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Sample records for hydrothermal synthesis

  1. Hydrothermal organic synthesis experiments

    NASA Technical Reports Server (NTRS)

    Shock, Everett L.

    1992-01-01

    Ways in which heat is useful in organic synthesis experiments are described, and experiments on the hydrothermal destruction and synthesis of organic compounds are discussed. It is pointed out that, if heat can overcome kinetic barriers to the formation of metastable states from reduced or oxidized starting materials, abiotic synthesis under hydrothermal conditions is a distinct possibility. However, carefully controlled experiments which replicate the descriptive variables of natural hydrothermal systems have not yet been conducted with the aim of testing the hypothesis of hydrothermal organic systems.

  2. Hydrothermal synthesis of ammonium illite

    USGS Publications Warehouse

    Sucha, V.; Elsass, F.; Eberl, D.D.; Kuchta, L'.; Madejova, J.; Gates, W.P.; Komadel, P.

    1998-01-01

    Synthetic gel and glass of illitic composition, natural kaolinite, and mixed-layer illite-smectite were used as starting materials for hydrothermal synthesis of ammonium illite. Ammonium illite was prepared from synthetic gel by hydrothermal treatment at 300??C. The onset of crystallization began within 3 h, and well-crystallized ammonium illite appeared at 24 h. Increasing reaction time (up to four weeks) led to many illite layers per crystal. In the presence of equivalent proportions of potassium and ammonium, the gel was transformed to illite with equimolar contents of K and NH4. In contrast, synthesis using glass under the same conditions resulted in a mixture of mixed-layer ammonium illite-smectite with large expandability and discrete illite. Hydrothermal treatments of the fine fractions of natural kaolinite and illite-smectite produced ammonium illite from kaolinite but the illite-smectite remained unchanged.

  3. Hydrothermal organic synthesis experiments

    NASA Technical Reports Server (NTRS)

    Shock, Everett L.

    1992-01-01

    The serious scientific debate about spontaneous generation which raged for centuries reached a climax in the nineteenth century with the work of Spallanzani, Schwann, Tyndall, and Pasteur. These investigators demonstrated that spontaneous generation from dead organic matter does not occur. Although no aspects of these experiments addressed the issue of whether organic compounds could be synthesized abiotically, the impact of the experiments was great enough to cause many investigators to assume that life and its organic compounds were somehow fundamentally different than inorganic compounds. Meanwhile, other nineteenth-century investigators were showing that organic compounds could indeed be synthesized from inorganic compounds. In 1828 Friedrich Wohler synthesized urea in an attempt to form ammonium cyanate by heating a solution containing ammonia and cyanic acid. This experiment is generally recognized to be the first to bridge the artificial gap between organic and inorganic chemistry, but it also showed the usefulness of heat in organic synthesis. Not only does an increase in temperature enhance the rate of urea synthesis, but Walker and Hambly showed that equilibrium between urea and ammonium cyanate was attainable and reversible at 100 C. Wohler's synthesis of urea, and subsequent syntheses of organic compounds from inorganic compounds over the next several decades dealt serious blows to the 'vital force' concept which held that: (1) organic compounds owe their formation to the action of a special force in living organisms; and (2) forces which determine the behavior of inorganic compounds play no part in living systems. Nevertheless, such progress was overshadowed by Pasteur's refutation of spontaneous generation which nearly extinguished experimental investigations into the origins of life for several decades. Vitalism was dealt a deadly blow in the 1950's with Miller's famous spark-discharge experiments which were undertaken in the framework of the Oparin

  4. Thermodynamics of Strecker synthesis in hydrothermal systems

    NASA Technical Reports Server (NTRS)

    Schulte, Mitchell; Shock, Everett

    1995-01-01

    Submarine hydrothermal systems on the early Earth may have been the sites from which life emerged. The potential for Strecker synthesis to produce biomolecules (amino and hydroxy acids) from starting compounds (ketones, aldehydes, HCN and ammonia) in such environments is evaluated quantitatively using thermodynamic data and parameters for the revised Helgeson-Kirkham-Flowers (HKF) equation of state. Although there is an overwhelming thermodynamic drive to form biomolecules by the Strecker synthesis at hydrothermal conditions, the availability and concentration of starting compounds limit the efficiency and productivity of Strecker reactions. Mechanisms for concentrating reactant compounds could help overcome this problem, but other mechanisms for production of biomolecules may have been required to produce the required compounds on the early Earth. Geochemical constraints imposed by hydrothermal systems provide important clues for determining the potential of these and other systems as sites for the emergence of life.

  5. Peptide synthesis in early earth hydrothermal systems

    USGS Publications Warehouse

    Lemke, K.H.; Rosenbauer, R.J.; Bird, D.K.

    2009-01-01

    We report here results from experiments and thermodynamic calculations that demonstrate a rapid, temperature-enhanced synthesis of oligopeptides from the condensation of aqueous glycine. Experiments were conducted in custom-made hydrothermal reactors, and organic compounds were characterized with ultraviolet-visible procedures. A comparison of peptide yields at 260??C with those obtained at more moderate temperatures (160??C) gives evidence of a significant (13 kJ ?? mol-1) exergonic shift. In contrast to previous hydrothermal studies, we demonstrate that peptide synthesis is favored in hydrothermal fluids and that rates of peptide hydrolysis are controlled by the stability of the parent amino acid, with a critical dependence on reactor surface composition. From our study, we predict that rapid recycling of product peptides from cool into near-supercritical fluids in mid-ocean ridge hydrothermal systems will enhance peptide chain elongation. It is anticipated that the abundant hydrothermal systems on early Earth could have provided a substantial source of biomolecules required for the origin of life. Astrobiology 9, 141-146. ?? 2009 Mary Ann Liebert, Inc. 2009.

  6. Zinc stannate nanostructures: hydrothermal synthesis

    PubMed Central

    Baruah, Sunandan; Dutta, Joydeep

    2011-01-01

    Nanostructured binary semiconducting metal oxides have received much attention in the last decade owing to their unique properties rendering them suitable for a wide range of applications. In the quest to further improve the physical and chemical properties, an interest in ternary complex oxides has become noticeable in recent times. Zinc stannate or zinc tin oxide (ZTO) is a class of ternary oxides that are known for their stable properties under extreme conditions, higher electron mobility compared to its binary counterparts and other interesting optical properties. The material is thus ideal for applications from solar cells and sensors to photocatalysts. Among the different methods of synthesizing ZTO nanostructures, the hydrothermal method is an attractive green process that is carried out at low temperatures. In this review, we summarize the conditions leading to the growth of different ZTO nanostructures using the hydrothermal method and delve into a few of its applications reported in the literature. PMID:27877377

  7. Hydrothermal synthesis of hydroxyapatite rods

    NASA Astrophysics Data System (ADS)

    Zhang, Xing; Vecchio, Kenneth S.

    2007-10-01

    Hydroxyapatite (HAP) rods were synthesized from dicalcium phosphate anhydrous (CaHPO 4, DCPA) and calcium carbonate (CaCO 3) by the hydrothermal method from 120 to 180 °C. Both cuttlebone (aragonite polymorph of CaCO 3) and CaCO 3 chemical (calcite polymorph of CaCO 3) were used as CaCO 3 sources. The nucleation and growth of HAP rods mainly occurred on DCPA particles, while some HAP rods also grew from aragonite particles. The nucleation and growth of β-tricalcium phosphate (β-TCP) particles on the surface of calcite particles were observed at the beginning of the reaction of DCPA and calcite, and some HAP rods were also found to grow out of β-TCP particles. After the hydrothermal reaction at 140 °C for 24 h, most products are HAP with a small amount of β-TCP synthesized as a byproduct. The HAP rods synthesized were ˜200 nm in width and several microns in length. The reaction mechanism and growth process of HAP rods are discussed.

  8. Garnet phosphors prepared via hydrothermal synthesis

    SciTech Connect

    Phillips, M.L.F.; Walko, R.J.; Shea, L.E.

    1996-05-01

    This project studied hydrothermal synthesis as a route to producing green-emitting cathodoluminescent phosphorus isostructural with yttrium aluminum garnet (Y{sub 3}Al{sub 5}O{sub 12}, or YAG). Aqueous precipitation of Y, Gd, Al, Ga, and Tb salts produced amorphous gels, which were heated with water at 600 C and 3,200 bar to produce crystalline YAG:Tb, Y{sub 3}Ga{sub 5}O{sub 12}:Tb, Y{sub 3}Al{sub 3}Ga{sub 2}O{sub 12}:Tb, and Gd{sub 3}Ga{sub 5}O{sub 12}:Tb powders. Process parameters were identified that yielded submicron YAG:Tb and Y{sub 3}Ga{sub 5}O{sub 12}:Tb powders without grinding. Cathodoluminescent efficiencies were measured as functions of power density at 600 V, using both the hydrothermal garnets and identical phosphor compositions synthesized at high temperatures. Saturation behavior was independent of synthetic technique, however, the hydrothermal phosphorus were less susceptible to damage (irreversible efficiency loss) at very high power densities (up to 0.1 W/cm{sup 2}). The fine grain sizes available with hydrothermal synthesis make it an attractive method for preparing garnet phosphorus for field emission, projection, and head-up displays.

  9. Hydrothermal synthesis of bismuth germanium oxide

    SciTech Connect

    Boyle, Timothy J.

    2016-12-13

    A method for the hydrothermal synthesis of bismuth germanium oxide comprises dissolving a bismuth precursor (e.g., bismuth nitrate pentahydrate) and a germanium precursor (e.g., germanium dioxide) in water and heating the aqueous solution to an elevated reaction temperature for a length of time sufficient to produce the eulytite phase of bismuth germanium oxide (E-BGO) with high yield. The E-BGO produced can be used as a scintillator material. For example, the air stability and radioluminescence response suggest that the E-BGO can be employed for medical applications.

  10. Hydrothermal synthesis map of bismuth titanates

    SciTech Connect

    Sardar, Kripasindhu; Walton, Richard I.

    2012-05-15

    The hydrothermal synthesis of four bismuth titanate materials from common bismuth and titanium precursors under hydrothermal conditions is described. Reaction of NaBiO{sub 3}{center_dot}2H{sub 2}O and anatase TiO{sub 2} in concentrated NaOH solution at 240 Degree-Sign C is shown to produce perovskite and sillenite phases Na{sub 0.5}Bi{sub 0.5}TiO{sub 3} and Bi{sub 12}TiO{sub 20}, depending on the ratio of metal precursors used. When KOH solution is used and a 1:1 ratio of the same precursors, a pyrochlore Bi{sub 1.43}Ti{sub 2}O{sub 6}(OH){sub 0.29}(H{sub 2}O){sub 0.66} is formed. The use of a mixture of HNO{sub 3} and NaOH is shown to facilitate the formation of the Aurivillius-type bismuth titanate Bi{sub 4}Ti{sub 3}O{sub 12}. The phases have been isolated separately as phase-pure powders and profile refinement of powder X-ray diffraction data allows comparisons with comparable materials reported in the literature. Analysis of Bi L{sub III}-edge X-ray absorption near edge structure (XANES) spectra of the materials shows the oxidation state of bismuth is +3 in all of the hydrothermally derived products. - Graphical abstract: Use of NaBiO{sub 3}{center_dot}2H{sub 2}O and TiO{sub 2} as reagents under hydrothermal conditions allows the phase-pure preparation of four crystalline bismuth titanate materials. Highlights: Black-Right-Pointing-Pointer NaBiO{sub 3} and TiO{sub 2} under hydrothermal conditions allow formation of bismuth titanates. Black-Right-Pointing-Pointer Synthesis of four distint phases has been mapped. Black-Right-Pointing-Pointer Bi LIII-edge XANES shows Bi is reduced to oxidation state +3 in all materials. Black-Right-Pointing-Pointer A new hydrated bismuth titanate pyrochlore has been isolated.

  11. Recent progress in hydrothermal synthesis of zinc oxide nanomaterials.

    PubMed

    Djurisic, A B; Chen, X Y; Leung, Y H

    2012-06-01

    Hydrothermal synthesis is of considerable interest due to its low cost, simplicity and relatively low growth temperature (typically below 200 °C). Since the synthesis is performed in aqueous solutions (no organic solvents), it can also be safe and environmentally friendly (depending on precursor chemicals). Consequently, it has been a subject of intense research in recent years. In this article, we review recent progress in hydrothermal synthesis of zinc oxide nanomaterials, with focus on practical relevance for a variety of applications.

  12. Hydrothermal synthesis of lutetium disilicate nanoparticles

    SciTech Connect

    Tang Xiaoping; Gao Yanfeng; Chen Hongfei; Luo Hongjie

    2012-04-15

    A simple, low-cost hydrothermal method was developed to synthesize irregular-and rod-shaped lutetium disilicate (Lu{sub 2}Si{sub 2}O{sub 7}) powders with sizes ranging from 71 to 340 nm. The synthesis temperature was 260 Degree-Sign C, which is nearly 1300 Degree-Sign C lower than that required for the solid-state reaction. The results indicated that both the hydrothermal temperature and pH values had great influences on the composition, crystalline phase and morphology of the powders. The formation mechanism, basic thermophysical properties, stability and anticorrosion properties of the Lu{sub 2}Si{sub 2}O{sub 7} powders were also investigated. The obtained powders possessed low thermal conductivity, a suitable thermal expansion coefficient (3.92-5.17 Multiplication-Sign 10{sup -6} K{sup -1}) with the silicon-based substrate and excellent thermal and structural stability. During hot corrosion testing, the surfaces of the samples appeared to react with the water and molten salt vapors, but no serious failure occurred. - Graphical abstract: An image for the as-prepared Lu{sub 2}Si{sub 2}O{sub 7} powders (left) and XRD pattern (right) (inset shows the SEM graph of powders). Highlights: Black-Right-Pointing-Pointer We synthesized Lu{sub 2}Si{sub 2}O{sub 7} powders via a hydrothermal process at 260 Degree-Sign C. Black-Right-Pointing-Pointer Crystalline phase and morphology of the powders changed with experimental parameter. Black-Right-Pointing-Pointer Hot corrosion was determined in an airflow environment containing alkaline vapor.

  13. Synthesis of Nanoparticles via Solvothermal and Hydrothermal Methods

    SciTech Connect

    Li, Jianlin; Wu, Qingliu; Wu, Ji

    2015-01-01

    This chapter summarizes the synthesis of various types of nanoparticles as well as surface modifications of nanomaterials using hydrothermal and solvothermal methods. First, the definition, history, instrumentation, and mechanism of hydrothermal and solvothermal methods as well as the important parameters af-fecting the nucleation and crystal growth of nanomaterials are briefly introduced. Then the specific hydrothermal and solvothermal methods used to grow oxides, Group II-VI, III-V, IV, transitional metals, and metal-organic framework nanoparticles are summarized. Finally, the hydrothermal and solvothermal strategies used for the surface modification of nanomaterials are discussed.

  14. Energetics of amino acid synthesis in hydrothermal ecosystems

    NASA Technical Reports Server (NTRS)

    Amend, J. P.; Shock, E. L.

    1998-01-01

    Thermodynamic calculations showed that the autotrophic synthesis of all 20 protein-forming amino acids was energetically favored in hot (100 degrees C), moderately reduced, submarine hydrothermal solutions relative to the synthesis in cold (18 degrees C), oxidized, surface seawater. The net synthesis reactions of 11 amino acids were exergonic in the hydrothermal solution, but all were endergonic in surface seawater. The synthesis of the requisite amino acids of nine thermophilic and hyperthermophilic proteins in a 100 degreesC hydrothermal solution yielded between 600 and 8000 kilojoules per mole of protein, which is energy that is available to drive the intracellular synthesis of enzymes and other biopolymers in hyperthermophiles thriving in these ecosystems.

  15. Hydrothermal synthesis of pyrochlores and their characterization

    NASA Astrophysics Data System (ADS)

    Redkin, Alexander F.; Ionov, Andrey M.; Kotova, Nataliya P.

    2013-10-01

    Pyrochlores, microlites, and U-betafites of pyrochlore group minerals were obtained from mixing experiments of the corresponding oxides and fluorides by hydrothermal synthesis at T = 800 °C and P = 200 MPa in the solution of 1.0 M NaF. The presence of U4+ in pyrochlore does not affect the cell parameter, which for the phases of pyrochlore-microlite series is 10.42 ± 0.01 Å. In a system with an excess of UO2, pyrochlores and microlites, containing uranium up to 0.2-0.3 atoms per formula unit (apfu), are formed. In the uranium-free system of betafites composition, perovskites and Ti-bearing pyrochlores are formed. U-pyrochlores of betafite series, containing 2Ti = Nb + Ta in moles, have cubic cell parameters of 10.26 ± 0.02 Å and U4+ isomorphic capacity of 0.4-0.5 apfu. In the pyrochlore structure, U4+ may substitute for Ca2+ and Na+ cations in the eightfold site. In pyrochlores of pyrochlore-microlite series, Ca2+ is replaced by U4+, while in pyrochlores of betafite series, U4+ replaces Na+. Phases with pyrochlore structure, containing U5+ and U6+ in the sixfold site, usually occupied by Nb5+, Ta5+, and Ti4+, are formed under oxidizing conditions (Cu-Cu2O buffer). They are characterized by low content of Nb5+, Ta5+ (<0.1 apfu), and anomalous behavior of the crystal lattice (compression, instead of expansion). Under natural conditions, the formation of pyrochlores containing a significant amount of U5+ and U6+ is unlikely.

  16. Hydrothermal synthesis of ytterbium silicate nanoparticles.

    PubMed

    Chen, Hongfei; Gao, Yanfeng; Liu, Yun; Luo, Hongjie

    2010-02-15

    A simple, low-cost hydrothermal method was developed to synthesize 20-nm-diameter single-crystalline ytterbium silicate (Yb(2)Si(2)O(7) and Yb(2)SiO(5)) nanoparticles at 200 degrees C. This is nearly 1000 degrees C lower than that for the typical sol-gel route to ytterbium silicate powders. Obtained powders showed very low thermal conductivity, a suitable thermal expansion coefficient, and excellent thermal/structural stability, suggesting a potential application to environmental and thermal barrier coatings. Special focus was placed on assessing the hydrothermal reaction mechanism for particle formation.

  17. Peptide synthesis under Enceladus hydrothermal condition

    NASA Astrophysics Data System (ADS)

    Fujishima, Kosuke; Takano, Yoshinori; Takai, Ken; Takahagi, Wataru; Adachi, Keito; Shibuya, Takazo; Tomita, Masaru

    2016-07-01

    Enceladus is one of the moons of Saturn, and it has been known to harbor interior ocean beneath the icy crust. The mass spectrometry data obtained by Cassini spacecraft indicates the presence of salty, and most likely alkaline ocean containing various organic compounds. While geochemical and other radiation related processes for in situ production of organics remain elusive, thermally unaltered carbonaceous chondrites, consisting the main body of Enceladus are known to be enriched with organic matters potentially including the building blocks of life (e.g., amino acids and amino acid precursors). Assuming that abiotic amino acids exist in the Enceladus alkaline seawater, we hypothesized that water-rock interaction may contribute to condensation of localized amino acids leading to peptide formation. In order to test this hypothesis, we have developed the Enceladus hydrothermal reactor based on the chemical constraints obtained through previous experimental and theoretical studies. We have added six different amino acids and introduced a thermal fluctuation system simulating the periodic tidal heating of the interior chondritic core. Total, eight sea water samples were obtained over the course of 147 days of experiment. While detection of peptide using Capillary Electrophoresis Time-of-Flight Mass Spectrometry (CE-TOF/MS) is still at the preliminary stage, so far pH monitoring and H2 and CO2 Gas Chromatography Mass Spectrometry (GC-MS) data clearly indicated the occurrence of serpentinization/carbonation reaction. Here, we discuss the interaction between aqueous alteration reactions and thermal cycling processes for the role of abiotic peptide formation under the Enceladus hydrothermal condition.

  18. Final storage of radioactive cesium by pollucite hydrothermal synthesis

    PubMed Central

    Yokomori, Yoshinobu; Asazuki, Kazuhito; Kamiya, Natsumi; Yano, Yudai; Akamatsu, Koki; Toda, Tetsuya; Aruga, Atsushi; Kaneo, Yoshiaki; Matsuoka, Seiko; Nishi, Koji; Matsumoto, Satoshi

    2014-01-01

    The Fukushima nuclear accident has highlighted the importance of finding a better final storage method for radioactive cesium species. Cs is highly soluble in water, and can easily exchange with other alkali ions in zeolites or clays to form stable complexes. However, Cs+ is released from Cs+ complexes into water when surrounded by an excess of water. Pollucite may be the best final storage option for Cs+, but its typical synthesis requires heating to about 1200°C in air. Here, we show that the hydrothermal synthesis of pollucite can be completed at 300°C in three hours from any zeolite or clay. Furthermore, our procedure does not require ion exchange before synthesis. Radioactive Cs is usually found in complexes with clays. At that time, this method only requires calcium hydroxide, water, and three hours of hydrothermal synthesis, so the process is both inexpensive and practical for large-scale application. Pollucite is an analog of analcime zeolite, and contains a channel system 2.8 Å in diameter, which is formed by 6-oxygen rings. As the diameter of Cs+ is 3.34 Å and each Cs+ exists independently within a separate portion of the channel, Cs+ cannot exit the pollucite framework without breaking it. PMID:24569302

  19. Energetics of Amino Acid Synthesis in Alkaline Hydrothermal Environments.

    PubMed

    Kitadai, Norio

    2015-12-01

    Alkaline hydrothermal systems have received considerable attention as candidates for the origin and evolution of life on the primitive Earth. Nevertheless, sufficient information has not yet been obtained for the thermodynamic properties of amino acids, which are necessary components for life, at high temperatures and alkaline pH. These properties were estimated using experimental high-temperature volume and heat capacity data reported in the literature for several amino acids, together with correlation algorithms and the revised Helgeson-Kirkham-Flowers (HKF) equations of state. This approach enabled determination of a complete set of the standard molal thermodynamic data and the revised HKF parameters for the 20 protein amino acids in their zwitterionic and ionization states. The obtained dataset was then used to evaluate the energetics of amino acid syntheses from simple inorganic precursors (CO2, H2, NH3 and H2S) in a simulated alkaline hydrothermal system on the Hadean Earth. Results show that mixing between CO2-rich seawater and the H2-rich hydrothermal fluid can produce energetically favorable conditions for amino acid syntheses, particularly in the lower-temperature region of such systems. Together with data related to the pH and temperature dependences of the energetics of amino acid polymerizations presented in earlier reports, these results suggest the following. Hadean alkaline hydrothermal settings, where steep pH and temperature gradients may have existed between cool, slightly acidic Hadean ocean water and hot, alkaline hydrothermal fluids at the vent-ocean interface, may be energetically the most suitable environment for the synthesis and polymerization of amino acids.

  20. Energetics of Amino Acid Synthesis in Alkaline Hydrothermal Environments

    NASA Astrophysics Data System (ADS)

    Kitadai, Norio

    2015-12-01

    Alkaline hydrothermal systems have received considerable attention as candidates for the origin and evolution of life on the primitive Earth. Nevertheless, sufficient information has not yet been obtained for the thermodynamic properties of amino acids, which are necessary components for life, at high temperatures and alkaline pH. These properties were estimated using experimental high-temperature volume and heat capacity data reported in the literature for several amino acids, together with correlation algorithms and the revised Helgeson-Kirkham-Flowers (HKF) equations of state. This approach enabled determination of a complete set of the standard molal thermodynamic data and the revised HKF parameters for the 20 protein amino acids in their zwitterionic and ionization states. The obtained dataset was then used to evaluate the energetics of amino acid syntheses from simple inorganic precursors (CO2, H2, NH3 and H2S) in a simulated alkaline hydrothermal system on the Hadean Earth. Results show that mixing between CO2-rich seawater and the H2-rich hydrothermal fluid can produce energetically favorable conditions for amino acid syntheses, particularly in the lower-temperature region of such systems. Together with data related to the pH and temperature dependences of the energetics of amino acid polymerizations presented in earlier reports, these results suggest the following. Hadean alkaline hydrothermal settings, where steep pH and temperature gradients may have existed between cool, slightly acidic Hadean ocean water and hot, alkaline hydrothermal fluids at the vent-ocean interface, may be energetically the most suitable environment for the synthesis and polymerization of amino acids.

  1. Hydrothermal synthesis and characterization of zirconia based catalysts

    SciTech Connect

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

    2013-07-15

    In this work, three equimolar mixed oxides ZrO{sub 2}/CeO{sub 2}, ZrO{sub 2}/TiO{sub 2}, ZrO{sub 2}/La{sub 2}O{sub 3} and a reference ZrO{sub 2} have been synthesized by hydrothermal method. The structural and surface properties of these materials have been fully characterized by X-ray diffraction, transmission electron microscopy, surface area measurement, chemical analysis, XPS, infrared spectroscopy after adsorption of pyridine and adsorption microcalorimetry of NH{sub 3} and SO{sub 2} probe molecules. All investigated mixed oxides are amphoteric and possess redox centers on their surface. Moreover, hydrothermal synthesis leads to catalysts with higher surface area and with better acid–base properties than classical coprecipitation method. Both Lewis and Brønsted acid sites are present on the surface of the mixed oxides. Compared to the other samples, the ZrO{sub 2}/TiO{sub 2} material appears to be the best candidate for further application in acid–base catalysis. - Graphical abstract: Mesoporous amorphous phase with a high surface area of titania zirconia mixed oxide obtained by hydrothermal preparation. - Highlights: • Three zirconia based catalysts and a reference were prepared by hydrothermal synthesis. • Mixed oxides present larger surface areas than the reference ZrO{sub 2}. • ZrO{sub 2}/TiO{sub 2} catalyst presents a mesoporous structure with high surface area. • ZrO{sub 2}/TiO{sub 2} catalyst presents simultaneously strong acidic and basic properties.

  2. Pathways for abiotic organic synthesis at submarine hydrothermal fields

    PubMed Central

    McDermott, Jill M.; Seewald, Jeffrey S.; German, Christopher R.; Sylva, Sean P.

    2015-01-01

    Arguments for an abiotic origin of low-molecular weight organic compounds in deep-sea hot springs are compelling owing to implications for the sustenance of deep biosphere microbial communities and their potential role in the origin of life. Theory predicts that warm H2-rich fluids, like those emanating from serpentinizing hydrothermal systems, create a favorable thermodynamic drive for the abiotic generation of organic compounds from inorganic precursors. Here, we constrain two distinct reaction pathways for abiotic organic synthesis in the natural environment at the Von Damm hydrothermal field and delineate spatially where inorganic carbon is converted into bioavailable reduced carbon. We reveal that carbon transformation reactions in a single system can progress over hours, days, and up to thousands of years. Previous studies have suggested that CH4 and higher hydrocarbons in ultramafic hydrothermal systems were dependent on H2 generation during active serpentinization. Rather, our results indicate that CH4 found in vent fluids is formed in H2-rich fluid inclusions, and higher n-alkanes may likely be derived from the same source. This finding implies that, in contrast with current paradigms, these compounds may form independently of actively circulating serpentinizing fluids in ultramafic-influenced systems. Conversely, widespread production of formate by ΣCO2 reduction at Von Damm occurs rapidly during shallow subsurface mixing of the same fluids, which may support anaerobic methanogenesis. Our finding of abiogenic formate in deep-sea hot springs has significant implications for microbial life strategies in the present-day deep biosphere as well as early life on Earth and beyond. PMID:26056279

  3. Pathways for abiotic organic synthesis at submarine hydrothermal fields.

    PubMed

    McDermott, Jill M; Seewald, Jeffrey S; German, Christopher R; Sylva, Sean P

    2015-06-23

    Arguments for an abiotic origin of low-molecular weight organic compounds in deep-sea hot springs are compelling owing to implications for the sustenance of deep biosphere microbial communities and their potential role in the origin of life. Theory predicts that warm H2-rich fluids, like those emanating from serpentinizing hydrothermal systems, create a favorable thermodynamic drive for the abiotic generation of organic compounds from inorganic precursors. Here, we constrain two distinct reaction pathways for abiotic organic synthesis in the natural environment at the Von Damm hydrothermal field and delineate spatially where inorganic carbon is converted into bioavailable reduced carbon. We reveal that carbon transformation reactions in a single system can progress over hours, days, and up to thousands of years. Previous studies have suggested that CH4 and higher hydrocarbons in ultramafic hydrothermal systems were dependent on H2 generation during active serpentinization. Rather, our results indicate that CH4 found in vent fluids is formed in H2-rich fluid inclusions, and higher n-alkanes may likely be derived from the same source. This finding implies that, in contrast with current paradigms, these compounds may form independently of actively circulating serpentinizing fluids in ultramafic-influenced systems. Conversely, widespread production of formate by ΣCO2 reduction at Von Damm occurs rapidly during shallow subsurface mixing of the same fluids, which may support anaerobic methanogenesis. Our finding of abiogenic formate in deep-sea hot springs has significant implications for microbial life strategies in the present-day deep biosphere as well as early life on Earth and beyond.

  4. Hydrothermal synthesis and characterization of zirconia based catalysts

    NASA Astrophysics Data System (ADS)

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

    2013-07-01

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

  5. Microwave-hydrothermal synthesis of perovskite bismuth ferrite nanoparticles

    SciTech Connect

    Biasotto, G.; Simoes, A.Z.; Foschini, C.R.; Zaghete, M.A.; Varela, J.A.; Longo, E.

    2011-12-15

    Highlights: Black-Right-Pointing-Pointer BiFeO{sub 3} (BFO) nanoparticles were grown by hydrothermal microwave method (HTMW). Black-Right-Pointing-Pointer The soaking time is effective in improving phase formation. Black-Right-Pointing-Pointer Rietveld refinement reveals an orthorhombic structure. Black-Right-Pointing-Pointer The observed magnetism of the BFO crystallites is a consequence of particle size. Black-Right-Pointing-Pointer The HTMW is a genuine technique for low temperatures and short times of synthesis. -- Abstract: Hydrothermal microwave method (HTMW) was used to synthesize crystalline bismuth ferrite (BiFeO{sub 3}) nanoparticles (BFO) in the temperature of 180 Degree-Sign C with times ranging from 5 min to 1 h. BFO nanoparticles were characterized by means of X-ray analyses, FT-IR, Raman spectroscopy, TG-DTA and FE-SEM. X-ray diffraction results indicated that longer soaking time was benefit to refraining the formation of any impurity phases and growing BFO crystallites into almost single-phase perovskites. Typical FT-IR spectra for BFO nanoparticles presented well defined bands, indicating a substantial short-range order in the system. TG-DTA analyses confirmed the presence of lattice OH{sup -} groups, commonly found in materials obtained by HTMW process. Compared with the conventional solid-state reaction process, submicron BFO crystallites with better homogeneity could be produced at the temperature as low as 180 Degree-Sign C. These results show that the HTMW synthesis route is rapid, cost effective, and could be used as an alternative to obtain BFO nanoparticles in the temperature of 180 Degree-Sign C for 1 h.

  6. Effects of hydrothermal temperature and time on hydrothermal synthesis of colloidal hydroxyapatite nanorods in the presence of sodium citrate.

    PubMed

    Jin, Xiaoying; Chen, Xiaohu; Cheng, Yute; Wang, Longshen; Hu, Bing; Tan, Junjun

    2015-07-15

    In this paper, colloidal hydrophilic hydroxyapatite nanorods were synthesized in the presence of sodium citrate via thermal-decomplexing method. The influences of hydrothermal temperature and time on the synthesis of HA nanorods were characterized in terms of structure, size, morphology, and colloidal stability through TEM, XRD, zeta potential, DLS and long-term standing test. Results show that increasing hydrothermal temperature and prolonging hydrothermal time would evidently improve crystallinity and enlarge size of HA nanorods but decrease the colloidal stability of nanorods. It is worth noting that the effect of raising the hydrothermal temperature and time on diameter increase is far greater than that on length increase; meanwhile, the colloidal stability would be seriously deteriorated when the hydrothermal temperature is over 180 °C for 24 h or when the hydrothermal temperature is 150 °C for over 48 h, in these cases, dispersion of HA nanorods would apparently settle within 2 months. The origin responding to the results is that although the charge density of HA nanorods is not obviously affected, the dynamic diameters of HA particles increase greatly, which reduces colloidal stability of the dispersion. This work provides new insights into the role of hydrothermal temperature and time on tailoring morphology, crystallinity and colloidal stability of HA nanorods. Moreover, it would be helpful to optimize the experimental procedure both on scientific and industrial applications related to HA. For example, on the premise of satisfying the necessary requirements including crystallinity, size, morphology and colloid stability, it is feasible to compress the consumption of experimental time through raising the hydrothermal temperature, or vice versa.

  7. The hydrothermal synthesis of tetragonal tungsten bronze-based catalysts for the selective oxidation of hydrocarbons.

    PubMed

    Botella, Pablo; Solsona, Benjamín; García-González, Ester; González-Calbet, José M; López Nieto, José M

    2007-12-21

    Mixed metal oxides with tetragonal tungsten bronze (TTB) structure, showing high activity and selectivity for the gas phase partial oxidation of olefins, have been prepared by hydrothermal synthesis from Keggin-type heteropolyacids.

  8. Synthesis of hydrogen cyanide under simulated hydrothermal conditions

    NASA Astrophysics Data System (ADS)

    Pinedo-González, Paulina

    Nitrogen is a fundamental element for life, where is present in structural (e.g., proteins), catalytic (e.g., enzymes and ribozymes), energy transfer (e.g., ATP) and information storage (RNA and DNA) biomolecules. Atmospheric and planetary models suggest that nitrogen was abundant in the early atmospheres of Earth as dinitrogen (N2 ), an inert gas under normal atmospheric conditions. To be available for prebiotic synthesis it must be converted into hydrogen cyanide (HCN), ammonia (NH3 ) and/or nitric oxide (NO), in a process referred to as nitrogen fixation. Due to the strength of the triple bond in N2 , nitrogen fixation, while thermodynamically favored is kinetically restricted. In a reducing atmosphere dominated by CH4 -N2 , thunderstorm lightning efficiently produces HCN and NH3 (Stribling and Miller, 1987). Nevertheless, photochemical and geochemical constraints strongly suggest that the early atmosphere was weakly reducing, dominated by CO2 and N2 with traces of CH4 , CO, and H2 (Kasting, 1993). Under these conditions, HCN is no longer synthesized in the lightning channel and instead NO is formed (Navarro-Gonźlez, et al., 2001). In volcanic plumes, where magmatic gases a were more reducing than in the atmosphere, NO can also be formed by the lava heat (Mather et al., 2004) or volcanic lightning (Navarro-Gonźlez et al., 1998). Surprisingly, dinitrogen can be a reduced to NH3 in hydrothermal systems (Brandes et al., 1998), but the formation of HCN and its derivates were not investigated. The present work explores the possibility of the formation of HCN as well as other nitrile derivatives catalyzed by mineral surfaces in hydrothermal vents. To simulate a hydrothermal atmosphere, the experiments were carried out in a stainless steel Parr R minireactor with a 0.1 M NH4 HCO3 solution (200 ml) with or without a mineral surface exposed at 1 bar at temperatures ranging from 100 to 375° C. Different mineral matrices are been investigated. Our preliminary results

  9. Hydrothermal synthesis of sodium bismuth titanate and titanate nanofibers

    NASA Astrophysics Data System (ADS)

    Kundu, Animesh

    A hydrothermal processing method was developed for the synthesis of sodium bismuth titanate powders and thin films from suitable precursors at 150°C. Oxide precursors were best suited for preparing pure phase materials. The sodium bismuth titanate powders consisted of cube shaped crystals. A modified solution-reprecitation model involving partial dissolution of the precursors was proposed to explain the growth of these particles. The thin films were prepared on strontium titanate (100) substrate. A sample holder was specially designed and fabricated to secure the substrates in the reaction vessel. The result was a relatively smooth film of thickness ≤550 nm. The films were essentially single crystalline and had strong epitaxial relationship with the substrate. Titanate nanofibers (NaxH yTinO2n+1° zH2O) were known to form under similar hydrothermal conditions as sodium bismuth titanate powders. Detail research revealed that the pure hydroxide and oxide precursors tend to form sodium bismuth titanate powders or thin films. Titanate nanofibers were the predominant product when any other ions or organics were present in the precursor. Much faster reaction kinetics for the formation of nanofibers was observed when certain organic compounds were added deliberately with the precursors. Accordingly, a hydrothermal process was developed for converting the precursors to titanate nanofibers in a significantly shorter time than reported in the literature. A thin film consisting of vertically aligned nanofibers was prepared on titanium substrate at 150°C in as little as 30 minutes. Complete conversion of starting precursors to free standing nanofibers was achieved in ˜8 hours at 150°C. The as-prepared nanofibers were some form of sodium titanate. They were converted to hydrogen titanate by ion exchange. Differential Scanning calorimetric experiments were performed to understand the thermal evolution of the fibers. The hydrogen titanate fibers underwent structural

  10. Rational synthesis of multifunctional mixed metal oxides by hydrothermal techniques

    NASA Astrophysics Data System (ADS)

    Stampler, Evan Scott

    Low temperature (<350°C) and pressure (<20 atm) hydrothermal methods have been developed for the synthesis of bismuth copper oxide chalcogenides, hexagonal rare-earth manganites, and silver delafossites with mixed cations on the B-site. These materials are of particular interest because they combine multiple functional properties, such as transparency and conductivity, or magnetism and ferroelectricity, in a single-phase material, thus enabling innovative technological applications. Phase-pure products were achieved by the appropriate combination of starting reagents, pH, and reaction temperature to control the solubility of the reactants. Phase-pure BiCuOS and BiCuOSe have been synthesized in high yield by a single-step hydrothermal reaction at low temperature (250°C) and pressure (< 20 atm). A reaction temperature of 250°C was sufficiently high to solubilize both Bi2O3 ([Bi3+] ≈ 10 -3 M) and Cu2O ([Cu+] ≈ 10-4 M) and stabilize monovalent copper species in solution, yet remains low enough to prevent the oxidation of sulfide and selenide. BiCuOS (Eg = 1.09 eV) and BiCuOSe (Eg = 0.75 eV) have smaller band gaps compared to the p-type transparent conductor LaCuOS (Eg = 3.1 eV) but have significantly higher room temperature conductivities (sigma ≈ 0.08 S cm-1 and 3.3 S cm-1, respectively). The high molar solubility of Mn2O3 ([Mn 3+] ≈ 10-3 M) and the slightly amphoteric character of the late rare-earth sesquioxides were exploited in the hydrothermal synthesis of rare-earth manganites, LnMnO3 (Ln=Ho-Lu and Y). While alkaline conditions were necessary for the solubilization of manganese, a reaction temperature approximately 50°C above the transition temperature of the respective rare-earth trihydroxide (100-300°C) accelerated the transition to the more reactive and soluble rare-earth oxide hydroxide and the subsequent reaction to yield the LnMnO3 phase. The high solubility of Ag2O, [Ag+] ≈ 10 -2.5 M, enabled the synthesis of two new silver delafossite

  11. Direct Hydrothermal Synthesis of Carbonaceous Silver Nanocables for Electrocatalytic Applications.

    PubMed

    Chen, Chuyang; Suryanto, Bryan Harry Rahmat; Zhao, Chuan; Jiang, Xuchuan; Yu, Aibing

    2015-08-05

    This study demonstrates a facile but efficient hydrothermal method for the direct synthesis of both carbonaceous silver (Ag@C core-shell) nanocables and carbonaceous nanotubes under mild conditions (<180 °C). The carbonaceous tubes can be formed by removal of the silver cores via an etching process under temperature control (60-140 °C). The structure and composition are characterized using various advanced microscopic and spectroscopic techniques. The pertinent variables such as temperature, reaction time, and surfactants that can affect the formation and growth of the nanocables and nanotubes are investigated and optimized. It is found that cetyltrimethylammonium bromide plays multiple roles in the formation of Ag@C nanocables and carbonaceous nanotubes including: a shape controller for metallic Ag wires and Ag@C cables, a source of Br(-) ions to form insoluble AgBr and then Ag crystals, an etching agent of silver cores to form carbonaceous tubes, and an inducer to refill silver particles into the carbonaceous tubes to form core-shell structures. The formation mechanism of carbonaceous silver nanostructures depending upon temperature is also discussed. Finally, the electrocatalytic performance of the as-prepared Ag@C nanocables is assessed for the oxidation reduction reaction and found to be very active but much less costly than the commonly used platinum catalysts. The findings should be useful for designing and constructing carbonaceous-metal nanostructures with potential applications in conductive materials, catalysts, and biosensors.

  12. Lipid synthesis under hydrothermal conditions by Fischer-Tropsch-type reactions

    NASA Technical Reports Server (NTRS)

    McCollom, T. M.; Ritter, G.; Simoneit, B. R.

    1999-01-01

    Ever since their discovery in the late 1970's, mid-ocean-ridge hydrothermal systems have received a great deal of attention as a possible site for the origin of life on Earth (and environments analogous to mid-ocean-ridge hydrothermal systems are postulated to have been sites where life could have originated or Mars and elsewhere as well). Because no modern-day terrestrial hydrothermal systems are free from the influence of organic compounds derived from biologic processes, laboratory experiments provide the best opportunity for confirmation of the potential for organic synthesis in hydrothermal systems. Here we report on the formation of lipid compounds during Fischer-Tropsch-type synthesis from aqueous solutions of formic acid or oxalic acid. Optimum synthesis occurs in stainless steel vessels by heating at 175 degrees C for 2-3 days and produces lipid compounds ranging from C2 to > C35 which consist of n-alkanols, n-alkanoic acids, n-alkenes, n-alkanes and alkanones. The precursor carbon sources used are either formic acid or oxalic acid, which disproportionate to H2, CO2 and probably CO. Both carbon sources yield the same lipid classes with essentially the same ranges of compounds. The synthesis reactions were confirmed by using 13C labeled precursor acids.

  13. Conventional and microwave hydrothermal synthesis of monodispersed metal oxide nanoparticles at liquid-liquid interface

    EPA Science Inventory

    Monodispersed nanoparticles of metal oxide including ferrites MFe2O4 (M=, Ni, Co, Mn) and γ-Fe2O3, Ta2O5 etc. have been synthesized using a water-toluene interface under both conventional and microwave hydrothermal conditions. This general synthesis procedure uses readily availab...

  14. Hydrothermal method of synthesis of rare-earth tantalates and niobates

    DOEpatents

    Nyman, May D; Rohwer, Lauren E.S.; Martin, James E

    2012-10-16

    A hydrothermal method of synthesis of a family of rare-earth Group 5 oxides, where the Group 5 oxide is a niobate or tantalate. The rare-earth Group 5 oxides can be doped with suitable emitter ions to form nanophosphors.

  15. Hydrothermal synthesis and photoluminescent properties of stacked indium sulfide superstructures.

    PubMed

    Xing, Yan; Zhang, Hongjie; Song, Shuyan; Feng, Jing; Lei, Yongqian; Zhao, Lijun; Li, Meiye

    2008-03-28

    Unusual hierarchical stacked superstructures of cubic beta-In2S3 were fabricated via a facile hydrothermal process in the presence of a surfactant cetyltrimethylammonium bromide CTAB; the 3D superstructures were developed by helical propagation of surface steps from microflakes of 10-20 nm thickness.

  16. Prebiotic Synthesis of Glycine from Ethanolamine in Simulated Archean Alkaline Hydrothermal Vents.

    PubMed

    Zhang, Xianlong; Tian, Ge; Gao, Jing; Han, Mei; Su, Rui; Wang, Yanxiang; Feng, Shouhua

    2016-09-23

    Submarine hydrothermal vents are generally considered as the likely habitats for the origin and evolution of early life on Earth. In recent years, a novel hydrothermal system in Archean subseafloor has been proposed. In this model, highly alkaline and high temperature hydrothermal fluids were generated in basalt-hosted hydrothermal vents, where H2 and CO2 could be abundantly provided. These extreme conditions could have played an irreplaceable role in the early evolution of life. Nevertheless, sufficient information has not yet been obtained for the abiotic synthesis of amino acids, which are indispensable components of life, at high temperature and alkaline condition. This study aims to propose a new method for the synthesis of glycine in simulated Archean submarine alkaline vent systems. We investigated the formation of glycine from ethanolamine under conditions of high temperature (80-160 °C) and highly alkaline solutions (pH = 9.70). Experiments were performed in an anaerobic environment under mild pressure (0.1-8.0 MPa) at the same time. The results suggested that the formation of glycine from ethanolamine occurred rapidly and efficiently in the presence of metal powders, and was favored by high temperatures and high pressures. The experiment provides a new pathway for prebiotic glycine formation and points out the phenomenal influence of high-temperature alkaline hydrothermal vents in origin of life in the early ocean.

  17. Prebiotic Synthesis of Glycine from Ethanolamine in Simulated Archean Alkaline Hydrothermal Vents

    NASA Astrophysics Data System (ADS)

    Zhang, Xianlong; Tian, Ge; Gao, Jing; Han, Mei; Su, Rui; Wang, Yanxiang; Feng, Shouhua

    2016-09-01

    Submarine hydrothermal vents are generally considered as the likely habitats for the origin and evolution of early life on Earth. In recent years, a novel hydrothermal system in Archean subseafloor has been proposed. In this model, highly alkaline and high temperature hydrothermal fluids were generated in basalt-hosted hydrothermal vents, where H2 and CO2 could be abundantly provided. These extreme conditions could have played an irreplaceable role in the early evolution of life. Nevertheless, sufficient information has not yet been obtained for the abiotic synthesis of amino acids, which are indispensable components of life, at high temperature and alkaline condition. This study aims to propose a new method for the synthesis of glycine in simulated Archean submarine alkaline vent systems. We investigated the formation of glycine from ethanolamine under conditions of high temperature (80-160 °C) and highly alkaline solutions (pH = 9.70). Experiments were performed in an anaerobic environment under mild pressure (0.1-8.0 MPa) at the same time. The results suggested that the formation of glycine from ethanolamine occurred rapidly and efficiently in the presence of metal powders, and was favored by high temperatures and high pressures. The experiment provides a new pathway for prebiotic glycine formation and points out the phenomenal influence of high-temperature alkaline hydrothermal vents in origin of life in the early ocean.

  18. Microemulsion-mediated hydrothermal synthesis and characterization of nanosize rutile and anatase particles

    SciTech Connect

    Wu, M.; Long, J.; Huang, A.; Luo, Y.; Feng, S.; Xu, R.

    1999-12-21

    Uniform nanoparticles of rutile and anatase were prepared, respectively, by a new approach, a microemulsion-mediated method, in which the microemulsion medium was further treated by hydrothermal reaction. Herein, the combined procedure of microemulsion and hydrothermal synthesis to prepare nanoparticles is referred to as a microemulsion-mediated hydrothermal (MMH) method. This MMH method could lead to the formation of crystalline titania powders under much milder reaction conditions than the normally reported microemulsion-mediated methods, in which posttreatment of calcination was necessary. In this work, a kind of solution was formed by dissolving tetrabutyl titanate into hydrochloric acid or nitric acid, and the solution was dispersed in an organic phase for the preparation of the microemulsion medium. The aqueous cores of water/Triton X-100/hexanol/cyclohexane microemulsions were used as constrained microreactors for a controlled growth of titania particles under hydrothermal conditions. The product of hydrothermal synthesis was separated and dried for characterization. The phase components and the morphologies and grain sizes of products were determined by X-ray diffraction (XRD) and by transmission electron microscopy (TEM). The effects of changing the variables of the reaction conditions, such as the use of acid, the concentrations of acid, the reaction temperatures, and/or the reaction times on the phases and morphologies of the titania product are described.

  19. Synthesis of lithium cobalt oxide by single-step soft hydrothermal method

    SciTech Connect

    Kumar Bokinala, Kiran; Pollet, M.; Artemenko, A.; Miclau, M.; Grozescu, I

    2013-02-15

    Lithium cobalt double oxide LiCoO{sub 2} was synthesized at 220 Degree-Sign C by soft hydrothermal method using Co(OH){sub 2} and LiOH as precursors, LiOH/NaOH as mineralizers and H{sub 2}O{sub 2} as oxidant. The soft hydrothermal synthesis method offers the dual advantage of a much lower synthesis time and a higher purity in comparison with other synthesis methods. The compound was identified by X-ray diffraction and its purity was checked by magnetic and electron magnetic resonance measurements. The grain morphology was studied by Scanning Electron Microscopy and an exponential growth of particle size with synthesis time was observed. - Graphical abstract: Concave cuboctohedrons obtained after 60 h reaction time. Highlights: Black-Right-Pointing-Pointer An optimized soft hydrothermal method for a fast synthesis of high purity LiCoO{sub 2} compound is reported. Black-Right-Pointing-Pointer Both lamellar and cuboctahedral particles could be stabilized. Black-Right-Pointing-Pointer Secondary phases content is lower than 0.1%. Black-Right-Pointing-Pointer Close to surface defects were evidenced using EMR.

  20. Evaluating experimental artifacts in hydrothermal prebiotic synthesis experiments

    NASA Technical Reports Server (NTRS)

    Smirnov, Alexander; Schoonen, Martin A A.

    2003-01-01

    Control experiments with ultra pure deionized water were conducted to evaluate the organic contamination in hydrothermal prebiotic experiments. Different combinations of reaction vessel material, sampling tubing and stirring were tested and the amounts of organic contaminants determined. All tested types of polymer tubing were proven to introduce organic contaminants (formate, acetate and propionate ions) into the reacting solution. Stainless steel has a catalytic effect on the decomposition of formate, consistent with earlier work at high temperatures and pressures.

  1. Experimental Investigation of Organic Synthesis in Hydrothermal Environments

    NASA Technical Reports Server (NTRS)

    Shock, Everett L.

    1998-01-01

    Seafloor hydrothermal systems may be the most likely locations on the early Earth for the emergence of life. Because of the disequilibrium inherent in such dynamic, mixing environments, abundant chemical energy would have been available for formation of the building blocks of life. In addition, theoretical studies suggest that organic compounds in these conditions would reach metastable states, due to kinetic barriers to the formation of stable equilibrium products (CO2 and methane). The speciation of organic carbon in metastable states is highly dependent on the oxidation state, pH, temperature, pressure and bulk composition of the system. The goal of our research is to investigate the effects of a number external variables on the formation, transformation, and stability of organic compounds at hydrothermal conditions. We have begun experimental work to attempt to control the oxidation state of simulated hydrothermal systems by using buffers composed of mineral powders and gas mixtures. We are also beginning to test the stability of organic compounds under these conditions. The experiments are being performed using the hydrothermal bomb apparatus at the U.S. Geological Survey in Menlo Park, CA and the supercritical water oxidizer (SCWO) at NASA Ames Research Center in Moffet Field, CA. The amino acids decomposed rapidly. Even after the approximately 15 minutes between addition of the amino acids and the first sampling, no amino acids were detected in the PPM system by GC- MS, while in the FeFeO system the amino acids were present at a level of less than 50% of original. Carboxylic acids, ammonia, and CO2 were the main products, along with some unidentified compounds. The ratios of carboxylic acids and concentrations of other products seem to have remained stable during the experiments, consistent with observations of other metastable systems and theoretical predictions.

  2. Evaluating experimental artifacts in hydrothermal prebiotic synthesis experiments.

    PubMed

    Smirnov, Alexander; Schoonen, Martin A A

    2003-04-01

    Control experiments with ultra pure deionized water were conducted to evaluate the organic contamination in hydrothermal prebiotic experiments. Different combinations of reaction vessel material, sampling tubing and stirring were tested and the amounts of organic contaminants determined. All tested types of polymer tubing were proven to introduce organic contaminants (formate, acetate and propionate ions) into the reacting solution. Stainless steel has a catalytic effect on the decomposition of formate, consistent with earlier work at high temperatures and pressures.

  3. Experimental Investigation of Organic Synthesis in Hydrothermal Environments

    NASA Technical Reports Server (NTRS)

    Shock, Everett L.

    1998-01-01

    The results of the investigation were presented at a Astrobiology Institute General Meeting. Seafloor hydrothermal systems may be the most likely locations on the early Earth for the emergence of life. Because of the disequilibrium inherent in such dynamic, mixing environments, abundant chemical energy would have been available for formation of the building blocks of life. In addition, theoretical studies suggest that organic compounds in these conditions would reach metastable states, due to kinetic barriers to the formation of stable equilibrium products (CO2 and methane). The speciation of organic carbon in metastable states is highly dependent on the oxidation state, pH, temperature, pressure and bulk composition of the system. The goal of our research is to investigate the effects of a number external variables on the formation, transformation, and stability of organic compounds at hydrothermal conditions. We have begun experimental work to attempt to control the oxidation state of simulated hydrothermal systems by using buffers composed of mineral powders and gas mixtures. We are also beginning to test the stability of organic compounds under these conditions.

  4. Hydrothermal synthesis of hollow silica spheres under acidic conditions.

    PubMed

    Yu, Qiyu; Wang, Pengpeng; Hu, Shi; Hui, Junfeng; Zhuang, Jing; Wang, Xun

    2011-06-07

    It is well-known that silica can be etched in alkaline media or in a unique hydrofluoric acid (HF) solution, which is widely used to prepare various kinds of hollow nanostructures (including silica hollow structures) via silica-templating methods. In our experiments, we found that stöber silica spheres could be etched in generic acidic media in a well-controlled way under hydrothermal conditions, forming well-defined hollow/rattle-type silica spheres. Furthermore, some salts such as NaCl and Na(2)SO(4) were found to be favorable for the formation of hollow/rattle-type silica spheres.

  5. Hydrothermal synthesis of hydroxyapatite nanorods using pyridoxal-5′-phosphate as a phosphorus source

    SciTech Connect

    Zhao, Xin-Yu; Zhu, Ying-Jie Lu, Bing-Qiang; Chen, Feng; Qi, Chao; Zhao, Jing; Wu, Jin

    2014-07-01

    Graphical abstract: Hydroxyapatite nanorods are synthesized using biocompatible biomolecule pyridoxal-5′-phosphate as a new organic phosphorus source by the hydrothermal method. - Highlights: • Hydrothermal synthesis of hydroxyapatite nanorods is reported. • Biocompatible pyridoxal-5′-phosphate is used as an organic phosphorus source. • This method is simple, surfactant-free and environmentally friendly. - Abstract: Hydroxyapatite nanorods are synthesized by the hydrothermal method using biocompatible biomolecule pyridoxal-5′-phosphate (PLP) as a new organic phosphorus source. In this method, PLP biomolecules are hydrolyzed to produce phosphate ions under hydrothermal conditions, and these phosphate ions react with pre-existing calcium ions to form hydroxyapatite nanorods. The effects of experimental conditions including hydrothermal temperature and time on the morphology and crystal phase of the products are investigated. This method is simple, surfactant-free and environmentally friendly. The products are characterized by X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared (FTIR) spectroscopy, and thermogravimetric (TG) analysis.

  6. Hydrothermal synthesis of nanostructured graphene/polyaniline composites as high-capacitance electrode materials for supercapacitors

    NASA Astrophysics Data System (ADS)

    Wang, Ronghua; Han, Meng; Zhao, Qiannan; Ren, Zonglin; Guo, Xiaolong; Xu, Chaohe; Hu, Ning; Lu, Li

    2017-03-01

    As known to all, hydrothermal synthesis is a powerful technique for preparing inorganic and organic materials or composites with different architectures. In this reports, by controlling hydrothermal conditions, nanostructured polyaniline (PANi) in different morphologies were composited with graphene sheets (GNS) and used as electrode materials of supercapacitors. Specifically, ultrathin PANi layers with total thickness of 10–20 nm are uniformly composited with GNS by a two-step hydrothermal-assistant chemical oxidation polymerization process; while PANi nanofibers with diameter of 50~100 nm are obtained by a one-step direct hydrothermal process. Benefitting from the ultrathin layer and porous structure, the sheet-like GNS/PANi composites can deliver specific capacitances of 532.3 to 304.9 F/g at scan rates of 2 to 50 mV/s. And also, this active material showed very good stability with capacitance retention as high as ~99.6% at scan rate of 50 mV/s, indicating a great potential for using in supercapacitors. Furthermore, the effects of hydrothermal temperatures on the electrochemical performances were systematically studied and discussed.

  7. Hydrothermal synthesis of nanostructured graphene/polyaniline composites as high-capacitance electrode materials for supercapacitors.

    PubMed

    Wang, Ronghua; Han, Meng; Zhao, Qiannan; Ren, Zonglin; Guo, Xiaolong; Xu, Chaohe; Hu, Ning; Lu, Li

    2017-03-14

    As known to all, hydrothermal synthesis is a powerful technique for preparing inorganic and organic materials or composites with different architectures. In this reports, by controlling hydrothermal conditions, nanostructured polyaniline (PANi) in different morphologies were composited with graphene sheets (GNS) and used as electrode materials of supercapacitors. Specifically, ultrathin PANi layers with total thickness of 10-20 nm are uniformly composited with GNS by a two-step hydrothermal-assistant chemical oxidation polymerization process; while PANi nanofibers with diameter of 50~100 nm are obtained by a one-step direct hydrothermal process. Benefitting from the ultrathin layer and porous structure, the sheet-like GNS/PANi composites can deliver specific capacitances of 532.3 to 304.9 F/g at scan rates of 2 to 50 mV/s. And also, this active material showed very good stability with capacitance retention as high as ~99.6% at scan rate of 50 mV/s, indicating a great potential for using in supercapacitors. Furthermore, the effects of hydrothermal temperatures on the electrochemical performances were systematically studied and discussed.

  8. Hydrothermal synthesis of nanostructured graphene/polyaniline composites as high-capacitance electrode materials for supercapacitors

    PubMed Central

    Wang, Ronghua; Han, Meng; Zhao, Qiannan; Ren, Zonglin; Guo, Xiaolong; Xu, Chaohe; Hu, Ning; Lu, Li

    2017-01-01

    As known to all, hydrothermal synthesis is a powerful technique for preparing inorganic and organic materials or composites with different architectures. In this reports, by controlling hydrothermal conditions, nanostructured polyaniline (PANi) in different morphologies were composited with graphene sheets (GNS) and used as electrode materials of supercapacitors. Specifically, ultrathin PANi layers with total thickness of 10–20 nm are uniformly composited with GNS by a two-step hydrothermal-assistant chemical oxidation polymerization process; while PANi nanofibers with diameter of 50~100 nm are obtained by a one-step direct hydrothermal process. Benefitting from the ultrathin layer and porous structure, the sheet-like GNS/PANi composites can deliver specific capacitances of 532.3 to 304.9 F/g at scan rates of 2 to 50 mV/s. And also, this active material showed very good stability with capacitance retention as high as ~99.6% at scan rate of 50 mV/s, indicating a great potential for using in supercapacitors. Furthermore, the effects of hydrothermal temperatures on the electrochemical performances were systematically studied and discussed. PMID:28291246

  9. Stable Carbon Isotopic Signatures of Abiotic Organics from Hydrothermal Synthesis Experiments

    NASA Technical Reports Server (NTRS)

    Stern, Jennifer C.; Summers, David P.; Kubo, Mike; Yassar, Saima

    2006-01-01

    Stable carbon isotopes can be powerful biogeochemical markers in the study of life's origins. Biogenic carbon fixation produces organics that are depleted in C-13 by about -20 to -30%0. Less attention has been paid to the isotopic signatures of abiotic processes. The possibility of abiotic processes producing organics with morphologies and isotopic signatures in the biogenic range has been at the center of recent debate over the Earth's earliest microfossils. The abiotic synthesis of organic compounds in hydrothermal environments is one possible source of endogenous organic matter to the prebiotic earth. Simulated hydrothermal settings have been shown to synthesize, among other things, single chain amphiphiles and simple lipids from a mix of CO, CO2, and H2. A key characteristic of these amphiphilic molecules is the ability to self-assemble in aqueous phases into more organized structures called vesicles, which form a selectively permeable boundary and serve the function of containing and concentrating other organic molecules. The ability to form cell like structures also makes these compounds more likely to be mistaken for biogenic. Hydrothermal simulation experiments were conducted from oxalic or formic acid in water at 175 C for 72 hr. The molecular and isotopic composition of the products of these reactions were determined and compared to biogenic fractionations . Preliminary results indicate isotopic fractionation during abiotic hydrocarbon synthesis in hydrothermal environments is on par with biological carbon fixation.

  10. Hydrothermal synthesis of single crystals of transition metal vanadates in the glaserite phase

    SciTech Connect

    Sanjeewa, Liurukara D.; McMillen, Colin D.; Willett, Daniel; Chumanov, George; Kolis, Joseph W.

    2016-04-15

    A series of transition metal vanadate crystals were prepared using a high temperature (580 °C) hydrothermal method. The compounds all had the general formula A{sub 2}AEM(VO{sub 4}){sub 2} (A=K, Na, Li; AE=Ba, Sr; M=Co, Fe, Mn). They are all variations of the glaserite structural type and range in symmetry from P-3m1 to P-3 to P2{sub 1}/c. Most of the derivatives contain a planar three-fold rotation operation, making them possible spin frustration candidates. Single crystal structural analyses were performed on many of the derivatives to obtain a detailed understanding of the distortions of the tetrahedral building blocks that accommodate the symmetry distortions. A hydrothermal growth method was developed to grow high quality single crystals of sizes up to 2–3 mm/edge. This method can be generalized for large crystal growth to enable magnetic and neutron diffraction studies that require relatively large single crystals. - Highlights: • The hydrothermal synthesis of glaserite-type vanadates is demonstrated. • Synthesis from stoichiometric component reactions yields 0.2–0.5 mm size crystals. • Hydrothermal recrystallization of glaserite powder yields 2–3 mm size crystals. • The structure varies according to the alkali and alkaline earth metals selected. • Ideal (P-3m1) and distorted (P-3 and P2{sub 1}/c) glaserite structures are observed.

  11. Hydrothermal synthesis, growth, and properties of a new chloride iodate

    NASA Astrophysics Data System (ADS)

    Zhao, Wenwu; Pan, Shilie; Dong, Lingyun; Yang, Zhihua; Dong, Xiaoyu; Chen, Zhaohui; Zhang, Min; Zhang, Fangfang

    2013-10-01

    A new chloride iodate, K2Bi(IO3)4Cl, has been synthesized using hydrothermal method from the KIO3-BiCl3 system. It crystallizes in the monoclinic system, space group P21/c with unit-cell parameters a = 11.216(3) Å, b = 12.260(3) Å, c = 10.444(2) Å, Z = 4, V = 1352.2(5) Å3. The material exhibits a three-dimensional structure consisting of interlocking iodide-linked infinite ∞[Bi(IO3)4] layer with interlayer potassium cations and chloride ions for charge balance. The powder X-ray diffraction pattern of the K2Bi(IO3)4Cl has been measured. Functional groups presented in the sample were identified by Fourier transform infrared spectrum. Thermal analysis and elemental analysis were also performed on the reported material.

  12. Vanadium oxides nanostructures: Hydrothermal synthesis and electrochemical properties

    SciTech Connect

    Mjejri, I.; Etteyeb, N.; Sediri, F.

    2014-12-15

    Highlights: • Vanadium oxides nanostructures were synthesized hydrothermally. • Reversible redox behavior with doping/dedoping process. • Doping/dedoping is easier for Li{sup +} to Na{sup +}. • Energy-related applications such as cathodes in lithium batteries. - Abstract: A facile and template-free one-pot strategy is applied to synthesize nanostructured vanadium oxide particles via a hydrothermal methodology. X-ray diffraction (XRD), scanning electron microscope (SEM), Fourier transforms infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) have been used to characterize the structure and morphology of the samples. The products are gradually changed from sheet-shaped VO{sub 2}(B) to rod-like V{sub 3}O{sub 7}·H{sub 2}O with decreasing cyclohexanediol as both protective and reducing agent. The specific surface area of the VO{sub 2}(B) nanosheets and V{sub 3}O{sub 7}·H{sub 2}O nanorods was found to be 22 and 16 m{sup 2} g{sup −1}, respectively. Thin films of VO{sub 2}(B) and V{sub 3}O{sub 7}·H{sub 2}O deposited on ITO substrates were electrochemically characterized by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The voltammograms show reversible redox behavior with doping/dedoping process corresponding to reversible cation intercalation/de-intercalation into the crystal lattice of the nanorods/nanosheets. This process is easier for the small Li{sup +} cation than larger ones Na{sup +}.

  13. Hydrothermal synthesis and characterization of CuFeO2 Delafossite Crystals

    NASA Astrophysics Data System (ADS)

    Sarabia, M.; Rojas, S.; Lopez-Cabana, Z.; Villalba, R.; Gonzalez, G.; Cabrera, A. L.

    2015-03-01

    In this study we synthetized CuFeO2 compounds using as precursors Cu2O and FeOOH with fused NaOH. The synthesis takes place is a Teflon vessel lasting 97 (Synthesis I) or 48 hrs (Synthesis II) at 210 °C. The compound obtained were analyzed for crystal structure and morphology with Raman Sprectroscopy, X-Ray Diffraction (XRD), X-Ray Photoelectron Spectroscopy (XPS), Scanning Electron Microscopy (SEM), Energy Dispersive Spectroscopy (EDS). Optical properties were obtained by UV-Vis Spectroscopy and Gas adsorption measured with a Quartz-Crystal Microbalance (QCM). Our results show that this type of hydrothermal synthesis is capable to recreate the Delafossite structure of this copper-iron oxide. This material chemisorbs water and carbon dioxide. Funds FONDECyT 1130372.

  14. Hydrothermal Synthesis and Catalytic Application of Ultrathin Rhodium Nanosheet Nanoassemblies.

    PubMed

    Bai, Juan; Xu, Guang-Rui; Xing, Shi-Hui; Zeng, Jing-Hui; Jiang, Jia-Xing; Chen, Yu

    2016-12-14

    Ultrathin noble metal nanosheets with atomic thickness exhibit abnormal electronic, surfacial, and photonic properties due to the unique two-dimensional (2D) confinement effect, which have attracted intensive research attention in catalysis/electrocatalysis. In this work, the well-defined ultrathin Rh nanosheet nanoassemblies with dendritic morphology are synthesized by a facile hydrothermal method with assistance of poly(allylamine hydrochloride) (PAH), where PAH effectively acts as the complexant and shape-directing agent. Transmission electron microscopy and atomic force microscopy images reveal the thickness of 2D Rh nanosheet with (111) planes is only ca. 0.8-1.1 nm. Nitrogen adsorption-desorption measurement displays the specific surface area of the as-prepared ultrathin Rh nanosheet nanoassemblies is 139.4 m(2) g(-1), which is much bigger than that of homemade Rh black (19.8 m(2) g(-1)). Detailed catalytic investigations display the as-prepared ultrathin Rh nanosheet nanoassemblies have nearly 20.4-fold enhancement in mass-activity for the hydrolysis of ammonia borane as compared with homemade Rh black.

  15. Microwave-hydrothermal process for the synthesis of rutile

    SciTech Connect

    Baldassari, Sara; Komarneni, Sridhar . E-mail: komarneni@psu.edu; Mariani, Emilia; Villa, Carla

    2005-11-03

    The synthesis of pure rutile titanium dioxide is not an easy achievement, as the crystallization process generally leads to mixtures of two or even three phases; moreover the synthetic processes normally used by industry require harsh reaction conditions. We carried out the synthesis of titanium dioxide from an aqueous titanium tetrachloride solution under microwave irradiation in the reaction time range of 5-120 min. We mostly obtained mixtures of rutile and anatase, but obtained single-phase rutile after a 2-h treatment at 160 deg. C; transmission electron micrographs revealed well-dispersed spherical nanoparticles. We also investigated the effects of dilution and addition of a dispersant (polyvinylpyrrolidone) on phase crystallization and particle shape.

  16. VentDB: A Global Online Synthesis Database of Seafloor Hydrothermal Spring Geochemistry

    NASA Astrophysics Data System (ADS)

    Mottl, M. J.; Lehnert, K. A.; Johansson, A. K.; Hsu, L.

    2011-12-01

    Chemical data for seafloor hydrothermal springs are fundamental to the study of mid-ocean ridge and seafloor processes, ocean water chemistry, and global geochemical cycles, as well as vent ecosystems and the sub-seafloor biosphere. So far, these data have been accessible only in the scientific literature or in online data catalogs where they are widely dispersed in individual data tables, and are often insufficiently documented for re-use. We have developed VentDB as an online data system for geochemical data for hydrothermal springs that will facilitate access and analysis of these data. VentDB uses the concept and architecture of the popular PetDB database for seafloor igneous and metamorphic rock geochemistry (www.petdb.org) to provide easy and fast access to a global synthesis of seafloor hydrothermal spring geochemical data. The VentDB database contains concentrations of major and trace species, dissolved gases, and radiogenic and isotopic ratios for hydrothermal vents on the seafloor. Further chemical or physical properties of hydrothermal springs can be included in the future if desired. The database comprises both the calculated hydrothermal end-member solution compositions as estimated by extrapolation of the concentrations of individual chemical species to a Mg concentration of zero, and the raw data for hydrothermal solution samples as collected, where available. Data quality is documented by including information for the raw analytical data about the analytical method, precision, and reference material measurements, and quality control parameters for end-member compositions including the lowest Mg measured in any sample, the number of samples and correlation coefficient of the linear regression, and the charge balance for the extrapolated zero-Mg composition. The database also includes information about the sampled locations (geospatial coordinates, vent or vent field names, names of other physiographic features), temperature, flow and vent type

  17. Hydrothermal synthesis of TiO2 nanostructure films and their photoelectrochemical properties

    NASA Astrophysics Data System (ADS)

    Miao, Hui; Hu, Xiaoyun; Fan, Jun; Li, Chaoben; Sun, Qian; Hao, Yuanyuan; Zhang, Guowei; Bai, Jintao; Hou, Xun

    2015-12-01

    In this study, anatase TiO2 nanostructured films were successfully prepared via Ti foil-assisted hydrothermal synthesis method without any surfactants. With the increase of hydrothermal time from 3 to 12 h, the surface morphologies of the films changed from nanotubes to nanoflowers and the thickness of the films increased from 2.5 to 4.2 μm. The nanoflowers were seated on a layer of oriented nanotubes and consisted of nanosheets. Both nanotubes and nanosheets were multi-walled, comprising interconnected [TiO6] octahedra. Ti foil and acid-treated Ti foil both formed pieces of thin films on the surface with nanotubes and nanoflowers, respectively. Photoelectrochemistry tests showed that the photocurrent response of the nanotube film was nearly 13.8 μA/cm2, which was approximately three times higher than that of nanoflowers film. This indicates that the nanotubes more successfully transferred electrons to the surface of the film as a result of nanotubes providing direct pathways for electrons from the point of injection to the Ti foil electrode. The ultraviolet (UV)-visible-near infrared (NIR) absorption spectra indicated that the nanotube film had a narrower band gap as compared to the nanoflower film. In other words, a relatively low hydrothermal treatment temperature or relatively short hydrothermal treatment time is better for preparing excellent photocurrent response films.

  18. In situ hydrothermal synthesis of tetrazole coordination polymers with interesting physical properties.

    PubMed

    Zhao, Hong; Qu, Zhi-Rong; Ye, Heng-Yun; Xiong, Ren-Gen

    2008-01-01

    Tetrazole compounds have been studied for more than one hundred years and applied in various areas. Several years ago Sharpless and his co-workers reported an environmentally friendly process for the preparation of 5-substituted 1H-tetrazoles in water with zinc salt as catalysts. To reveal the exact role of the zinc salt in this reaction, a series of hydrothermal reactions aimed at trapping and characterizing the solid intermediates were investigated. This study allowed us to obtain a myriad interesting metal-organic coordination polymers that not only partially showed the role of the metal species in the synthesis of tetrazole compounds but also provided a class of complexes displaying interesting chemical and physical properties such as second harmonic generation (SHG), fluorescence, ferroelectric and dielectric behaviors. In this tutorial review, we will mainly focus on tetrazole coordination compounds synthesized by in situ hydrothermal methods. First, we will discuss the synthesis and crystal structures of these compounds. Their various properties will be mentioned and we will show the applications of tetrazole coordination compounds in organic synthesis. Finally, we will outline some expectations in this area of chemistry. The direct coordination chemistry of tetrazoles to metal ions and in situ synthesis of tetrazole through cycloaddition between organotin azide and organic cyano group will be not discussed in this review.

  19. Hydrothermal synthesis of alpha- and beta-HgS nanostructures

    NASA Astrophysics Data System (ADS)

    Galain, Isabel; María, Pérez Barthaburu; Ivana, Aguiar; Laura, Fornaro

    2017-01-01

    We synthesized HgS nanostructures by the hydrothermal method in order to use them as electron acceptors in hybrid organic-inorganic solar cells. We employed different mercury sources (HgO and Hg(CH3COO)2) and polyvinylpyrrolidone (PVP) or hexadecanethiol (HDT) as stabilizing/capping agent for controlling size, crystallinity, morphology and stability of the obtained nanostructures. We also used thiourea as sulfur source, and a temperature of 180 °C during 6 h. Synthesized nanostructures were characterized by powder X-Ray Diffraction, Diffuse Reflectance Infrared Fourier Transform and Transmission Electron Microscopy. When PVP acts as stabilizing agent, the mercury source has influence on the size -but not in morphology- of the beta-HgS obtained nansostructures. HDT has control over nanostructures' size and depending on the relation Hg:HDT, we obtained a mixture of alpha and beta HgS which can be advantageous in the application in solar cells, due their absorption in different spectral regions. The smallest nanostructures obtained have a mean diameter of 20 nm when using HDT as capping agent. Also, we deposited the aforementioned nanostructures onto flat glass substrates by the spin coating technique as a first approach of an active layer of a solar cell. The depositions were characterized by atomic force microscopy. We obtained smaller particle deposition and higher particle density -but a lower area coverage (5%) - in samples with HDT as capping agent. This work presents promising results on nanostructures for future application on hybrid solar cells. Further efforts will be focused on the deposition of organic-inorganic layers.

  20. Sonochemical and hydrothermal synthesis of PbTe nanostructures with the aid of a novel capping agent

    SciTech Connect

    Fard-Fini, Shahla Ahmadian; Salavati-Niasari, Masoud; Mohandes, Fatemeh

    2013-10-15

    Graphical abstract: - Highlights: • PbTe nanostructures were prepared with the aid of Schiff-base compound. • Sonochemical and hydrothermal methods were employed to fabricate PbTe nanostrucrues. • The effect of preparation parameters on the morphology of PbTe was investigated. - Abstract: In this work, a new Schiff-base compound derived from 1,8-diamino-3,6-dioxaoctane and 2-hydroxy-1-naphthaldehyde marked as (2-HyNa)-(DaDo) was synthesized, characterized, and then used as capping agent for the preparation of PbTe nanostructures. To fabricate PbTe nanostructures, two different synthesis methods; hydrothermal and sonochemical routes, were applied. To further investigate, the effect of preparation parameters like reaction time and temperature in hydrothermal synthesis and sonication time in the presence of ultrasound irradiation on the morphology and purity of the final products was tested. The products were analyzed with the aid of SEM, TEM, XRD, FT-IR, and EDS. Based on the obtained results, it was found that pure cubic phased PbTe nanostructures have been obtained by hydrothermal and sonochemical approaches. Besides, SEM images showed that cubic-like and rod-like PbTe nanostructures have been formed by hydrothermal and sonochemical methods, respectively. Sonochemical synthesis of PbTe nanostructures was favorable, because the synthesis time of sonochemical method was shorter than that of hydrothermal method.

  1. Direct synthesis of thermochromic VO{sub 2} through hydrothermal reaction

    SciTech Connect

    Alie, David; Gedvilas, Lynn; Wang, Zhiwei; Tenent, Robert; Engtrakul, Chaiwat; Yan, Yanfa; Shaheen, Sean E.; Dillon, Anne C.; Ban, Chunmei

    2014-04-01

    Thermochromic VO{sub 2} was directly synthesized using hydrothermal techniques. The effects of formation conditions on the structure and morphology of the final product were studied through X-ray diffraction (XRD), and scanning electron microscopy (SEM). Unique hollow sphere morphology was observed for the synthesized VO{sub 2} powders. Ex-situ XRD studies after heat treatment confirmed the thermal stability of the VO{sub 2} structure. Thermochromic properties, as a consequence of the reversible structural transformation between monoclinic VO{sub 2} and tetragonal phases, were observed by Fourier transform infrared spectroscopy (FTIR). - Graphical abstract: Thermochromic VO{sub 2} crystals with hollow spherical and asterisk shape were directly synthesized using hydrothermal techniques. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) studies confirmed the thermal stability and the reversible thermochromic properties of the VO{sub 2} structure. - Highlights: • One-step synthesis of thermochromic VO{sub 2} monoclinic phase, and VO{sub 2} (A and B phases) using hydrothermal technique. VO{sub 2} (A), VO{sub 2} (B). • Identification of the relationship between synthesis conditions and the morphology/structure of the final products. • Formation of VO{sub 2} monoclinic phase with an interesting hollow sphere shape. • Demonstration of superior thermal stability of the VO{sub 2} monoclinic phase. • Characterizing the thermochromic properties of VO{sub 2} monoclinic phase.

  2. Simple mass production of zinc oxide nanostructures via low-temperature hydrothermal synthesis

    NASA Astrophysics Data System (ADS)

    Ghasaban, Samaneh; Atai, Mohammad; Imani, Mohammad

    2017-03-01

    The specific properties of zinc oxide (ZnO) nanoparticles have attracted much attention within the scientific community as a useful material for biomedical applications. Hydrothermal synthesis is known as a useful method to produce nanostructures with certain particle size and morphology however, scaling up the reaction is still a challenging task. In this research, large scale hydrothermal synthesis of ZnO nanostructures (60 g) was performed in a 5 l stainless steel autoclave by reaction between anionic (ammonia or sodium hydroxide) and cationic (zinc acetate dehydrate) precursors in low temperature. Hydrothermal reaction temperature and time were decreased to 115 °C and 2 or 6 h. In batch repetitions, the same morphologies (plate- and needle-like) with reproducible particle size were obtained. The nanostructures formed were analyzed by powder x-ray diffraction, Fourier-transform infrared spectroscopy, energy dispersive x-ray analysis, scanning electron microscopy and BET analysis. The nanostructures formed were antibacterially active against Staphylococcus aureus.

  3. Highly aligned arrays of high aspect ratio barium titanate nanowires via hydrothermal synthesis

    SciTech Connect

    Bowland, Christopher C.; Zhou, Zhi; Malakooti, Mohammad H.; Sodano, Henry A.

    2015-06-01

    We report on the development of a hydrothermal synthesis procedure that results in the growth of highly aligned arrays of high aspect ratio barium titanate nanowires. Using a multiple step, scalable hydrothermal reaction, a textured titanium dioxide film is deposited on titanium foil upon which highly aligned nanowires are grown via homoepitaxy and converted to barium titanate. Scanning electron microscope images clearly illustrate the effect the textured film has on the degree of orientation of the nanowires. The alignment of nanowires is quantified by calculating the Herman's Orientation Factor, which reveals a 58% improvement in orientation as compared to growth in the absence of the textured film. The ferroelectric properties of barium titanate combined with the development of this scalable growth procedure provide a powerful route towards increasing the efficiency and performance of nanowire-based devices in future real-world applications such as sensing and power harvesting.

  4. Titanium dioxide nanoparticles: Impact of increasing ionic strength during synthesis, reflux, and hydrothermal aging

    SciTech Connect

    Isley, Sara L.; Jordan, David S.; Penn, R. Lee

    2009-01-08

    This work investigates the role of ionic strength during synthesis, reflux, and hydrothermal aging of sol-gel synthesized titanium dioxide. Research presented here uses X-ray diffraction data and Rietveld refinements to quantify anatase, brookite, and rutile phases as functions of synthetic and aging variables. In addition, the Scherrer equation is used to obtain average crystallite sizes for each phase quantified. Results presented in this work demonstrate that the most control over the sol-gel products can be obtained by modifying the pH during hydrolysis. In addition, while varying the ionic strength during reflux and hydrothermal aging can result in enhanced control over the crystalline phase and crystallite size, the most control can be achieved by varying the ionic strength during synthesis. Finally, sol-gel synthesis at low pH (-0.6) and high-chloride concentration (3 M NaCl) produced a heterogeneous sample composed of nanocrystalline anatase (3.8 nm) and rutile (2.9 nm)

  5. Rapid hydrothermal flow synthesis and characterisation of carbonate- and silicate-substituted calcium phosphates.

    PubMed

    Chaudhry, Aqif A; Knowles, Jonathan C; Rehman, Ihtesham; Darr, Jawwad A

    2013-09-01

    A range of crystalline and nano-sized carbonate- and silicate-substituted hydroxyapatite has been successfully produced by using continuous hydrothermal flow synthesis technology. Ion-substituted calcium phosphates are better candidates for bone replacement applications (due to improved bioactivity) as compared to phase-pure hydroxyapatite. Urea was used as a carbonate source for synthesising phase pure carbonated hydroxyapatite (CO₃-HA) with ≈5 wt% substituted carbonate content (sample 7.5CO₃-HA) and it was found that a further increase in urea concentration in solution resulted in biphasic mixtures of carbonate-substituted hydroxyapatite and calcium carbonate. Transmission electron microscopy images revealed that the particle size of hydroxyapatite decreased with increasing urea concentration. Energy-dispersive X-ray spectroscopy result revealed a calcium deficient apatite with Ca:P molar ratio of 1.45 (±0.04) in sample 7.5CO₃-HA. For silicate-substituted hydroxyapatite (SiO₄-HA) silicon acetate was used as a silicate ion source. It was observed that a substitution threshold of ∼1.1 wt% exists for synthesis of SiO₄-HA in the continuous hydrothermal flow synthesis system, which could be due to the decreasing yields with progressive increase in silicon acetate concentration. All the as-precipitated powders (without any additional heat treatments) were analysed using techniques including Transmission electron microscopy, X-ray powder diffraction, Differential scanning calorimetry, Thermogravimetric analysis, Raman spectroscopy and Fourier transform infrared spectroscopy.

  6. Pyrophosphate synthesis in iron mineral films and membranes simulating prebiotic submarine hydrothermal precipitates

    NASA Astrophysics Data System (ADS)

    Barge, Laura M.; Doloboff, Ivria J.; Russell, Michael J.; VanderVelde, David; White, Lauren M.; Stucky, Galen D.; Baum, Marc M.; Zeytounian, John; Kidd, Richard; Kanik, Isik

    2014-03-01

    Cells use three main ways of generating energy currency to drive metabolism: (i) conversion of adenosine diphosphate (ADP) to adenosine triphosphate (ATP) by the proton motive force through the rotor-stator ATP synthase; (ii) the synthesis of inorganic phosphate˜phosphate bonds via proton (or sodium) pyrophosphate synthase; or (iii) substrate-level phosphorylation through the direct donation from an active phosphoryl donor. A mechanism to produce a pyrophosphate bond as “energy currency” in prebiotic systems is one of the most important considerations for origin of life research. Baltscheffsky (1996) suggests that inorganic pyrophosphate (PO74-; PPi) may have preceded ATP/ADP as an energy storage molecule in earliest life, produced by an H+ pyrophosphatase. Here we test the hypothesis that PPi could be synthesized in inorganic precipitates simulating hydrothermal chimney structures transected by thermal and/or ionic gradients. Appreciable yields of PPi were obtained via substrate phosphorylation by acetyl phosphate within the iron sulfide/silicate precipitates at temperatures expected for an alkaline hydrothermal system. The formation of PPi only occurred in the solid phase, i.e. when both Pi and the phosphoryl donor were precipitated with Fe-sulfides or Fe-silicates. The amount of Ac-Pi incorporated into the precipitate was a significant factor in the amount of PPi that could form, and phosphate species were more effectively incorporated into the precipitate at higher temperatures (⩾50 to >85 °C). Thus, we expect that the hydrothermal precipitate would be more enriched in phosphate (and especially, Ac-Pi) near the inner margins of a hydrothermal mound where PPi formation would be at a maximum. Iron sulfide and iron silicate precipitates effectively stabilized Ac-Pi and PPi against hydrolysis (relative to hydrolysis in aqueous solution). Thus it is plausible that PPi could accumulate as an energy currency up to useful concentrations for early life in a

  7. Hydrothermal Synthesis and Photoluminescence of Boron Nitride Quantum Dots

    NASA Astrophysics Data System (ADS)

    Li, Hongling; Tay, Roland Yingjie; Tsang, Siu Hon; Teo, Edwin Hang Tong

    Boron nitride quantum dots (BNQDs), as a new member of heavy metal-free quantum dots, have attracted great interest owing to its unique structure as well as fascinating physical/chemical properties. However, it is still a challenge to controllably synthesize high quality BNQDs with high quantum yield (QY), uniform size and strong luminescence. Here we present a facile and effective approach to controllablly fabricate BNQDs by snoication-solvothermal technique. Encouragingly, the as-prepared BNQDs possess strong blue luminescence with high QY of up to 19.5%, which can be attributed to the synergic effect of size, surface chemistry and edge defects. In addition, the size of the BNQDs could be controlled with a narrow size distribution of 1.32 nm and the smallest average size achieved is 2.62 nm with an average thickness of ~3 atomic layers. Furthermore, the as-prepared BNQDs are non-toxic to cells and show nanosecond-scaled lifetimes and little photobleaching effect. Therefore, it is believed that BNQDs are promising as one of the novel heavy metal-free QDs for multi-purpose applications in a range of fields. Moreover, this synthesis concept is expected to open a new window to controllably prepare other heavy metal-free QDs, as well as to understand their luminescence mechanism.

  8. Hydrothermal synthesis of NiWO4 crystals for high performance non-enzymatic glucose biosensors

    PubMed Central

    Mani, Sivakumar; Vediyappan, Veeramani; Chen, Shen-Ming; Madhu, Rajesh; Pitchaimani, Veerakumar; Chang, Jia-Yaw; Liu, Shang-Bin

    2016-01-01

    A facile hydrothermal route for the synthesis of ordered NiWO4 nanocrystals, which show promising applications as high performance non-enzymatic glucose sensor is reported. The NiWO4-modified electrodes showed excellent sensitivity (269.6 μA mM−1 cm−2) and low detection limit (0.18 μM) for detection of glucose with desirable selectivity, stability, and tolerance to interference, rendering their prospective applications as cost-effective, enzyme-free glucose sensors. PMID:27087561

  9. One-step hydrothermal synthesis of nitrogen-doped nanocarbons: albumine directing the carbonization of glucose.

    PubMed

    Baccile, Niki; Antonietti, Markus; Titirici, Maria-Magdalena

    2010-02-22

    We present a simple and green one-step pathway towards nitrogen-doped carbon nanostructures with controlled mesoporosity through hydrothermal treatment of glucose in the presence of model proteins. Performing the reaction with different amounts of egg white ovalbumin protein (OvA), carbonaceous nanoparticles or continuous nanosponges with high specific surface areas can be efficiently produced. The nitrogen content of the structures is rather high (up to 8 wt%) and can be kept constant up to 950 degrees C, while oxygen elimination and graphitization of the carbon material occurs. We demonstrate here that sustainable natural resources can be efficiently used in the synthesis of pure high-potential nanomaterials.

  10. Hydrothermal Synthesis of Ultrasmall Pt Nanoparticles as Highly Active Electrocatalysts for Methanol Oxidation

    PubMed Central

    Ji, Wenhai; Qi, Weihong; Tang, Shasha; Peng, Hongcheng; Li, Siqi

    2015-01-01

    Ultrasmall nanoparticles, with sizes in the 1–3 nm range, exhibit unique properties distinct from those of free molecules and larger-sized nanoparticles. Demonstrating that the hydrothermal method can serve as a facile method for the synthesis of platinum nanoparticles, we successfully synthesized ultrasmall Pt nanoparticles with an average size of 2.45 nm, with the aid of poly(vinyl pyrrolidone) (PVP) as reducing agents and capping agents. Because of the size effect, these ultrasmall Pt nanoparticles exhibit a high activity toward the methanol oxidation reaction.

  11. Hydrothermal synthesis of NiWO4 crystals for high performance non-enzymatic glucose biosensors

    NASA Astrophysics Data System (ADS)

    Mani, Sivakumar; Vediyappan, Veeramani; Chen, Shen-Ming; Madhu, Rajesh; Pitchaimani, Veerakumar; Chang, Jia-Yaw; Liu, Shang-Bin

    2016-04-01

    A facile hydrothermal route for the synthesis of ordered NiWO4 nanocrystals, which show promising applications as high performance non-enzymatic glucose sensor is reported. The NiWO4-modified electrodes showed excellent sensitivity (269.6 μA mM-1 cm-2) and low detection limit (0.18 μM) for detection of glucose with desirable selectivity, stability, and tolerance to interference, rendering their prospective applications as cost-effective, enzyme-free glucose sensors.

  12. Confined-Pyrolysis as an Experimental Method for Hydrothermal Organic Synthesis

    NASA Technical Reports Server (NTRS)

    Leif, Roald N.; Simoneit, Bernd R. T.

    1995-01-01

    A closed pyrolysis system has been developed as a tool for studying the reactions of organic compounds under extreme hydrothermal conditions. Small high pressure stainless steel vessels in which the ratio of sediment or sample to water has been adjusted to eliminate the headspace at peak experimental conditions confines the organic components to the bulk solid matrix and eliminates the partitioning of the organic compounds away from the inorganic components during the experiment. Confined pyrolysis experiments were performed to simulate thermally driven catagenetic changes in sedimentary organic matter using a solids to water ratio of 3.4 to 1. The extent of alteration was measured by monitoring the steroid and triterpenoid biomarkers and polycyclic aromatic hydrocarbon distributions. These pyrolysis experiments duplicated the hydrothermal transformations observed in nature. Molecular probe experiments using alkadienes, alkenes and alkanes in H2O and D2O elucidated the isomerization and hydrogenation reactions of aliphatic and the competing oxidative reactions occurring under hydrothermal conditions. This confined pyrolysis technique is being applied to test experiments on organic synthesis of relevance to chemical evolution for the origin of life.

  13. One-step synthesis of hydrothermally stable mesoporous aluminosilicates with strong acidity

    NASA Astrophysics Data System (ADS)

    Yang, Dongjiang; Xu, Yao; Wu, Dong; Sun, Yuhan

    2008-09-01

    Using tetraethylorthosilicate (TEOS), polymethylhydrosiloxane (PMHS) and aluminium isopropoxide (AIP) as the reactants, through a one-step nonsurfactant route based on PMHS-TEOS-AIP co-polycondensation, hydrothermally stable mesoporous aluminosilicates with different Si/Al molar ratios were successfully prepared. All samples exclusively showed narrow pore size distribution centered at 3.6 nm. To assess the hydrothermal stability, samples were subjected to 100 °C distilled water for 300 h. The boiled mesoporous aluminosilicates have nearly the same N 2 adsorption-desorption isotherms and the same pore size distributions as those newly synthesized ones, indicating excellent hydrothermal stability. The 29Si MAS NMR spectra confirmed that PMHS and TEOS have jointly condensed and CH 3 groups have been introduced into the materials. The 27Al MAS NMR spectra indicated that Al atoms have been incorporated in the mesopore frameworks. The NH 3 temperature-programmed desorption showed strong acidity. Due to the existence of large amount of CH 3 groups, the mesoporous aluminosilicates obtained good hydrophobicity. Owing to the relatively large pore and the strong acidity provided by the uniform four-coordinated Al atoms, the excellent catalytic performance for 1,3,5-triisopropylbenzene cracking was acquired easily. The materials may be a profitable complement for the synthesis of solid acid catalysts.

  14. Facile mesoporous template-assisted hydrothermal synthesis of ordered mesoporous magnesium silicate as an efficient adsorbent

    NASA Astrophysics Data System (ADS)

    Lu, Qingshan; Li, Qiang; Zhang, Jingjing; Li, Jingfeng; Lu, Jinhua

    2016-01-01

    Mesoporous materials with unique structure as well as special morphology have potential applications in pollutant adsorption. In this work, using mesoporous silica SBA-15 filled with carbon (C@SBA-15) as both silicon source and assisted template, the ordered mesoporous magnesium silicate (Mg3Si4O9(OH)4) has been fabricated at 140 °C by a novel and facile hydrothermal method. During the hydrothermal process, the magnesium silicate grew along the silica walls at the expense of consuming silica and deposited on the carbon surface of the C@SBA-15. Meanwhile, the rigid carbon inside the pores of the SBA-15 supported the magnesium silicate as mesoporous walls under hydrothermal condition. The obtained magnesium silicate possessed ordered mesoporous structure, high specific surface area of 446 m2/g, large pore volume of 0.84 cm3/g, and hierarchical structure assembled with ultrathin nanosheets of 15 nm in thickness. These characteristics endow the ordered mesoporous magnesium silicate with the fast adsorption rate and high adsorption capacity of 382 mg/g for methylene blue. In addition, this synthesis method opens a new approach to fabricate other ordered mesoporous silicates.

  15. Hydrothermal synthesis, characterization and up/down-conversion luminescence of barium rare earth fluoride nanocrystals

    SciTech Connect

    Jia, Li-Ping; Zhang, Qiang; Yan, Bing

    2014-07-01

    Graphical abstract: Lanthanide ions doped bare earth rare earth fluoride nanocrystals are synthesized by hydrothermal technology and characterized. The down/up-conversion luminescence of them are discussed. - Highlights: • Mixed hydrothermal system H{sub 2}O–OA (EDA)–O-A(LO-A) is used for synthesis. • Barium rare earth fluoride nanocrystals are synthesized comprehensively. • Luminescence for down-conversion and up-conversion are obtained for these systems. - Abstract: Mixed hydrothermal system H{sub 2}O–OA (EDA)–O-A(LO-A) is developed to synthesize barium rare earth fluorides nanocrystals (OA = oleylamine, EDA = ethylenediamine, O-A = oleic acid and LO-A = linoleic acid). They are presented as BaREF{sub 5} (RE = Ce, Pr, Nd, Eu, Gd, Tb, Dy, Y, Tm, Lu) and Ba{sub 2}REF{sub 7} (RE = La, Sm, Ho, Er, Yb). The influence of reaction parameters (rare earth species, hydrothermal system and temperature) is checked on the phase and shape evolution of the fluoride nanocrystals. It is found that reaction time and temperature of these nanocrystals using EDA (180 °C, 6 h) is lower than those of them using OA (220 °C, 10 h). The photoluminescence properties of these fluorides activated by some rare earth ions (Nd{sup 3+}, Eu{sup 3+}, Tb{sup 3+}) are studied, and especially up-conversion luminescence of the four fluoride nanocrystal systems (Ba{sub 2}LaF{sub 7}:Yb, Tm(Er), Ba{sub 2}REF{sub 7}:Yb, Tm(Er) (RE = Gd, Y, Lu)) is observed.

  16. A novel microwave applicator for tailoring the energy input for hydrothermal synthesis of zeolites.

    PubMed

    Stenzel, C; Brinkmann, M; Müller, J; Schertlen, R; Venot, Y; Wiesbeck, W

    2001-01-01

    A new applicator system for microwave heating of aqueous solutions for the hydrothermal synthesis of zeolite crystals has been developed and experimentally characterized. It is based on a short-ended coaxial waveguide with the solution being inserted as a lossy dielectric. The electrical and thermal design of the autoclave has been optimized by numerical simulations of the E-field and of the temperature distribution respectively. Different reference temperature profiles--a homogeneous and a gradient one--could be established within the zeolite solution and were held constant over time. From temperature measurements at various positions in the solution the two reference profiles could be verified. Temperature differences of less than 15 degrees C have been measured within the homogeneous autoclave whereas differences up to 55 degrees C have been found in the gradient autoclave. In the first synthesis experiments using this applicator zeolite crystals of the zeolite A and VPI-5-type could be successfully crystallized.

  17. Hydrothermal synthesis of a novel uranium oxalate/glycolate via in-situ ligand formation.

    PubMed

    Knope, Karah E; Cahill, Christopher L

    2007-08-06

    A novel templated uranium oxalate/glycolate, (UO2)4(O)2(C2O4)(H2C2O3)2.2[(C8H20)N] (a = 7.9230(8) A, b = 13.3793(13) A, c = 17.4141(18) A, beta = 96.006(2) degrees , monoclinic, P21/n, Z = 2), has been synthesized under hydrothermal conditions via in-situ ligand synthesis. The oxalate and glycolate anions have been formed through the oxidation of 1,4-diazabicyclo[2.2.2]octane, which proceeds through intermediates such as piperazine and ethylene glycol. Reported herein is the synthesis of this compound, crystal structure, and mechanistic information regarding the oxidation pathway.

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

    NASA Technical Reports Server (NTRS)

    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.

  19. Hydrothermal synthesis of ultrafine barium hexaferrite nanoparticles and the preparation of their stable suspensions.

    PubMed

    Primc, D; Makovec, D; Lisjak, D; Drofenik, M

    2009-08-05

    The hydrothermal treatment of an appropriate suspension of Ba and Fe hydroxides in the presence of a large excess of OH(-) results in the formation of Ba hexaferrite at temperatures as low as 150 degrees C. This low formation temperature enables the synthesis of uniform, ultrafine Ba hexaferrite nanoparticles. These nanoparticles have a disc-like shape, approximately 10 nm wide, but only approximately 3 nm thick. When the temperature of the hydrothermal treatment is increased, large platelet Ba hexaferrite crystals appear as a consequence of secondary re-crystallization (Ostwald ripening). In this work, this undesired process of secondary re-crystallization has been evaluated. We show that the secondary re-crystallization can be totally suppressed with the use of an oleic acid surfactant. The addition of oleic acid enabled the synthesis of uniform, ultrafine nanoparticles at temperatures up to 240 degrees C. The nanoparticles were hydrophobic and could be suspended in nonpolar liquids to form relatively concentrated ferrofluids. Such stable suspensions of hexaferrite nanoparticles will be technologically important, especially as precursors for the preparation of new nanostructured materials, for example nanocomposites or nanostructured ceramic films.

  20. Evaluating reaction pathways of hydrothermal abiotic organic synthesis at elevated temperatures and pressures using carbon isotopes

    NASA Astrophysics Data System (ADS)

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

    2015-04-01

    Experiments were performed to better understand the role of environmental factors on reaction pathways and corresponding carbon isotope fractionations during abiotic hydrothermal synthesis of organic compounds using piston cylinder apparatus at 750 °C and 5.5 kbars. Chemical compositions of experimental products and corresponding carbon isotopic values were obtained by a Pyrolysis-GC-MS-IRMS system. Alkanes (methane and ethane), straight-chain saturated alcohols (ethanol and n-butanol) and monocarboxylic acids (formic and acetic acids) were generated with ethanol being the only organic compound with higher δ13C than CO2. CO was not detected in experimental products owing to the favorable water-gas shift reaction under high water pressure conditions. The pattern of δ13C values of CO2, carboxylic acids and alkanes are consistent with their equilibrium isotope relationships: CO2 > carboxylic acids > alkanes, but the magnitude of the fractionation among them is higher than predicted isotope equilibrium values. In particular, the isotopic fractionation between CO2 and CH4 remained constant at ∼31‰, indicating a kinetic effect during CO2 reduction processes. No "isotope reversal" of δ13C values for alkanes or carboxylic acids was observed, which indicates a different reaction pathway than what is typically observed during Fischer-Tropsch synthesis under gas phase conditions. Under constraints imposed in experiments, the anomalous 13C isotope enrichment in ethanol suggests that hydroxymethylene is the organic intermediate, and that the generation of other organic compounds enriched in 12C were facilitated by subsequent Rayleigh fractionation of hydroxymethylene reacting with H2 and/or H2O. Carbon isotope fractionation data obtained in this study are instrumental in assessing the controlling factors on abiotic formation of organic compounds in hydrothermal systems. Knowledge on how environmental conditions affect reaction pathways of abiotic synthesis of organic

  1. Rapid hydrothermal flow synthesis and characterisation of carbonate- and silicate-substituted calcium phosphates

    PubMed Central

    Knowles, Jonathan C; Rehman, Ihtesham; Darr, Jawwad A

    2013-01-01

    A range of crystalline and nano-sized carbonate- and silicate-substituted hydroxyapatite has been successfully produced by using continuous hydrothermal flow synthesis technology. Ion-substituted calcium phosphates are better candidates for bone replacement applications (due to improved bioactivity) as compared to phase-pure hydroxyapatite. Urea was used as a carbonate source for synthesising phase pure carbonated hydroxyapatite (CO3-HA) with ≈5 wt% substituted carbonate content (sample 7.5CO3-HA) and it was found that a further increase in urea concentration in solution resulted in biphasic mixtures of carbonate-substituted hydroxyapatite and calcium carbonate. Transmission electron microscopy images revealed that the particle size of hydroxyapatite decreased with increasing urea concentration. Energy-dispersive X-ray spectroscopy result revealed a calcium deficient apatite with Ca:P molar ratio of 1.45 (±0.04) in sample 7.5CO3-HA. For silicate-substituted hydroxyapatite (SiO4-HA) silicon acetate was used as a silicate ion source. It was observed that a substitution threshold of ∼1.1 wt% exists for synthesis of SiO4-HA in the continuous hydrothermal flow synthesis system, which could be due to the decreasing yields with progressive increase in silicon acetate concentration. All the as-precipitated powders (without any additional heat treatments) were analysed using techniques including Transmission electron microscopy, X-ray powder diffraction, Differential scanning calorimetry, Thermogravimetric analysis, Raman spectroscopy and Fourier transform infrared spectroscopy. PMID:22983020

  2. Two chain gallium fluorodiphosphates: synthesis, structure solution, and their transient presence during the hydrothermal crystallisation of a microporous gallium fluorophosphate.

    PubMed

    Millange, Franck; Walton, Richard I; Guillou, Nathalie; Loiseau, Thierry; O'Hare, Dermot; Férey, Gérard

    2002-04-21

    Two novel gallium fluorodiphosphates have been isolated and their structures solved ab initio from powder X-ray diffraction data; the materials readily interconvert under hydrothermal conditions, and are metastable with respect to an open-framework zeolitic gallium fluorophosphate, during the synthesis of which they are present as transient intermediates.

  3. Hydrothermal Synthesis and Processing of Barium Titanate Nanoparticles Embedded in Polymer Films.

    PubMed

    Toomey, Michael D; Gao, Kai; Mendis, Gamini P; Slamovich, Elliott B; Howarter, John A

    2015-12-30

    Barium titanate nanoparticles embedded in flexible polymer films were synthesized using hydrothermal processing methods. The resulting films were characterized with respect to material composition, size distribution of nanoparticles, and spatial location of particles within the polymer film. Synthesis conditions were varied based on the mechanical properties of the polymer films, ratio of polymer to barium titanate precursors, and length of aging time between initial formulations of the solution to final processing of nanoparticles. Block copolymers of poly(styrene-co-maleic anhydride) (SMAh) were used to spatially separate titanium precursors based on specific chemical interactions with the maleic anhydride moiety. However, the glassy nature of this copolymer restricted mobility of the titanium precursors during hydrothermal processing. The addition of rubbery butadiene moieties, through mixing of the SMAh with poly(styrene-butadiene-styrene) (SBS) copolymer, increased the nanoparticle dispersion as a result of greater diffusivity of the titanium precursor via higher mobility of the polymer matrix. Additionally, an aminosilane was used as a means to retard cross-linking in polymer-metalorganic solutions, as the titanium precursor molecules were shown to react and form networks prior to hydrothermal processing. By adding small amounts of competing aminosilane, excessive cross-linking was prevented without significantly impacting the quality and composition of the final barium titanate nanoparticles. X-ray diffraction and X-ray photoelectron spectroscopy were used to verify nanoparticle compositions. Particle sizes within the polymer films were measured to be 108 ± 5 nm, 100 ± 6 nm, and 60 ± 5 nm under different synthetic conditions using electron microscopy. Flexibility of the films was assessed through measurement of the glass transition temperature using dynamic mechanical analysis. Dielectric permittivity was measured using an impedance analyzer.

  4. Hydrothermal synthesis and structural investigation of a new polymorph form of NdBO3

    NASA Astrophysics Data System (ADS)

    Tekin, Berna; Güler, Halil

    2012-09-01

    The present work deals with the hydrothermal synthesis of a new polymorph form of neodymium orthoborate, NdBO3. It was obtained by dissolving 0.1875g B2O3 in 20 ml distilled water and later added to 1.8125 g Nd2O3 and the mixture was transferred to a teflon autoclave. The hydrothermal reaction was performed at 230 °C for 72 h. Characterizations of the sample were carried out by using X-Ray Powder Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR) and Thermal Analysis (DTA/TG) techniques. NdBO3 was crystallized in monoclinic system and unit cell parameters were calculated as a=11.726(1) Å, b= 6.759(2) Å, c= 9.909(4) Å, β= 114.50(0)°, and space group of C2/c. It was confirmed that NdBO3 was isostructural with the form of Er doped YBO3 (a=11.3138(3) Å, b=6.5403(2) Å, c= 9.5499(2) Å and β= 112.902(1)°) at room temperature. The other significant invention of NdBO3 was thermally stable up to 700 °C, but if the specimen was heated at 780 °C for 4 h, the monoclinic crystal structure was transformed to the aragonite form of NdBO3 (ICDD 12-756).

  5. Hydrothermal synthesis of mesoporous metal oxide arrays with enhanced properties for electrochemical energy storage

    SciTech Connect

    Xiao, Anguo Zhou, Shibiao; Zuo, Chenggang; Zhuan, Yongbing; Ding, Xiang

    2015-01-15

    Highlights: • NiO mesoporous nanowall arrays are prepared via hydrothermal method. • Mesoporous nanowall arrays are favorable for fast ion/electron transfer. • NiO mesoporous nanowall arrays show good supercapacitor performance. - Abstract: Mesoporous nanowall NiO arrays are prepared by a facile hydrothermal synthesis method with a following annealing process. The NiO nanowall shows continuous mesopores ranging from 5 to 10 nm and grows vertically on the substrate forming a porous net-like structure with macropores of 20–300 nm. A plausible mechanism is proposed for the growth of mesoporous nanowall NiO arrays. As cathode material of pseudocapacitors, the as-prepared mesoporous nanowall NiO arrays show good pseudocapacitive performances with a high capacitance of 600 F g{sup −1} at 2 A g{sup −1} and impressive high-rate capability with a specific capacitance of 338 F g{sup −1} at 40 A g{sup −1}. In addition, the mesoporous nanowall NiO arrays possess good cycling stability. After 6000 cycles at 2 A g{sup −1}, a high capacitance of 660 F g{sup −1} is attained, and no obvious degradation is observed. The good electrochemical performance is attributed to its highly porous morphology, which provides large reaction surface and short ion diffusion paths, leading to enhanced electrochemical properties.

  6. Direct hydrothermal synthesis of hierarchically porous siliceous zeolite by using alkoxysilylated nonionic surfactant.

    PubMed

    Mukti, Rino R; Hirahara, Hirotomo; Sugawara, Ayae; Shimojima, Atsushi; Okubo, Tatsuya

    2010-02-16

    A hierarchically porous siliceous MFI zeolite (silicalite-1) with narrow mesoporosity has been hydrothermally synthesized by using trialkoxysilylated alkyl poly(oxyethylene ether) as mesopore-directing agent. A mesostructured silica-surfactant composite was formed at the early stage of the reaction, and zeolite crystallization proceeded during subsequent hydrothermal treatment. The scanning electron microscopy (SEM) and transmission electron microscopy (TEM) observations of the crystallized products showed that micro- and mesopores were hierarchically assembled in unique particle morphology with rugged surfaces. Solid-state (29)Si and (13)C NMR revealed that the covalent bonds between the zeolite framework and mesopore-directing agent were present in the products before calcination. The use of nonsilylated alkyl poly(oxyethylene ether) or a silylated alkytrimethyl-ammonium-type cationic surfactant for the synthesis of silicalite-1 resulted in a mixture of mesoporous silica and zeolite as the final product, which suggests that the covalent interaction and nonelectrostatic charge matching interaction favor the formation of hierarchically mesoporous siliceous zeolite. This alkoxysilylated nonionic surfactant can also be extended to synthesize aluminosilicate MFI zeolite (ZSM-5).

  7. Hydrothermal synthesis and luminescence properties of KLa):Eu3+ phosphor

    NASA Astrophysics Data System (ADS)

    Yang, Zaifa; Sun, Yumei; Han, Liu; Xu, Denghui; Sun, Jiayue

    2016-04-01

    KLa):Eu3+ phosphors were prepared by the hydrothermal method. The after tuning of synthesis time and the ratio of the ethylene glycol to water ratio made the phosphor present different morphologies, including peanut-like shape and spheres. The samples were characterized by x-ray diffraction (XRD), scanning electron microscope (SEM), diffuse reflectance spectrum, and fluorescence spectrum. Under the excitation of 397 nm near-ultraviolet, the typical red emission produced by Eu3+ ions can be observed. And the phosphors show strong red light around 612 nm, attributed to D→F transition of Eu ion. The luminescence properties of the as-prepared phosphors were studied based on changing the synthesis condition. It is found that the synthesis time and the changing of the ratio of ethylene glycol to water play the crucial role in the formation of morphology. The optimum dopant concentration of Eu ions in KLa):Eu3+ is around 7 mol. %. Moreover, the fluorescence decay curve and thermal stability of luminescence were also investigated in detail. The Commission International de I'Eclairage coordinates of KLa):0.07Eu3+ located in the red reddish region. All the results suggest that KLa):0.07Eu3+ might be a promising reddish-orange emitting phosphor used in white light-emitting diodes (w-LED).

  8. Hydrothermal synthesis and properties of controlled α-Fe2O3 nanostructures in HEPES solution.

    PubMed

    Li, Hui; Lu, Zhong; Li, Qin; So, Man-Ho; Che, Chi-Ming; Chen, Rong

    2011-09-05

    A facile, template-free, and environmentally friendly hydrothermal strategy was explored for the controllable synthesis of α-Fe(2)O(3) nanostructures in HEPES solution (HEPES=2-[4-(2-hydroxyethyl)-1-piperazinyl]ethanesulfonic acid). The effects of experimental parameters including HEPES/FeCl(3) molar ratio, pH value, reaction temperature, and reaction time on the formation of α-Fe(2)O(3) nanostructures have been investigated systematically. Based on the observations of the products, the function of HEPES in the reaction is discussed. The different α-Fe(2)O(3) nanostructures possess different optical, magnetic properties, and photocatalytic activities, depending on the shape and size of the sample. In addition, a novel and facile approach was developed for the synthesis of Au/α-Fe(2)O(3) and Ag/α-Fe(2)O(3) nanocomposites in HEPES buffer solution; this verified the dual function of HEPES both as reductant and stabilizer. This work provides a new strategy for the controllable synthesis of transition metal oxide nanostructures and metal-supported nanocomposites, and gives a strong evidence of the relationship between the property and morphology/size of nanomaterials.

  9. Quality and high yield synthesis of Ag nanowires by microwave-assisted hydrothermal method.

    PubMed

    Meléndrez, Manuel F; Medina, Carlos; Solis-Pomar, Francisco; Flores, Paulo; Paulraj, Mani; Pérez-Tijerina, Eduardo

    2015-01-01

    Silver nanowires (Ag-NWs) were obtained using microwave-assisted hydrothermal method (MAH). The main advantage of the method is its high NWs production which is greater than 90%. It is also easy, fast, and highly reproducible process. One of the drawbacks presented so far in the synthesis of nanostructures by polyol path is the high temperature used in the process, which is superior than the boiling point of solvent (ethylene glycol), and also its excessive reaction time. Here, Ag-NWs with diameters of 70 to 110 nm were synthesized in 5 min in large quantities. Results showed that dimensions and shape of nanowires were very susceptible to changes with reaction parameters. The reactor power and reactor fill capacity were important for the synthesis. It was found that the reaction time needs to be decreased because of the NWs which start to deform and break up due to significant increase in the pressure's system. Energy-dispersive X-ray spectroscopy and electron diffraction analysis (SAED) did not show corresponding phases of AgO. Some aspects about synthesis parameters which are related to the percent yield and size of nanowires are also discussed.

  10. Hydrothermal Synthesis of Nanoclusters of ZnS Comprised on Nanowires

    PubMed Central

    Ibupoto, Zafar Hussain; Khun, Kimleang; Liu, Xianjie; Willander, Magnus

    2013-01-01

    Cetyltrimethyl ammonium bromide cationic (CTAB) surfactant was used as template for the synthesis of nanoclusters of ZnS composed of nanowires, by hydrothermal method. The structural and morphological studies were performed by using X-ray diffraction (XRD), scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM) techniques. The synthesized ZnS nanoclusters are composed of nanowires and high yield on the substrate was observed. The ZnS nanocrystalline consists of hexagonal phase and polycrystalline in nature. The chemical composition of ZnS nanoclusters composed of nanowires was studied by X-ray photo electron microscopy (XPS). This investigation has shown that the ZnS nanoclusters are composed of Zn and S atoms.

  11. Vaterite-type YBO 3:Eu 3+ crystals: hydrothermal synthesis, morphology and photoluminescence properties

    NASA Astrophysics Data System (ADS)

    Zhang, Jie; Lin, Jun

    2004-10-01

    Vaterite-type YBO 3:Eu 3+ crystals with interesting flower and hedgehog fungus-like structures composed of nanosheets were obtained by controlled crystallization of Y 2O 3 and Eu 2O 3 in H 3BO 3 solutions under acidic hydrothermal (HT) conditions. Nanosheets of uniform thicknesses were formed by preferential crystal growth along the (1 0 0) crystallographic plane and specific three-dimensional structures were further developed through a homocentric growth mechanism. Optical emission measurements showed that the HT-grown nanosheet crystals exhibited a higher ratio of the emitted red-to-orange light ratio than crystals grown from solid-state reactions. The photoluminescence intensity and emission lifetimes were also studied as a function of the Eu 3+ dopant concentration and the HT synthesis temperature. The effect of some additives: a chelating ligand, a surfactant and a polymer, on the YBO 3:Eu 3+ crystals morphology was also investigated.

  12. Synthesis and Electronic Transport of Hydrothermally Synthesized p-Type Na-Doped SnSe

    NASA Astrophysics Data System (ADS)

    Yang, Zong-Ren; Chen, Wei-Hao; Liu, Chia-Jyi

    2016-11-01

    A series of polycrystalline Sn1-x Na x Se with x = 0.00, 0.02, 0.04 and 0.10 were fabricated using hydrothermal synthesis followed by evacuated-and-encapsulated sintering. The as-fabricated materials were characterized using powder x-ray diffraction and electronic transport. The resulting materials were single phase. Partial replacement of Na for Sn leads to a simultaneous increase of electrical conductivity and thermopower. The x = 0.04 sample has the largest power factor among the series of the samples. Upon partial replacement of Na for Sn, the power factor is significantly enhanced as compared to the undoped SnSe. The maximum ZT value of ˜0.4 was achieved for Sn0.96Na0.04Se at 550 K.

  13. Green hydrothermal synthesis and optical properties of γ-Gd2S3 nanoparticles

    NASA Astrophysics Data System (ADS)

    Khajuria, Sonika; Ladol, Jigmet; Sanotra, Sumit; Sheikh, Haq Nawaz

    2016-06-01

    Green synthesis of γ-Gd2S3 nanoparticles was carried out using low-temperature hydrothermal route in autoclave. A 1:1 mixture of ionic liquid 1-ethyl-3-methylimidazolium ethyl sulfate, ([EMIM][EtSO4]), and water was used as a solvent. Synthesized nanoparticles were characterized by x-ray powder diffraction (XRPD), scanning electron microscopy (SEM), UV-visible spectroscopy (UV-vis), particle size by dynamic light scattering (DLS) technique, and photoluminescence (PL) studies. XRPD suggests cubic Th3P4-type structure for obtained Gd2S3 nanoparticles. The size of synthesized nanoparticles is about 86 nm. Optical band gap for these nanoparticles estimated from electronic spectrum is 2.95 eV which shows blue shift from values reported for bulk Gd2S3 due to pronounced quantum mechanical effect. These nanoparticles show sharp emission peak at 385 nm and a broad shoulder at 475 nm when excited at 260 nm.

  14. Synthesis of polyethylenimine (PEI) functionalized silver nanoparticles by a hydrothermal method and their antibacterial activity study.

    PubMed

    Liu, Zhiguo; Wang, Yuanlin; Zu, Yuangang; Fu, Yujie; Li, Na; Guo, Na; Liu, Ruisi; Zhang, Yiming

    2014-09-01

    In this study, we report a facile, one-step hydrothermal method to synthesize PEI-functionalized Ag nanoparticles in which no extra reducing agent is needed and PEI serves as a reducing agent and a stabilizing agent. The obtained Ag colloids have been characterized by TEM, UV absorption spectra and laser particle size analyzer. We found that the size of Ag nanoparticles can be tuned through the alteration of the temperature and growth mode. Under an acidic condition, PEI-functionalized Ag nanoparticles are positively charged. More importantly, the Ag colloids exhibited stronger antibacterial activity in the bactericidal test. Its bactericidal efficiency exceeds the commonly used antibacterial agents such as Erythromycin, chloramphenicol and penicillin as well as AgNO3 solution. These results prove that our synthesis method is very efficient to produce a stable PEI-functionalized Ag colloid with excellent antibacterial activity.

  15. Hydrothermal synthesis of Ni(12)P(5) hollow microspheres, characterization and photocatalytic degradation property.

    PubMed

    Li, Jun; Ni, Yonghong; Liao, Kaiming; Hong, Jianming

    2009-04-01

    In this paper, we report the successful synthesis of Ni(12)P(5) hollow spheres via a facile hydrothermal route, employing white phosphorus (WP) and nickel nitrate as the reactants in the presence of hexamethylenetetramine (HMT) and polyethylene glycol 10000 (PEG-10000). The phase and morphology of the product were characterized by means of powder X-ray diffraction (XRD), energy dispersive spectrometry (EDS), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). HMT and surfactant (PEG-10000) played important roles in the formation of Ni(12)P(5) hollow microspheres. Furthermore, research also showed that the as-prepared Ni(12)P(5) hollow spheres could photocatalytically degrade some organic dyes such as Safranine T and Pyronine B under irradiation of 365 nm UV light.

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

    SciTech Connect

    Edalati, Khatereh; Shakiba, Atefeh; Vahdati-Khaki, Jalil; Zebarjad, Seyed Mojtaba

    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.

  17. Hydrothermal synthesis of hydrocarbons at low temperature. Implications for sustaining a biosphere in Europa

    NASA Astrophysics Data System (ADS)

    Navarro-Gonzalez, Rafael; Montoya, Lilia; Davis, Wanda; McKay, Chris

    Observational evidence from Earth-borne systems and space missions as well as theoretical arguments suggest that Jupiter's satellite Europa could be geologically active today and may possess an ocean of liquid water of about 100 km deep underneath the icy surface about 10 km thickness. The existence of an aqueous ocean is an important requirement for life, as we know it. However, a biosphere also depends of an adequate energy source to drive the most fundamental biological processes such as metabolism, growth, reproduction, etc. Methanogenesis associated with hydrothermal vents may potentially drive a biosphere in an European ocean. We report here on the production of a large variety of hydrocarbons in hydrothermal systems at low temperatures (150° C). The chemical composition of the hydrothermal vent gases was derived from a thermochemical model that assumes that Europa had a cometary (solar, less H) abundance at high temperatures characteristic of a vent. Specifically the following gas mixture was used: 45% CO2 , 45% CH4, and 10 % N2 . A 500 ml stainless steel reactor was filled with 200 ml triply distilled water and the gas mixture at 1 bar at 25° C. In some experiments 3 g of pyrite were added into the reaction vessel. The system was heated for 24 hrs in the temperature range from 100 to 375° C. At the completion of the experiment, the reaction was quenched to 25° C and the gas mixture was analyzed by GC-FTIR-MS techniques. In the absence of pyrite, methane is oxidized to carbon dioxide with the possible production of hydrogen. In contrast in the presence of pyrite, methane is converted into a suite of hydrocarbons from C2 to C7 containing all possible isomers. The production of these compounds was found at temperatures as low as 150° C. In order to get a better understanding of the chemical mechanism involved in the synthesis of hydrocarbons and explore the effect on the initial oxidation state of the carbon used, we performed additional experiments in

  18. Hydrothermal reactions: From the synthesis of ligand to new lanthanide 3D-coordination polymers

    SciTech Connect

    Silva, Fausthon Fred da; Fernandes de Oliveira, Carlos Alberto; Lago Falcão, Eduardo Henrique; Gatto, Claudia Cristina; Bezerra da Costa, Nivan; Oliveira Freire, Ricardo; Chojnacki, Jarosław; Alves Júnior, Severino

    2013-11-15

    The organic ligand 2,5-piperazinedione-1,4-diacetic acid (H{sub 2}PDA) was synthesized under hydrothermal conditions starting from the iminodiacetic acid and catalyzed by oxalic acid. The X-ray powder diffraction data indicates that the compound crystallizes in the P2{sub 1}/c monoclinic system as reported in the literature. The ligand was also characterized by elemental analysis, magnetic nuclear resonance, infrared spectroscopy and thermogravimetric analysis. Two new coordination networks based on lanthanide ions were obtained with this ligand using hydrothermal reaction. In addition to single-crystal X-ray diffraction, the compounds were characterized by infrared spectroscopy, thermogravimetric analysis, scanning electron microscopy and elemental analysis. Single-crystal XRD showed that the compounds are isostructural, crystallizing in P2{sub 1}/n monoclinic system with chemical formula [Ln(PDA){sub 1.5}(H{sub 2}O)](H{sub 2}O){sub 3} (Ln=Gd{sup 3+}(1) and Eu{sup 3+}(2)).The luminescence properties of both compounds were studied. In the compound (1), a broad emission band was observed at 479 nm, redshifted by 70 nm in comparison of the free ligand. In (2), the typical f–f transition was observed with a maximum peak at 618 nm, related with the red emission of the europium ions. Computational methods were performed to simulate the crystal structure of (2). The theoretical calculations of the intensity parameters are in good agreement with the experimental values. - Graphical abstract: Scheme of obtaining the ligand 2,5-piperazinedione-1,4-diacetic acid (H{sub 2}PDA) and two new isostructural 3D-coordination polymers [Ln(PDA){sub 1.5}(H{sub 2}O)](H{sub 2}O){sub 3} (Ln=Gd{sup 3+} and Eu{sup 3+}) by hydrothermal synthesis. Display Omitted - Highlights: • The ligand 2,5-piperazinedione-1,4-diacetic acid was synthetized using the hydrothermic method and characterized. • Two new 3D-coordination polymers with this ligand containing Gd{sup 3+} and Eu{sup 3+} ions

  19. Hierarchically nanostructured hydroxyapatite: hydrothermal synthesis, morphology control, growth mechanism, and biological activity

    PubMed Central

    Ma, Ming-Guo

    2012-01-01

    Hierarchically nanosized hydroxyapatite (HA) with flower-like structure assembled from nanosheets consisting of nanorod building blocks was successfully synthesized by using CaCl2, NaH2PO4, and potassium sodium tartrate via a hydrothermal method at 200°C for 24 hours. The effects of heating time and heating temperature on the products were investigated. As a chelating ligand and template molecule, the potassium sodium tartrate plays a key role in the formation of hierarchically nanostructured HA. On the basis of experimental results, a possible mechanism based on soft-template and self-assembly was proposed for the formation and growth of the hierarchically nanostructured HA. Cytotoxicity experiments indicated that the hierarchically nanostructured HA had good biocompatibility. It was shown by in-vitro experiments that mesenchymal stem cells could attach to the hierarchically nanostructured HA after being cultured for 48 hours. Objective The purpose of this study was to develop facile and effective methods for the synthesis of novel hydroxyapatite (HA) with hierarchical nanostructures assembled from independent and discrete nanobuilding blocks. Methods A simple hydrothermal approach was applied to synthesize HA by using CaCl2, NaH2PO4, and potassium sodium tartrate at 200°C for 24 hours. The cell cytotoxicity of the hierarchically nanostructured HA was tested by MTT (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) assay. Results HA displayed the flower-like structure assembled from nanosheets consisting of nanorod building blocks. The potassium sodium tartrate was used as a chelating ligand, inducing the formation and self-assembly of HA nanorods. The heating time and heating temperature influenced the aggregation and morphology of HA. The cell viability did not decrease with the increasing concentration of hierarchically nanostructured HA added. Conclusion A novel, simple and reliable hydrothermal route had been developed for the synthesis of

  20. Synthesis of copper-core/carbon-sheath nanocables by a surfactant-assisted hydrothermal reduction/carbonization process.

    PubMed

    Deng, Bin; Xu, An-Wu; Chen, Guang-Yi; Song, Rui-Qi; Chen, Liuping

    2006-06-22

    A simple hydrothermal method has been developed for the one-step synthesis of copper-core/carbon-sheath nanocables in solution. The obtained nanostructures were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and high-resolution TEM (HRTEM), Raman, and UV-vis spectrum analysis. These copper@carbon nanocables formed through the hydrothermal reduction/carbonization in the presence of surfactant cetyltrimethylammonium bromide (CTAB) acting as the structure-directing agent by hydrothermal treatment. HRTEM and selected-area electron diffraction (SAED) indicate that the resulted Cu nanowires had the preferred [110] growth direction. The influence of the reaction temperature, reaction time, and pH on the final products was investigated in detail. The possible formation mechanism for copper-core/carbon-sheath nanocables was also proposed. Amorphous carbon nanotubes can be obtained by etching the copper core in the nanocables.

  1. Optimization of hydrothermal synthesis of pure phase zeolite Na-P1 from South African coal fly ashes.

    PubMed

    Musyoka, Nicholas M; Petrik, Leslie F; Gitari, Wilson M; Balfour, Gillian; Hums, Eric

    2012-01-01

    This study was aimed at optimizing the synthesis conditions for pure phase zeolite Na-P1 from three coal fly ashes obtained from power stations in the Mpumalanga province of South Africa. Synthesis variables evaluated were: hydrothermal treatment time (12-48 hours), temperature (100-160°C) and varying molar quantities of water during the hydrothermal treatment step (H(2)O:SiO(2) molar ratio ranged between 0-0.49). The optimum synthesis conditions for preparing pure phase zeolite Na-P1 were achieved when the molar regime was 1 SiO(2): 0.36 Al(2)O(3): 0.59 NaOH: 0.49 H(2)O and ageing was done at 47°C for 48 hours. The optimum hydrothermal treatment time and temperature was 48 hours and 140°C, respectively. Fly ashes sourced from two coal-fired power plants (A, B) were found to produce nearly same high purity zeolite Na-P1 under identical conditions whereas the third fly ash (C) lead to a low quality zeolite Na-P1 under these conditions. The cation exchange capacity for the high pure phase was found to be 4.11 meq/g. These results highlight the fact that adjustment of reactant composition and presynthesis or synthesis parameters, improved quality of zeolite Na-P1 can be achieved and hence an improved potential for application of zeolites prepared from coal fly ash.

  2. Influence of hydrothermal synthesis parameters on the properties of hydroxyapatite nanoparticles

    PubMed Central

    Wojnarowicz, Jacek; Chodara, Agnieszka; Chudoba, Tadeusz; Gierlotka, Stanislaw; Lojkowski, Witold

    2016-01-01

    Hydroxyapatite (HAp) nanoparticles of tunable diameter were obtained by the precipitation method at room temperature and by microwave hydrothermal synthesis (MHS). The following parameters of the obtained nanostructured HAp were determined: pycnometric density, specific surface area, phase purity, lattice parameters, particle size, particle size distribution, water content, and structure. HAp nanoparticle morphology and structure were determined using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). X-ray diffraction measurements confirmed crystalline HAp was synthesized, which was pure in terms of phase. It was shown that by changing the synthesis parameters, the diameter of HAp nanoparticles could be controlled. The average diameter of the HAp nanoparticles was determined by Scherrer’s equation via the Nanopowder XRD Processor Demo web application, which interprets the results of specific surface area and TEM measurements using the dark-field technique. The obtained nanoparticles with average particle diameter ranging from 8–39 nm were characterized by having homogeneous morphology with a needle shape and a narrow particle size distribution. Strong similarities were found when comparing the properties of some types of nanostructured hydroxyapatite with natural occurring apatite found in animal bones and teeth. PMID:28144510

  3. Influence of hydrothermal synthesis parameters on the properties of hydroxyapatite nanoparticles.

    PubMed

    Kuśnieruk, Sylwia; Wojnarowicz, Jacek; Chodara, Agnieszka; Chudoba, Tadeusz; Gierlotka, Stanislaw; Lojkowski, Witold

    2016-01-01

    Hydroxyapatite (HAp) nanoparticles of tunable diameter were obtained by the precipitation method at room temperature and by microwave hydrothermal synthesis (MHS). The following parameters of the obtained nanostructured HAp were determined: pycnometric density, specific surface area, phase purity, lattice parameters, particle size, particle size distribution, water content, and structure. HAp nanoparticle morphology and structure were determined using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). X-ray diffraction measurements confirmed crystalline HAp was synthesized, which was pure in terms of phase. It was shown that by changing the synthesis parameters, the diameter of HAp nanoparticles could be controlled. The average diameter of the HAp nanoparticles was determined by Scherrer's equation via the Nanopowder XRD Processor Demo web application, which interprets the results of specific surface area and TEM measurements using the dark-field technique. The obtained nanoparticles with average particle diameter ranging from 8-39 nm were characterized by having homogeneous morphology with a needle shape and a narrow particle size distribution. Strong similarities were found when comparing the properties of some types of nanostructured hydroxyapatite with natural occurring apatite found in animal bones and teeth.

  4. Hydrothermal Synthesis and Characterization of Ni-Al Montmorillonite-Like Phyllosilicates

    PubMed Central

    Reinholdt, Marc X.; Brendlé, Jocelyne; Tuilier, Marie-Hélène; Kaliaguine, Serge; Ambroise, Emmanuelle

    2013-01-01

    This work describes the first hydrothermal synthesis in fluoride medium of Ni-Al montmorillonite-like phyllosilicates, in which the only metallic elements in the octahedral sheet are Ni and Al. X-ray diffraction , chemical analysis, thermogravimetric and differential thermal analysis, scanning electron microscopy and transmission electron microscopy confirm that the synthesized samples are montmorillonite-like phyllosilicates having the expected chemical composition. The specific surface areas of the samples are relatively large (>100 m2 g−1) compared to naturally occurring montmorillonites. 29Si and 27Al nuclear magnetic resonance (NMR) indicate substitutions of Al for Si in the tetrahedral sheet. 19F NMR and Ni K-edge extended X-ray absorption fine structure (EXAFS) local probes highlight a clustering of the metal elements and of the vacancies in the octahedral sheet of the samples. These Ni-Al phyllosilicates exhibit a higher local order than in previously synthesized Zn-Al phyllosilicates. Unlike natural montmorillonites, where the distribution of transition metal cations ensures a charge equilibrium allowing a stability of the framework, synthetic montmorillonites entail clustering and instability of the lattice when the content of divalent element in the octahedral sheet exceeds ca. 20%. Synthesis of Ni-Al montmorillonite-like phyllosilicates, was successfully achieved for the first time. These new synthetic materials may find potential applications as catalysts or as materials with magnetic, optical or staining properties. PMID:28348321

  5. Synthesis of non-aggregated nicotinic acid coated magnetite nanorods via hydrothermal technique

    NASA Astrophysics Data System (ADS)

    Attallah, Olivia A.; Girgis, E.; Abdel-Mottaleb, Mohamed M. S. A.

    2016-02-01

    Non-aggregated magnetite nanorods with average diameters of 20-30 nm and lengths of up to 350 nm were synthesized via in situ, template free hydrothermal technique. These nanorods capped with different concentrations (1, 1.5, 2 and 2.5 g) of nicotinic acid (vitamin B3); possessed good magnetic properties and easy dispersion in aqueous solutions. Our new synthesis technique maintained the uniform shape of the nanorods even with increasing the coating material concentration. The effect of nicotinic acid on the shape, particle size, chemical structure and magnetic properties of the prepared nanorods was evaluated using different characterization methods. The length of nanorods increased from 270 nm to 350 nm in nicotinic acid coated nanorods. Goethite and magnetite phases with different ratios were the dominant phases in the coated samples while a pure magnetite phase was observed in the uncoated one. Nicotinic acid coated magnetic nanorods showed a significant decrease in saturation magnetization than uncoated samples (55 emu/g) reaching 4 emu/g in 2.5 g nicotinic acid coated sample. The novel synthesis technique proved its potentiality to prepare coated metal oxides with one dimensional nanostructure which can function effectively in different biological applications.

  6. Biomolecule-assisted hydrothermal synthesis of silver bismuth sulfide with nanostructures

    SciTech Connect

    Kaowphong, Sulawan

    2012-05-15

    Silver bismuth sulfide (AgBiS{sub 2}) nanostructures were successfully prepared via a simple biomolecule-assisted hydrothermal synthesis at 200 Degree-Sign C for 12-72 h. Silver nitrate, bismuth nitrate and L-cysteine were used as starting materials. Here, the biomolecule, L-cysteine, was served as the sulfide source and a complexing agent. The products, characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM), were cubic AgBiS{sub 2} nanoparticles with a diameter range of about 20-75 nm. It was found that their crystallinity and particle size increased with increasing reaction time. The energy dispersive X-ray spectroscopy (EDX) and inductively coupled plasma optical emission spectrophotometry (ICP-OES) analyses were used to confirm the stoichiometry of AgBiS{sub 2}. The optical band gap of the AgBiS{sub 2} nanoparticles, calculated from UV-vis spectra, was 3.0 eV which indicated a strong blue shift because of the quantum confinement effect. A possible formation mechanism of the AgBiS{sub 2} nanoparticles was also discussed. - Graphical abstract: The optical band gap of the as-prepared AgBiS{sub 2} nanoparticles displays a strong blue shift comparing to the 2.46 eV of bulk AgBiS{sub 2} caused by the quantum confinement effects. Highlights: Black-Right-Pointing-Pointer A simple biomolecule-assisted hydrothermal method is developed to prepare AgBiS{sub 2}. Black-Right-Pointing-Pointer L-Cysteine is served as the sulfide source and a complexing agent. Black-Right-Pointing-Pointer Increase in band gap of the AgBiS{sub 2} nanoparticles attributes to the quantum confinement effects.

  7. Sodium dodecyl benzene sulfonate-assisted synthesis through a hydrothermal reaction

    SciTech Connect

    Sobhani, Azam; Salavati-Niasari, Masoud

    2012-08-15

    Graphical abstract: Reaction of a SeCl{sub 4} aqueous solution with a NiCl{sub 2}·6H{sub 2}O aqueous solution in presence of sodium dodecyl benzene sulfonate (SDBS) as capping agent and hydrazine (N{sub 2}H{sub 4}·H{sub 2}O) as reductant, produces nanosized nickel selenide through a hydrothermal method. The effect of temperature, reaction time and amounts of reductant on the morphology, particle sizes of NiSe nanostructures has been investigated. Highlights: ► NiSe nanostructures were synthesized by hydrothermal method. ► A novel Se source was used to synthesize NiSe. ► SDBS as capping agent plays a crucial role on the morphology of products. ► A mixture of Ni{sub 3}Se{sub 2} and NiSe was prepared in the presence of 2 ml hydrazine. ► A pure phase of NiSe was prepared in the presence of 4 or 6 ml hydrazine. -- Abstract: The effects of the anionic surfactant on the morphology, size and crystallization of NiSe precipitated from NiCl{sub 2}·6H{sub 2}O and SeCl{sub 4} in presence of hydrazine (N{sub 2}H{sub 4}·H{sub 2}O) as reductant were investigated. The products have been successfully synthesized in presence of sodium dodecyl benzene sulfonate (SDBS) as surfactant via an improved hydrothermal route. A variety of synthesis parameters, such as reaction time and temperature, capping agent and amount of reducing agent have a significant effect on the particle size, phase purity and morphology of the obtained products. The sample size became bigger with decreasing reaction temperature and increasing reaction time. In the presence of 2 ml hydrazine, the samples were found to be the mixture of Ni{sub 3}Se{sub 2} and NiSe. With increasing the reaction time and amount of hydrazine a pure phase of hexagonal NiSe was obtained. X-ray diffraction analysis (XRD), scanning electron microscope (SEM) and transmission electron microscopy (TEM) images indicate phase, particle size and morphology of the products. Chemical composition and purity of the products were

  8. Pathways for synthesis of new selenium-containing oxo-compounds: Chemical vapor transport reactions, hydrothermal techniques and evaporation method

    NASA Astrophysics Data System (ADS)

    Kovrugin, Vadim M.; Colmont, Marie; Siidra, Oleg I.; Gurzhiy, Vladislav V.; Krivovichev, Sergey V.; Mentré, Olivier

    2017-01-01

    Due to the low and close melting and sublimation temperatures (340 and 350 °C, respectively), the crystal growth of selenates and/or selenites is generally achieved using either chemical vapor transport routes, hydrothermal methods due to the good solubility and reactivity of (SeO3)2- anions or isothermal evaporation synthesis. Here we report examples many new crystal structures obtained using these synthesis routes. Particularly, description of each process is given with theoretical and practical information assorted with description of selected structures.

  9. Hydrothermal synthesis and thermal evolution of carbonate-fluorhydroxyapatite scaffold from cuttlefish bones.

    PubMed

    Tkalčec, Emilija; Popović, Jasminka; Orlić, Sebastijan; Milardović, Stjepan; Ivanković, Hrvoje

    2014-09-01

    Phase composition, crystal structure and morphology of carbonated fluor/hydroxyapatite synthesized hydrothermally from aragonitic cuttlefish bones were studied by powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM) combined with energy dispersive X-ray spectroscopy (EDS). The product of synthesis has been characterized as carbonated fluor/hydroxyapatite with carbonate incorporated inside channel (A-type) and substituted for the PO4(3-) group (B-type). The vibration band at 874 cm(-1) assigned to bending (ν2) mode undoubtedly confirmed carbonate substituted for PO4(3-) group, while the band at 880 cm(-1) was attributed to A-type carbonate substitution. The additional sharp and intense band at 865 cm(-1) considered as "non-apatitic" carbonate substitution is not assigned with certainty so far. Evolution of CO2 from tetrahedral (PO4(3-)) sites with the increase in heat-treatment temperature is evident by the changes in tetrahedral bond lengths and angles, as obtained by the Rietveld structure refinement. Also, changes in the isotropic temperature parameters for the 2a site point to A-type carbonate incorporation as well.

  10. High-throughput continuous hydrothermal synthesis of an entire nanoceramic phase diagram.

    PubMed

    Weng, Xiaole; Cockcroft, Jeremy K; Hyett, Geoffrey; Vickers, Martin; Boldrin, Paul; Tang, Chiu C; Thompson, Stephen P; Parker, Julia E; Knowles, Jonathan C; Rehman, Ihtesham; Parkin, Ivan; Evans, Julian R G; Darr, Jawwad A

    2009-01-01

    A novel High-Throughput Continuous Hydrothermal (HiTCH) flow synthesis reactor was used to make directly and rapidly a 66-sample nanoparticle library (entire phase diagram) of nanocrystalline Ce(x)Zr(y)Y(z)O(2-delta) in less than 12 h. High resolution PXRD data were obtained for the entire heat-treated library (at 1000 degrees C/1 h) in less than a day using the new robotic beamline I11, located at Diamond Light Source (DLS). This allowed Rietveld-quality powder X-ray diffraction (PXRD) data collection of the entire 66-sample library in <1 day. Consequently, the authors rapidly mapped out phase behavior and sintering behaviors for the entire library. Out of the entire 66-sample heat-treated library, the PXRD data suggests that 43 possess the fluorite structure, of which 30 (out of 36) are ternary compositions. The speed, quantity and quality of data obtained by our new approach, offers an exciting new development which will allow structure-property relationships to be accessed for nanoceramics in much shorter time periods.

  11. Yttrium-succinates coordination polymers: Hydrothermal synthesis, crystal structure and thermal decomposition

    SciTech Connect

    Amghouz, Zakariae; Roces, Laura; Garcia-Granda, Santiago; Garcia, Jose R.; Souhail, Badredine; Mafra, Luis; Shi, Fa-nian; Rocha, Joao

    2009-12-15

    New polymeric yttrium-succinates, Y{sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}(H{sub 2}O){sub 4}.6H{sub 2}O and Y{sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}(H{sub 2}O){sub 2}, have been synthesized, and their structures (solved by single crystal XRD) are compared with that of Y{sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}(H{sub 2}O){sub 2}.H{sub 2}O. Three compounds were obtained as single phases, and their thermal behaviour is described. - Graphical abstract: In the field of coordination polymers or MOF's, few studies report on the polymorphs of Ln(III)-succinic acid. Here, we describe the hydrothermal synthesis and structural characterization of two novel yttrium-succinates coordination polymers, respectively 2D and 3D, Y{sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}(H{sub 2}O){sub 4}.6H{sub 2}O and Y{sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}(H{sub 2}O){sub 2}.

  12. Hydrothermal synthesis spherical TiO2 and its photo-degradation property on salicylic acid

    NASA Astrophysics Data System (ADS)

    Guo, Wenlu; Liu, Xiaolin; Huo, Pengwei; Gao, Xun; Wu, Di; Lu, Ziyang; Yan, Yongsheng

    2012-07-01

    Anatase TiO2 spheres have been prepared using hydrothermal synthesis. The prepared spheres were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and UV-vis diffuse reflectance spectra (UV-vis DRS). The TiO2 consisted of well-defined spheres with size of 3-5 μm. The photocatalytic activity of spherical TiO2 was determined by degradation of salicylic acid under visible light irradiation. It was revealed that the degradation rate of the spherical TiO2 which was processed at 150 °C for 48 h could reach 81.758%. And the kinetics of photocatalytic degradation obeyed first-order kinetic, which the rate constant value was 0.01716 S-1 of the salicylic acid onto TiO2 (temperature: 150, time: 48 h). The kinetics of adsorption followed the pseudo-second-order model and the rate constant was 1.2695 g mg-1 of the salicylic acid onto TiO2 (temperature: 150, time: 48 h).

  13. Microwave technique applied to the hydrothermal synthesis and sintering of calcia stabilized zirconia nanoparticles

    NASA Astrophysics Data System (ADS)

    Rizzuti, Antonino; Corradi, Anna; Leonelli, Cristina; Rosa, Roberto; Pielaszek, Roman; Lojkowski, Witold

    2010-01-01

    This study is focused on the synthesis of zirconia nanopowders stabilized by 6%mol calcia prepared under hydrothermal conditions using microwave technology. Sodium hydroxide-based hydrolysis of zirconyl chloride solution containing calcium nitrate followed by microwave irradiation at the temperature of 220 °C for 30 min was sufficient to obtain white powders of crystalline calcia stabilized zirconia. By means of X-ray diffraction and transmission electron microscopy, it was shown that tetragonal zirconia nanocrystallites with a size of ca 7 nm and diameter/standard deviation ratio of 0.10 were formed. The effects of the [Ca2+] and [NaOH] as well as temperature and time of microwave irradiation on the density and specific surface area were evaluated. Sintering test of the tetragonal nanopowders at 1,300 °C in air was performed in a monomode microwave applicator. The sample was sintered to the density of 95% and the grain size, analyzed by field emission scanning electron microscopy, was in the range from 90 to 170 nm.

  14. Synthesis of dittmarite/Mg(OH)2 composite coating on AZ31 using hydrothermal treatment

    NASA Astrophysics Data System (ADS)

    Zhao, Qing; Mahmood, Waqas; Zhu, Yanying

    2016-03-01

    In this work, we have used hydrothermal method for the synthesis of dittmarite/Mg(OH)2 composite (DMC) layer on AZ31 alloy of magnesium. The synthesized coating was characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and energy dispersive X-ray spectroscopy (EDS). In a test immersion into the Hank's mixture for 31 days, the synthesized coating inhibited corrosion of AZ31 significantly and the amorphous calcium apatite precursor deposited on the coating surface. In another tape test, we noticed strong adhesion between the coating and substrate that eventually concludes that the synthesized coating is hydrophilic and a promising candidate to be used in the absorbable implant materials. Besides, the cytotoxicity of the AZ31 alloy with DMC coating, grown under different conditions on L-929 cells in vitro was examined indirectly through the growth inhibition method (MTT assay). The cytotoxicity of the deposited coating lie between 0 ∼ 1 that indicates it as a promising biomaterial.

  15. Hydrothermal synthesis of ZTO/graphene nanocomposite with excellent photocatalytic activity under visible light irradiation.

    PubMed

    Ben Ali, Monaam; Yolcu, Haci Hasan; Elhouichet, Habib; Sieber, Brigitte; Addad, Ahmed; Boussekey, Luc; Moreau, Myriam; Férid, Mokhtar; Szunerits, Sabine; Boukherroub, Rabah

    2016-07-01

    A facile and efficient one-step hydrothermal approach for the synthesis of Zn2SnO4 nanoparticles/reduced graphene oxide (ZTO/rGO) nanocomposites using zinc acetate, tin chloride and graphene oxide (GO) as precursors, and sodium hydroxide as reducing agent has been developed. This approach allows simultaneous reduction of GO and growth of spinel ZTO nanoparticles (NPs) on the rGO sheets. The morphology and microstructure characterizations of ZTO/rGO nanocomposites revealed that this method leads to close interfacial contact of ZTO NPs and rGO and efficient dispersion of ZTO NPs on the surface of rGO sheets. The photocatalytic activity of the ZTO/rGO nanocomposite was investigated for the reduction of rhodamine B under visible light irradiation. Compared to pure ZTO NPs, ZTO/rGO nanocomposite exhibited superior photocatalytic activity with a full degradation of rhodamine B within 15min. The enhanced photocatalytic performance of ZTO/rGO was mainly attributed to excellent electron trapping and effective adsorption properties of rGO.

  16. Hydrothermal synthesis of copper coordination polymers based on molybdates: Chemistry issues

    NASA Astrophysics Data System (ADS)

    Pavani, K.; Ramanan, A.; Whittingham, M. S.

    2006-08-01

    Crystal engineering of metal organic coordination polymers or metal organic frameworks have been attracting unprecedented efforts in the past few years due to potential applications in the area of catalysis, gas separation and storage. Hydrothermal synthesis is a popular soft chemical route employed by a number of researchers to grow suitable single crystals for unambiguous structural characterization. The structural diversity of the various solid frameworks is attributed to the choice of metal, its ability to exist in multiple oxidation states exhibiting different coordination geometry and multidentate nature of organic ligands. Polyoxomolybdate is another interesting class of inorganic materials that are potential catalysts. A contemporary theme is to develop porous solids combining the acidic properties of oligomeric molybdates integrated with first-row transition metal ions that can form coordination polymers with suitable multidentate ligands. A bottleneck to this problem is to develop reliable synthetic protocols that can produce reproducible materials with designed structural characteristics. In this paper, we present our results on the formation of self-assembled metal organic hybrid solids from acidified aqueous molybdate solution containing cupric ions and one of the multidentate organic ligands (pyrazine, 2-pyrazine carboxylic acid or isonicotinic acid). We propose a molecular mechanism to rationalize the formation of solids.

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

    NASA Astrophysics Data System (ADS)

    Bhavani, P.; Rajababu, C. H.; Arif, M. D.; Reddy, I. Venkata Subba; Reddy, N. Ramamanohar

    2017-03-01

    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 (MS) of 103.017 emu/g and low remanant magnetization (Mr) of 0.22 emu/g with coercivity (Hc) of 70.9 Oe, which may be attributed to the smaller magnetic domains (dm) and dead magnetic layer thickness (t).

  18. Synthesis and characterization of mesoporous MgO by template-free hydrothermal method

    SciTech Connect

    Cui, Hongmei; Wu, Xiaofeng; Chen, Yunfa; Boughton, R.I.

    2014-02-01

    Highlights: • A simple synthesis of porous MgO with diameter size from 3 to 10 μm without any templates. • Effect of temperature and time were investigated. • Systematic characterization by TG/DTA, XRD, SEM, TEM, and nitrogen adsorption–desorption isotherm of MgO. • A possible formation and crystal growth mechanism of mesopores MgO is proposed. - Abstract: Mesoporous MgO particles have been synthesized through a novel template-free hydrothermal co-precipitation method using a Mg(NO{sub 3}){sub 2} solution as the magnesium source and NaCO{sub 3} as precipitant. The samples were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and N{sub 2} adsorption–desorption analysis. The results indicate that the MgO samples have a disordered mesoporous structure, a large BET surface area, and a large pore volume. The effect of reaction temperature on the MgO product BET surface area was studied. A possible formation and crystal growth mechanism for mesoporous MgO is proposed.

  19. Synthesis and growth of hematite nanodiscs through a facile hydrothermal approach

    NASA Astrophysics Data System (ADS)

    Jiang, X. C.; Yu, A. B.; Yang, W. R.; Ding, Y.; Xu, C. X.; Lam, S.

    2010-03-01

    This study reports a facile hydrothermal method for the synthesis of monodispersed hematite (α-Fe2O3) nanodiscs under mild conditions. The method has features such as no use of surfactants, no toxic precursors, and no requirements of high-temperature decomposition of iron precursors in non-polar solvents. By this method, α-Fe2O3 nanodiscs were achieved with diameter of 50 ± 10 nm and thickness of 6.5 nm by the hydrolysis of ferric chloride. The particle characteristics (e.g., shape, size, and distribution) and functional properties (e.g., magnetic and catalytic properties) were investigated by various advanced techniques, including TEM, AFM, XRD, BET, and SQUID. Such nanodiscs were proved to show unique magnetic properties, i.e., superparamagnetic property at a low temperature (e.g., 20 K) but ferromagnetic property at a room temperature ( 300 K). They also exhibit low-temperature (<623 K) catalytic activity in CO oxidation because of extremely clean surfaces due to non-involvement of surfactants, compared with those spheres and ellipsoids capped by PVP molecules.

  20. Hydrothermal Synthesis and Characterization of a Metal-Organic Framework by Thermogravimetric Analysis, Powder X-Ray Diffraction, and Infrared Spectroscopy: An Integrative Inorganic Chemistry Experiment

    ERIC Educational Resources Information Center

    Crane, Johanna L.; Anderson, Kelly E.; Conway, Samantha G.

    2015-01-01

    This advanced undergraduate laboratory experiment involves the synthesis and characterization of a metal-organic framework with microporous channels that are held intact via hydrogen bonding of the coordinated water molecules. The hydrothermal synthesis of Co[subscript 3](BTC)[subscript 2]·12H[subscript 2]O (BTC = 1,3,5-benzene tricarboxylic acid)…

  1. Flower-like NiO structures: Controlled hydrothermal synthesis and electrochemical characteristic

    SciTech Connect

    Chai, Hui; Chen, Xuan; Jia, Dianzeng; Bao, Shujuan; Zhou, Wanyong

    2012-12-15

    Graphical abstract: Flower-like porous NiO was obtained via thermal decomposition of the precursor prepared by a hydrothermal process using hexamethylenetetramine and polyethylene glycol as hydrolysis-controlling agent and surfactant, respectively. The morphology and microstructure of as-synthesized NiO were characterized by X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results of electrochemical measurements demonstrated that the flower-like porous NiO has high capacity (340 F g{sup −1}) with excellent cycling performance as electrode materials of electrochemical capacitors (ECs), which may be attributed to the unique microstrcture of NiO. Data analyses indicated that NiO with novel porous structure attractive for practical and large-scale applications in electrochemical capacitors. Display Omitted Highlights: ► Synthesis and characterization of NiO with novel porous structure is presented in this work. ► The electrochemical performance of product was examined. ► NiO with excellent performance as electrode materials may be due to the unique microstrcture. ► NiO with novel porous structure attractive for practical with high capacity (340 F g{sup −1}). -- Abstract: Flower-like porous NiO was obtained by thermal decomposition of the precursor prepared by a hydrothermal process with hexamethylenetetramine and polyethylene glycol as hydrolysis-controlling agent and surfactant, respectively. The morphology and microstructure of as-synthesized NiO were characterized by X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The resulting structures of NiO exhibited porous like petal building blocks. The electrochemical measurements’ results demonstrated that flower-like porous NiO has high capacity (340 F g{sup −1}) with excellent cycling performance as electrode materials for

  2. Performances of ZnO-Based Dye Sensitized Solar Cells Fabricated by Hydrothermal Synthesis and Sol-Gel Technique

    NASA Astrophysics Data System (ADS)

    Zhu, Li; Fan, Yu-Qing; Zhao, Mao-Cong; Wu, Min; Zhang, Jia-Yu; Xu, Chun-Xiang; Cui, Yi-Ping

    2009-01-01

    ZnO is introduced as an alternative to TiO2 in dye sensitized solar cells (DSSCs) due to its band gap similar to TiO2, higher electron mobility, and flexible procedures of preparations. Several samples of ZnO films are prepared with the hydrothermal synthesis method and the sol-gel technique, respectively. These ZnO films were assembled as photoanodes in DSSCs using N3 dye as the sensitizer. The ZnO-based cells prepared by the hydrothermal synthesis show typical current source characteristics, whose fill factor (FF) is 0.44 and photo-to-electric power conversion efficiency is 0.34%. On the other hand, all the samples prepared with the sol-gel technique show accompanied source characteristics with relatively higher power conversion efficiencies (1%) but a lower FF (0.26). X-ray diffraction (XRD) and atomic force microscopy (AFM) measurements indicate that the sol-gel samples have small particles sizes. Therefore, sol-gel samples could adsorb more dye molecules to generate high conversion efficiencies. At the same time, more grain boundaries make it more possible for injected electrons to recombine with the oxidized electrolyte. Hydrothermal samples have bigger grains, so they show poor conversion efficiency and relatively high FF.

  3. One-pot hydrothermal synthesis of zeolite/sodium tantalate composite and its photodegradation of methyl orange

    SciTech Connect

    Gu, Xiaoli; Lu, Haiqiang; Kan, Chun; Yao, Jianfeng

    2015-08-15

    Highlights: • Sodalite/NaTaO{sub 3} composite is prepared by a one-pot hydrothermal synthesis. • Enhanced photodegradation is achieved due to the heterogeneous doping effect. • Structure distortion is found for NaTaO{sub 3} after removing sodalite by acid washing. - Abstract: Sodalite/NaTaO{sub 3} composite was prepared by a one-pot hydrothermal synthesis method. Sodalite and NaTaO{sub 3} grow interpenetrated, and the resulting composites have similar morphology as the pure sodalite. The sodalite/NaTaO{sub 3} composite has a lower band gap of 3.35 eV due to the heterogeneous doping effect, and exhibits an enhanced photodegradation of methyl orange under UV irradiation as compared to the pure NaTaO{sub 3}. A slight structure distortion is found for NaTaO{sub 3} after removing sodalite by acid washing the sodalite/NaTaO{sub 3} composite, and such result further confirms the co-growth of the two crystals. This one-pot hydrothermal method opens up new avenues for the preparation of photocatalytic composites.

  4. Hydrothermal synthesis of nanocubes of sillenite type compounds for photovoltaic applications and solar energy conversion of carbon dioxide to fuels

    SciTech Connect

    Subramanian, Vaidyanathan; Murugesan, Sankaran

    2014-04-29

    The present invention relates to formation of nanocubes of sillenite type compounds, such as bismuth titanate, i.e., Bi.sub.12TiO.sub.20, nanocubes, via a hydrothermal synthesis process, with the resulting compound(s) having multifunctional properties such as being useful in solar energy conversion, environmental remediation, and/or energy storage, for example. In one embodiment, a hydrothermal method is disclosed that transforms nanoparticles of TiO.sub.2 to bismuth titanate, i.e., Bi.sub.12TiO.sub.20, nanocubes, optionally loaded with palladium nanoparticles. The method includes reacting titanium dioxide nanotubes with a bismuth salt in an acidic bath at a temperature sufficient and for a time sufficient to form bismuth titanate crystals, which are subsequently annealed to form bismuth titanate nanocubes. After annealing, the bismuth titanate nanocubes may be optionally loaded with nano-sized metal particles, e.g., nanosized palladium particles.

  5. Hydrothermal synthesis of manganese phosphate/graphene foam composite for electrochemical supercapacitor applications.

    PubMed

    Mirghni, Abdulmajid Abdallah; Madito, Moshawe Jack; Masikhwa, Tshifhiwa Moureen; Oyedotun, Kabir O; Bello, Abdulhakeem; Manyala, Ncholu

    2017-05-15

    Manganese phosphate (Mn3(PO4)2 hexagonal micro-rods and (Mn3(PO4)2 with different graphene foam (GF) mass loading up to 150mg were prepared by facile hydrothermal method. The characterization of the as-prepared samples proved the successful synthesis of Mn3(PO4)2 hexagonal micro-rods and Mn3(PO4)2/GF composites. It was observed that the specific capacitance of Mn3(PO4)2/GF composites with different GF mass loading increases with mass loading up to 100mg, and then decreases with increasing mass loading up to 150mg. The specific capacitance of Mn3(PO4)2/100mg GF electrode was calculated to be 270Fg(-1) as compared to 41Fg(-1) of the pristine sample at a current density of 0.5Ag(-1) in a three-electrode cell configuration using 6M KOH. Furthermore, the electrochemical performance of the Mn3(PO4)2/100mg GF electrode was evaluated in a two-electrode asymmetric cell device where Mn3(PO4)2/100mg GF electrode was used as a positive electrode and activated carbon (AC) from coconut shell as a negative electrode. AC//Mn3(PO4)2/100mg GF asymmetric cell device was tested within the potential window of 0.0-1.4V, and showed excellent cycling stability with 96% capacitance retention over 10,000 galvanostatic charge-discharge cycles at a current density of 2Ag(-1).

  6. NiO nanowall array prepared by a hydrothermal synthesis method and its enhanced electrochemical performance for lithium ion batteries

    SciTech Connect

    Cao, F.; Pan, G.X.; Tang, P.S.; Chen, H.F.

    2013-03-15

    Graphical abstract: Self-supported NiO nanowall array is fabricated by a facile hydrothermal synthesis method and exhibits noticeable Li ion battery performance with good cycle life and high capacity. Highlights: ► NiO nanowall array is prepared by a hydrothermal synthesis method. ► NiO nanowall array with high capacity as anode material for Li ion battery. ► Nanowall array structure is favorable for fast ion/electron transfer. - Abstract: Free-standing quasi-single-crystalline NiO nanowall array is successfully fabricated via a simple hydrothermal synthesis method. The as-prepared NiO film exhibits a highly porous nanowall structure composed of many interconnected nanoflakes with thicknesses of ∼20 nm. The NiO nanowalls arrange vertically to the substrate resulting in the formation of extended porous net-like structure with pores of 30–300 nm. As anode material for lithium ion batteries, the quasi-single-crystalline NiO nanowall array exhibits pretty good electrochemical performances with high capacity, weaker polarization, higher coulombic efficiency and better cycling performance as compared to the dense polycrystalline NiO film. The quasi-single-crystalline NiO nanowall array presents an initial coulombic efficiency of 76% and good cycling life with a capacity of 564 mAh g{sup −1} at 0.5 A g{sup −1} after 50 cycles, higher than that of the dense polycrystalline NiO film (358 mAh g{sup −1}). The enhanced performance is due to the unique nanowall array structure providing faster ion/electron transport and better morphological stability.

  7. Hydrothermal synthesis for new multifunctional materials: A few examples of phosphates and phosphonate-based hybrid materials

    NASA Astrophysics Data System (ADS)

    Rueff, Jean-Michel; Poienar, Maria; Guesdon, Anne; Martin, Christine; Maignan, Antoine; Jaffrès, Paul-Alain

    2016-04-01

    Novel physical or chemical properties are expected in a great variety of materials, in connection with the dimensionality of their structures and/or with their nanostructures, hierarchical superstructures etc. In the search of new advanced materials, the hydrothermal technique plays a crucial role, mimicking the nature able to produce fractal, hyperbranched, urchin-like or snow flake structures. In this short review including new results, this will be illustrated by examples selected in two types of materials, phosphates and phosphonates, prepared by this method. The importance of the synthesis parameters will be highlighted for a magnetic iron based phosphates and for hybrids containing phosphonates organic building units crystallizing in different structural types.

  8. High-throughput continuous hydrothermal synthesis of nanomaterials (part II): unveiling the as-prepared CexZryYzO2-δ phase diagram.

    PubMed

    Quesada-Cabrera, Raul; Weng, Xiaole; Hyett, Geoff; Clark, Robin J H; Wang, Xue Z; Darr, Jawwad A

    2013-09-09

    High-throughput continuous hydrothermal flow synthesis was used to manufacture 66 unique nanostructured oxide samples in the Ce-Zr-Y-O system. This synthesis approach resulted in a significant increase in throughput compared to that of conventional batch or continuous hydrothermal synthesis methods. The as-prepared library samples were placed into a wellplate for both automated high-throughput powder X-ray diffraction and Raman spectroscopy data collection, which allowed comprehensive structural characterization and phase mapping. The data suggested that a continuous cubic-like phase field connects all three Ce-Zr-O, Ce-Y-O, and Y-Zr-O binary systems together with a smooth and steady transition between the structures of neighboring compositions. The continuous hydrothermal process led to as-prepared crystallite sizes in the range of 2-7 nm (as determined by using the Scherrer equation).

  9. One-step synthesis of amino-functionalized fluorescent carbon nanoparticles by hydrothermal carbonization of chitosan.

    PubMed

    Yang, Yunhua; Cui, Jianghu; Zheng, Mingtao; Hu, Chaofan; Tan, Shaozao; Xiao, Yong; Yang, Qu; Liu, Yingliang

    2012-01-11

    Highly amino-functionalized fluorescent carbon nanoparticles (CNPs) were fabricated by hydrothermal carbonization of chitosan at a mild temperature. They were applied to bioimaging of human lung adenocarcinoma A549 cells, showing low cytotoxicity and excellent biocompatibility.

  10. Ammonium mediated hydrothermal synthesis of nanostructured hematite (α-Fe{sub 2}O{sub 3}) particles

    SciTech Connect

    Wang, Xiaoge

    2012-09-15

    Highlights: ► Hydrothermal synthesis of nanostructured hematite (α-Fe{sub 2}O{sub 3}) particles. ► NH{sub 4}OH mediated direct transformation of micro-rod hematite to ellipsoidal particles. ► Ellipsoids formed by controlled aggregation, rather than directional growth. -- Abstract: Uniform α-Fe{sub 2}O{sub 3} particles of different shapes have been synthesized through hydrothermal process. The additives, the type of Fe(III) salts and reaction conditions in hydrothermal process were thoroughly investigated. The crystalline structure and morphology of the as-synthesized powder have been characterized by using X-ray powder diffraction, scanning electron microscopy and field emission scanning electron microscopy. Rod and ellipsoidal-shaped α-Fe{sub 2}O{sub 3} were obtained with ferric chloride as a precursor, while only irregular-shaped particles were synthesized by using ferric nitrate as precursors in the absence of NH{sub 4}OH. Direct transformation of micro-rod hematite to ellipsoidal particles with FeCl{sub 3} as precursor was also observed by adding NH{sub 4}OH. It is shown that the nanorod was formed through presumed directional aggregation of rapidly formed nucleus, while the formation of ellipsoidal hematite particles may undergo a nucleation–aggregation–dissolution–recrystallization process in the presence of ammonium.

  11. One-pot hydrothermal synthesis of Nitrogen-doped graphene as high-performance anode materials for lithium ion batteries

    PubMed Central

    Xing, Zheng; Ju, Zhicheng; Zhao, Yulong; Wan, Jialu; Zhu, Yabo; Qiang, Yinghuai; Qian, Yitai

    2016-01-01

    Nitrogen-doped (N-doped) graphene has been prepared by a simple one-step hydrothermal approach using hexamethylenetetramine (HMTA) as single carbon and nitrogen source. In this hydrothermal process, HMTA pyrolyzes at high temperature and the N-doped graphene subsequently self-assembles on the surface of MgO particles (formed by the Mg powder reacting with H2O) during which graphene synthesis and nitrogen doping are simultaneously achieved. The as-synthesized graphene with incorporation of nitrogen groups possesses unique structure including thin layer thickness, high surface area, mesopores and vacancies. These structural features and their synergistic effects could not only improve ions and electrons transportation with nanometer-scale diffusion distances but also promote the penetration of electrolyte. The N-doped graphene exhibits high reversible capacity, superior rate capability as well as long-term cycling stability, which demonstrate that the N-doped graphene with great potential to be an efficient electrode material. The experimental results provide a new hydrothermal route to synthesize N-doped graphene with potential application for advanced energy storage, as well as useful information to design new graphene materials. PMID:27184859

  12. One-step synthesis of high quality kesterite Cu2ZnSnS4 nanocrystals - a hydrothermal approach.

    PubMed

    Tiong, Vincent Tiing; Bell, John; Wang, Hongxia

    2014-01-01

    The present work demonstrates a systematic approach for the synthesis of pure kesterite-phase Cu2ZnSnS4 (CZTS) nanocrystals with a uniform size distribution by a one-step, thioglycolic acid (TGA)-assisted hydrothermal route. The formation mechanism and the role of TGA in the formation of CZTS compound were thoroughly studied. It has been found that TGA interacted with Cu(2+) to form Cu(+) at the initial reaction stage and controlled the crystal-growth of CZTS nanocrystals during the hydrothermal reaction. The consequence of the reduction of Cu(2+) to Cu(+) led to the formation Cu2- x S nuclei, which acted as the crystal framework for the formation of CZTS compound. CZTS was formed by the diffusion of Zn(2+) and Sn(4+) cations to the lattice of Cu2- x S during the hydrothermal reaction. The as-synthesized CZTS nanocrystals exhibited strong light absorption over the range of wavelength beyond 1000 nm. The band gap of the material was determined to be 1.51 eV, which is optimal for application in photoelectric energy conversion device.

  13. One-step synthesis of high quality kesterite Cu2ZnSnS4 nanocrystals – a hydrothermal approach

    PubMed Central

    Tiong, Vincent Tiing; Bell, John

    2014-01-01

    Summary The present work demonstrates a systematic approach for the synthesis of pure kesterite-phase Cu2ZnSnS4 (CZTS) nanocrystals with a uniform size distribution by a one-step, thioglycolic acid (TGA)-assisted hydrothermal route. The formation mechanism and the role of TGA in the formation of CZTS compound were thoroughly studied. It has been found that TGA interacted with Cu2+ to form Cu+ at the initial reaction stage and controlled the crystal-growth of CZTS nanocrystals during the hydrothermal reaction. The consequence of the reduction of Cu2+ to Cu+ led to the formation Cu2− xS nuclei, which acted as the crystal framework for the formation of CZTS compound. CZTS was formed by the diffusion of Zn2+ and Sn4+ cations to the lattice of Cu2− xS during the hydrothermal reaction. The as-synthesized CZTS nanocrystals exhibited strong light absorption over the range of wavelength beyond 1000 nm. The band gap of the material was determined to be 1.51 eV, which is optimal for application in photoelectric energy conversion device. PMID:24778970

  14. One-pot hydrothermal synthesis of Nitrogen-doped graphene as high-performance anode materials for lithium ion batteries

    NASA Astrophysics Data System (ADS)

    Xing, Zheng; Ju, Zhicheng; Zhao, Yulong; Wan, Jialu; Zhu, Yabo; Qiang, Yinghuai; Qian, Yitai

    2016-05-01

    Nitrogen-doped (N-doped) graphene has been prepared by a simple one-step hydrothermal approach using hexamethylenetetramine (HMTA) as single carbon and nitrogen source. In this hydrothermal process, HMTA pyrolyzes at high temperature and the N-doped graphene subsequently self-assembles on the surface of MgO particles (formed by the Mg powder reacting with H2O) during which graphene synthesis and nitrogen doping are simultaneously achieved. The as-synthesized graphene with incorporation of nitrogen groups possesses unique structure including thin layer thickness, high surface area, mesopores and vacancies. These structural features and their synergistic effects could not only improve ions and electrons transportation with nanometer-scale diffusion distances but also promote the penetration of electrolyte. The N-doped graphene exhibits high reversible capacity, superior rate capability as well as long-term cycling stability, which demonstrate that the N-doped graphene with great potential to be an efficient electrode material. The experimental results provide a new hydrothermal route to synthesize N-doped graphene with potential application for advanced energy storage, as well as useful information to design new graphene materials.

  15. SDS-assisted hydrothermal synthesis of porous CdIn2S4 microspheres

    NASA Astrophysics Data System (ADS)

    Bai, X. F.; Li, J. S.; Wu, W.

    2017-02-01

    The porous CdIn2S4 microspheres were synthesized via a sodium dodecyl sulfate (SDS)-assisted hydrothermal technology. The as-prepared CdIn2S4 products were characterized by X-ray diffraction, field emission scanning electron microscopy and UV-Vis diffusive reflectance spectroscopy. The results showed that hydrothermal time and the surfactant addition had great effect on the structure, morphology and optical property of CdIn2S4 products.

  16. Functionalized TiO2 nanoparticles by single-step hydrothermal synthesis: the role of the silane coupling agents

    PubMed Central

    Dalod, Antoine R M; Henriksen, Lars; Grande, Tor

    2017-01-01

    A simple, robust and versatile hydrothermal synthesis route to in situ functionalized TiO2 nanoparticles was developed using titanium(IV) isopropoxide as Ti-precursor and selected silane coupling agents (3-aminopropyltriethoxysilane (APTES), 3-(2-aminoethylamino)propyldimethoxymethylsilane (AEAPS), and n-decyltriethoxysilane (DTES)). Spherical nanoparticles (ca. 9 nm) with narrow size distribution were obtained by using DTES or by synthesis performed without silane coupling agents. Rod-like nanoparticles along with 9 nm spherical nanoparticles were formed using aminosilane coupling agents because of a combination of oriented attachment of nanoparticles and specific adsorption of the aminosilane on crystallographic faces of anatase nanoparticles. The nanoparticles were functionalized in situ and became hydrophobic as silanes reacted to form covalent bonds on the surface of TiO2. The versatility of the aqueous synthesis route was demonstrated, and by selecting the type of silane coupling agent the surface properties of the TiO2 nanoparticles could be tailored. This synthesis route has been further developed into a two-step synthesis to TiO2–SiO2 core–shell nanoparticles. Combustion of the silane coupling agents up to 700 °C leads to the formation of a nanometric amorphous SiO2 layer, preventing growth and phase transition of the in situ functionalized nanoparticles. PMID:28243569

  17. A nontoxic and low-cost hydrothermal route for synthesis of hierarchical Cu2ZnSnS4 particles

    PubMed Central

    2014-01-01

    We explore a facile and nontoxic hydrothermal route for synthesis of a Cu2ZnSnS4 nanocrystalline material by using l-cysteine as the sulfur source and ethylenediaminetetraacetic acid (EDTA) as the complexing agent. The effects of the amount of EDTA, the mole ratio of the three metal ions, and the hydrothermal temperature and time on the phase composition of the obtained product have been systematically investigated. The addition of EDTA and an excessive dose of ZnCl2 in the hydrothermal reaction system favor the generation of kesterite Cu2ZnSnS4. Pure kesterite Cu2ZnSnS4 has been synthesized at 180°C for 12 h from the reaction system containing 2 mmol of EDTA at 2:2:1 of Cu/Zn/Sn. It is confirmed by Raman spectroscopy that those binary and ternary phases are absent in the kesterite Cu2ZnSnS4 product. The kesterite Cu2ZnSnS4 material synthesized by the hydrothermal process consists of flower-like particles with 250 to 400 nm in size. It is revealed that the flower-like particles are assembled from single-crystal Cu2ZnSnS4 nanoflakes with ca. 20 nm in size. The band gap of the Cu2ZnSnS4 nanocrystalline material is estimated to be 1.55 eV. The films fabricated from the hierarchical Cu2ZnSnS4 particles exhibit fast photocurrent responses under intermittent visible-light irradiation, implying that they show potentials for use in solar cells and photocatalysis. PMID:24855463

  18. A nontoxic and low-cost hydrothermal route for synthesis of hierarchical Cu2ZnSnS4 particles.

    PubMed

    Xia, Yu; Chen, Zhihong; Zhang, Zhengguo; Fang, Xiaoming; Liang, Guozheng

    2014-01-01

    We explore a facile and nontoxic hydrothermal route for synthesis of a Cu2ZnSnS4 nanocrystalline material by using l-cysteine as the sulfur source and ethylenediaminetetraacetic acid (EDTA) as the complexing agent. The effects of the amount of EDTA, the mole ratio of the three metal ions, and the hydrothermal temperature and time on the phase composition of the obtained product have been systematically investigated. The addition of EDTA and an excessive dose of ZnCl2 in the hydrothermal reaction system favor the generation of kesterite Cu2ZnSnS4. Pure kesterite Cu2ZnSnS4 has been synthesized at 180°C for 12 h from the reaction system containing 2 mmol of EDTA at 2:2:1 of Cu/Zn/Sn. It is confirmed by Raman spectroscopy that those binary and ternary phases are absent in the kesterite Cu2ZnSnS4 product. The kesterite Cu2ZnSnS4 material synthesized by the hydrothermal process consists of flower-like particles with 250 to 400 nm in size. It is revealed that the flower-like particles are assembled from single-crystal Cu2ZnSnS4 nanoflakes with ca. 20 nm in size. The band gap of the Cu2ZnSnS4 nanocrystalline material is estimated to be 1.55 eV. The films fabricated from the hierarchical Cu2ZnSnS4 particles exhibit fast photocurrent responses under intermittent visible-light irradiation, implying that they show potentials for use in solar cells and photocatalysis.

  19. High-strength nanograined and translucent hydroxyapatite monoliths via continuous hydrothermal synthesis and optimized spark plasma sintering.

    PubMed

    Chaudhry, Aqif A; Yan, Haixue; Gong, Kenan; Inam, Fawad; Viola, Giuseppe; Reece, Mike J; Goodall, Josephine B M; ur Rehman, Ihtesham; McNeil-Watson, Fraser K; Corbett, Jason C W; Knowles, Jonathan C; Darr, Jawwad A

    2011-02-01

    The synthesis of high-strength, completely dense nanograined hydroxyapatite (bioceramic) monoliths is a challenge as high temperatures or long sintering times are often required. In this study, nanorods of hydroxyapatite (HA) and calcium-deficient HA (made using a novel continuous hydrothermal flow synthesis method) were consolidated using spark plasma sintering (SPS) up to full theoretical density in ∼5 min at temperatures up to 1000°C. After significant optimization of the SPS heating and loading cycles, fully dense HA discs were obtained which were translucent, suggesting very high densities. Significantly high three-point flexural strength values for such materials (up to 158 MPa) were measured. Freeze-fracturing of disks followed by scanning electron microscopy investigation revealed selected samples possessed sub-200 nm sized grains and no visible pores, suggesting they were fully dense.

  20. Carbon Isotopes of Alkanes in Hydrothermal Abiotic Organic Synthesis Processes at High Temperatures and Pressures: An Experimental Study

    NASA Technical Reports Server (NTRS)

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

    2010-01-01

    Observation of methane in the Martian atmosphere has been reported by different detection techniques [1-4]. With more evidence showing extensive water-rock interaction in Martian history [5-7], abiotic formation by Fischer-Tropsch Type (FTT) synthesis during serpentization reactions may be one possible process responsible for methane generation on Mars [8, 9]. While the experimental studies performed to date leave little doubt that chemical reactions exist for the abiotic synthesis of organic compounds by mineral surface-catalyzed reactions [10-12], little is known about the reaction pathways by which CO2 and/or CO are reduced under hydrothermal conditions. Carbon and hydrogen isotope measurements of alkanes have been used as an effective tool to constrain the origin and reaction pathways of hydrocarbon formation. Alkanes generated by thermal breakdown of high molecular weight organic compounds have carbon and hydrogen isotopic signatures completely distinct from those formed abiotically [13-15]. Recent experimental studies, however, showed that different abiogenic hydrocarbon formation processes (e.g., polymerization vs. depolymerization) may have different carbon and hydrogen isotopic patterns [16]. Results from previous experiments studying decomposition of higher molecular weight organic compounds (lignite) also suggested that pressure could be a crucial factor affecting fractionation of carbon isotopes [17]. Under high pressure conditions, no experimental data are available describing fractionation of carbon isotope during mineral catalyzed FTT synthesis. Thus, hydrothermal experiments present an excellent opportunity to provide the requisite carbon isotope data. Such data can also be used to identify reaction pathways of abiotic organic synthesis under experimental conditions.

  1. Two new cobalt-zinc orthophosphate monohydrates: hydrothermal synthesis, crystal structures and thermal investigation.

    PubMed

    Sørensen, Morten B; Hazell, Rita G; Bentien, Anders; Bond, Andrew D; Jensen, Torben R

    2005-02-07

    Two new cobalt zinc orthophosphate hydrates with similar chemical formula, (CoxZn(1-x))3(PO4)2.H2O, but different composition and structure, have been prepared by systematic hydrothermal synthesis from the system nCo(CH3COO)2 : (1 -n)Zn(CH(3)COO)2 : 3.5H3PO4 : 2.1(CH3)2NH(CH2)3NH2:144H2O (0

  2. Hydrothermal synthesis of manganese oxides/carbon nanotubes composites as anode materials for lithium ion batteries

    SciTech Connect

    Xu, Shou-Dong; Zhu, Ya-Bo; Zhuang, Quan-Chao; Wu, Chao

    2013-09-01

    Graphical abstract: Carbon nanotubes in the composites not only accommodate the volume change during charge/discharge processes, but also provide a good electron conducting network at high power rates, resulting in high reversible capacity of the electrodes. - Highlights: • MnO/CNTs composites are obtained by heating Mn{sub 3}O{sub 4}/CNTs at 500 °C for 3 h in flowing Ar/H{sub 2}. • MnO/CNTs electrode exhibits higher specific capacity at the current density of 100 mAh g{sup −1} and a better cycle performance. • Enhancement of cyclability of MnO/CNTs electrode can be attributed to the presence of CNTs in the composites. - Abstract: Mn{sub 3}O{sub 4} nanoparticles and Mn{sub 3}O{sub 4}/carbon nanotubes (CNTs) composites are prepared via a hydrothermal synthesis method. MnO and MnO/CNTs composites are obtained by heating Mn{sub 3}O{sub 4} and Mn{sub 3}O{sub 4}/CNTs at 500 for 3 h in flowing Ar/H{sub 2}. The phase structure, composition and morphology of the composites are characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM). The electrochemical properties of the composite electrodes are studied by performing cyclic voltammetry (CV), galvanostatic charge and discharge tests. The results reveal that the Mn{sub 3}O{sub 4}/CNTs and MnO/CNTs electrodes exhibit higher specific capacity at the current density of 100 mAh g{sup −1} and a better cycle performance than pure Mn{sub 3}O{sub 4} and MnO electrodes. The excellent electrochemical properties of Mn{sub 3}O{sub 4}/CNTs and MnO/CNTs electrodes can be attributed to the presence of CNTs in the composites offering an electron conducting network and suppressing the volume expansion of Mn{sub 3}O{sub 4} and MnO particles efficiently during the charge and discharge processes.

  3. Phase stability and rapid consolidation of hydroxyapatite-zirconia nano-coprecipitates made using continuous hydrothermal flow synthesis.

    PubMed

    Chaudhry, Aqif A; Yan, Haixue; Viola, Giuseppe; Reece, Mike J; Knowles, Jonathan C; Gong, Kenan; Rehman, Ihtesham; Darr, Jawwad A

    2012-07-01

    A rapid and continuous hydrothermal route for the synthesis of nano-sized hydroxyapatite rods co-precipitated with calcium-doped zirconia nanoparticles using a superheated water flow at 450°C and 24.1 MPa as a crystallizing medium is described. Hydroxyapatite and calcium-doped zirconia phases in the powder mixtures could be clearly identified based on particle size and morphology under transmission electron microscopy. Retention of a nanostructure after sintering is crucial to load-bearing applications of hydroxyapatite-based ceramics. Therefore, rapid consolidation of the co-precipitates was investigated using a spark plasma sintering furnace under a range of processing conditions. Samples nominally containing 5 and 10 wt% calcium-doped zirconia and hydroxyapatite made with Ca:P solution molar ratio 2.5 showed excellent thermal stability (investigated using in situ variable temperature X-ray diffraction) and were sintered via spark plasma sintering to >96% sintered densities at 1000°C resulting in hydroxyapatite and calcium-doped zirconia as the only two phases. Mechanical tests of spark plasma sintering sintered samples (containing 10 wt% calcium-doped zirconia) revealed a three-pt flexural strength of 107.7 MPa and Weibull modulus of 9.9. The complementary nature of the spark plasma sintering technique and continuous hydrothermal flow synthesis (which results in retention of a nanostructure even after sintering at elevated temperatures) was hence showcased.

  4. Template-directed preparation of two-layer porous NiO film via hydrothermal synthesis for lithium ion batteries

    SciTech Connect

    Chen, Z.; Xiao, A.; Chen, Y.; Zuo, C.; Zhou, S.; Li, L.

    2012-08-15

    Graphical abstract: A two-layer porous NiO film is prepared via hydrothermal synthesis method based on monolayer polystyrene sphere template and shows noticeable Li battery performance with good cycle life and high capacity. Highlights: ► Two-layer porous NiO film is prepared via monolayer polystyrene spheres template. ► NiO film with high capacity as anode material for lithium ion batteries. ► Two-layer porous structure is favorable for fast lithium ion and electron transfer. -- Abstract: A two-layer porous NiO film is prepared by hydrothermal synthesis method through self-assembled monolayer polystyrene spheres template. The substructure of the NiO film is composed of ordered close-packed hollow-sphere array and the superstructure is made up of randomly NiO nanoflakes. The electrochemical properties are measured by galvanostatic charge/discharge tests and cyclic voltammetric analysis (CV). As anode material for lithium ion batteries, the two-layer porous NiO film exhibits high initial coulombic efficiency of 75%, high reversible capacity and rather good cycling performance. The discharge capacity of the two-layer porous NiO film is 501 mAh g{sup −1} at 0.5 C after 50 cycles. The two-layer porous architecture is responsible for the enhancement of electrochemical properties.

  5. Hydrothermal Synthesis of BiFeO3 Nanoparticles for Visible Light Photocatalytic Applications.

    PubMed

    Niu, Feng; Gao, Tong; Zhang, Ning; Chen, Zhi; Huang, Qiaoli; Qin, Laishun; Sun, Xingguo; Huang, Yuexiang

    2015-12-01

    Bismuth ferrite is a promising material for visible light response photocatalytic applications due to its narrow band gap. In this work, single crystalline BiFeO3 nanoparticles were prepared by a modified hydrothermal process. The effects of hydrothermal temperature, reaction time and precursor xerogel amoumt on the as-prepared BiFeO3 particle size and morphology were investigated by XRD, TEM and HRTEM. The XRD analysis reveals that single crystalline BiFeO3 particles can be obtained when the hydrothermal temperature is kept below 220 degrees C. TEM observation showed that the as-formed BFO particles are in a square or rectangle-like shape and that the particle size is increased with increasing hydrothermal temperature. The hydrothermal reaction time and the amount of xerogel could also influence the as-formed BFO particle morphology and size. The band gap of the as-prepared BFO nanoparticles was identified by UV-vis diffuse reflectance spectrum. The measurement of photodegradation of methyl orange dye in an aqueous solution revealed that the as-prepared BFO nanoparticles exhibit photocatalytic activity under visible light irradiation.

  6. Hydrothermal synthesis of assembled sphere-like WO3 architectures and their gas-sensing properties

    NASA Astrophysics Data System (ADS)

    Zhang, Hejing; Liu, Tianmo; Huang, Long; Guo, Weiwei; Liu, Dejun; Zeng, Wen

    2012-04-01

    Unique assembled sphere-like WO3 architectures were successfully synthesized through a facile hydrothermal method in the presence of malic acid followed by subsequent heat treatment. We found that malic acid played a significant role in governing morphologies of WO3·xH2O precursors during hydrothermal process. A possible formation mechanism was also proposed in detail. Experimental results showed that the optimized hydrothermal precursor could be dehydrated to mixed composition of hexagonal and monoclinic WO3 with the unique sphere-like porous architecture after being annealed at 400 °C for 2.5 h. Besides, gas-sensing measurement indicated that the well-defined 3D assembled sphere-like architectures exhibited the highest sensor response to ethanol at the optimal temperature of 250 °C among the samples.

  7. Chelating ligand-mediated hydrothermal synthesis of samarium orthovanadate with decavanadate as vanadium source.

    PubMed

    Li, Quanguo; Zuo, Wenli; Li, Feng

    2013-01-01

    A new ethylenediaminetetraacetic acid- (EDTA-) mediated hydrothermal route to prepare chrysanthemum-shaped samarium orthovanadate (SmVO₄) nanocrystals with decavanadate (K₆V₁₀O₂₈·9H₂O) as vanadium source has been developed. The present hydrothermal approach is simple and reproducible and employs a relatively mild reaction temperature. The EDTA, pH value, and temperature of the reaction systems play important roles in determining the morphologies and growth process of the SmVO₄ products. The products have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), photoluminescence spectra (PL), and UV-Vis spectroscopy.

  8. A hybrid Mg-Al layered double hydroxide/graphene nanostructure obtained via hydrothermal synthesis

    NASA Astrophysics Data System (ADS)

    Zhao, Xiaodong; Cao, Jian-Ping; Zhao, Jun; Hu, Guo-Hua; Dang, Zhi-Min

    2014-06-01

    A hybrid Mg-Al layered double hydroxide/graphene (LDH-GR) material nanostructure has been fabricated by employing the hydrothermal treatment at 140 °C for 10 h. Graphene oxide is simultaneously reduced to graphene during the hydrothermal treatment. The LDH and LDH-GR have high degree of crystallinity and assembled layer structure, which is attributed to electrostatic interaction mechanism. The obtained hybrid nanostructure materials can be used as flame retardant or conductor of electricity and heat due to the combination of different properties arising from graphene and LDH.

  9. Hydrothermal synthesis of sodium tungstate nanorods and nanobundles in the presence of sodium sulfate

    SciTech Connect

    Cao Guangxiang; Song Xinyu; Yu Haiyun; Fan Chunhua; Yin Zhilei; Sun Sixiu . E-mail: ssx@sdu.edu.cn

    2006-02-02

    Sodium tungstate nanorods and nanobundles have been successfully prepared, for the first time, through a simple salt-assisted hydrothermal route based on the reaction between Na{sub 2}WO{sub 4} and HCl in aqueous solution. The resultant sodium tungstate nanorods and nanobundles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and selected area electronic diffraction (SAED) techniques. The ingredients of the sample have been detected by energy-dispersive spectrum (EDS) method. It is found that hydrothermal temperature and time play important roles in the control of the morphology and size of the products.

  10. Bulk Synthesis of Monodisperse Ferrite Nanoparticles at Water-Organic Interfaces under Conventional and Microwave Hydrothermal Treatment and Their Surface Functionalization

    EPA Science Inventory

    Synthesis of monodisperse MFe2O4 (M=, Ni, Co, Mn) and γ-Fe2O3 nanoparticles at a water-toluene interface under conventional as well as microwave hydrothermal conditions using readily available nitrate or chloride salts and oleic acid as the dispersing agent is described. The ens...

  11. Synthesis of ZrO{sub 2} nanoparticles by hydrothermal treatment

    SciTech Connect

    Machmudah, Siti Widiyastuti, W. Prastuti, Okky Putri Nurtono, Tantular Winardi, Sugeng; Wahyudiono,; Kanda, Hideki; Goto, Motonobu

    2014-02-24

    Zirconium oxide (zirconia, ZrO{sub 2}) is the most common material used for electrolyte of solid oxide fuel cells (SOFCs). Zirconia has attracted attention for applications in optical coatings, buffer layers for growing superconductors, thermal-shield, corrosion resistant coatings, ionic conductors, and oxygen sensors, and for potential applications including transparent optical devices and electrochemical capacitor electrodes, fuel cells, catalysts, and advanced ceramics. In this work, zirconia particles were synthesized from ZrCl{sub 4} precursor with hydrothermal treatment in a batch reactor. Hydrothermal treatment may allow obtaining nanoparticles and sintered materials with controlled chemical and structural characteristics. Hydrothermal treatment was carried out at temperatures of 150 – 200°C with precursor concentration of 0.1 – 0.5 M. Zirconia particles obtained from this treatment were analyzed by using SEM, PSD and XRD to characterize the morphology, particle size distribution, and crystallinity, respectively. Based on the analysis, the size of zirconia particles were around 200 nm and it became smaller with decreasing precursor concentration. The increasing temperature caused the particles formed having uniform size. Zirconia particles formed by hydrothermal treatment were monoclinic, tetragonal and cubic crystal.

  12. Surfactant-Assisted Hydrothermal Synthesis of Single Phase Pyrite FeS2 Nanocrystals

    SciTech Connect

    Wadia, Cyrus; Wu, Yue; Gul, Sheraz; Volkman, Steven; Guo, Jinghua; Alivisatos, Paul

    2009-03-27

    Iron pyrite nanocrystals with high purity have been synthesized through a surfactant-assisted hydrothermal reaction under optimum pH value. These pyrite nanocrystals represent a new group of well-defined nanoscale structures for high-performance photovoltaic solar cells based on non-toxic and earth abundant materials.

  13. Hydrothermal synthesis of the first organically templated open-framework uranium phosphate.

    PubMed

    Danis, J A; Runde, W H; Scott, B; Fettinger, J; Eichhorn, B

    2001-11-21

    [(C2H5)2NH2]2[(UO2)5(PO4)4] was prepared from U3O8, HONEt2 and phosphoric acid under hydrothermal conditions (180 degrees C, 5 days) and represents the first three-dimensional open-framework uranium phosphate prepared to date.

  14. Polymer Assisted Core-shell Ag-C nanoparticles Synthesis via Green hydrothermal Technique

    NASA Astrophysics Data System (ADS)

    Williams, James; Mishra, Sanjay

    2009-03-01

    Core-Shell Ag-C nanoparticles were synthesized in the presence of glucose through a one-pot green hydrothermal wet chemical process. An aqueous solution of glucose and Ag nitrate was hydrothermally treated to produce porous carbonaceous shell over silver core nanoparticles. The growth of carbon shells was regulated by either of the polymers (poly) vinyl pyrrolidone (PVP) or poly vinyl alcohol (PVA). The two polymers were compared to take a measure of different tunable sizes of cores, and shells. The effects of hydrothermal temperature, time, and concentration of reagents on the final formation of nanostructures were studied using UV-vis extinction spectra, transmission electron microscope, and Raman spectroscopy. The polymer molecules were found to be incorporated into carbonaceous shell. The resulting opacity of the shell was found to be hydrothermal time and temperature dependent. The shell structure was found to be more uniform with PVP than PVA. Furthermore, the polymer concentration was found to influence size and shape of the core-silver particles as well. The core-shelled nanoparticles have surfaces with organic groups capable of assembling with different reagents that could be useful in drug-delivery, optical nanodevices or biochemistry.

  15. Hydrothermal synthesis of fine stabilized superparamagnetic nanoparticles of Zn2+ substituted manganese ferrite

    NASA Astrophysics Data System (ADS)

    Zahraei, Maryam; Monshi, Ahmad; Morales, Maria del Puerto; Shahbazi-Gahrouei, Daryoush; Amirnasr, Mehdi; Behdadfar, Behshid

    2015-11-01

    Superparamagnetic Zn2+ substituted manganese ferrite Mn1-xZnxFe2O4 (x=0.3, 0.35, 0.4 and 0.45) nanoparticles (NPs) were synthesized via a direct, efficient and environmental friendly hydrothermal method. The synthesized NPs were characterized by X-ray powder diffractometry (XRD), transmission electron microscopy (TEM), thermo-gravimetry (TG) and vibrating sample magnetometry (VSM). The effects of various parameters such as the pH of reaction mixture, time and temperature of hydrothermal treatment and Zn substitution on the spinel phase formation, the magnetization, and the size of resulting NPs are discussed. The Zn2+ substituted manganese ferrite NPs obtained from hydrothermal process crystallized mainly in the spinel phase. Nevertheless, without citrate ions, the hematite phase appeared in the product. The monophase Zn2+ substituted manganese ferrite NPs hydrothermally prepared in the presence of citric acid had mean particle size of 7 nm and a narrow size distribution. Furthermore, the synthesized NPs can be used to prepare ferrofluids for biomedical applications due to their small size, good stability in aqueous medium (pH 7) and also high magnetization value.

  16. Synthesis of magnetic nickel spinel ferrite nanospheres by a reverse emulsion-assisted hydrothermal process

    SciTech Connect

    Zhang Jilin; Shi Jianxin; Gong Menglian

    2009-08-15

    Nickel ferrite nanospheres were successfully synthesized by a reverse emulsion-assisted hydrothermal method. The reverse emulsion was composed of water, cetyltrimethyl ammonium bromide, polyoxyethylene(10)nonyl phenyl ether, iso-amyl alcohol and hexane. During the hydrothermal process, beta-FeO(OH) and Ni{sub 0.75}Fe{sub 0.25}(CO{sub 3}){sub 0.125}(OH){sub 2}.0.38H{sub 2}O (INCHH) nanorods formed first and then transformed into nickel spinel ferrite nanospheres. The phase transformation mechanism is proposed based on the results of X-ray powder diffraction, transmission electron microscopy and energy-dispersive X-ray spectroscopy, etc. Nickel ferrite may form at the end of the INCHH nanorods or from the solution accompanied by the dissolution of beta-FeO(OH) and INCHH nanorods. The X-ray photoelectron spectroscopy analysis shows that a few Fe{sup 3+} ions have been reduced to Fe{sup 2+} ions during the formation of nickel ferrite. The maximum magnetization of the nickel ferrite nanospheres obtained after hydrothermal reaction for 30 h is 55.01 emu/g, which is close to that of bulk NiFe{sub 2}O{sub 4}. - Graphical abstract: Nickel ferrite nanospheres were obtained through a reverse emulsion-assisted hydrothermal process. The phase transformation as a function of reaction time was studied based on the XRD, TEM and EDS analyses.

  17. Synthesis and characterization of porous ZnO nanoparticles by hydrothermal treatment of as pure aqueous precursor

    SciTech Connect

    Sahoo, Trilochan; Kim, Myoung; Baek, Jong Hyeob; Jeon, Seong-Ran; Kim, Jin Soo; Yu, Yeon-Tae; Lee, Cheul-Ro; Lee, In-Hwan

    2011-04-15

    Graphical abstract: ZnO nanocrystals are predominately prepared by soft chemical methods such as sol-gel and hydrothermal. Although hydrothermal approach is very simple, complexing agents or mineralizers such as alkali metal hydroxide are generally used. There is always a high probability that these cations will be incorporated within the nanocrystals. Such unintentional doping is detrimental to the intrinsic property of the material and will impede its effective application. Here we report a very simple and effective hydrothermal approach to synthesize ZnO nanocrystal without employing any mineralizers. Research highlights: The manuscript reports synthesis of ZnO nanoparticle by simple thermal treatment of aqueous precursor without using any assisting mineralizing agent. The highlights of the findings are as follows: {yields} Aqueous synthesis of ZnO nanoparticles is demonstrated without using any mineralizer. {yields} The method minimizes the risk of unintentional doping due to mineralizers. {yields} The synthesized ZnO nanoparticles had a non-uniform mesoporous structure. {yields} The porous ZnO nanoparticls exhibited size dependent optical absorption. -- Abstract: The presence of the complexing agents in the growth solution poses risk of the unintentional doping in the synthesized product and hence is likely to adversely affect the intrinsic properties. Herein we report the synthesis of ZnO nanoparticles with porous microstructure using pure aqueous precursor. Crystalline ZnO nanoparticles were synthesized by thermal treatment of aqueous solution of zinc acetate in an open bath. The size of the nanocrystals was controlled by changing the initial precursor concentration. The structural and optical properties of the synthesized nanocrystals were analyzed by X-ray diffraction, high resolution transmission electron microscopy, UV-vis absorption and room temperature photoluminescence measurement techniques. The TEM and UV-vis spectral signature analyses confirmed

  18. Two-Step Hydrothermal Synthesis of Bifunctional Hematite-Silver Heterodimer Nanoparticles for Potential Antibacterial and Anticancer Applications

    NASA Astrophysics Data System (ADS)

    Trang, Vu Thi; Tam, Le Thi; Phan, Vu Ngoc; Van Quy, Nguyen; Huy, Tran Quang; Le, Anh-Tuan

    2017-01-01

    In recent years, the development of composite nanostructures containing noble metal and magnetic nanocrystals has attracted much interest because they offer a promising avenue for multifunctional applications in nanomedicine and pharmacotherapy. In this work, we present a facile two-step hydrothermal approach for the synthesis of bifunctional heterodimer nanoparticles (HDNPs) composed of hematite nanocubes (α-Fe2O3 NCs) and silver nanoparticles (Ag-NPs). The formation and magnetic property of α-Fe2O3-Ag HDNPs was analyzed by transmission electron microscopy, x-ray diffraction and vibrating sample magnetometer. Interestingly, the hydrothermal-synthesized α-Fe2O3-Ag HDNPs were found to display significant antibacterial activity against three types of infectious bacteria. The cytotoxicity of α-Fe2O3-Ag nanocomposite against lung cancer A549 cell line was investigated and compared with that of pure α-Fe2O3 NCs and Ag-NPs. The obtained results reveal that the α-Fe2O3-Ag nanocomposite exhibited higher anticancer performance than that of pure Ag-NPs, whereas pure α-Fe2O3 NCs were not cytotoxic to the tested cells. The inhibitory concentration (IC50) of the α-Fe2O3-Ag nanocomposite was found at 20.94 μg/mL. With the aforementioned properties, α-Fe2O3-Ag HDNPs showed a high potential as a multifunctional material for advanced biomedicine and nanotherapy applications.

  19. Hydrothermal synthesis of nanostructured manganese oxide as cathodic catalyst in a microbial fuel cell fed with leachate.

    PubMed

    Haoran, Yuan; Lifang, Deng; Tao, Lu; Yong, Chen

    2014-01-01

    Much effort has been devoted to the synthesis of novel nanostructured MnO2 materials because of their unique properties and potential applications as cathode catalyst in Microbial fuel cell. Hybrid MnO2 nanostructures were fabricated by a simple hydrothermal method in this study. Their crystal structures, morphology, and electrochemical characters were carried out by FESEM, N2-adsorption-desorption, and CV, indicating that the hydrothermally synthesized MnO2 (HSM) was structured by nanorods of high aspect ratio and multivalve nanoflowers and more positive than the naturally synthesized MnO2 (NSM), accompanied by a noticeable increase in oxygen reduction peak current. When the HSM was employed as the cathode catalyst in air-cathode MFC which fed with leachate, a maximum power density of 119.07 mW/m(2) was delivered, 64.68% higher than that with the NSM as cathode catalyst. Furthermore, the HSM via a 4-e pathway, but the NSM via a 2-e pathway in alkaline solution, and as 4-e pathway is a more efficient oxygen reduction reaction, the HSM was more positive than NSM. Our study provides useful information on facile preparation of cost-effective cathodic catalyst in air-cathode MFC for wastewater treatment.

  20. Hydrothermal Synthesis of Nanostructured Manganese Oxide as Cathodic Catalyst in a Microbial Fuel Cell Fed with Leachate

    PubMed Central

    Haoran, Yuan; Lifang, Deng; Tao, Lu; Yong, Chen

    2014-01-01

    Much effort has been devoted to the synthesis of novel nanostructured MnO2 materials because of their unique properties and potential applications as cathode catalyst in Microbial fuel cell. Hybrid MnO2 nanostructures were fabricated by a simple hydrothermal method in this study. Their crystal structures, morphology, and electrochemical characters were carried out by FESEM, N2-adsorption-desorption, and CV, indicating that the hydrothermally synthesized MnO2 (HSM) was structured by nanorods of high aspect ratio and multivalve nanoflowers and more positive than the naturally synthesized MnO2 (NSM), accompanied by a noticeable increase in oxygen reduction peak current. When the HSM was employed as the cathode catalyst in air-cathode MFC which fed with leachate, a maximum power density of 119.07 mW/m2 was delivered, 64.68% higher than that with the NSM as cathode catalyst. Furthermore, the HSM via a 4-e pathway, but the NSM via a 2-e pathway in alkaline solution, and as 4-e pathway is a more efficient oxygen reduction reaction, the HSM was more positive than NSM. Our study provides useful information on facile preparation of cost-effective cathodic catalyst in air-cathode MFC for wastewater treatment. PMID:24723824

  1. Selective synthesis of vitamin K3 over mesoporous NbSBA-15 catalysts synthesized by an efficient hydrothermal method.

    PubMed

    Selvaraj, M; Park, D-W; Kim, I; Kawi, S; Ha, C S

    2012-08-28

    Well hexagonally ordered NbSBA-15 catalysts synthesized by an efficient hydrothermal method were used, for the first time, for the selective synthesis of vitamin K(3) by liquid-phase oxidation of 2-methyl-1-naphthol (2MN1-OH) under various reaction conditions. The recyclable NbSBA-15 catalysts were also reused to find their catalytic activities. To investigate the leaching of non-framework niobium species on the surface of silica networks, the results of original and recyclable NbSBA-15 catalysts were correlated and compared. To find an optimum condition for the selective synthesis of vitamin K(3), the washed NbSBA-15(2.2pH) was extensively used in this reaction with various reaction parameters such as temperature, time and ratios of reactant (2M1N-OH to H(2)O(2)), and the obtained results were also demonstrated. Additionally, the liquid-phase oxidation of 2M1N-OH was carried out with different solvents to find the best solvent with a good catalytic activity. Based on the all catalytic studies, the vitamin K(3) selectivity (97.3%) is higher in NbSBA-15(2.2pH) than that of other NbSBA-15 catalysts, and the NbSBA-15(2.2pH) is found to be a highly active and eco-friendly heterogeneous catalyst for the selective synthesis of vitamin K(3).

  2. Hydrothermal synthesis of Mo-doped VO2/TiO2 composite nanocrystals with enhanced thermochromic performance.

    PubMed

    Li, Dengbing; Li, Ming; Pan, Jing; Luo, Yuanyuan; Wu, Hao; Zhang, Yunxia; Li, Guanghai

    2014-05-14

    This paper reports a one-step TiO2 seed-assistant hydrothermal synthesis of Mo-doped VO2(M)/TiO2 composite nanocrystals. It was found that excess Mo doping can promote formation of the VO2(M) phase, and rutile TiO2 seed is beneficial to morphology control, size reduction, and infrared modulation of Mo-doped VO2(M) nanocrystals. The Mo-doped VO2 nanocrystals epitaxially grow on TiO2 seeds and have a quasi-spherical shape with size down to 20 nm and a nearly 35% infrared modulation near room temperature. The findings of this work demonstrate important progress in the near-room-temperature thermochromic performance of VO2(M) nanomaterials, which will find potential application in constructing VO2(M) nanocrystal-based smart window coatings.

  3. Controllable synthesis of CuFe2O4 nanostructures through simple hydrothermal method in the presence of thioglycolic acid

    NASA Astrophysics Data System (ADS)

    Paramasivan, P.; Venkatesh, P.

    2016-10-01

    In this paper a novel and simple route for the preparation of copper ferrite (CuFe2O4) is proposed. The present investigation reports, the novel synthesis of CuFe2O4 samples C1, C2, C3 and C4 using hydrothermal method and its physicochemical characterization. In order to elucidate the relationship between the constituent, structure, magnetic and PL properties product's particle size, morphological and structural properties were characterized by the X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM), photoluminescence (PL) and magnetic properties. The crystallization, surface morphology, magnetic properties and luminescence properties of the samples have been investigated. The relatively high Ms of the samples suggests that this method is suitable for preparing high-quality nanocrystalline copper ferrites for practical applications. Different mechanisms to explain the obtained results and the correlation between magnetism and structure are discussed.

  4. Controllable Synthesis of Single-Crystalline CdO and Cd(OH)2Nanowires by a Simple Hydrothermal Approach

    PubMed Central

    2010-01-01

    Single-crystalline Cd(OH)2 or CdO nanowires can be selectively synthesized at 150 °C by a simple hydrothermal method using aqueous Cd(NO3)2 as precursor. The method is biosafe, and compared to the conventional oil-water surfactant approach, more environmental-benign. As revealed by the XRD results, CdO or Cd(OH)2 nanowires can be generated in high purity by varying the time of synthesis. The results of FESEM and HRTEM analysis show that the CdO nanowires are formed in bundles. Over the CdO-nanowire bundles, photoluminescence at ~517 nm attributable to near band-edge emission of CdO was recorded. Based on the experimental results, a possible growth mechanism of the products is proposed. PMID:20672033

  5. Green synthesis of silver nanoparticles in aloe vera plant extract prepared by a hydrothermal method and their synergistic antibacterial activity

    PubMed Central

    Phromviyo, Nutthakritta; Boueroy, Parichart; Chompoosor, Apiwat

    2016-01-01

    Background There is worldwide interest in silver nanoparticles (AgNPs) synthesized by various chemical reactions for use in applications exploiting their antibacterial activity, even though these processes exhibit a broad range of toxicity in vertebrates and invertebrates alike. To avoid the chemical toxicity, biosynthesis (green synthesis) of metal nanoparticles is proposed as a cost-effective and environmental friendly alternative. Aloe vera leaf extract is a medicinal agent with multiple properties including an antibacterial effect. Moreover the constituents of aloe vera leaves include lignin, hemicellulose, and pectins which can be used in the reduction of silver ions to produce as AgNPs@aloe vera (AgNPs@AV) with antibacterial activity. Methods AgNPs were prepared by an eco-friendly hydrothermal method using an aloe vera plant extract solution as both a reducing and stabilizing agent. AgNPs@AV were characterized using XRD and SEM. Additionally, an agar well diffusion method was used to screen for antimicrobial activity. MIC and MBC were used to correlate the concentration of AgNPs@AV its bactericidal effect. SEM was used to investigate bacterial inactivation. Then the toxicity with human cells was investigated using an MTT assay. Results The synthesized AgNPs were crystalline with sizes of 70.70 ± 22-192.02 ± 53 nm as revealed using XRD and SEM. The sizes of AgNPs can be varied through alteration of times and temperatures used in their synthesis. These AgNPs were investigated for potential use as an antibacterial agent to inhibit pathogenic bacteria. Their antibacterial activity was tested on S. epidermidis and P. aeruginosa. The results showed that AgNPs had a high antibacterial which depended on their synthesis conditions, particularly when processed at 100 oC for 6 h and 200 oC for 12 h. The cytotoxicity of AgNPs was determined using human PBMCs revealing no obvious cytotoxicity. These results indicated that AgNPs@AV can be effectively utilized in

  6. Controllable Low-Temperature Hydrothermal Synthesis and Gas-Sensing Investigation of Crystalline SnO2 Nanoparticles

    NASA Astrophysics Data System (ADS)

    Lu, Ping; Hu, Xiulan; Huang, Huihong; Hu, Ning; Zhang, Jianbo; Shen, Xiaodong

    2016-04-01

    SnO2 nanoparticles have been successfully synthesized by a facile hydrothermal method from SnCl2·2H2O, hexamethylenetetramine, and trisodium citrate in water at 120 °C for 12 h. The effects of surfactant and precipitant on SnO2 synthesis were investigated. SnO2 nanoparticles can be synthesized in the temperature range of 120-180 °C with long reaction time in the presence of trisodium citrate. When NaOH was used as precipitant instead of hexamethylenetetramine, it is difficult to obtain SnO2 nanoparticles at 120 °C in the presence of trisodium citrate. SnO2 nanoparticles with an average size of about 5 nm show good crystallinity and excellent sensitivity to ethanol and acetaldehyde in about 55% relative humidity.

  7. One step microwaved-assisted hydrothermal synthesis of nitrogen doped graphene for high performance of supercapacitor

    NASA Astrophysics Data System (ADS)

    Sari, Fitri Nur Indah; Ting, Jyh-Ming

    2015-11-01

    Nitrogen doped graphene (NDG) has been synthesized using a microwave-assisted hydrothermal (MHT) method within only several minute. In the method, homemade graphene oxide was reduced using ethylene glycol (EG) to obtain the graphene while ammonia liquid was used as the nitrogen source. However, it was found that the reduction and doping simultaneously occurred and the addition of ammonia further enhanced the reduction. The reduction and doping were examined through various analysis and the mechanisms were proposed. The effects of the hydrothermal temperature and time on the reduction and doping were discussed. It was also shown that the doping leads to enhanced specific capacitance by as much as 54%, a high specific energy density of 42.8 W h kg-1 at a power density of 4330 W kg-1, and excellent long term stability up to 98% retention after 1000 cycles at wide working voltage of 1.6 V in 2 M H2SO4.

  8. One-step synthesis of novel biacidic carbon via hydrothermal carbonization

    SciTech Connect

    Xiao Huiquan; Guo Yingxue; Liang Xuezheng; Qi Chenze

    2010-07-15

    The novel biacidic carbon has been synthesized via one-step hydrothermal carbonization of glucose, citric acid, and hydroxyethylsulfonic acid at 180 {sup o}C for only 4 h. The novel carbon had an acidity of 1.7 mmol/g with the carbonyl to sulfonic acid groups molar ratio of 1:3, which was confirmed by IR, XPS, TPD, SEM, and BET analyses. The catalytic activities of the carbon were investigated through esterification and oxathioketalization. The results showed that the carbon owned the comparable activities to sulfuric acid, which indicated that the carbon holds great potential for the green processes. - Graphical abstract: The novel biacidic carbon has been synthesized via one-step hydrothermal carbonization. Both the sulfonic and carbonyl acid groups were introduced to the carbon during the carbonization processes.

  9. Hydrothermal synthesis of SrCO 3:Eu 3+/Tb 3+ microneedles and their luminescence properties

    NASA Astrophysics Data System (ADS)

    Yang, Jun; Liu, Xiaoming; Li, Chunxia; Quan, Zewei; Kong, Deyan; Lin, Jun

    2007-05-01

    SrCO 3:Eu 3+/Tb 3+ microneedles that grow along the a-axis were successfully prepared through a large-scale and facile hydrothermal method without any template and further annealing treatment. X-ray diffraction (XRD), scanning electron microscopy (SEM), and photoluminescence (PL) spectra as well kinetic decays, were used to characterize the samples. The preferential growth along a-axis for SrCO 3:Eu 3+/Tb 3+ microneedles has been proposed through analysis of the XRD patterns of samples obtained at different hydrothermal treatment time. Under ultraviolet excitation, the SrCO 3:Eu 3+ and SrCO 3:Tb 3+ microneedle samples show a strong red and green emission corresponding to the 5D 0- 7F J ( J=1, 2, 3, 4) transitions of Eu 3+ and the 5D 4- 7F J ( J=6, 5, 4, 3) transitions of Tb 3+, respectively, which have potential applications in lighting fields.

  10. Hydrothermal synthesis and electrochemical performance of NiO microspheres with different nanoscale building blocks

    SciTech Connect

    Wang Ling; Hao Yanjing; Zhao Yan; Lai Qiongyu; Xu Xiaoyun

    2010-11-15

    NiO microspheres were successfully obtained by calcining the Ni(OH){sub 2} precursor, which were synthesized via the hydrothermal reaction of nickel chloride, glucose and ammonia. The products were characterized by TGA, XRD and SEM. The influences of glucose and reaction temperature on the morphologies of NiO samples were investigated. Moreover, the possible growth mechanism for the spherical morphology was proposed. The charge/discharge test showed that the as-prepared NiO microspheres composed of nanoparticles can serve as an ideal electrode material for supercapacitor due to the spherical hollow structure. -- Graphical Abstract: Fig. 5 is the SEM image of NiO that was prepared in the different hydrothermal reaction temperatures. It showed that reaction temperature played a crucial role for the morphology of products.

  11. Hydrothermal Synthesis of Lanthanide Stannates Pyrochlore Nanocrystals for Catalytic Combustion of Soot Particulates

    PubMed Central

    2015-01-01

    Nanocrystalline La2Sn2O7 and La2Sn1.8Co0.2O7 with a phase-pure pyrochlore structure were synthesized by a hydrothermal method, and their catalytic activity was investigated for soot combustion. The as-synthesized catalysts presented relatively larger surface area, and pore volume, which was benefit to the gas molecule diffusion in the reaction. A uniform spherical structure with particle size of 200–500 nm was found in SEM. The samples via hydrothermal route are more active for catalytic soot combustion, ascribing to the spherical morphology, high surface area and improved oxygen mobility. After Co, the reducibility was improved and surface oxygen vacancy was produced, resulting in the enhanced activity and selectivity to CO2 formation. PMID:26090513

  12. Interfacial hydrothermal synthesis of SnO{sub 2} nanorods towards photocatalytic degradation of methyl orange

    SciTech Connect

    Hou, L.R. Lian, L.; Zhou, L.; Zhang, L.H.; Yuan, C.Z.

    2014-12-15

    Highlights: • Efficient interfacial hydrothermal strategy was developed. • 1D SnO{sub 2} nanorods as an advanced photocatalyst. • SnO{sub 2} nanorods exhibit photocatalytic degradation of the MO. - Abstract: One-dimensional (1D) SnO{sub 2} nanorods (NRs) have been successfully synthesized by means of an efficient interfacial hydrothermal strategy. The resulting product was physically characterized by X-ray powder diffraction, scanning electron microscopy, transmission electron microscope, etc. The as-fabricated SnO{sub 2} NRs exhibited excellent photocatalytic degradation of the methyl orange with high degradation efficiency of 99.3% with only 60 min ultra violet light irradiation. Meanwhile, the 1D SnO{sub 2} NRs exhibited intriguing photostability after four recycles.

  13. Selected-control synthesis of dysprosium hydroxide and oxide nanorods by adjusting hydrothermal temperature

    SciTech Connect

    Song Xuchun Zheng Yifan; Wang Yun

    2008-05-06

    Dysprosium hydroxide and oxide nanorods were prepared directly from commercial bulk Dy{sub 2}O{sub 3} crystals by facile hydrothermal process at 130 and 210 deg. C, respectively. The as-synthesized dysprosium hydroxide and oxide nanorods were investigated by various techniques of XRD, TEM, SEM, and EDS. In the process, the temperature was found to play important roles in determining produce dysprosium hydroxide and oxide nanorods.

  14. Facile synthesis of air-stable Prussian white microcubes via a hydrothermal method

    SciTech Connect

    Hu, M.; Jiang, J.S.

    2011-05-15

    Research highlights: {yields} We have synthesized Prussian white microcubes in large quantities by a facile hydrothermal method for the first time. {yields} It is the first report about air-stable PW. {yields} The shape of crystals strongly depended on the concentration of K{sub 4}[Fe(CN){sub 6}], the hydrothermal temperature and the reaction duration. {yields} A layer-by-layer growth mechanism was proposed to explain the formation of PW microcubes. -- Abstract: Air-stable Prussian white (PW) microcubes were fabricated by the slow dissociation of K{sub 4}[Fe(CN){sub 6}] under hydrothermal condition without the protection of inert atmosphere. Moessbauer spectra and Fourier transform infrared (FT-IR) spectrum were used to characterize the composition of PW. X-ray diffraction (XRD) identified the obtained PW was monoclinic, and the purity was high. Scanning electron microscopy (SEM) images indicated the cubes were composed by solid cubes and hollow cubes. The shape of crystals strongly depended on the concentration of K{sub 4}[Fe(CN){sub 6}], the hydrothermal temperature as well as the reaction duration. The lower concentration and lower temperature resulted in perfect cubic crystals, while the higher concentration or the higher temperature resulted in irregular cubic crystals. After exposing in air for 2 months, no oxidation of PW occurred. To explain the formation of the PW microcubes, a layer-by-layer growth mechanism was put forward based on the low dissociation rate of K{sub 4}[Fe(CN){sub 6}]. The partially solubility of PW in water caused the formation of hollow cubes.

  15. Synthesis of Silver-Strontium Titanate Hybrid Nanoparticles by Sol-Gel-Hydrothermal Method

    PubMed Central

    Ueno, Shintaro; Nakashima, Kouichi; Sakamoto, Yasunao; Wada, Satoshi

    2015-01-01

    Silver (Ag) nanoparticle-loaded strontium titanate (SrTiO3) nanoparticles were attempted to be synthesized by a sol-gel-hydrothermal method. We prepared the titanium oxide precursor gels incorporated with Ag+ and Sr2+ ions with various molar ratios, and they were successfully converted into the Ag-SrTiO3 hybrid nanoparticles by the hydrothermal treatment at 230 °C in strontium hydroxide aqueous solutions. The morphology of the SrTiO3 nanoparticles is dendritic in the presence and absence of Ag+ ions. The precursor gels, which act as the high reactive precursor, give rise to high nucleation and growth rates under the hydrothermal conditions, and the resultant diffusion-limited aggregation phenomena facilitate the dendritic growth of SrTiO3. From the field-emission transmission electron microscope observation of these Ag-SrTiO3 hybrid nanoparticles, the Ag nanoparticles with a size of a few tens of nanometers are distributed without severe agglomeration, owing to the competitive formation reactions of Ag and SrTiO3.

  16. An Anion-Induced Hydrothermal Oriented-Explosive Strategy for the Synthesis of Porous Upconversion Nanocrystals

    PubMed Central

    Qiu, Peiyu; Sun, Rongjin; Gao, Guo; Zhang, Chunlei; Chen, Bin; Yan, Naishun; Yin, Ting; Liu, Yanlei; Zhang, Jingjing; Yang, Yao; Cui, Daxiang

    2015-01-01

    Rare-earth (RE)-doped upconversion nanocrystals (UCNCs) are deemed as the promising candidates of luminescent nanoprobe for biological imaging and labeling. A number of methods have been used for the fabrication of UCNCs, but their assembly into porous architectures with desired size, shape and crystallographic phase remains a long-term challenging task. Here we report a facile, anion-induced hydrothermal oriented-explosive method to simultaneously control size, shape and phase of porous UCNCs. Our results confirmed the anion-induced hydrothermal oriented-explosion porous structure, size and phase transition for the cubic/hexagonal phase of NaLuF4 and NaGdF4 nanocrystals with various sizes and shapes. This general method is very important not only for successfully preparing lanthanide doped porous UCNCs, but also for clarifying the formation process of porous UCNCs in the hydrothermal system. The synthesized UCNCs were used for in vitro and in vivo CT imaging, and could be acted as the potential CT contrast agents. PMID:25767613

  17. Synthesis and electrochemical performance of Ti3C2Tx with hydrothermal process

    NASA Astrophysics Data System (ADS)

    Wang, Libo; Zhang, Heng; Wang, Bo; Shen, Changjie; Zhang, Chuanxiang; Hu, Qianku; Zhou, Aiguo; Liu, Baozhong

    2016-09-01

    In this study, a simple hydrothermal method has been developed to prepare Ti3C2Tx from Ti3AlC2 as a high-performance electrode material for supercapacitors. This method is environmentally friendly and has a low level of danger. The morphology and structure of the Ti3C2Tx can be controlled by hydrothermal reaction time, temperature and NH4F amounts. The prepared Ti3C2Tx was characterized by X-ray diffraction, field emission scanning electron microscopy, Raman spectroscopy, X-ray photoelectron spectroscopy and Brunauer-Emmet-Teller. The results show that the prepared Ti3C2Tx is terminated by O, OH, and F groups. The electrochemical properties of the Ti3C2Tx sample exhibit specific capacitance up to 141 Fcm-3 in 3 M KOH aqueous electrolyte, and even after 1000 cycles, no significant degradation of the volumetric capacitance was observed. These results indicate that the Ti3C2Tx material prepared by this hydrothermal method can be used in high performance supercapacitors.

  18. Hydrothermal synthesis of nanostructured SnO particles through crystal growth in the presence of gelatin

    SciTech Connect

    Uchiyama, Hiroaki Nakanishi, Shunsuke; Kozuka, Hiromitsu

    2014-09-15

    Crystalline SnO particles were obtained from Sn{sub 6}O{sub 4}(OH){sub 4} by the hydrothermal treatment in aqueous solutions containing gelatin at 150 °C for 24 h, where the morphologies of the SnO products changed from blocks to layered disks, stacked plates and unshaped aggregates with increasing amount of gelatin in the solutions. Such morphological changes of SnO particles were thought to be attributed to the suppression of the growth of SnO crystals by the adsorbed gelatin. - Graphical abstract: Nanostructured SnO particles were obtained from Sn{sub 6}O{sub 4}(OH){sub 4} by the hydrothermal treatment in gelatin solutions. - Highlights: • SnO particles were prepared from Sn{sub 6}O{sub 4}(OH){sub 4} by the hydrothermal treatment. • The adsorption of gelatin suppressed the growth of SnO crystals. • The shape of SnO particles depends on the amount of gelatin. • Blocks, disks, stacked plates and unshaped aggregates were obtained.

  19. Conventional hydrothermal synthesis of Na-A zeolite from cupola slag and aluminum sludge.

    PubMed

    Anuwattana, Rewadee; Khummongkol, Pojanie

    2009-07-15

    Na-A type zeolites were prepared from two industrial wastes: the solid by-product of cupola slag and aluminum sludge from an aluminum plating plant. Two preparation methods using the same starting material compositions were carried out. In the first method, alkaline fusion was introduced, followed by the hydrothermal treatment to obtain sodium aluminosilicate which was then crystallized in NaOH solution under the condition of 90+/-3 degrees C for 1-9h with different H(2)O/SiO2 ratios. The result shows that higher H(2)O/SiO2 ratio increases the rate of crystallization. The largest amount of crystallinity for Na-A was found at 3h. In the second method, alkaline hydrothermal treatment without fusion was carried out in the same condition as the first method. No Na-A zeolite was obtained by this method. The changes of the dissolved amounts of Si(4+) and Al(3+) in 3M NaOH were investigated during the hydrothermal reaction.

  20. Optimization of reaction parameters in hydrothermal synthesis: a strategy towards the formation of CuS hexagonal plates

    PubMed Central

    2013-01-01

    Background For decades, copper sulphide has been renowned as the superior optical and semiconductor materials. Its potential applications can be ranged from solar cells, lithium-ion batteries, sensors, and catalyst systems. The synthesis methodologies of copper sulphide with different controlled morphology have been widely explored in the literature. Nevertheless, the understanding on the formation chemistry of CuS is still limited. The ultimate approach undertaking in this article is to investigate the formation of CuS hexagonal plates via the optimization of reaction parameters in hydrothermal reaction between copper (II) nitrate and sodium thiosulphate without appending any assistant agent. Results Covellite (CuS) hexagonal plates were formed at copper ion: thiosulphate ion (Cu2+:S2O32−) mole ratio of 1:2 under hydrothermal treatment of 155°C for 12 hours. For synthesis conducted at reaction temperature lower than 155°C, copper sulphate (CuSO4), krohnite (NaCu2(SO4)(H2O)2] and cyclooctasulphur (S8) were present as main impurities with covellite (CuS). When Cu2+:S2O32− mole ratio was varied to 1: 1 and 1: 1.5, phase pure plate-like natrochalcite [NaCu2(SO4)(H2O)] and digenite (Cu9S5) were produced respectively. Meanwhile, mixed phases of covellite (CuS) and cyclooctasulphur (S8) were both identified when Cu2+:S2O32− mole ratio was varied to 1: 2.5, 1: 3 and 1: 5 as well as when reaction time was shortened to 1 hour. Conclusions CuS hexagonal plates with a mean edge length of 1 μm, thickness of 100 nm and average crystallite size of approximately (45 ± 2) nm (Scherrer estimation) were successfully synthesized via assisting agent- free hydrothermal method. Under a suitable Cu2+:S2O32− mole ratio, we evidenced that the formation of covellite (CuS) is feasible regardless of the reaction temperature applied. However, a series of impurities were attested with CuS if reaction temperature was not elevated high enough for the additional crystallite

  1. 1-Dodecane-sulfonic-acid-sodium-salt(LAS) assisted hydrothermal synthesis of CdxZn1-xS solid solution as efficient photocatalysts under visible light irradiation

    NASA Astrophysics Data System (ADS)

    Jia, B.; Guo, L. J.

    2010-03-01

    With anionic surfactant LAS assisted, series of zinc cadmium sulfide semiconductor photocatalysts were synthesized by hydrothermal method. These products were characterized by X-ray diffraction (XRD), UV-Vis absorption spectra (UV-Vis) and scanning electron microscopy (FESEM). The photocatalytic activities of as-prepared samples were evaluated by photocatalytic hydrogen production from water under visible-light irradiation. The best synthesis parameters are: Composition 0.9:0.1 (Cd:Zn molar ratio), Temperature 160 °C, Hydrothermal Time 48 Hour, LAS Concentration 1.7 mmol/L, the maximum visible-light-catalytic hydrogen production rate is 161.25 μmol/h (λ>430 nm) which is higher than those of by coprecipitation method. The experiment results indicate that surfactant assisted hydrothermal method is an effective way to get highly active CdZnS solid solution photocatalyst.

  2. Synthesis of Bi2WO6/Bi2O3 composite with enhanced photocatalytic activity by a facile one-step hydrothermal synthesis route.

    PubMed

    Wang, Tianye; Zhang, Fengjun; Xiao, Guosheng; Zhong, Shuang; Lu, Cong

    2015-01-01

    In this study, the characterization and photocatalytic activity of Bi2WO6/Bi2O3 under visible-light irradiation was investigated in detail. The results suggested that Bi2WO6/Bi2O3 can be synthesized by a facile one-pot hydrothermal route using a super big 200 mL Teflon-lined autoclave with optimal sodium oleate/Bi molar ratio of 1.25. Through the characterization of Bi2WO6/Bi2O3 by X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy, Fourier transform infrared, UV-vis diffuse reflectance spectra and Photoluminescence spectra, it was found that the as-prepared composite possessed smaller crystallite size and higher visible-light responsive than the pure Bi2WO6. Moreover, it was expected that the as-prepared composites exhibited enhanced photocatalytic activity for the degradation of Rhodamine B under visible-light irradiation, which could be ascribed to their improved light absorption property and the reduced recombination of the photogenerated electrons and holes during the photocatalytic reaction. In general, this study could provide a principle method to synthesize Bi2WO6/Bi2O3 with enhanced photocatalytic activity by one-step hydrothermal synthesis route for environmental purification.

  3. Microwave Hydrothermal Synthesis of Terbium Ions Complexed with Porous Graphene for Effective Absorbent for Organic Dye

    NASA Astrophysics Data System (ADS)

    Chen, Keqin; Gao, Hui; Bai, Bowei; Liu, Wenjing; Li, Xiaolong

    2017-03-01

    A luminescent terbium ions/reduced graphene oxide complex (Tb-RGO) was successfully and rapidly synthesized by the microwave hydrothermal reaction via the interactions between terbium ions and the active oxygen functional groups of graphene oxide. The as-prepared material was porous stacked by multilayer graphene in all directions. Thus, the resulting product owed the high specific surface area, high adsorption capacity and ultra-fast adsorption rate. Combined with the characteristic photoluminescence derived from terbium ions, the material has potential applications in biosensing and environmental protection.

  4. Hydrothermal synthesis of micrometer sized HgMoO4 flowers formed by nanorods

    NASA Astrophysics Data System (ADS)

    Jia, Run-Ping; Zhang, Ying-Qiang

    2010-10-01

    Micrometer sized HgMoO4 flowers formed by nanorods were prepared by a selected hydrothermal method using a mixture of ethanol and water as a reaction medium, which were characterized by scanning electron microscopy, X-ray diffractometer (XRD), FT-IR spectrometry, photoluminescence spectrometry, and UV-visible spectrometry. Results indicated that the micrometer sized flowers consisted of mercury molybdate nanorods, and the monoclinic wolframite-type structure of the flowers was confirmed by both XRD and FT-IR spectrometry. A blue shift of the photoluminescence peaks and a broadening of XRD peaks were observed, which increased with ethanol fraction in the reaction medium.

  5. Hydrothermal Synthesis and Biocompatibility Study of Highly Crystalline Carbonated Hydroxyapatite Nanorods

    NASA Astrophysics Data System (ADS)

    Xue, Caibao; Chen, Yingzhi; Huang, Yongzhuo; Zhu, Peizhi

    2015-08-01

    Highly crystalline carbonated hydroxyapatite (CHA) nanorods with different carbonate contents were synthesized by a novel hydrothermal method. The crystallinity and chemical structure of synthesized nanorods were studied by Fourier transform infrared spectroscopy (FTIR), X-ray photo-electronic spectroscopy (XPS), X-ray diffraction (XRD), Raman spectroscopy, and transmission electron microscopy (TEM). The biocompatibility of synthesized CHA nanorods was evaluated by cell viability and alkaline phosphatase (ALP) activity of MG-63 cell line. The biocompatibility evaluation results show that these CHA nanorods are biologically active apatites and potentially promising bone-substitute biomaterials for orthopedic application.

  6. Hydrothermal synthesis and magnetic properties of ErCrO{sub 4} nanoparticles

    SciTech Connect

    Sundarayya, Y. Kumar, K. Ashwini Sondge, Rajesh Srinath, S. Kaul, S. N.

    2014-04-24

    Homogeneous single phase ErCrO{sub 4} nanoparticles have been synthesized by a modified sol-gel followed by hydrothermal method. X-ray diffraction reveals that the compound crystallizes into tetragonal structure with space group I41/amd. The average crystallite size was estimated to be 21(1) nm. Morphological analysis of the sample confirms uniform particles of size 20 nm. DC magnetic measurements show that ErCrO{sub 4} undergoes a paramagnetic-antiferromagnetic transition at 16 K, due to the superexchange Er-O-Cr-O-Er antiferromagnetic interactions.

  7. D-penicillamine assisted hydrothermal synthesis of Bi2S3 nanoflowers and their electrochemical application.

    PubMed

    Zhang, Ming; Chen, De-Jun; Wang, Rui-Zhi; Feng, Jiu-Ju; Bai, Zhengyu; Wang, Ai-Jun

    2013-10-01

    Single crystalline flower-like Bi2S3 nanostructures were successfully synthesized via a simple, facile and green hydrothermal method, with the assistance of D-penicillamine. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM), and found their morphologies mainly depend on the ratios of Bi(3+) to D-penicillamine, as well as the reaction temperature and time. And the possible growth mechanism has been discussed in some detail. In addition, the as-prepared Bi2S3 nanoflowers show good hydrogen storage ability. This strategy can be potentially expanded to prepare other metal chalcogenides materials.

  8. Microwave Hydrothermal Synthesis of Terbium Ions Complexed with Porous Graphene for Effective Absorbent for Organic Dye.

    PubMed

    Chen, Keqin; Gao, Hui; Bai, Bowei; Liu, Wenjing; Li, Xiaolong

    2017-12-01

    A luminescent terbium ions/reduced graphene oxide complex (Tb-RGO) was successfully and rapidly synthesized by the microwave hydrothermal reaction via the interactions between terbium ions and the active oxygen functional groups of graphene oxide. The as-prepared material was porous stacked by multilayer graphene in all directions. Thus, the resulting product owed the high specific surface area, high adsorption capacity and ultra-fast adsorption rate. Combined with the characteristic photoluminescence derived from terbium ions, the material has potential applications in biosensing and environmental protection.

  9. Hydrothermal synthesis and characterization of orchid-like MnO 2 nanostructures

    NASA Astrophysics Data System (ADS)

    Li, Xueliang; Li, Wenjie; Chen, Xiangying; Shi, Chengwu

    2006-12-01

    Orchid-like Cr-doped MnO 2 nanostructures have been synthesized via a hydrothermal method, using KClO 3 as the oxidant. The as-obtained samples were characterized by X-ray diffraction (XRD), X-ray photoelectron spectra (XPS), transmission electron microscopy (TEM) and field emission scanning electron microscopy (FE-SEM). Results show that the morphologies of orchid-like MnO 2 are made up of nanorods. The influences of chromium in the solution on the morphology of the products are discussed. The electrochemical characterization was carried out by cyclic voltammetry, which indicated that the products were excellent electrode material for super-capacitor.

  10. Controlled hydrothermal synthesis of CeO2 nanospheres and their excellent magnetic properties

    NASA Astrophysics Data System (ADS)

    Niu, Xiaofei

    2017-04-01

    Monodisperse spherical CeO2 nanostructures with irregular and rough surfaces have successfully been synthesized via a facile hydrothermal technology. XRD, SEM, XPS, Raman scattering, and M-H curves were employed to characterize the samples. The results showed that the spherical CeO2 nanostructures have a cubic fluorite structure and that there are Ce3+ ions and oxygen vacancies in the surface of the samples. The M-H curve of CeO2 nanospheres exhibits excellent room-temperature ferromagnetism (RT-FM), which is likely ascribed to the effects of the Ce3+ ions and oxygen vacancies.

  11. Synthesis and Characterization of Strontium Carbonate Nanostructures via Simple Hydrothermal Method

    NASA Astrophysics Data System (ADS)

    Asgari-Fard, Zahra; Sabet, Mohammad; Salavati-Niasari, Masoud

    2016-02-01

    Strontium carbonate (SrCO3) nanostructures were synthesized via simple hydrothermal method by Sr(NO3)2, ethylenediamine and hydrazine as reagents. The products were characterized with X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) and Fourier transform infrared spectroscopy (FT-IR). Different parameter's effects on the product size and morphology were investigated. It was found that reagent concentration, reaction time and temperature play key roles in morphology of the obtained product.

  12. Recyclable rhodium nanoparticles: green hydrothermal synthesis, characterization, and highly catalytic performance in reduction of nitroarenes.

    PubMed

    Lee, Yohan; Jang, Seongwan; Cho, Chang-Woo; Bae, Jong-Seong; Park, Sungkyun; Park, Kang Hyun

    2013-11-01

    In this work, rhodium nanoparticles were synthesized using hydrothermal method that is simple and easy to manipulate reaction and use nontoxic supercritical water. The rhodium nanoparticles were formed in uniform size and shape. These Rh NPs also acted as a efficient heterogenous catalyst in reduction of 4-nitrophenol to 4-aminophenol. Moreover, the rhodium nanoparticles can be recycled without any loss in catalytic activity, and showed highly catalytic activity for various nitroarenes. Therefore, this method will contribute greatly to the development of environmental field and be suitable for use in the industry.

  13. Selective growth of vertical ZnO nanowires with the control of hydrothermal synthesis and nano-imprint technology.

    PubMed

    Song, Jaejin; Baek, Seonghoon; Lee, Heon; Lim, Sangwoo

    2009-06-01

    Nano-imprint technology is one of the most advanced technologies for the fabrication of nano-size patterning. In this study, nano-imprint technology was used for the selective growth of ZnO nanowires on the Si wafer. When the poly methyl-methacrylate (PMMA) was first patterned by a nano-imprint process and ZnO seed layer was deposited and patterned by lift-off, ZnO nanowires were not vertically grown on the whole area of the patterned seed layer. Synthesis in zinc sulfate solution exhibited well-structured ZnO nanowires compared to the zinc nitrate solution, but uniformly aligned vertical growth of ZnO nanowires was not observed in either cases. On the other hand, when the PMMA was patterned using a nano-imprint process in the presence of seed layer, and ZnO nanowires were synthesized in zinc sulfate solution, selective growth of vertically aligned ZnO nanowires on 0.5 microm pattern sizes was achieved. The observation in this study suggests that the selective growth of ZnO nanowires on a defined pattern size can be obtained with the modification of pattering sequence and the control of low temperature hydrothermal synthesis of ZnO nanowires.

  14. Hydrothermal synthesis and metal ions doping effects of single-crystal Mn{sub 3}O{sub 4}

    SciTech Connect

    Kuang, Lili; Dong, Ruiting; Zhang, Zhanyang; Feng, Liang; Wang, Fan Wen, Yanxuan

    2013-09-01

    Graphical abstract: - Highlights: • Dopant species and dopant/Mn molar ratio affect the shape of Mn{sub 3}O{sub 4} microcrystal. • For Cu and Ni doped Mn{sub 3}O{sub 4}, the spontaneous valence changes of dopant taken place. • An apparent change in the energy bandgap of Mn{sub 3}O{sub 4} with the metal doping. - Abstract: Synthesis of undoped and transition metal ion doped Mn{sub 3}O{sub 4} microcrystals were achieved through a simple hydrothermal route. The morphologies and structures of the obtained products were characterized using X-ray diffraction, X-ray photoemission spectroscopy and scanning electron microscopy. Results revealed that the low volume percentage of ethanol in the precursor solution limited formation of Mn{sup 2+}, while the introduction of doping ions into the precursor solution caused a direct synthesis of single phase Mn{sub 3}O{sub 4} crystals. For Cu and Ni doping ions, the spontaneous valence changes during the doping process were taken place. The possible doping mechanisms for the formation of single-phase Mn{sub 3}O{sub 4} were discussed briefly. UV–vis spectroscopic studies showed an apparent change in the energy bandgap of Mn{sub 3}O{sub 4} with the metal doping.

  15. Selected-control hydrothermal synthesis and formation mechanism of monazite- and zircon-type LaVO(4) nanocrystals.

    PubMed

    Fan, Weiliu; Song, Xinyu; Bu, Yuxiang; Sun, Sixiu; Zhao, Xian

    2006-11-23

    Selective-controlled structure and shape of LaVO(4) nanocrystals were successfully synthesized by a simple hydrothermal method without the presence of catalysts or templates. It was found that tuning the pH of the growth solution was a crucial step for the control of the structure transformation, that is, from monoclinic (m-) to tetragonal (t-) phase, and morphology evolution of LaVO(4) nanocrystals. Further studies demonstrated that the morphology of the product had a strong dependence on the initial lanthanum sources. In the La(NO(3))(3) or LaCl(3) reaction system, pure t-LaVO(4) nanorods with uniform diameters about 10 nm could be obtained. But when using La(2)(SO(4))(3) as the lanthanum source, we can get t-LaVO(4) nanowiskers with broomlike morphology. The detailed systematic study had shown that a special dissolution-recrystallization transformation mechanism as well as an Ostwald ripening process was responsible for the phase control and anisotropic morphology evolution of the LaVO(4) nanocrystals. As a result, the controlled synthesis of m- and t-LaVO(4) not only has great theoretical significance in studying the polymorph control and selective synthesis of inorganic materials but also benefits the potential applications based on LaVO(4) nanocrystals owing to the unusual luminescent properties induced by structural transformation.

  16. Nitrogen-doped graphene/ZnSe nanocomposites: hydrothermal synthesis and their enhanced electrochemical and photocatalytic activities.

    PubMed

    Chen, Ping; Xiao, Tian-Yuan; Li, Hui-Hui; Yang, Jing-Jing; Wang, Zheng; Yao, Hong-Bin; Yu, Shu-Hong

    2012-01-24

    Nitrogen-doped graphene (GN) has great potential applications in many fields because doping with nitrogen can alter the electrical properties of graphene. It is still a challenge to develop a convenient method for synthesis of GN sheets. In this paper, we first report the synthesis of a nitrogen-doped graphene/ZnSe nanocomposite (GN-ZnSe) by a one-pot hydrothermal process at low temperature using graphene oxide nanosheets and [ZnSe](DETA)(0.5) nanobelts as precursors. ZnSe nanorods composed of ZnSe nanoparticles were found to deposit on the surface of the GN sheets. The results demonstrated that [ZnSe](DETA)(0.5) nanobelts were used not only as the source of ZnSe nanoparticles but also as the nitrogen source. Interestingly, it was found that the as-prepared nanocomposites exhibit remarkably enhanced electrochemical performance for oxygen reduction reaction and photocatalytic activities for the bleaching of methyl orange dye under visible-light irradiation. This facile and catalyst-free approach for depositing ZnSe nanoparticles onto the graphene sheets may provide an alternative way for preparation of other nanocomposites based on GN sheets under mild conditions, which show their potential applications in wastewater treatment, fuel cells, energy storage, nanodevices, and so on.

  17. Pencil-like zinc oxide micro/nano-scale structures: Hydrothermal synthesis, optical and photocatalytic properties

    SciTech Connect

    Moulahi, A.; Sediri, F.

    2013-10-15

    Graphical abstract: - Highlights: • Zinc oxide micro/nanopencils have been synthesized hydrothermally. • Photocatalytic activity has been evaluated by the degradation of methylene blue under UV light irradiation. • ZnO nanopencils exhibit much higher photocatalytic activity than the commercial ZnO. - Abstract: Zinc oxide micro/nanopencils have been successfully synthesized by hydrothermal process using zinc acetate and diamines as structure-directing agents. The morphology, the structure, the crystallinity and the composition of the materials were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). The optical properties of synthesized ZnO were investigated by UV–vis spectroscopy. The photocatalytic activity of the material has been evaluated by the degradation of methylene blue under UV irradiation. As a result, after the lapse of 150 min, around 82% bleaching was observed, with ZnO nanopencils yielding more photodegradation compared to that of commercial ZnO (61%)

  18. Facile synthesis of graphene/ZnO nanocomposites by low temperature hydrothermal method

    SciTech Connect

    Saravanakumar, Balasubramaniam; Mohan, Rajneesh; Kim, Sang-Jae

    2013-02-15

    Highlights: ► Graphene/ZnO nanocomposites were prepared by low temperature hydrothermal method. ► Rhodamine-B degraded by using graphene/ZnO nanocomposites. ► ZnO anchored well on the surface of graphene. -- Abstract: Graphene/ZnO nanocomposites have been synthesized using hydrothermal method at two different temperatures 80 and 90 °C. The structure, morphology and optical properties of as synthesized nanocomposites were analyzed through X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), Fourier transform infrared spectroscopy, transmission electron microscopy (TEM) and UV–vis absorbance spectroscopy. The XRD pattern confirmed the formation of graphene decorated by hexagonal ZnO with high crystallinity. FESEM image revealed that the sheet like graphene decorated with ZnO in homogeneously. Decoration of quasi-spherical ZnO nanoparticles on graphene sheet was confirmed by TEM. The characteristic absorbance peaks of graphene/ZnO nanocomposites were observed in UV visible spectra. The photocatalytic degradation experiment was performed against rhodamine-B dye and showed good catalytic activity for both samples. The graphene/ZnO nanocomposites showed higher catalytic activity then ZnO nanoparticles. The GZN-90 sample showed more catalytic activity than GZN-80 due to higher density of ZnO in graphene surface generates large number of photo-induced electron.

  19. Hydrothermal synthesis and magnetic properties of {alpha}-MnO{sub 2} nanowires

    SciTech Connect

    Zhao, J.G.; Yin, J.Z.; Yang, S.G.

    2012-03-15

    Highlights: Black-Right-Pointing-Pointer {alpha}-MnO{sub 2} nanowires were synthesized through the hydrothermal method. Black-Right-Pointing-Pointer Ferromagnetism was observed in the {alpha}-MnO{sub 2} nanowires at 5 K. Black-Right-Pointing-Pointer The N{sub 2} adsorption-desorption experiment shows that surface area of {alpha}-MnO{sub 2} nanowires is 160.4 m{sup 2} g{sup -1}. -- Abstract: In the present study, one-dimensional (1D) {alpha}-MnO{sub 2} nanowires with width of 50-60 nm, length about several micrometers have been successfully prepared under hydrothermal conditions in the presence of sodium carboxymethyl cellulose. The samples were characterized by X-ray diffraction, scanning electron microscope, superconducting quantum interference device and N{sub 2} adsorption-desorption experiment. The magnetic measurement reveals that the {alpha}-MnO{sub 2} nanowires exhibit a ferromagnetic behavior at 5 K and a paramagnetic behavior at 300 K. The N{sub 2} adsorption-desorption experiment shows that surface area is 160.4 m{sup 2} g{sup -1}, which is even larger than those of mesoporous nanostructures. At the same time, the possible formation mechanism for the formation of {alpha}-MnO{sub 2} nanowires has been proposed according to the experimental results.

  20. Hydrothermal synthesis of cerium titanate nanorods and its application in visible light photocatalysis

    SciTech Connect

    Pei, L.Z. Liu, H.D.; Lin, N.; Yu, H.Y.

    2015-01-15

    Highlights: • Cerium titanate nanorods have been synthesized by a simple hydrothermal process. • The size of the cerium titanate nanorods can be controlled by growth conditions. • Cerium titanate nanorods exhibit good photocatalytic activities for methyl blue. - Abstract: Cerium titanate nanorods have been prepared via a hydrothermal process using sodium dodecyl sulfate (SDS) as the surfactant. The cerium titanate nanorods have been analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), and ultraviolet–visible (UV–vis) diffuse reflectance spectrum. XRD shows that the nanorods are composed of CeTi{sub 21}O{sub 38} phase. Electron microscopy observations indicate that the nanorods have good single crystalline nature. The diameter and length of the nanorods are about 50–200 nm and 1–2 μm, respectively. Cerium titanate nanorods have a band gap of 2.65 eV. The photocatalytic activities of the nanorods have been investigated by degrading methylene blue (MB) under visible light irradiation. MB solution with the concentration of 10 mg L{sup −1} can be degraded totally with the irradiation time increasing to 240 min. Cerium titanate nanorods exhibit great potential in photocatalytic degradation of MB under visible light irradiation.

  1. Direct synthesis of silver/polymer/carbon nanocables via a simple hydrothermal route

    SciTech Connect

    Jin Mingshang; Kuang Qin Jiang Zhiyuan; Xu Tao; Xie Zhaoxiong Zheng Lansun

    2008-09-15

    High-yield silver/polymer/carbon nanocables were synthesized via a one-step simple hydrothermal route by using silver chloride and glucose as precursors. High-resolution TEM and element mapping proved that as-prepared nanocables consist of a silver nanowire core, a polymer inner shell, and a graphitic carbon outer shell. A three-step growth mechanism was proposed to explain the growth of such three-layer nanocables, i.e. the formation of silver nanowires, the glycosidation of glucose molecules on silver nanowire surface and the carbonization of the outmost glycosidation layer. We believe that reaction temperature plays the key role in the polymerization of glucose and sequent surface-carbonization. - Graphical abstract: High-yield silver/polymer/carbon coaxial nanocables were synthesized via a one-step simple hydrothermal route by using silver chloride and glucose as precursors. Our experiments indicate that such novel nanostructures formed through the growth mechanism that the silver nanowires grow first, and then glycosidation of glucose occurs on the silver nanowire surfaces, and finally the partial carbonization occurs on the outmost surface of the polymer layer.

  2. HYDROTHERMAL SYNTHESIS OF α-MoO3 NANORODS FOR NO2 DETECTION

    NASA Astrophysics Data System (ADS)

    Bai, Shouli; Chen, Song; Tian, Yuan; Luo, Ruixian; Li, Dianqing; Chen, Aifan

    2012-12-01

    Thermodynamically stable molybdenum trioxide nanorods have been successfully synthesized by a simple hydrothermal process. The product exhibits high-quality, single-crystalline layered orthorhombic structure (α-MoO3), and aspect ratio over 20 by characterizations of X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM) and Fourier transform infrared (FT-IR). The growth mechanism of α-MoO3 nanorods can be understood by electroneutral and dehydration reaction, which is highly dependent on solution acidity and hydrothermal temperature. The sensing tests show that the sensor based on MoO3 nanorods exhibits high sensitivity to NO2 and is not interferred by CO and CH4, which makes this kind sensor a competitive candidate for NO2 detection. The intrinsic sensing performance of MoO3 maybe arise from its nonstoichiometry of MoO3 owing to the presence of Mo5+ and oxygen vacancy in MoO3 lattice, which has been confirmed by X-ray photoelectron spectroscopy (XPS) analysis. The sensing mechanism of MoO3 for NO2 is also discussed.

  3. Hydrothermal reactions: From the synthesis of ligand to new lanthanide 3D-coordination polymers

    NASA Astrophysics Data System (ADS)

    da Silva, Fausthon Fred; de Oliveira, Carlos Alberto Fernandes; Falcão, Eduardo Henrique Lago; Gatto, Claudia Cristina; da Costa, Nivan Bezerra; Freire, Ricardo Oliveira; Chojnacki, Jarosław; Alves Júnior, Severino

    2013-11-01

    The organic ligand 2,5-piperazinedione-1,4-diacetic acid (H2PDA) was synthesized under hydrothermal conditions starting from the iminodiacetic acid and catalyzed by oxalic acid. The X-ray powder diffraction data indicates that the compound crystallizes in the P21/c monoclinic system as reported in the literature. The ligand was also characterized by elemental analysis, magnetic nuclear resonance, infrared spectroscopy and thermogravimetric analysis. Two new coordination networks based on lanthanide ions were obtained with this ligand using hydrothermal reaction. In addition to single-crystal X-ray diffraction, the compounds were characterized by infrared spectroscopy, thermogravimetric analysis, scanning electron microscopy and elemental analysis. Single-crystal XRD showed that the compounds are isostructural, crystallizing in P21/n monoclinic system with chemical formula [Ln(PDA)1.5(H2O)](H2O)3 (Ln=Gd3+(1) and Eu3+(2)).The luminescence properties of both compounds were studied. In the compound (1), a broad emission band was observed at 479 nm, redshifted by 70 nm in comparison of the free ligand. In (2), the typical f-f transition was observed with a maximum peak at 618 nm, related with the red emission of the europium ions. Computational methods were performed to simulate the crystal structure of (2). The theoretical calculations of the intensity parameters are in good agreement with the experimental values.

  4. Hydrothermal synthesis of BaTiO 3 nanoparticles using a supercritical continuous flow reaction system

    NASA Astrophysics Data System (ADS)

    Hayashi, Hiromichi; Noguchi, Takio; Islam, Nazrul M.; Hakuta, Yukiya; Imai, Yusuke; Ueno, Nobuhiko

    2010-06-01

    Highly crystalline BaTiO 3 nanoparticle was synthesized rapidly by hydrothermal reaction in supercritical water using a continuous flow reactor. The reactants of TiO 2 sol (or TiCl 4)/Ba(NO 3) 2 mixed solution and KOH solution were used as starting materials and that was heated quickly up to 400 °C under the pressure of 30 MPa for 8 ms as reaction time. The XRD results revealed that the crystal phase of the obtained particles was cubic BaTiO 3, indicating that the hydrothermal reaction in supercritical water was successfully proceeded under present reaction conditions. Primarily particle size of the BaTiO 3 nanoparticle was determined by means of BET surface area, as small as less than 10 nm with decreasing the reaction pH. In contrast, dispersed particle size in solution measured by DLS (dynamic light scattering) technique decreased from 260 to 90 nm with increasing the reactants concentration. Aggregation of BaTiO 3 nanoparticles might be depressed in the presence of coexisting nitrate anions.

  5. Synthesis of hydrothermally stable, hierarchically mesoporous aluminosilicate Al-SBA-1 and their catalytic properties

    NASA Astrophysics Data System (ADS)

    Li, Na; Wang, Jin-Gui; Xu, Jian-Xiong; Liu, Jin-Yu; Zhou, Hui-Jing; Sun, Ping-Chuan; Chen, Tie-Hong

    2012-03-01

    Hydrothermally stable mesoporous aluminosilicates Al-SBA-1 with hierarchical pore structure have been successfully synthesized under alkaline condition at 120 °C by employing organic mesomorphous complexes of polyelectrolyte (poly(acrylic acid) (PAA)) and cationic surfactant (hexadecyl pyridinium chloride (CPC)) as template. The Si/Al ratio could be as high as 5 and the incorporation of Al into the silica framework did not disturb the well-ordered cubic Pm3&cmb.macr;n mesostructure. Meanwhile, the incorporation of Al could greatly increase the specific surface area and pore volume of the samples. The Al-SBA-1 materials exhibited a high hydrothermal stability and remained stable even after being treated in boiling water for 10 days. The catalytic activity of the Al-SBA-1 materials was investigated by employing the Friedel-Crafts alkylation of toluene with benzyl alcohol as a model reaction and they exhibited excellent catalytic property due to the incorporated acid sites and the hierarchically mesoporous structure.

  6. Hydrothermal synthesis and formation mechanism of hexagonal yttrium hydroxide fluoride nanobundles

    SciTech Connect

    Tian, Li; Sun, QiLiang; Zhao, RuiNi; He, HuiLin; Xue, JianRong; Lin, Jun

    2013-11-15

    Graphical abstract: The formation of yttrium hydroxide fluorides nanobundles can be expressed as a precipitation transformation from cubic NaYF{sub 4} to hexagonal NaYF{sub 4} and to hexagonal Y(OH){sub 2.02}F{sub 0.98} owing to ion exchange. - Highlights: • Novel Y(OH){sub 2.02}F{sub 0.98} nanobundles have been successfully prepared by hydrothermal method. • The branched nanobundles composed of numerous oriented-attached nanoparticles has been studied. • The growth mechanism is proposed to be ion exchange and precipitation transformation. - Abstract: This article presents the fabrication of hexagonal yttrium hydroxide fluoride nanobundles via one-pot hydrothermal process, using yttrium nitrate, sodium hydroxide and ammonia fluoride as raw materials to react in propanetriol solvent. The X-ray diffraction pattern clearly reveals that the grown product is pure yttrium hydroxide fluoride, namely Y(OH){sub 2.02}F{sub 0.98}. The morphology and microstructure of the synthesized product is testified to be nanobundles composed of numerous oriented-attached nanoparticles as observed from the field emission scanning electron microscopy (FESEM). The chemical composition was analyzed by the energy dispersive spectrum (EDS), confirming the phase transformation of the products which was clearly consistent with the result of XRD analysis. It is proposed that the growth of yttrium hydroxide fluoride nanobundles be attributed to ion exchange and precipitation transformation.

  7. A Facile Hydrothermal Route for Synthesis of ZnS Hollow Spheres with Photocatalytic Degradation of Dyes Under Visible Light

    NASA Astrophysics Data System (ADS)

    Han, Zh.; Wang, N.; Zhang, H.; Yang, X.

    2017-01-01

    A facile hydrothermal method was employed for the synthesis of ZnS hollow spheres by using thioglycolic acid (TGA) as a capping agent under hydrothermal condition. The obtained products were characterized by X-ray powder diffraction (XRD) and X-ray Photoelectron Spectroscopy (XPS). No diffraction peaks from other crystalline forms were detected, the synthesized ZnS hierarchical hollow spheres were relatively pure. The photocatalytic activities of as-synthesized samples were evaluated by the degradation of methyl orange (MO) and rhodamine B (RhB) under the condition of visible-light irradiation. The higher the initial MO and RhB concentrations, the longer it takes to reach the same residual concentration, implying that the apparent rates of MO and RhB degradation decrease with increase in the initial MO and RhB concentration. The increase of photocatalyst dosage from 0.2 to 0.6 g/L results in a sharp increase of the photodegradation efficiency from 68.50 to 92.66% after 180 min of visible-light irradiation for MO degradation, and the increase of photocatalyst dosage from 0.2 to 0.4 g/L results in a distinct increase of the photodegradation efficiency from 65.72 to 90.85% after 180 min of visible-light irradiation for RhB. The elution of intermediates generated in the photocatalytic mineralization of MO and RhB resulted in an increase in total organic carbon (TOC) level, leading to the difference between TOC removal rate and MO and RhB decolorization rates.

  8. Photocatalytic activity of Li-doped TiO{sub 2} nanoparticles: Synthesis via ionic liquid-assisted hydrothermal route

    SciTech Connect

    Ravishankar, T.N.; Nagaraju, G.; Dupont, Jairton

    2016-06-15

    Highlights: • TiO{sub 2}: Li nanoparticles were synthesized via an ionic liquid-assisted hydrothermal method. • The doping of Li to anatase TiO{sub 2} affects the properties of the resultant product. • TiO{sub 2}: Li nanoparticles were used as a photocatalyst for the degradation of dye. • TiO{sub 2}: Li nanoparticles were used as sensor, and antibacterial agent. • TiO{sub 2}: Li were used as reducing agent for the reduction of Cr{sup 6+} to Cr{sup 3+}. - Abstract: We have proposed a simple one pot synthesis of lithium-doped TiO{sub 2} nanoparticles (TiO{sub 2}:Li) via an ionic liquid-assisted hydrothermal method and their potential use as a photocatalyst for the degradation of organic dye, as well as the reduction of toxic Cr{sup 6+} to non toxic Cr{sup 3+}. The structure of TiO{sub 2}:Li nanoparticles was examined by XRD, FTIR, XPS, Raman, UV–vis, Photoluminescence spectroscopy and morphology by SEM and TEM. The incorporation of Li into anatase-phase TiO{sub 2} affected the optical properties of the resultant TiO{sub 2} nanoparticles. The photocatalytic activity of the TiO{sub 2}:Li nanoparticles was determined by degradation of trypan blue. Degradation studies showed improved photocatalytic activity of TiO{sub 2}:Li nanoparticles compared to TiO{sub 2} nanoparticles and bulk TiO{sub 2}. TiO{sub 2}:Li nanoparticles also functioned as a detoxification agent which was confirmed by the reduction of Cr{sup 6+} to Cr{sup 3+}.

  9. Template-free hydrothermal derived cobalt oxide nanopowders: Synthesis, characterization, and removal of organic dyes

    SciTech Connect

    Nassar, Mostafa Y.; Ahmed, Ibrahim S.

    2012-09-15

    Graphical abstract: XRD patterns of the products obtained by hydrothermal treatment at 160 °C for 24 h, and at different [Co{sup 2+}]/[CO{sub 3}{sup 2−}] ratios: (a) 1:6, (b) 1:3, (c) 1:1.5, (d) 1:1, (e) 1:0.5. Highlights: ► Spinel cobalt oxide nanoparticles with different morphologies were prepared by hydrothermal approach. ► The optical characteristics of the as-prepared cobalt oxide revealed the presence of two band gaps. ► Adsorption of methylene blue dye on Co{sub 3}O{sub 4} was investigated and the percent uptake was found to be >99% in 24 h. -- Abstract: Pure spinel cobalt oxide nanoparticles were prepared through hydrothermal approach using different counter ions. First, the pure and uniform cobalt carbonate (with particle size of 21.8–29.8 nm) were prepared in high yield (94%) in an autoclave in absence unfriendly organic surfactants or solvents by adjusting different experimental parameters such as: pH, reaction time, temperature, counter ions, and (Co{sup 2+}:CO{sub 3}{sup 2−}) molar ratios. Thence, the spinel Co{sub 3}O{sub 4} (with mean particle size of 30.5–47.35 nm) was produced by thermal decomposition of cobalt carbonate in air at 500 °C for 3 h. The products were characterized by powder X-ray diffraction (XRD), Fourier transform infrared (FTIR), transmission electron microscope (TEM), scanning electron microscope (SEM), and thermal analysis (TA). Also, the optical characteristics of the as-prepared Co{sub 3}O{sub 4} nanoparticles revealed the presence of two band gaps (1.45–1.47, and 1.83–1.93 eV). Additionally, adsorption of methylene blue dye on Co{sub 3}O{sub 4} nanoparticles was investigated and the uptake% was found to be >99% in 24 h.

  10. Hydrothermal synthesis of iron phosphate microspheres constructed by mesoporous polyhedral nanocrystals

    SciTech Connect

    Song, Haojie; Sun, Yali; Jia, Xiaohua

    2015-09-15

    Novel monodispersed Fe{sub 5}(PO{sub 4}){sub 4}(OH){sub 3}·2H{sub 2}O microspheres with the diameters of several micrometers were prepared by a facile one-step hydrothermal method without using any templates, only employing FeCl{sub 3}·6H{sub 2}O and NaNH{sub 4}HPO{sub 4} as the initial materials. The obtained samples were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), and high-resolution transmission electron microscopy (HR-TEM), respectively. The characterizations revealed that the as-prepared microspheres are constructed by the polyhedral nanoparticles with an average diameter of 100 nm. The corresponding FePO{sub 4} microspheres assembled by mesoporous polyhedral nanocrystals can be easily obtained by calcining a sphere-like Fe{sub 5}(PO{sub 4}){sub 4}(OH){sub 3}·2H{sub 2}O precursor. - Graphical abstract: Novel monodispersed Fe{sub 5}(PO{sub 4}){sub 4}(OH){sub 3}·H{sub 2}O microspheres with a diameter of several micrometers were successfully obtained by a simple, template-free hydrothermal route. FePO{sub 4} microspheres constructed by mesoporous polyhedral FePO{sub 4} nanocrystals could be easily prepared by calcining an Fe{sub 5}(PO{sub 4}){sub 4}(OH){sub 3}·2H{sub 2}O precursor. Display Omitted - Highlights: • Monodispersed Fe{sub 5}(PO{sub 4}){sub 4}(OH){sub 3}·2H{sub 2}O microspheres were prepared by a facile hydrothermal method without using any templates • Fe{sub 5}(PO{sub 4}){sub 4}(OH){sub 3}·2H{sub 2}O microspheres present a novel morphology, which was constructed by closely polyhedral nanoparticles. • The FePO{sub 4} microspheres assembled by mesoporous polyhedral nanocrystals obtained by calcining Fe{sub 5}(PO{sub 4}){sub 4}(OH){sub 3}·2H{sub 2}O precursor.

  11. Hydrothermal synthesis and characterization of fluorine & manganese co-doped PZT based cuboidal shaped powder

    NASA Astrophysics Data System (ADS)

    Nawaz, H.; Shuaib, M.; Saleem, M.; Rauf, A.; Aleem, A.

    2016-08-01

    Cuboidal shaped PZT powder particles based composition Pb0.89(Ba, Sr)0.11(Zr0.52Ti0.48)O3 co- doped with 1 mol% manganese and 2 mol% fluorine was prepared through hydrothermal route. 200-250nm size cuboidal particles were observed under FE-SEM. XRD technique revealed that the perovskite type ceramic structure has a dominant rhombohedral phase. The resultant powder particles were then spray dried, uniaxially pressed and sintered at different temperatures to achieve maximum theoretical density. 98% density was obtained in the pellets at a sintering temperature of 1190°C with an average grain size of 1-3um. The electrical properties of sintered samples were also measured before and after poling to evaluate the effect of dopants on piezoelectric properties.

  12. Synthesis of highly magnetic graphite-encapsulated FeCo nanoparticles using a hydrothermal process.

    PubMed

    Lee, Seung Jae; Cho, Jee-Hyun; Lee, Chulhyun; Cho, Janggeun; Kim, Yong-Rok; Park, Joung Kyu

    2011-09-16

    The graphite encapsulation of metal alloy magnetic nanoparticles has attracted attention for biological applications because of the high magnetization of the encapsulated particles. However, most of the synthetic methods have limitations in terms of scalability and economics because of the demanding synthetic conditions and low yields. Here, we show that well controlled graphite-encapsulated FeCo core-shell nanoparticles can be synthesized by a hydrothermal method, simply by mixing Fe/Co with sucrose as a carbon source. Various Fe/Co metal ratios were used to determine the compositional dependence of the saturation magnetization and relaxivity coefficient. Transmission electron microscopy indicated that the particle sizes were 7 nm. In order to test the capability of graphite-encapsulated FeCo nanoparticles as magnetic resonance imaging (MRI) contrast agents, these nanoparticles were solubilized in water by the nonspecific physical adsorption of sodium dodecylbenzene sulfonate.

  13. Hydrothermal synthesis and photoelectrochemical properties of In2S3 thin films with a wedgelike structure

    NASA Astrophysics Data System (ADS)

    Zhang, Lina; Zhang, Wei; Yang, Haibin; Fu, Wuyou; Li, Minghui; Zhao, Hui; Ma, Jinwen

    2012-09-01

    Indium sulfide (In2S3) thin films with a wedgelike structure were prepared on fluorine-doped tin oxide (FTO) substrate by a facile hydrothermal method. By properly monitoring the experimental conditions, including the reaction time, concentrations of tartaric acid, precursor concentration ratio and the reaction temperature, the In2S3 films with different morphologies and thickness could be obtained, and the growth mechanism of β-In2S3 films was also proposed in this work. Furthermore, UV-vis absorption study revealed that the absorption range broadened with the growth of the In2S3 crystals. In addition, a photocurrent of 0.48 mA cm-2 was obtained under 100 mW cm-2 UV-visible illuminations of the wedgelike In2S3 thin films.

  14. Synthesis of pyrite FeS2 nanorods by simple hydrothermal method and its photocatalytic activity

    NASA Astrophysics Data System (ADS)

    Morales-Gallardo, M. V.; Ayala, A. M.; Pal, Mou; Cortes Jacome, M. A.; Toledo Antonio, J. A.; Mathews, N. R.

    2016-09-01

    In this work, FeS2 nanorods were synthetized by hydrothermal method. The advantages of our process were the high yield, simplicity and reproducibility. The material was studied in detail using different experimental tools such as XRD, SEM, HRTEM, EDXS, XPS, Raman, and UV-vis reflectance. XRD pattern and Raman data revealed good crystalline quality for the as synthesized pyrite FeS2. SEM analysis displayed the rod-like morphologies of FeS2 which seemed to grow radially from a center giving a flower-like appearance. From TEM images the approximate length and diameter of nano-rods were determined as 275 and 15 nm respectively. The material showed excellent photocatalytic activity which was assessed from the degradation of the methlyene blue.

  15. Rapid hydrothermal synthesis of VO2 (B) and its conversion to thermochromic VO2 (M1).

    PubMed

    Popuri, Srinivasa Rao; Miclau, Marinela; Artemenko, Alla; Labrugere, Christine; Villesuzanne, Antoine; Pollet, Michaël

    2013-05-06

    The present study provides a rapid way to obtain VO2 (B) under economical and environmentally friendly conditions. VO2 (B) is one of the well-known polymorphs of vanadium dioxide and is a promising cathode material for aqueous lithium ion batteries. VO2 (B) was successfully synthesized by rapid single-step hydrothermal process using V2O5 and citric acid as precursors. The present study shows that phase-pure VO2 (B) polytype can be easily obtained at 180 °C for 2 h and 220 °C for 1 h, that is, the lowest combination of temperature and duration reported so far. The obtained VO2 (B) is characterized by X-ray powder diffraction, high-resolution scanning electron microscopy, and Fourier transform infrared spectroscopy. In addition, we present an indirect way to obtain VO2 (M1) by annealing VO2 (B) under vacuum for 1 h.

  16. Synthesis and characterization of WO{sub 3} nanostructures prepared by an aged-hydrothermal method

    SciTech Connect

    Huirache-Acuna, R.; Paraguay-Delgado, F.; Albiter, M.A.; Lara-Romero, J.; Martinez-Sanchez, R.

    2009-09-15

    Nanostructures of tungsten trioxide (WO{sub 3}) have been successfully synthesized by using an aged route at low temperature (60 deg. C) followed by a hydrothermal method at 200 deg. C for 48 h under well controlled conditions. The material was studied by X-ray diffraction (XRD), scanning electron microscopy (SEM) and Energy Dispersive Spectroscopy (EDS), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). Specific Surface Area (S{sub BET}) were measured by using the BET method. The lengths of the WO{sub 3} nanostructures obtained are between 30 and 200 nm and their diameters are from 20 to 70 nm. The growth direction of the tungsten oxide nanostructures was determined along [010] axis with an inter-planar distance of 0.38 nm.

  17. Hydrothermal synthesis of magnetic mesoporous carbon microspheres from carboxymethylcellulose and nickel acetate

    NASA Astrophysics Data System (ADS)

    Wu, Qiong; Li, Wei; Tan, Jia; Nan, Xi; Liu, Shouxin

    2015-03-01

    Paramagnetic mesoporous carbon spheres with diameters of 1-3 μm were synthesized through the hydrothermal carbonization of carboxymethylcellulose with nickel acetate, followed by high-temperature carbonization in a N2 atmosphere. Monodisperse Ni particles of average size of 2-5 nm were doped into the carbon matrix, and covered the entrances of pores. Ni particles existed as metallic nickel and nickel oxide with ordered lattice structures. The effect of Ni content on the specific surface area, mesopore percentage, and magnetic and adsorption properties were investigated. The highest vitamin B12 adsorption capacity of 103 mg/g was achieved for the sample prepared using 0.04 g of nickel acetate. The Freundlich and Langmuir isotherm models were used to determine the equilibrium uptakes of vitamin B12. Vitamin B12 was physically adsorbed as a monolayer on the carbon spheres. The carbon spheres were easily separated on account of their magnetism.

  18. Hydrothermal synthesis and acetylene sensing properties of variety low dimensional zinc oxide nanostructures.

    PubMed

    Zhou, Qu; Chen, Weigen; Peng, Shudi; Zeng, Wen

    2014-01-01

    Various morphologies of low dimensional ZnO nanostructures, including spheres, rods, sheets, and wires, were successfully synthesized using a simple and facile hydrothermal method assisted with different surfactants. Zinc acetate dihydrate was chosen as the precursors of ZnO nanostructures. We found that polyethylene glycol (PEG), polyvinylpyrrolidone (PVP), glycine, and ethylene glycol (EG) play critical roles in the morphologies and microstructures of the synthesized nanostructures, and a series of possible growth processes were discussed in detail. Gas sensors were fabricated using screen-printing technology, and their sensing properties towards acetylene gas (C2H2), one of the most important arc discharge characteristic gases dissolved in oil-filled power equipments, were systematically measured. The ZnO nanowires based sensor exhibits excellent C2H2 sensing behaviors than those of ZnO nanosheets, nanorods, and nanospheres, indicating a feasible way to develop high-performance C2H2 gas sensor for practical application.

  19. ZnO nanorod array random lasers fabricated by a laser-induced hydrothermal synthesis

    NASA Astrophysics Data System (ADS)

    Fujiwara, Hideki; Suzuki, Takemasa; Niyuki, Ryo; Sasaki, Keiji

    2016-10-01

    We demonstrate random lasing in ZnO nanorod array (NRA) structures fabricated by a laser-induced hydrothermal growth, which would make it possible to control structural parameters, such as diameter, length, density and so on, by adjusting the laser irradiation time and intensity. To realize low-threshold ZnO NRA random lasers, we attempt to optimize the structure by changing the laser irradiation time (growth time). From the results, we confirmed that the fabricated ZnO NRAs after CO2 laser annealing could induce UV random lasing and their thresholds strongly depend on the growth time. Thus, we succeed to realize ZnO NRA random lasers and suggest the possibility to control the random lasing properties by adjusting the irradiated laser conditions.

  20. Rare earth fluoride nano-/microstructures: hydrothermal synthesis, luminescent properties and applications.

    PubMed

    Zhao, Qian; Xu, Zhenhe; Sun, Yaguang

    2014-02-01

    Rare earth fluoride materials have attracted wide interest and come to the forefront in nanophotonics due to their distinct electrical, optical and magnetic properties as well as their potential applications in diverse fields such as optical telecommunication, lasers, biochemical probes, infrared quantum counters, and medical diagnostics. This review presents a comprehensive overview of the flourishing field of rare earth fluorides materials in the past decade. We summarize the recent research progress on the preparation, morphology, luminescent properties and application of rare earth fluoride-based luminescent materials by hydrothermal systems. Various rare earth fluoride materials are obtained by fine-tuning of experimental conditions, such as capping agents, fluoride source, acidity, temperature and reaction time. The controlled morphology, luminescent properties and application of the rare earth fluorides are briefly discussed with typical examples.

  1. Amino acids assisted hydrothermal synthesis of hierarchically structured ZnO with enhanced photocatalytic activities

    NASA Astrophysics Data System (ADS)

    Guo, Yanxia; Lin, Siwen; Li, Xuan; Liu, Yuping

    2016-10-01

    Novel hierarchically structured ZnO, including rose-like, dandelion-like and flower-like, have been synthesized through a simple hydrothermal process using different amino acids (glutamine, histidine and glycine) as structure-directing agents and urea as deposition agent, followed by subsequent calcination. Amino acids played a crucial role in the formation of hierarchically structured ZnO, and different amino acids could induce different exquisite shapes and assembly ways, as well as more oxygen defects. The prepared hierarchically structured ZnO exhibited excellent photocatalytic activities for the photodegradation of Rhodamine B, which was associated with their special hierarchical structures, large BET surface area and the existence of more oxygen defects. Amino acid-assisted growth mechanism of hierarchically structured ZnO was also discussed.

  2. Hydrothermal Synthesis and Acetylene Sensing Properties of Variety Low Dimensional Zinc Oxide Nanostructures

    PubMed Central

    Chen, Weigen; Peng, Shudi; Zeng, Wen

    2014-01-01

    Various morphologies of low dimensional ZnO nanostructures, including spheres, rods, sheets, and wires, were successfully synthesized using a simple and facile hydrothermal method assisted with different surfactants. Zinc acetate dihydrate was chosen as the precursors of ZnO nanostructures. We found that polyethylene glycol (PEG), polyvinylpyrrolidone (PVP), glycine, and ethylene glycol (EG) play critical roles in the morphologies and microstructures of the synthesized nanostructures, and a series of possible growth processes were discussed in detail. Gas sensors were fabricated using screen-printing technology, and their sensing properties towards acetylene gas (C2H2), one of the most important arc discharge characteristic gases dissolved in oil-filled power equipments, were systematically measured. The ZnO nanowires based sensor exhibits excellent C2H2 sensing behaviors than those of ZnO nanosheets, nanorods, and nanospheres, indicating a feasible way to develop high-performance C2H2 gas sensor for practical application. PMID:24672324

  3. Hydrothermal reactions of pyruvic acid: synthesis, selection, and self-assembly of amphiphilic molecules.

    PubMed

    Hazen, Robert M; Deamer, David W

    2007-04-01

    Selection and self-assembly of organic compounds in aqueous phases must have been a primary process leading to emergent molecular complexity and ultimately to the origin of life. Facile reactions of pyruvic acid under hydrothermal conditions produce a complex mixture of larger organic molecules, some of which are amphiphiles that readily self-assemble into cell-sized vesicular structures. Chemical characterization of major components of this mixture reveals similarities to the suite of organic compounds present in the Murchison carbonaceous chondrite, some of whose molecules also self-assemble into membranous vesicles. Physical properties of the products are thus relevant to understanding the prebiotic emergence of molecular complexity. These results suggest that a robust family of prebiotic reaction pathways produces similar products over a range of geochemical and astrochemical environments.

  4. Synthesis and characterization of hydrothermally grown ZnO nanomaterials for biomedical applications

    NASA Astrophysics Data System (ADS)

    Shearin, Austin; Bhaumik, Anagh; Wanekaya, Adam; Delong, Robert; Ghosh, Kartik; Missouri State University Team

    2014-03-01

    Nanomaterials have been of recent importance in the biomedical field due to their use in drug delivery applications, magnetic resonance imaging, and cell separation. Intrinsically nanomaterials of ZnO are having low cytotoxicity and genotoxicity which is suitable for several biomedical applications. The aim of this work has been to synthesize high quality ZnO nanostructures using hydrothermal process with varied growth parameters. X-ray diffraction studies on the high quality synthesized materials confirmed the hexagonal crystal structure as well as the nano-crystallite size of ZnO. Raman spectroscopy has been done on the nanostructured ZnO to understand the different phonon modes present in the molecule. Scanning electron microscopy was used to observe shape and size of the synthesized nanomaterials. Future work to be done is to study interaction kinetics between ZnO nanostructures with biomolecules such as ATP, RNA and protein.

  5. Highly Crystalline FeCO3 Microparticle Synthesis by Hydrothermal Decomposition of Fe-EDTA Complex

    NASA Astrophysics Data System (ADS)

    Chirita, M.; Banica, R.; Ieta, A.; Bucur, A.; Sfiarloaga, P.; Ursu, D. H.; Grozescu, I.

    2010-08-01

    In this article, we present an experimental procedure to synthesize highly crystalline FeCO3 by hydrothermal decomposition of Fe(III)-EDTA complex, starting from Ferric Ammonium Sulfate and Na4EDTA main precursors in urea presence. The structure, morphology and composition of the powders were obtained using X-ray powder diffraction and scanning electron microscopy. The peaks were founded, indicate that the synthesized products autoclaved 22 h at 250 °C are pure FeCO3, which was well proved experimentally from EDAX further investigated. The size with appreciatively 100 μm was evaluated by SEM images. Magnetic characterization confirmed the magnetic characteristics of FeCO3. This procedure allowed the FeCO3 microparticles formation with good and stabile crystallographic characteristics.

  6. Hydrothermal synthesis of h-MoO3 microrods and their gas sensing properties to ethanol

    NASA Astrophysics Data System (ADS)

    Liu, Yueli; Yang, Shuang; Lu, Yu; Podval'naya, Natal'ya V.; Chen, Wen; Zakharova, Galina S.

    2015-12-01

    Hexagonal molybdenum trioxide (h-MoO3) microrods were successfully synthesized via a novel and facile hydrothermal route from peroxomolybdate solution with the presence of NH4Cl as the mineralizer. A variety of the techniques including X-ray diffraction (XRD), scanning electron microscopy (SEM), differential scanning calorimetry combined with the thermal gravimetric analysis (DSC-TG) were used to characterize the product. The gas sensing test indicates that h-MoO3 microrods have a good response to 5-500 ppm ethanol in the range of 273-380 °C, and the optimum operating temperature is 332 °C with a high sensitivity of 8.24 to 500 ppm ethanol. Moreover, it also has a good selectivity toward ethanol gas if compared with other gases, such as ammonia, methanol and toluene. The sensing mechanism of h-MoO3 microrods to ethanol was also discussed.

  7. Hydrothermal synthesis of graphene-LaFeO3 composite supported with Cu-Co nanocatalyst for higher alcohol synthesis from syngas

    NASA Astrophysics Data System (ADS)

    Niu, T.; Liu, G. L.; Chen, Y.; Yang, J.; Wu, Jiang; Cao, Y.; Liu, Y.

    2016-02-01

    The composite of graphene and a perovskite-type oxide (PTO) should be an attractive new material, owing to the special properties of graphene and the flexibility of PTO. Both graphene and PTO are promising support for some metallic nanoparticles. Therefore, in this work, taking LaFeO3 as the representative for PTO, a novel composite of graphene sheets-LaFeO3 has been prepared by using hydrothermal synthesis, and bimetallic nanoparticles of Cu-Co have been loaded on the composite. The resultant catalyst is applied to higher alcohols synthesis (HAS) from syngas. The morphology, structure and the state of the bimetallic composite catalyst are characterized by using techniques of SEM, TEM, AFM, XRD, TPR, Raman and N2 adsorption-desorption. For the graphene-LaFeO3 support, the graphene sheets are embedded into the bulk LaFeO3 or uniformly deposited on the surface of the LaFeO3 grains, resulting in high specific surface area. And the mass transferring ability of the bimetallic catalyst is optimized by uniform mixing of graphene and LaFeO3 and the formation of the mesopores. For the active component, the Cu-Co alloy nanoparticles are highly dispersed on the graphene-LaFeO3 composite, which leads to the high activity, high selectivity and excellent stability to higher alcohols.

  8. In situ ligand synthesis with the UO{sub 2}{sup 2+} cation under hydrothermal conditions

    SciTech Connect

    Frisch, Mark; Cahill, Christopher L.

    2007-09-15

    A novel uranium (VI) coordination polymer, (UO{sub 2}){sub 2}(C{sub 2}O{sub 4})(C{sub 5}H{sub 6}NO{sub 3}){sub 2} (1), has been prepared under the hydrothermal reaction of uranium nitrate hexahydrate and L-pyroglutamic acid. Compound 1 (monoclinic, C2/c, a=22.541(6) A, b=5.7428(15) A, c=15.815(4) A, {beta}=119.112(4){sup o}, Z=4, R{sub 1}=0.0237, wR{sub 2}=0.0367) consists of uranium pentagonal bipyramids linked via L-pyroglutamate and oxalate anions to form an overall two-dimensional (2D) structure. With the absence of oxalic acid within the starting materials, the oxalate anions are hypothesized to form in situ whereby decarboxylation of L-pyroglutamic acid occurs followed by coupling of CO{sub 2} to form the oxalate linkages as observed in the crystal structure. Addition of copper (II) to this system appears to promote oxalate formation in that synthetic moolooite (Cu(C{sub 2}O{sub 4}).nH{sub 2}O; 0{<=}n{<=}1) and a known uranyl oxalate [(UO{sub 2}){sub 2}(C{sub 2}O{sub 4})(OH){sub 2}(H{sub 2}O){sub 2}.H{sub 2}O], co-crystallize in significant quantity. Compound 1 exhibits the characteristic uranyl emission spectrum upon either direct uranyl excitation or ligand excitation, the latter of which shows an increase in relative intensity. This subsequent increase in the intensity indicates an energy transfer from the ligand to the uranyl cations thus illustrating an example of the antenna effect in the solid state. - Graphical abstract: A novel homometallic coordination polymer (UO{sub 2}){sub 2}(C{sub 2}O{sub 4})(C{sub 5}H{sub 6}NO{sub 3}){sub 2}, in the uranium-L-pyroglutamic acid system has been synthesized under hydrothermal conditions. The title compound consists of uranium pentagonal bipyramids bridged through both L-pyroglutamate and oxalate linkages to produce a 3D crystal structure. The oxalate anions are theorized to result from decarboxylation of L-pyroglutamic acid followed by subsequent coupling of CO{sub 2}.

  9. Hydrothermal synthesis and characteristics of anions-doped calcium molybdate red powder phosphors

    SciTech Connect

    Shi, Shikao; Zhang, Yan; Liu, Qing; Zhou, Ji

    2013-10-15

    Graphical abstract: - Highlights: • Four anion-doped CaMoO{sub 4}:Eu{sup 3+} red phosphors were prepared by hydrothermal approach. • Some samples exhibit nearly spherical morphology and well-distributed fine particles. • The red luminescence can be obviously enhanced after certain amount of anion doping. • The improved phosphor system is a potential candidate for white LED applications. - Abstract: Applying hydrothermal and subsequent heat-treatment process, CaMoO{sub 4}:Eu{sup 3+} was doped with four anions (SiO{sub 3}{sup 2−}, PO{sub 4}{sup 3−}, SO{sub 4}{sup 2−} and ClO{sub 3}{sup −}) to prepare fine red powder phosphors. The introduction of small amount of anions into the host had little influence on the structure, which was confirmed by X-ray diffraction patterns. The anion-doped phosphor samples (except SiO{sub 3}{sup 2−}) exhibited nearly spherical morphology, and the particle sizes were in the range of 0.3–0.4 μm for SO{sub 4}{sup 2−}-doped samples, and 0.8–1.2 μm for PO{sub 4}{sup 3−} and ClO{sub 3}{sup −}-doped samples. Excited with 395 nm near-UV light, all samples showed typical Eu{sup 3+} red emission at 615 nm, and PO{sub 4}{sup 3−}, SO{sub 4}{sup 2−} and ClO{sub 3}{sup −}-doped samples enhanced the red luminescence as compared with the individual CaMoO{sub 4}:Eu{sup 3+} sample. In particular, relative emission intensity for optimum ClO{sub 3}{sup −}-doped phosphors reached more than 6-fold that of the commercial red phosphor, which is highly desirable for the powder phosphors used in the solid-state lighting industry.

  10. Synthesis of N-acetyl-L-cysteine-capped ZnCdSe quantum dots via hydrothermal method and their characterization

    PubMed Central

    Gao, Fang; Liu, Yuying; Fan, Yao; Zhao, Dan

    2014-01-01

    Compared with the most studied green-red emitting (530–650 nm) quantum dots (QDs), the preparation of short-wavelength-emitting QDs remains difficult. Besides, one of the representative short-wavelength QDs materials, ZnCdSe, has a shortcoming of high content of toxic cadmium metal. In this paper, we report the synthesis of high-quality water-soluble ZnCdSe QDs via optimized one-step hydrothermal method with a new thiol as ligand, within a short time of 65 min. The emission wavelength of prepared QDs is tunable in the range of 425–540 nm by merely controlling the molar ratio of Cd:Zn or Se:Zn, and the quantum yield reaches 35%. More importantly, the maximum Cd:Zn molar ratio has been reduced to 0.04:1.0, much lower than that reported in the literature (0.5:1.0), resulting in excellent biological compatibility of prepared QDs and thus their promising applications in biological fields. Moreover, the transmission electron microscopy was employed to examine the effect of Cd:Zn ratio on the size of prepared ZnCdSe QDs, which were also characterized by x-ray photoelectron spectroscopy and electron diffraction spectroscopy. PMID:27877713

  11. Microwave Treated Rapid Hydrothermal Synthesis Of Zno Nano-Flakes Array: The Effect Of Citric Acid As Capping Agent

    NASA Astrophysics Data System (ADS)

    Gopal Ram, S. D.; Ravi, G.; Kulandainathan, M. Anbu

    2010-10-01

    Microwave assisted hydrothermal synthesis of ZnO nanostructures with improved surface area by the addition of Citric Acid (CA) as a metal capping agent is reported. Citric acid is added to the mother precursor in three different concentrations for the preparation of ZnO nanostructure. The influence of the citric acid as a capping agent has been studied both in the preparation of ZnO nanopowders and in the ordered array formation on the precoated ZnO seed layer over glass substrates. The addition of this capping agent has shown up clearly in the morphology of the nanostructures. The X-ray diffraction patterns has shown a diminished crystallinity and a increased full width half maximum (FWHM) in the preferred oriented diffraction peak. The peak broadening is an indication of the reduced crystallite size. This cause of the inhibition in growth is realized to be the effect of capping action of citric acid. The optical property of the ZnO nanostructure was characterized by UV-vis-NIR spectroscopy.

  12. Sustainable Hydrothermal Carbonization Synthesis of Iron/Nitrogen-Doped Carbon Nanofiber Aerogels as Electrocatalysts for Oxygen Reduction.

    PubMed

    Song, Lu-Ting; Wu, Zhen-Yu; Zhou, Fei; Liang, Hai-Wei; Yu, Zi-You; Yu, Shu-Hong

    2016-12-01

    It is urgent to develop new kinds of low-cost and high-performance nonprecious metal (NPM) catalysts as alternatives to Pt-based catalysts for oxygen reduction reaction (ORR) in fuel cells and metal-air batteries, which have been proved to be efficient to meet the challenge of increase of global energy demand and CO2 emissions. Here, an economical and sustainable method is developed for the synthesis of Fe, N codoped carbon nanofibers (Fe-N/CNFs) aerogels as efficient NPM catalysts for ORR via a mild template-directed hydrothermal carbonization (HTC) process, where cost-effective biomass-derived d(+)-glucosamine hydrochloride and ferrous gluconate are used as precursors and recyclable ultrathin tellurium nanowires are used as templates. The prepared Fe/N-CNFs catalysts display outstanding ORR activity, i.e., onset potential of 0.88 V and half-wave potential of 0.78 V versus reversible hydrogen electrode in an alkaline medium, which is highly comparable to that of commercial Pt/C (20 wt% Pt) catalyst. Furthermore, the Fe/N-CNFs catalysts exhibit superior long-term stability and better tolerance to the methanol crossover effect than the Pt/C catalyst in both alkaline and acidic electrolytes. This work suggests the great promise of developing new families of NPM ORR catalysts by the economical and sustainable HTC process.

  13. Inspired by efficient cellulose-dissolving system: Facile one-pot synthesis of biomass-based hydrothermal magnetic carbonaceous materials.

    PubMed

    Ma, Jian-Feng; Xing, Jian-Xiong; Wang, Kun; Yang, Hai-Yan; Fei, Ben-Hua; Liu, Xing-E

    2017-05-15

    The core-shell structure of carbon encapsulated magnetic nanoparticles (CEMNs) displays unique properties. Enhancing the magnetization of iron core, in parallel, improving the encapsulation of carbon shell are the two major challenges in the synthesis of CEMNs. Inspired by efficient cellulose-dissolving system, carbon encapsulated magnetic nano-Fe3O4 particles (Fe3O4@C) with ∼10.0nm Fe3O4 cores and 1.9-3.3nm carbon shell, were successfully one-pot synthesized via a novel hydrothermal carbonization (HTC) process. The dissolving process in ionic liquids ([Emim]Ac and [Amim]Cl) completely cleaved the intra- and intermolecular H-bonds in cellulose, and favored the incorporation of Fe3O4 nanoparticles into the cellulose H-bonds systems during the regeneration process. Some stable linkages were formed in Fe3O4@C, taking Fe3O4 nanoparticles as a structure guiding agent. The morphology and properties of Fe3O4@C depended strongly on the type of carbon precursors and pyrolysis temperature. Well encapsulated nanostructure was obtained at HTC temperature 280°C, when [Emim]Ac-treated holocellulose was used as the carbon source. Meanwhile, the thickness of the amorphous shell and magnetization increased with HTC temperature. More importantly, a novel elements for understanding the growth mechanism for the Fe3O4@C composite under HTC conditions was proposed.

  14. A simple hydrothermal method for the large-scale synthesis of single-crystal potassium tungsten bronze nanowires.

    PubMed

    Gu, Zhanjun; Ma, Ying; Zhai, Tianyou; Gao, Bifen; Yang, Wensheng; Yao, Jiannian

    2006-10-10

    The large-scale synthesis of single-crystal K(x)WO(3) tungsten bronze nanowires has been successfully realized by a hydrothermal method under mild conditions. Uniform K(0.33)WO(3) nanowires with diameters of 5-25 nm and lengths of up to several micrometers are obtained. It is found that the morphology and crystallographic forms of the final products are strongly dependent on the sulfate and citric acid, which may act as structure-directing and soft-reducing agent, respectively. Some other influential factors on the growth of tungsten bronze nanowires, such as temperature and reaction time, are also discussed. It is worth noting that other alkali metal tungsten bronzes such as (NH(4))(x)WO(3), Rb(x)WO(3), and Cs(x)WO(3) could also be selectively synthesized by a similar route. Thus, this novel and efficient method could provide a potential mild route to selectively synthesize various tungsten bronze on-dimensional nanomaterials.

  15. Hydrothermal Synthesis of Silver Vanadium Oxide (Ag0.35V2O5) Nanobelts for Sensing Amines

    NASA Astrophysics Data System (ADS)

    Fu, Haitao; Xie, Hui; Yang, Xiaohong; An, Xizhong; Jiang, Xuchuan; Yu, Aibing

    2015-10-01

    A simple hydrothermal method for the synthesis of Ag0.35V2O5 nanobelts with the assistance of sodium dodecyl sulfate (SDS) is reported in this study. The experimental variables that may affect the nanoparticle structures were investigated. And several advanced techniques, such as TEM, HRTEM, X-ray diffraction (XRD), were used to characterize the morphology and composition of the as-prepared nanobelts. The mechanism of the formation and growth of Ag0.35V2O5 nanobelts was also investigated and discussed. The results show that SDS, as a weak reducing agent, plays a crucial role in the formation of Ag0.35V2O5. According to N2 sorption isothermals, the as-prepared Ag0.35V2O5 nanobelts are found to exhibit relative high surface area. The gas sensing performance of the Ag0.35V2O5 nanobelts towards organic amine was tested. It is found that the nanobelts show superior sensitivity of amine(s) to V2O5 particles, lower detection limit (5 ppm), and higher selectivity of amine versus ammonia at an optimized working temperature of ~260 °C. Moreover, the density functional theory (DFT) simulation was conducted to better understand the sensing mechanism. These findings may be useful in designing promising materials to detect amine gases for medical or food industrial applications.

  16. Synthesis of nanocrystalline barium-hexaferrite from nanocrystalline goethite using the hydrothermal method: Particle size evolution and magnetic properties

    SciTech Connect

    Penn, R.L.; Banfield, J.F.; Voigt, J.

    1997-03-01

    To characterize particle size/magnetic property relationships, 9 to 50 nm in diameter barium hexaferrite, BaFe{sub 12}O{sub 19} (BHF), particles were prepared using a new synthesis route. By replacing the conventional 50 to 100 nm particles of goethite with nanocrystalline goethite produced via the microwave anneal method of Knight and Sylva, nanocrystalline BHF was synthesized using the hydrothermal method. Evolution of particle size and morphology with respect to concentration and heat treatment time is reported. Hysteresis properties, including coercivity (0.2--1.0 kOe), magnetization saturation (0.1--33.4 emu/g), and magnetization remanence (0.004--22.5 emu/g) are discussed as a function of particle size. The magnetization saturation and remanence of the 7 nm particles is nearly zero, suggesting the superparamagnetic threshold size for BHF is around this size. In addition, the equilibrium morphology of BHF crystals was calculated to be truncated hexagonal prisms which was verified by experiment, and the isoelectric point, pH of 4.1, was measured for 18 nm BHF particles.

  17. Synthesis of nanocrystalline barium-hexaferrite from nanocrystalline goethite using the hydrothermal method: Particle size evolution and magnetic properties

    SciTech Connect

    Penn, R.L.; Banfield, J.F.; Voigt, J.

    1997-08-01

    To characterize particle size/magnetic property relationships, 9 to 50 nm in diameter barium hexaferrite, BaFe{sub 12}O{sub 19} (BHF), particles were prepared using a new synthesis route. By replacing the conventional 50 to 100 nm particles of goethite with nanocrystalline goethite produced via the microwave anneal method of Knight and Sylva, nanocrystalline BHF was synthesized using the hydrothermal method. Evolution of particle size and morphology with respect to concentration and heat treatment time is reported. Hysteresis properties, including coercivity (0.2--1.0 kOe), magnetization saturation (0.1--33.4 emu/g), and magnetization remanence (0.004--22.5 emu/g) are discussed as a function of particle size. The magnetization saturation and remanence of the 7 nm particles is nearly zero, suggesting the superparamagnetic threshold size for BHF is around this size. In addition, the equilibrium morphology of BHF crystals was calculated to be truncated hexagonal prisms which was verified by experiment, and the isoelectric point, pH of 4.1 was measured for 18 nm BHF particles.

  18. One-step synthesis of titanium oxide nanocrystal- rutile by hydrothermal method

    NASA Astrophysics Data System (ADS)

    Yan, Evyan Yang Chia; Zakaria, Sarani; Chia, Chin Hua

    2014-09-01

    Pure rutile phase titanium oxides (TiO2) nanocrystals were synthesized via hydrothermal method with titanium tetrachloride (TiCl4) and water (H2O) treated in an autoclave. The particle size and phase assemblages were characterized using Scanning electron microscopy (SEM) and X-ray diffraction (XRD) respectively. Band gap energy (Eg) of the nanocrystals was estimated from the Ultra violet - visible light (UV-vis) absorption spectra. It was demonstrated that TiO2 nanocrystals can be prepared through increasing of temperature and period of treatment. It is believed that the presence of acid chloride (HCl) as by-product during the hydrolysis played an important role in controlling the growth of morphology and crystal structures. The Eg of the samples were estimated from the plot of modified Kubelka-Munk function were in the range of 3.04 - 3.26eV for the samples synthesized at temperature ranging from 50 to 200°C for 16 hours.

  19. Hydrothermal synthesis of zinc oxide nanoparticles using rice as soft biotemplate

    PubMed Central

    2013-01-01

    Background Rice as a renewable, abundant bio-resource with unique characteristics can be used as a bio-template to synthesize various functional nanomaterials. Therefore, the effect of uncooked rice flour as bio-template on physico-chemical properties, especially the morphology of zinc oxide nanostructures was investigated in this study. The ZnO particles were synthesized through hydrothermal-biotemplate method using zinc acetate-sodium hydroxide and uncooked rice flour at various ratios as precursors at 120°C for 18 hours. Results The results indicate that rice as a bio-template can be used to modify the shape and size of zinc oxide particles. Different morphologies, namely flake-, flower-, rose-, star- and rod-like structures were obtained with particle size at micro- and nanometer range. Pore size and texture of the resulting zinc oxide particles were found to be template-dependent and the resulting specific surface area enhanced compared to the zinc oxide synthesized without rice under the same conditions. However, optical property particularly the band gap energy is generally quite similar. Conclusion Pure zinc oxide crystals were successfully synthesized using rice flour as biotemplate at various ratios of zinc salt to rice. The size- and shape-controlled capability of rice to assemble the ZnO particles can be employed for further useful practical applications. PMID:23919386

  20. Hydrothermal synthesis and structural characterization of ammonium ion-templated lanthanide(III) carboxylate-phosphonates

    PubMed Central

    Ayi, Ayi A.; Kinnibrugh, Tiffany L.; Clearfield, Abraham

    2014-01-01

    Using N-(phosphonomethyl) iminodiacetic acid (H4PMIDA), as a complexing agent, two new complexes, (NH4)La(PMIDA)(H2O)•H2O, 1 and (NH4)Yb(PMIDA), 2 have been synthesized hydrothermally. In both compounds, the metal ions are trapped by a three five-membered chelate rings by the chelating PMIDA anions giving a tricapped trigonal prismatic LaO8N and monocapped trigonal prismatic YbO6N geometries for 1 and 2, respectively. The structure of 1 consists of La(PMIDA)(H2O) chelating units, linked together by the phosphonate oxygen atoms O1 and O3 to form a chain along the c-axis. The chains are then connected together by the bridging phosphonate oxygen O2 to form a 2D layered structure with alternating 4- and 8-membered apertures. The structure of 2 consists Yb(PMIDA) chelating units, which are connected by alternating bridging carboxylate and phosphonate groups along the [010] direction forming chains with a corrugated pattern. The third phosphonate oxygen bridges the chains together along the [001] direction to build the two-dimensional layer with 4- and 6-membered apertures in the bc-plane. Under excitation of 330 nm, compound 2 shows a broad emission band at λmax = 460 nm. This emission is essentially in the blue luminescent region, which corresponds to ligand centered fluorescence. PMID:25414845

  1. Synthesis and Enhanced Photocatalytic Activity of Ce-Doped Zinc Oxide Nanorods by Hydrothermal Method

    NASA Astrophysics Data System (ADS)

    Aisah, N.; Gustiono, D.; Fauzia, V.; Sugihartono, I.; Nuryadi, R.

    2017-02-01

    Zinc oxide (ZnO) is a n-type semiconductor material which has a wide direct band gap energy of ∼ 3.3 eV, and other interesting optical properties, hence it’s potentially applied to various fields such as electronics, optoelectronics, sensors, photonic devices, and also photocatalyst. Dopant in ZnO nanostructures is an effective way to improve ZnO’s structural properties in various applications. In this study, undoped and Ce doped ZnO nanorods were synthesized on ITO coated glass substrates by ultrasonic spray pyrolysis for seeding deposition and hydrothermal methods at a temperature of 95 0C for 2 hours for growth. X-ray diffraction, field emission scanning electron microscopy (FESEM), UV-VIS and Photoluminescence spectroscopy were used to characterize the crystal structure, surface morphology and optical properties of ZnO nanorods and the photocatalytic activity test for methylene blue degradation. The experimental results showed that 3% Cerium dopant has produced hexagonal morphology ZnO nanorod growing more uniform on (002) crystal planes, increased the intensity of ultraviolet absorbance thereby increase the degradation speed of methylene blue.

  2. Controllable synthesis of hydroxyapatite nanocrystals via a dendrimer-assisted hydrothermal process

    SciTech Connect

    Zhou Zhuohua; Zhou, Ping-Le; Yang Shiping . E-mail: shipingy@shnu.edu.cn; Yu Xibin; Yang Liangzhun

    2007-09-04

    The morphology and size of hydroxyapatite Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2} (denoted HAP) can be controlled under hydrothermal treatment assisted with different dendrimers, such as carboxylic terminated poly(amidoamine) (PAMAM) and polyhydroxy terminated PAMAM. The structure and morphology were characterized by X-ray diffraction (XRD), infrared spectroscopy (IR) and transmission electron microscopy (TEM). IR spectra were also used to investigate the complexation of Ca{sup 2+} with PAMAM. The results revealed that the inner cores of the PAMAM dendrimers are hydrophilic and potentially open to calcium ions, since interior nitrogen moieties serve as complexation sites, especially in case of the polyhydroxy terminated PAMAM. And the reasonable mechanism of crystallization was proposed that it can be attributed to the localization of nucleation site: external or interior PAMAM. Additionally, the PAMAM dendrimer with carboxylic and polyhydroxy groups has an effective influence on the size and shape of hydroxyapatite (HAP) nanostructures. Different crystal morphology was accomplished by adsorption of different dendrimers onto specific faces of growing crystals, altering the relative growth rates of the different crystallographic faces and leading to different crystal habits.

  3. Hydrothermal synthesis, structure, and magnetic properties of Pu(SeO3)2

    SciTech Connect

    Bray, Travis H; Skanthakumar, S; Soderholm, L.; Sykora, Richard E.; Haire, Richard G.; Albrecht-Schmitt, Thomas E.

    2007-01-01

    The reaction between PuO2 and SeO2 under mild hydrothermal conditions results in the formation of Pu(SeO3)2 as brick-red prisms. This compound adopts the Ce(SeO3)2 structure type, and consists of one-dimensional chains of edge-sharing [PuO8] distorted bicapped trigonal prisms linked by [SeO3] units into a three-dimensional network. Crystallographic data: Pu(SeO3)2, monoclinic, space group P21/n, a 6.960(1) A , b 10.547(2) A , c 7.245(1) A , b 106.880(9)1, V 508.98(17) A 3, Z 4 (T 193 K), R(F) 2.92% for 83 parameters with 1140 re ections with I42s(I). Magnetic susceptibility data for Pu(SeO3)2 are linear from 35 to 320 K and yield an effective moment of 2.71(5) mB and a Weiss constant of -500(5) K.

  4. Hydrothermal synthesis and structural characterization of three inorganic organic composite sandwich-type phosphotungstates

    NASA Astrophysics Data System (ADS)

    Zhao, Jun-Wei; Zheng, Shou-Tian; Yang, Guo-Yu

    2007-12-01

    Three inorganic-organic composite sandwich-type phosphotungstates [Ni(tepa)(H 2O)] 4H 2[Ni 4(H 2O) 2( α- B-PW 9O 34) 2]·8H 2O ( 1), (enH 2) 3[Ni 2(H 2O) 10][Ni 4(H 2O) 2( α- B-PW 9O 34) 2]·en·8H 2O ( 2) and (enH 2) 10[Mn 4(H 2O) 2( α- B-PW 9O 34) 2] 2·20H 2O ( 3) (tepa=tetraethylenepentamine and en=ethylenediamine) have been synthesized by the hydrothermal reaction of the trivacant Keggin polyoxoanion [ α- A-PW 9O 34] 9- with Ni 2+ or Mn 2+ ions in the presence of tepa or en and structurally characterized by IR spectra, elemental analysis, thermogravimetric analysis and variable temperature magnetic susceptibility. X-ray crystallographic analyses indicate that they all contain the classical tetra- M sandwiched polyoxoanions [ M4(H 2O) 2( α- B-PW 9O 34) 2] 10- ( M=Ni 2+ or Mn 2+) and nickel-organoamine cations or organoamine cations work as the charge balance ions. The tetra- M clusters in 1, 2 and 3 exhibit the familiar structural type of a β-junction at the sites of metal incorporation. The study of magnetic property of 1 is indicative of a typical ferromagnetic coupling between Ni 2+ cations.

  5. Hydrothermal synthesis and characterization of titanium dioxide nanotubes as novel lithium adsorbents

    SciTech Connect

    Moazeni, Maryam; Hajipour, Hengameh; Askari, Masoud; Nusheh, Mohammad

    2015-01-15

    The ion exchange process is a promising method for lithium extraction from brine and seawater having low concentrations of this element. To achieve this goal, it is vital to use an effective adsorbent with maximum lithium adsorption potential together with a stable structure during extraction and insertion of the ions. In this study, titanium dioxide and then lithium titanate spinel with nanotube morphology was synthesized via a simple two-step hydrothermal process. The produced Li{sub 4}Ti{sub 5}O{sub 12} spinel ternary oxide nanotube with about 70 nm diameter was then treated with dilute acidic solution in order to prepare an adsorbent suitable for lithium adsorption from local brine. Morphological and phase analysis of the obtained nanostructured samples were done by using transmission and scanning electron microscopes along with X-ray diffraction. Lithium ion exchange capacity of this adsorbent was finally evaluated by means of adsorption isotherm. The results showed titanium dioxide adsorbent could recover 39.43 mg/g of the lithium present in 120 mg/L of lithium solution.

  6. Novel rapid synthesis of zinc oxide nanotubes via hydrothermal technique and antibacterial properties.

    PubMed

    Aal, Nadia Abdel; Al-Hazmi, Faten; Al-Ghamdi, Ahmed A; Al-Ghamdi, Attieh A; El-Tantawy, Farid; Yakuphanoglu, F

    2015-01-25

    ZnO nanotubes with the wurtzite structure have been successfully synthesized via simple hydrothermal solution route using zinc nitrate, urea and KOH for the first time. The structural, compositions and morphology architectures of the as synthesized ZnO nanotubes was performed using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS) and high resolution transmission scanning electron microscopy (HRTEM). TEM showed that ZnO nanotubes exhibited a wall thickness of less than 2 nm, with an average diameter of 17 nm and the length is 2 μm. In addition, the antibacterial activity of ZnO nanotubes was carried out in vitro against two kinds of bacteria: gram - negative bacteria (G -ve) i.e. Escherichia coli (E. coli) and gram - positive bacteria (G +ve) i.e. Staphylococcus aureus. Therefore, this work demonstrates that simply synthesized ZnO nanotubes have excellent potencies, being ideal antibacterial agents for many biomedical applications.

  7. Hydrothermal synthesis of platinum-group-metal nanoparticles by using HEPES as a reductant and stabilizer.

    PubMed

    So, Man-Ho; Ho, Chi-Ming; Chen, Rong; Che, Chi-Ming

    2010-06-01

    Platinum-group-metal (Ru, Os, Rh, Ir, Pd and Pt) nanoparticles are synthesized in an aqueous buffer solution of 4-(2-hydroxyethyl)-1-piperazineethanesulfonic acid (HEPES) (200 mM, pH 7.4) under hydrothermal conditions (180 degrees C). Monodispersed (monodispersity: 11-15%) metal nanoparticles were obtained with an average particle size of less than 5 nm (Ru: 1.8+/-0.2, Os: 1.6+/-0.2, Rh: 4.5+/-0.5, Ir: 2.0+/-0.3, Pd: 3.8+/-0.4, Pt: 1.9+/-0.2 nm). The size, monodispersity, and stability of the as-obtained metal nanoparticles were affected by the HEPES concentration, pH of the HEPES buffer solution, and reaction temperature. HEPES with two tertiary amines (piperazine groups) and terminal hydroxyl groups can act as a reductant and stabilizer. The HEPES molecules can bind to the surface of metal nanoparticles to prevent metal nanoparticles from aggregation. These platinum-group-metal nanoparticles could be deposited onto the surface of graphite, which catalyzed the aerobic oxidation of alcohols to aldehydes.

  8. Microwave-Assisted Hydrothermal Rapid Synthesis of Calcium Phosphates: Structural Control and Application in Protein Adsorption

    PubMed Central

    Cai, Zhu-Yun; Peng, Fan; Zi, Yun-Peng; Chen, Feng; Qian, Qi-Rong

    2015-01-01

    Synthetic calcium phosphate (CaP)-based materials have attracted much attention in the biomedical field. In this study, we have investigated the effect of pH values on CaP nanostructures prepared using a microwave-assisted hydrothermal method. The hierarchical nanosheet-assembled hydroxyapatite (HAP) nanostructure was prepared under weak acidic conditions (pH 5), while the HAP nanorod was prepared under neutral (pH 7) and weak alkali (pH 9) condition. However, when the pH value increases to 11, a mixed product of HAP nanorod and tri-calcium phosphate nanoparticle was obtained. The results indicated that the pH value of the initial reaction solution played an important role in the phase and structure of the CaP. Furthermore, the protein adsorption and release performance of the as-prepared CaP nanostructures were investigated by using hemoglobin (Hb) as a model protein. The sample that was prepared at pH = 11 and consisted of mixed morphologies of nanorods and nanoprisms showed a higher Hb protein adsorption capacity than the sample prepared at pH 5, which could be explained by its smaller size and dispersed structure. The results revealed the relatively high protein adsorption capacity of the as-prepared CaP nanostructures, which show promise for applications in various biomedical fields such as drug delivery and protein adsorption.

  9. Hydrothermal synthesis, phase structure, optical and photocatalytic properties of Zn2SnO4 nanoparticles.

    PubMed

    Ben Ali, Monaam; Barka-Bouaifel, Fatiha; Elhouichet, Habib; Sieber, Brigitte; Addad, Ahmed; Boussekey, Luc; Férid, Mokhtar; Boukherroub, Rabah

    2015-11-01

    Zinc stannate (Zn2SnO4 or ZTO) nanoparticles were synthesized via hydrothermal method using NaOH as a mineralizer. X-ray diffraction (XRD), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM) of the synthesized ZTO nanoparticles revealed the formation of highly pure ZTO phase with the spinel-like structure. The nanoparticles have spherical shape with an average size of about 25 nm. The Raman spectrum of the sample was dominated by the A(1g) vibration mode of pure ZTO phase. From UV-Vis measurement, a band gap E(g) of 3.465 eV was determined. The photocatalytic activity of the ZTO nanoparticles was evaluated for the photodegradation of rhodamine B (RhB) under visible light irradiation. The influence of catalyst concentration and irradiation time on the photocatalytic process was investigated. The ZTO catalyst showed the best photocatalytic performance at a concentration of 0.2 g/L, and the photodecomposition of RhB followed first-order kinetics with a rate constant k=0.0249 min(-1). The ZTO-assisted photocatalytic degradation of RhB occurred via two competitive processes: a photocatalytic process and a photosensitized process. The detection of hydroxyl radicals by fluorescence measurements suggests that these species play an important role in the photocatalytic process.

  10. Synthesis and Characterization of Nanostructure Transition Metal Oxides Extracted from Industrial Waste (EOFD) by Hydrothermal Method

    NASA Astrophysics Data System (ADS)

    Girisun, T. C. Sabari; Babeela, C.; Vidhya, V.

    2011-10-01

    Electric oil furnace dust (EOFD) is a solid waste generated in the collection of particulate material during steelmaking process in electric and oil furnaces. Over 7 million metric tons dust produced per annum in worldwide creates deep impacts like soil, ground water and ecology pollutions. This article reports the simple one step process for the extraction of nanostructured metal oxides from the industrial waste (EOFD) for the realization of low cost solar applications. By hydrothermal technique valuable metals were obtained in the form of metal oxides. Initially the presence of metals was identified by ICP analysis. XRD analysis confirms the formation of nano structured titanium oxide (TiO) along with traces of iron oxide (Fe2O3). The surface morphology and the particle size were analyzed by SEM analysis. Thus the metal oxides derived could be helpful to reduce the burden on the environment, increase the development of the source nano material and reduce the cost of raw materials for solar cell applications.

  11. One-step synthesis of titanium oxide nanocrystal- rutile by hydrothermal method

    SciTech Connect

    Yan, Evyan Yang Chia; Zakaria, Sarani; Chia, Chin Hua

    2014-09-03

    Pure rutile phase titanium oxides (TiO{sub 2}) nanocrystals were synthesized via hydrothermal method with titanium tetrachloride (TiCl{sub 4}) and water (H{sub 2}O) treated in an autoclave. The particle size and phase assemblages were characterized using Scanning electron microscopy (SEM) and X-ray diffraction (XRD) respectively. Band gap energy (E{sub g}) of the nanocrystals was estimated from the Ultra violet – visible light (UV-vis) absorption spectra. It was demonstrated that TiO{sub 2} nanocrystals can be prepared through increasing of temperature and period of treatment. It is believed that the presence of acid chloride (HCl) as by-product during the hydrolysis played an important role in controlling the growth of morphology and crystal structures. The E{sub g} of the samples were estimated from the plot of modified Kubelka-Munk function were in the range of 3.04 – 3.26eV for the samples synthesized at temperature ranging from 50 to 200°C for 16 hours.

  12. Lanthanum cerate (La2Ce2O7): hydrothermal synthesis, characterization and optical properties

    NASA Astrophysics Data System (ADS)

    Khademinia, Shahin; Behzad, Mahdi

    2015-03-01

    La2Ce2O7 nano-powders were synthesized via a hydrothermal reaction in a deionized water (S 1) and in a 2 M NaOH aqueous solution (S 2) at 180 °C for 48 h. La(NO3)3·H2O and (NH4)2Ce(NO3)6 were used in the stoichiometric 1:1 La:Ce molar ratio as raw materials. The obtained materials were crystallized in a cubic crystal structure with space group. The synthesized materials were characterized by powder X-ray diffraction technique and Fourier-transform infrared spectroscopy. To investigate the effect of the basic solution on the morphology of the obtained materials, the morphologies of the synthesized materials were studied by field emission scanning electron microscopy technique. The technique showed that the morphology of La2Ce2O7 samples changed from grain to rod-like structure in presence of the basic solution. Cell parameter refinements showed that these parameters were larger for S2 than those for S 1. Photoluminescence and ultraviolet visible spectra of the synthesized nanomaterials were also investigated.

  13. Controllable synthesis of ultrathin vanadium oxide nanobelts via an EDTA-mediated hydrothermal process

    NASA Astrophysics Data System (ADS)

    Yu-Xiang, Qin; Cheng, Liu; Wei-Wei, Xie; Meng-Yang, Cui

    2016-02-01

    Ultrathin VO2 nanobelts with rough alignment features are prepared on the induction layer-coated substrates by an ethylenediaminetetraacetic acid (EDTA)-mediated hydrothermal process. EDTA acts as a chelating reagent and capping agent to facilitate the one-dimensional (1D) preferential growth of ultrathin VO2 nanobelts with high crystallinities and good uniformities. The annealed induction layer and concentration of EDTA are found to play crucial roles in the formation of aligned and ultrathin nanobelts. Variation in EDTA concentration can change the VO2 morphology of ultrathin nanobelts into that of thick nanoplates. Mild annealing of ultrathin VO2 nanobelts at 350 °C in air results in the formation of V2O5 nanobelts with a nearly unchanged ultrathin structure. The nucleation and growth mechanism involved in the formations of nanobelts and nanoplates are proposed. The ethanol gas sensing properties of the V2O5 nanobelt networks-based sensor are investigated in a temperature range from 100 °C to 300 °C over ethanol concentrations ranging from 3 ppm to 500 ppm. The results indicate that the V2O5 nanobelt network sensor exhibits high sensitivity, good reversibility, and fast response-recovery characteristics with an optimal working temperature of 250 °C. Project supported by the National Natural Science Foundation of China (Grant Nos. 61274074, 61271070, and 61574100).

  14. Synthesis and photocatalysis properties of ZnO structures with different morphologies via hydrothermal method

    NASA Astrophysics Data System (ADS)

    Xie, Juan; Wang, Hu; Duan, Ming; Zhang, Liehui

    2011-05-01

    The special flower-like and sheet-like ZnO structures were successfully synthesized by hydrothermal method. The samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and energy dispersive spectroscopy (EDS). The photocatalytic activity of different morphologies of ZnO structures was evaluated by degradating of methyl orange (MO). The photocatalytic degradation process was monitored in terms of decolorization and total organic carbon (TOC) removals. The results indicated that the flower-like ZnO structures were consisted of numerous flower-like aggregates with the size of 2 μm. The sheet-like ZnO nanostructures were obtained by increasing the reaction time. They exhibited higher photodegradation efficiencies under UV light irradiation than flower-like ZnO structures due to the blue shift of the band gap. The photodegradation could be described as the pseudo-first-order kinetics with apparent rate constants ranging from 1.17 × 10 -2 to 3.42 × 10 -2 min -1, which were based on the morphology of the structures. The photodegradation was faster than the mineralization, indicating that the accumulation of by-products were resistant to photocatalytic degradation.

  15. Metastable monoclinic ZnMoO4: hydrothermal synthesis, optical properties and photocatalytic performance.

    PubMed

    Lv, Li; Tong, Wenming; Zhang, Yanbing; Su, Yiguo; Wang, Xiaojing

    2011-11-01

    Metastable monoclinic ZnMoO4 was successfully synthesized via a hydrothermal route with variation of reaction temperatures and time at pH value of 5.7. Systematic sample characterizations were carried out, including X-ray powder diffraction, scanning electron microscopy, Fourier transformed infrared spectra, UV-visible diffuse reflectance spectra, and photoluminescence spectra. The results show that all as-prepared ZnMoO4 samples were demonstrated to crystallize in a pure-phase of monoclinic wolframite structure. All samples were formed in plate-like morphology. Six IR active vibrational bands were observed in the wave number range of 400-900 cm(-1). The band gap of as-prepared ZnMoO4 was estimated to be 2.86 eV by Tauc equation. Photoluminescence measurement indicates that as-prepared ZnMoO4 exhibits a broad blue-green emission under excitation wavelength of 280 nm at room temperature. Photocatalytic activity of as-prepared ZnMoO4 was examined by monitoring the degradation of methyl orange dye in an aqueous solution under UV radiation of 365 nm. The as-prepared ZnMoO4 obtained at 180 degrees C for 40 h showed the best photocatalytic activity with completing degradation of MO in irradiation time of 120 min. Consequently, monoclinic ZnMoO4 proved to be an efficient near visible light photocatalyst.

  16. A hydrothermal synthesis of Pr3+ doped mesoporous TiO2 for UV light photocatalysis.

    PubMed

    Wang, Yong; Chen, Guihua; Shen, Qianhong; Yang, Hui; Li, Liquan; Song, Yanjiang

    2014-07-01

    Pr3+ doped mesoporous TiO2 photocatalysts with a different molar ratio of Pr to Ti were prepared by a hydrothermal method using triblock copolymer as the template. The as-prepared samples were systematically characterized by X-ray diffraction, N2 adsorption-desorption, X-ray photoelectron spectra, transmission electron microscopy and UV-visible diffuse reflectance spectroscopy. The characterizations indicated all the samples had mesoporous structure and narrow pore size distribution. Pr3+ doping enlarged the surface area and decreased the crystallite size. The surface area of the samples varied from 136 to 170 m2/g, and the average crystallite size ranged between 5.04 and 7.60 nm. The effect of Pr3+ doping amount on the photocatalytic activity of mesoporous TiO2 was evaluated by the degradation of methyl orange under UV light irradiation. The results showed that the suitable amount of Pr3+ doped samples exhibited the higher photocatalytic activity than mesoporous TiO2. Among the samples, 1 at.% Pr3+ doped mesoporous TiO2 showed the highest photocatalytic activity.

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

    PubMed

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

    2013-02-01

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

  18. Hydrothermal synthesis and NH3 gas sensing property of WO3 nanorods at low temperature

    NASA Astrophysics Data System (ADS)

    Dien Nguyen, Dac; Vuong Dang, Duc; Chien Nguyen, Duc

    2015-09-01

    One-dimensional self-assembled single-crystalline hexagonal tungsten trioxide (WO3) nanostructures were synthesized by wet chemical-assisted hydrothermal processing at 120 °C for 24 h using sodium tungstate and hydrochloric acid. Urchin-like hierarchical nanorods (petal size: ∼16 nm diameter and 110 nm length) were obtained. The samples were characterized by field emission scanning electron microscopy, transmission electron microscopy, energy dispersive x-ray spectroscopy and x-ray diffraction. Sensors based on WO3 nanorods were fabricated by coating them on SiO2/Si substrate attached with Pt interdigitated electrodes. NH3 gas-sensing properties of WO3 nanorods were measured at different temperatures ranging from 50 °C to 350 °C and the response was evaluated as a function of ammonia gas concentration. The gas-sensing results reveal that WO3 nanorods sensor exhibits high sensitivity and selectivity to NH3 at low operating temperature (50 °C). The maximum response reached at 50 °C was 192 for 250 ppm NH3, with response and recovery times of 10 min and 2 min, respectively.

  19. Amine ligand-based hydrothermal synthesis of Co3O4 nanoparticles, characterization and magnetic study

    NASA Astrophysics Data System (ADS)

    Mansournia, Mohammadreza; Rakhshan, Narges

    2016-12-01

    Cobalt(II,III) oxid (Co3O4) nanostructures have been successfully synthesized using [Co(NH3)6]Cl3 and [Co(en)3]Cl3 (en: ethylenediamine) as the single precursors via hydrothermal method, and CoCl2·6H2O through a facile ammonia-assisted approach. Indeed, ammine and en ligands, as well as ammonia vapor, act as the sources of hydroxide ion in the preparation of Co3O4 nanoparticles. The structure of products was confirmed by X-ray diffraction (XRD) technique and Fourier-transform infrared (FT-IR) spectroscopy and their morphologies were examined by scanning electron microscopy (SEM). The optical study of the as-prepared Co3O4 nanostructures using UV-Vis diffused reflectance spectroscopy (DRS) exhibited their semiconducting property by revealing one optical band gap in 3.3 eV. Moreover, the vibrating sample magnetometry (VSM) measurements showed a weak ferromagnetic behavior that could be attributed to uncompensated surface spins and/or finite-size effects. Further, the effects of the nature of the precursor, its concentration, temperature and reaction time on the size and morphology of the samples were studied in detail.

  20. Hydrothermal Synthesis and Ammonia Sensing Properties of WO3/Fe2O3 Nanorod Composites

    NASA Astrophysics Data System (ADS)

    Dien, Nguyen Dac; Phuoc, Luong Huu; Hien, Vu Xuan; Vuong, Dang Duc; Chien, Nguyen Duc

    2017-01-01

    WO3 nanorods (NRs) and α-Fe2O3 NRs were fabricated by hydrothermal treatment. Composites of these materials were created by mixing with ratios of 1:2, 1:1 and 2:1 in weight. Morphology, structure and composition characteristics of the WO3/Fe2O3 NRs composites were characterized by scanning electron microscopy, x-ray diffraction and energy dispersive x-ray spectroscopy analyses. The results of sensing measurements indicated that the sensor based on WO3:Fe2O3 with the ratio of 2:1 exhibited fairly good sensitivity toward NH3 at 300°C and the sensor based on WO3:Fe2O3 with the ratio of 1:1 can be used as a NH3 sensor with an operating temperature of 350°C. Selectivity and response-recovery times are suitable for practical applications. Finally, the mechanism for the improvement in the gas-sensing property was discussed.

  1. Hydrothermal synthesis of mixed zinc-cobalt ferrite nanoparticles: structural and magnetic properties

    NASA Astrophysics Data System (ADS)

    Coppola, P.; da Silva, F. G.; Gomide, G.; Paula, F. L. O.; Campos, A. F. C.; Perzynski, R.; Kern, C.; Depeyrot, J.; Aquino, R.

    2016-05-01

    We synthesize Zn-substituted cobalt ferrite (Zn x Co1- x Fe2O4, with 0 ≤ x ≤ 1) magnetic nanoparticles by a hydrothermal co-precipitation method in alkaline medium. The chemical composition is evaluated by atomic absorption spectroscopy and energy-dispersive X-ray spectroscopy techniques. The structure and morphology of the nanopaticles are investigated by X-ray diffraction (XRD) and transmission electron microscopy (TEM), respectively. XRD Rietveld refinements reveal the cation distribution among the tetrahedral (A) and octahedral (B) sites. It shows that up to x 0.5 zinc ions occupy preferably A-sites, above which Zn ions begin also a gradual occupancy of B-sites. TEM images show nanoparticles with different shapes varying from spheres, cubes, to octahedrons. Hysteresis loop properties are studied at 300 and 5 K. These properties are strongly influenced by the Zn and Co proportion in the nanoparticle composition. At 300 K, only samples with high Co content present hysteresis. At 5 K, the reduced remanent magnetization ratio ( M R/ M S) and the coercivity ( H C) suggest that nanoparticles with x < 0.5 have cubic anisotropy. A kink on the hysteresis loop, close to the remanence, is observed at low temperature. This feature is presumably associated to interplay between hard and soft anisotropy regimes in the powder samples.

  2. Nanobrick-like WO3 thin films: Hydrothermal synthesis and electrochromic application

    NASA Astrophysics Data System (ADS)

    Kondalkar, V. V.; Kharade, R. R.; Mali, S. S.; Mane, R. M.; Patil, P. B.; Patil, P. S.; Choudhury, S.; Bhosale, P. N.

    2014-09-01

    Nanobrick-like WO3 thin films have been synthesized via facile hydrothermal route. Nanostructured WO3 thin films were characterized using X-ray diffraction (XRD), UV-Vis-NIR spectrophotometer, scanning electron microscopy (SEM), atomic force microscopy (AFM) to investigate the intentional properties such as phase structure, optical properties and surface morphology. Moreover electrochromic (EC) performance of WO3 thin film was investigated in 0.5 M LiClO4/PC by means of cyclic voltammetry (CV), chronocoulometry (CC) and chronoamperometry (CA). The value of diffusion coefficient (D) was determined from anodic peak current and was found to be 1.51 × 10-9 cm2/s. The response time of 6.9 s for bleaching (tb) and 9.7 s for coloration (tc) was observed with excellent reversibility 76%. The coloration efficiency for nanobricks WO3 is 39.24 cm2/C. CIE 1931 L∗ab values for colored and bleached films were estimated at 2° observer using D-65 illumination. The electrochromic studies show highly reversible and the stable nature of WO3 thin film which provides a versatile and promising application towards the fabrication of smart windows.

  3. Synthesis and optical characteristics of yttrium-doped zinc oxide nanorod arrays grown by hydrothermal method.

    PubMed

    Park, Hyunggil; Kim, Younggyu; Ji, Iksoo; Lee, Sang-Heon; Kim, Jin Soo; Kim, Jin Soo; Leem, Jae-Young

    2014-11-01

    Yttrium-doped ZnO (YZO) nanorods were synthesized by hydrothermal growth on a quartz substrate with various post-annealing temperatures. To investigate the effects of post-annealing on the optical properties and parameters of the nanorods, X-ray diffractometry (XRD), photoluminescence (PL) measurement, and ultraviolet (UV)-visible spectroscopy were used. From the XRD investigation, the full width at half maximum (FWHM) and the dislocation density of the nanorods was found to increase with an increase in the post-annealing temperature. In the PL spectra, the intensity of the near band edge (NBE) emission peak in the UV region also increases with an increase in the temperature of post-annealing. The deep level emission (DLE) peak in the visible region changes with various post-annealing temperatures, and its intensity increases remarkably with post-annealing at 800 degrees C. In this paper, changes in the optical parameters of the nanorods caused by variation in the behavior of Y during post-annealing was investigated, with properties such as absorption coefficients, refractive indices, and dispersion parameters being obtained from transmittance and reflectance analysis.

  4. Hydrothermal synthesis of cobalt oxide porous nanoribbons anchored with reduced graphene oxide for hydrogen peroxide detection

    NASA Astrophysics Data System (ADS)

    Zhang, Xinmeng; Li, Kezhi; Li, Hejun; Lu, Jinhua; Fu, Qiangang; Zhang, Leilei

    2016-08-01

    A new Co3O4-reduced graphene oxide (Co3O4-rGO) nanostructure was successfully prepared by hydrothermal-synthesized Co3O4 porous nanoribbons with an approximate length of 6-17 μm, a width of 21-737 nm, and a thickness of 33-80 nm hybridizing with reduced graphene oxide. The electrochemical properties of the Co3O4-rGO-modified electrode were investigated by the cyclic voltammograms and amperometric current-time method. The modified electrode shows high electrochemical activity for the catalytic reduction and detection of H2O2 in alkaline medium. The nonenzymatic hydrogen peroxide sensor exhibits wide linear range of 1-18.5 mM ( R = 0.99439), high adsorption amount about 3.24 × 10-6 mol/cm2, and a low detection limit of 5.35 × 10-7 M ( S/ N = 3). In addition, the sensor has a fast response (<5 s), good long-term stability, excellent repeatability (3.22 % relative standard deviation), and high selectivity. These outstanding properties of the sensor derive from their particular hybrid structure and synergistic effects between rGO and Co3O4.

  5. Hexamethylenetetramine assisted hydrothermal synthesis of BiPO4 and its electrochemical properties for supercapacitors

    NASA Astrophysics Data System (ADS)

    Nithya, V. D.; Kalai Selvan, R.; Vasylechko, Leonid

    2015-11-01

    The well defined microstructures of BiPO4 were successfully synthesized by the facile hexamethylenetetramine (HMT) assisted hydrothermal method. The low temperature monoclinic BiPO4 structure with space group P21/n, were obtained from X-ray diffraction (XRD) for the pristine and HMT-assisted BiPO4 with 1, 3, 5 and 10 mmole concentration. A transformation from low temperature monazite-type phase to the high temperature SbPO4-type phase of BiPO4 was observed at the 10 mmole concentration. There was a variation in the morphology from polyhedron to octahedra-like and finally into cube shape upon an increase in concentration of HMT. The role of reaction time in the morphology of BiPO4 particles was investigated. The selected area electron diffraction (SAED) pattern elucidated the ordered dot pattern and the calculated d-spacing revealed the formation of BiPO4. An increased specific capacitance of HMT assisted materials (202 F/g) compared with pristine BiPO4 (89 F/g) at 5 mA/cm2 was observed upon morphological variation due to HMT addition.

  6. Influence of synthesis pH and oxidative strength of the catalyzing acid on the morphology and chemical structure of hydrothermal carbon.

    PubMed

    Reiche, Sylvia; Kowalew, Natalia; Schlögl, Robert

    2015-02-23

    A specific control of the morphology and chemical structure of hydrothermal carbon (HTC) is of crucial importance for its application, both in catalyst supports or electrochemical devices. Here we show how the morphology, that is, particles size and homogeneity, and the distribution of functional groups can be controlled by the control of the synthesis pH of the hydrothermal carbonization. A complementary analysis of liquid byproducts by HPLC provides useful information on the nature of the polymeric species produced during the poly-condensation in the hydrothermal process and reveals the potential implementation of the process into the biorefinery concept. The acidic byproducts levulinic acid and formic acid determine the hydrothermal carbonization autocatalytically by additional supply of protons to the reaction medium. Thus, for a starting pH>3, only minor structural differences can be detected for HTC. The use of oxidizing acids favors higher yields of HTC and improves carbonization towards higher condensed carbon domains. Scaling up the process in a stirred 2 L batch reactor favors carbonization leading to higher condensed carbonaceous products. The relative trends of pH variation are maintained.

  7. Hydrothermal synthesis of ZnO nanorod arrays for photocatalytic inactivation of bacteria

    NASA Astrophysics Data System (ADS)

    Akhavan, O.; Mehrabian, M.; Mirabbaszadeh, K.; Azimirad, R.

    2009-11-01

    Arrays of ZnO nanorods were synthesized on ZnO seed layer/glass substrates by a hydrothermal method at a low temperature of 70 °C. The effect of pH > 7 of the hydrated zinc nitrate-NaOH precursor on the morphology and topography (e.g. size, surface area and roughness), the optical characteristics (e.g. optical transmission and band-gap energy), hydrophilicity and antibacterial activity of the grown ZnO nanostructure and nanorod coatings were investigated. For pH = 11.33 of the precursor (NaOH concentration of 0.10M), a fast growth of ZnO nanorods on the seed layer (length of ~1 µm in 1.5 h) was observed. The fast growth of the ZnO nanorods resulted in a significant reduction in the optical band-gap energy of the nanorod coating, which was attributed to the formation of more defects in the nanorods during their fast growth. The surface of the ZnO nanorod arrays was relatively hydrophilic (with a water contact angle of 16°) even after the subtraction of their surface roughness effect (with a contact angle of ca 27°). This hydrophilicity of the ZnO nanorods was assigned to the observed surface OH bonds. These characteristics caused the ZnO nanorod arrays to show an excellent UV-induced photocatalytic degradation of Escherichia coli bacteria. Furthermore, the synthesized ZnO nanorods were found to be strong photo-induced antibacterial material, even without considering their high surface area ratio.

  8. Hydrothermal synthesis of copper based nanoparticles: antimicrobial screening and interaction with DNA.

    PubMed

    Giannousi, K; Lafazanis, K; Arvanitidis, J; Pantazaki, A; Dendrinou-Samara, C

    2014-04-01

    Copper based nanoparticles (Cu-based NPs) of different compositions and sizes have been hydrothermally synthesized by varying the reaction time in the presence of the biocompatible surfactants polyoxyethylene (20) sorbitan laurate (Tween 20) and polyethylene glycol 8000 (PEG 8000). Effective control of the above synthetic parameters gave rise to Cu, Cu2O and Cu/Cu2O NPs of 10-44 nm. The antibacterial activity of the NPs was screened against Gram-positive (Bacillus subtilis, Bacillus cereus, Staphylococcus aureus) and Gram-negative (Xanthomonas campestris, Escherichia coli) bacteria. The Cu-based NPs induce pDNA degradation in a dose-dependent manner as well as extensive ds CT-DNA degradation. Cu2O NPs of 16 nm and 12 nm exhibit the lowest IC50 values (2.13 μg/mL and 3.7 μg/mL) against B. cereus and B. subtilis, respectively. The agarose gel electrophoresis of ds CT-DNA treated with Cu2O NPs demonstrated degradation at high concentration. In lower concentrations, viscosity measurements indicated groove binding. In regard to the enhanced antibacterial effect and specificity of Cu2O NPs against the Gram-positive strains, the activity pathway was further explored and ROS production and lipid peroxidation verified. The released copper ions 5.15 mg/L in distilled water and 16.32 mg/L in nutrient medium, found below the critical value to inhibit bacterial growth and thus nanosized composition effect is predominant.

  9. Conformal BaTiO3 Films with High Piezoelectric Coupling through an Optimized Hydrothermal Synthesis.

    PubMed

    Zhou, Zhi; Bowland, Christopher C; Patterson, Brendan A; Malakooti, Mohammad H; Sodano, Henry A

    2016-08-24

    Two-dimensional (2D) ferroelectric films have vast applications due to their dielectric, ferroelectric, and piezoelectric properties that meet the requirements of sensors, nonvolatile ferroelectric random access memory (NVFeRAM) devices, and micro-electromechanical systems (MEMS). However, the small surface area of these 2D ferroelectric films has limited their ability to achieve higher memory storage density in NVFeRAM devices and more sensitive sensors and transducer. Thus, conformally deposited ferroelectric films have been actively studied for these applications in order to create three-dimensional (3D) structures, which lead to a larger surface area. Most of the current methods developed for the conformal deposition of ferroelectric films, such as metal-organic chemical vapor deposition (MOCVD) and plasma-enhanced vapor deposition (PECVD), are limited by high temperatures and unstable and toxic organic precursors. In this paper, an innovative fabrication method for barium titanate (BaTiO3) textured films with 3D architectures is introduced to alleviate these issues. This fabrication method is based on converting conformally grown rutile TiO2 nanowire arrays into BaTiO3 textured films using a simple two-step hydrothermal process which allows for thickness-controlled growth of conformal films on patterned silicon wafers coated with fluorine-doped tin oxide (FTO). Moreover, the processing parameters have been optimized to achieve a high piezoelectric coupling coefficient of 100 pm/V. This high piezoelectric response along with high relative dielectric constant (εr = 1600) of the conformally grown textured BaTiO3 films demonstrates their potential application in sensors, NVFeRAM, and MEMS.

  10. Influence of EDTA{sup 2-} on the hydrothermal synthesis of CdTe nanocrystallites

    SciTech Connect

    Gong Haibo; Hao Xiaopeng; Xu Xiangang

    2011-12-15

    Transformation from Te nanorods to CdTe nanoparticles was achieved with the assistance of EDTA as a ligand under hydrothermal conditions. Experimental results showed that at the beginning of reaction Te nucleated and grew into nanorods. With the proceeding of reaction, CdTe nucleus began to emerge on the surface, especially on the tips of Te nanorods. Finally, nearly monodispersed hexagonal CdTe nanoparticles with diameters of about 200 nm were obtained. The effects of EDTA on the morphology and formation of CdTe nanoparticles were discussed in consideration of the strong ligand-effect of EDTA, which greatly decreased the concentration of Cd{sup 2+}. Furthermore, the possible formation process of CdTe nanoparticles from Te nanorods was further proposed. The crystal structure and morphology of the products were investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM). - Graphical Abstract: Firstly, Te nucleated and grew into nanorods in the presence of EDTA{sup 2-}. Then CdTe nucleus began to emerge on Te nanorods and finally monodispersed CdTe nanoparticles were obtained. Highlights: Black-Right-Pointing-Pointer EDTA serves as a strong ligand with Cd{sup 2+}. Black-Right-Pointing-Pointer The existence of EDTA constrains the nucleation of CdTe and promotes the formation of Te nanorods. Black-Right-Pointing-Pointer With the proceeding of reaction, CdTe nucleus began to emerge on the surface, especially on the tips of Te nanorods. Black-Right-Pointing-Pointer Nearly monodispersed hexagonal CdTe nanoparticles with diameters of about 200 nm were finally obtained.

  11. Effect of Experimental Parameters on the Hydrothermal Synthesis of Bi2WO6 Nanostructures

    NASA Astrophysics Data System (ADS)

    Cui, Ziming; Yang, Hua; Wang, Bin; Li, Ruishan; Wang, Xiangxian

    2016-04-01

    Bi2WO6 nanostructures were synthesized by a hydrothermal route, where the effect of various experimental parameters on the products was investigated. It is demonstrated that the sample morphology and size is highly dependent on the NaOH content (or pH value). At C NaOH = 0-0.0175 mol (pH range of 1-4), the prepared samples present flower-like hierarchical microspheres which are constructed from thin nanosheets via the self-assembly process. The size of the hierarchical microspheres exhibits a decreasing trend with increasing the NaOH content, from 7 μm at C NaOH = 0 mol to 1.5 μm at C NaOH = 0.0175 mol. At C NaOH = 0.03-0.0545 mol (pH: 5-9), the prepared samples exhibit irregular flake-like structures, and their size increases with the increase in NaOH content. At C NaOH = 0.055-0.05525 mol (pH: 10-11), the prepared samples are composed of uniform sphere-like particles with an average size of 85 nm. Compared to the NaOH content, the reaction temperature and time has a relatively small effect on the product morphology and size. The photocatalytic activity of the samples was evaluated by degrading rhodamine B (RhB) under irradiation of simulated sunlight. Among these samples, the samples composed of flower-like hierarchical microspheres have relatively high photocatalytic activity. In particular, the microspheres prepared at C NaOH = 0.01 mol exhibit the highest photocatalytic activity, and the degradation percentage reaches 99 % after 2 h of irradiation.

  12. Microwave-assisted hydrothermal synthesis of zinc oxide particles starting from chloride precursor

    SciTech Connect

    Tseng, Chun-Chieh; Chou, Yu-Hsien; Liu, Chung-Ming; Liu, Yih-Ming; Ger, Ming-Der; Shu, Youn-Yuen

    2012-01-15

    Graphical abstract: Schematic of the mechanism for ZnO nanoparticles obtained by the calcination. Highlights: Black-Right-Pointing-Pointer Nanocrystalline ZnO particles were successfully prepared by a microwave-assisted method. Black-Right-Pointing-Pointer Sponge-like morphology of ZnO change to a net-like structure after thermal treatment. Black-Right-Pointing-Pointer The PL spectra exhibited a nearband-edge emission at 393 nm. -- Abstract: Zinc oxide (ZnO) was synthesized using a microwave assisted hydrothermal (MAH) process based on chloride/urea/water solution and under 800 W irradiation for 5 min. In the bath, Zn{sup 2+} ions reacted with the complex carbonate and hydroxide ions to form zinc carbonate hydroxide hydrate (Zn{sub 4}CO{sub 3}(OH){sub 6}{center_dot}H{sub 2}O), and the conversion from Zn{sub 4}CO{sub 3}(OH){sub 6}{center_dot}H{sub 2}O to ZnO was synchronously achieved by a MAH process. The as-prepared ZnO has a sponge-like morphology. However, the initial sponge-like morphology of ZnO could change to a net-like structure after thermal treatment, and compact nano-scale ZnO particles were finally obtained when the period of thermal treatment increased to 30 min. Pure ZnO nanoparticles was obtained from calcination of loose sponge-like ZnO particles at 500 Degree-Sign C. The analysis of optical properties of these ZnO nanoparticles showed that the intensity of 393 nm emission increased with the calcination temperature because the defects were reduced and the crystallinity was improved.

  13. Hydrothermal synthesis of two copper helical coordination polymers with acentric three-dimensional framework constructing from mixed pyridine carboxylates

    SciTech Connect

    Zhang Shuai; Cao Yanning; Zhang Hanhui Chai Xiaochuan; Chen Yiping

    2008-03-15

    Two copper helical coordination polymers, [Cu(2-pc)(3-pc)]{sub n}1 and [Cu(2-pc)(4-pc)]{sub n}2 (2-pc=2-pyridine carboxylate, 3-pc=3-pyridine carboxylate, 4-pc=4-pyridine carboxylate) have been hydrothermally synthesized directly from pyridine carboxylic acids and copper nitrate. The crystal structure were determined by single-crystal X-ray diffraction with the following data: compound 1, orthorhombic, P2{sub 1}2{sub 1}2{sub 1}, a=6.591(3) A, b=8.692(5) A, c=20.548(9) A, V=1177.2(9) A{sup 3}, Z=4; compound 2, orthorhombic, Pna2{sub 1}, a=21.160(10) A, b=9.095(5) A, c=6.401(3) A, V=1231.9(11) A{sup 3}, Z=4. The acentric three-dimensional (3D) framework of 1 is constructed from right-handed helical Cu(2-pc) chains and left-handed Cu(3-pc) helices. As for 2, Cu(2-pc) helical chains, in which left- and right-handed helices are coexisting, and Cu(4-pc) zigzag chains combined together to form acentric 3D architecture of 2 as well. Additionally, besides general spectral characterization, we first introduce generalized 2D correlation spectroscopy to explore the coordination polymers and ascertain the stretching vibration location of carboxylate groups of compounds 1 and 2. -- Abstract: Two copper helical coordination polymers, [Cu(2-pc)(3-pc)]{sub n}1 and [Cu(2-pc)(4-pc)]{sub n}2 have been obtained by hydrothermal synthesis. Both two compounds crystallized in non-centrosymmetric space groups, P2{sub 1}2{sub 1}2{sub 1} and Pna2{sub 1}, respectively. The 3D framework of 1 is constructed from right-handed helical Cu(2-pc) chains and left-handed Cu(3-pc) helices. As for 2, Cu(2-pc) helical chains, in which left- and right-handed helices are coexisting, and Cu(4-pc) zigzag chains combined together to form 3D architecture of 2 as well.

  14. Location of Framework Al Atoms in the Channels of ZSM-5: Effect of the (Hydrothermal) Synthesis.

    PubMed

    Pashkova, Veronika; Sklenak, Stepan; Klein, Petr; Urbanova, Martina; Dědeček, Jiří

    2016-03-14

    (27) Al 3Q MAS NMR and UV/Vis spectroscopy with bare Co(II) ions as probes of Al pairs in the zeolite framework were employed to analyze the location of framework Al atoms in the channel system of zeolite ZSM-5. Furthermore, the effect of Na(+) ions together with tetrapropylammonium cation (TPA(+)) in the ZSM-5 synthesis gel on the location of Al in the channel system was investigated. Zeolites prepared using exclusively TPA(+) as a structure-directing agent (i.e., in the absence of Na(+) ions) led to 55-90% of Al atoms located at the channel intersection, regardless the presence or absence of Al pairs [Al-O-(Si-O)2 -Al sequences in one ring] in the zeolite framework. The presence of Na(+) ions in the synthesis gel did not modify the Al location at the channel intersection (55-95% of Al atoms) and led only to changes in i) the distribution of framework Al atoms between Al pairs (decrease) and single isolated Al atoms (increase), and ii) the siting of Al in distinguishable framework tetrahedral sites.

  15. Hydrothermal Processing

    SciTech Connect

    Elliott, Douglas C.

    2011-03-11

    This chapter is a contribution to a book on Thermochemical Conversion of Biomass being edited by Prof. Robert Brown of Iowa State University. It describes both hydrothermal liquefaction and hydrothermal gasification of biomass to fuels.

  16. Surfactant-assisted hydrothermal crystallization of nanostructured lithium metasilicate (Li{sub 2}SiO{sub 3}) hollow spheres: (I) Synthesis, structural and microstructural characterization

    SciTech Connect

    Ortiz-Landeros, J.

    2011-05-15

    Lithium metasilicate (Li{sub 2}SiO{sub 3}) was successfully synthesized using a hydrothermal process in the presence of different surfactants with cationic, non-ionic and anionic characters. The samples obtained were compared to a sample prepared by the conventional solid-state reaction method. The structural and microstructural characterizations of different Li{sub 2}SiO{sub 3} powders were performed using various techniques. Diffraction analyses revealed the successful crystallization of pure Li{sub 2}SiO{sub 3} single phase by hydrothermal technique, even without further heat-treatments and independent of the surfactant used. Electron microscopy analyses revealed that Li{sub 2}SiO{sub 3} powders were composed of uniform micrometric particles with a hollow sphere morphology and nanostructured walls. Finally, different thermal analyses showed that Li{sub 2}SiO{sub 3} samples preserved their structure and microstructure after further thermal treatments. Specific aspects regarding the formation mechanism of the spherical aggregates under hydrothermal conditions are discussed, and there is a special emphasis on the effect of the synthesis pathway on the morphological characteristics. -- Graphical abstract: Li{sub 2}SiO{sub 3} was synthesized using a hydrothermal process in the presence of different surfactants. Li{sub 2}SiO{sub 3} powders were composed of uniform micrometric particles with a hollow sphere morphology and nanostructured walls. Display Omitted Highlights: {yields} Pure Li{sub 2}SiO{sub 3} was synthesized by the hydrothermal method. {yields} Surfactant addition produced microstructural and morphological variations. {yields} TEM reveled the generation of nanostructured hollow spheres.

  17. Hydrothermal synthesis of copper selenides with controllable phases and morphologies from an ionic liquid precursor

    NASA Astrophysics Data System (ADS)

    Liu, Xiaodi; Duan, Xiaochuan; Peng, Peng; Zheng, Wenjun

    2011-12-01

    Cu2-xSe nanocrystals and CuSe nanoflakes are successfully synthesized through a convenient hydrothermal method from an ionic liquid precursor 1-n-butyl-3-ethylimidazolium methylselenite ([BMIm][SeO2(OCH3)]). The phases and morphologies of the copper selenides can be controlled by simply changing the atom ratio of Cu/Se in the reactants and reaction temperature. Furthermore, it is found that the [BMIm][SeO2(OCH3)] not only serves as Se source but also has influence on the shapes of CuSe nanoflakes. The adsorption of alkyl imidazolium rings ([BMIm]+) onto the (0001) facets of covellite CuSe prohibits the growth in the [0001] direction, and CuSe nuclei growth mainly processes along the six symmetric directions (+/-[01&cmb.macr;11], +/-[101&cmb.macr;1&cmb.macr;], and +/-[1&cmb.macr;100]) to form flakelike CuSe. The obtained copper selenides are characterized by XRD, SEM, EDS, XPS, TEM, and HRTEM. The results indicate that the Cu2-xSe nanocrystals are nearly spherical particles with an average diameter of about 20 nm, the hexagonal CuSe nanoflakes are single crystals with an edge length of 100-400 nm and a thickness of 25-50 nm. The potential formation mechanism of the copper selenides is also proposed.Cu2-xSe nanocrystals and CuSe nanoflakes are successfully synthesized through a convenient hydrothermal method from an ionic liquid precursor 1-n-butyl-3-ethylimidazolium methylselenite ([BMIm][SeO2(OCH3)]). The phases and morphologies of the copper selenides can be controlled by simply changing the atom ratio of Cu/Se in the reactants and reaction temperature. Furthermore, it is found that the [BMIm][SeO2(OCH3)] not only serves as Se source but also has influence on the shapes of CuSe nanoflakes. The adsorption of alkyl imidazolium rings ([BMIm]+) onto the (0001) facets of covellite CuSe prohibits the growth in the [0001] direction, and CuSe nuclei growth mainly processes along the six symmetric directions (+/-[01&cmb.macr;11], +/-[101&cmb.macr;1&cmb.macr;], and +/-[1

  18. Hydrothermal synthesis of hydroxyapatite plates prepared using low molecular weight heparin (LMWH).

    PubMed

    Rajeswari, A; Kumar, V Ganesh; Karthick, V; Dhas, T Stalin; Potluri, Sri Lakshmi

    2013-11-01

    Materials with enhanced physical and biological properties have been used for biomedical applications and can be developed by functionalizing them using various components. Hydroxyapatite (HAP), among other available synthetic material, serves as one of the best tools in orthopaedics and ceramic coatings. The porous structure of HAP helps in bone cell regeneration, chemical integration of bone and also favours the interaction between bone and tissues. Herein, we have demonstrated a simple procedure for the synthesis of HAP using low molecular weight heparin (LMWH), a structural analogue of bone heparan sulphate proteoglycan. The presence of small sized HAP plates with well-defined structures was revealed using electron microscopic analysis. The phase purity of the synthesized HAP was evaluated using X-ray diffraction pattern obtained before and after immersion in simulated body fluid (SBF).

  19. Hydrothermal-hydrolysis synthesis and photocatalytic properties of nano-TiO2 with an adjustable crystalline structure.

    PubMed

    Zhang, Jinghuan; Xiao, Xin; Nan, Junmin

    2010-04-15

    Tri-phase (anatase, rutile, and brookite), bi-phase (anatase and rutile), and mono-phase (rutile) TiO(2) nanomaterials with different morphologies were successively synthesized using a hydrothermal-hydrolysis method and adjusting the Ti(4+)/Ti(3+) molar ratio in a precursor solution. The properties of the fabricated nanomaterials were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), photocatalytic reaction, and other techniques. It has been shown that TiO(2) nanorods can be obtained by increasing the Ti(4+)/Ti(3+) molar ratio in a precursor solution from 1:0 to 0.3:0.7. TiO(2) nanoparticles are formed if the Ti(3+) fraction in the solution is further increased. The selective synthesis of TiO(2) nanomaterials is explained by a decrease in the reaction rate and by changes in acidity with increasing Ti(3+) content. The tri-phase nanorods and bi-phase nanoparticles synthesized with Ti(4+)/Ti(3+) molar ratios from 1:0 to 0.8:0.2 and 0.2:0.8 to 0:1, respectively, have a higher degradation ability with respect to methylene blue aqueous solutions under UV irradiation at ambient temperature compared to purely rutile TiO(2) nanorods synthesized with Ti(4+)/Ti(3+) molar ratios from 0.7:0.3 to 0.3:0.7. The high photocatalytic activity of the multi-phase TiO(2) samples is primarily attributed to their larger band gap and suppressed recombination of photo-generated electron-hole pairs.

  20. High-temperature, high-pressure hydrothermal synthesis, characterization, and structural relationships of layered uranyl arsenates.

    PubMed

    Liu, Hsin-Kuan; Ramachandran, Eswaran; Chen, Yi-Hsin; Chang, Wen-Jung; Lii, Kwang-Hwa

    2014-09-02

    Five new uranyl arsenates, Na14[(UO2)5(AsO4)8]·2H2O (1), K6[(UO2)5O5(AsO4)2] (2a), K4[(UO2)3O2(AsO4)2] (2b), Rb4[(UO2)3O2(AsO4)2] (3), and Cs6[(UO2)5O2(AsO4)4] (4), were synthesized by high-temperature, high-pressure hydrothermal reactions at about 560 °C and 1440 bar and were characterized by single-crystal X-ray diffraction, thermogravimetric analysis, and photoluminescence spectroscopy. Crystal data for compound 1: triclinic, P1, a = 7.0005(3) Å, b = 12.1324(4) Å, c = 13.7428(5) Å, α = 64.175(2)°, β = 89.092(2)°, γ = 85.548(2)°, V = 1047.26(7) Å(3), Z = 1, R1 = 0.0185; compound 2a: monoclinic, P2₁/c, a = 6.8615(3) Å, b = 24.702(1) Å, c = 7.1269(3) Å, β = 98.749(2)°, V = 1193.89(9) Å(3), Z = 2, R1 = 0.0225; compound 2b: monoclinic, P2₁/c, a = 6.7852(3) Å, b = 17.3640(8) Å, c = 7.1151(3) Å, β = 98.801(3)°, V = 828.42(6) Å(3), Z = 2, R1 = 0.0269; compound 3: monoclinic, P2₁/m, a = 6.9783(3) Å, b = 17.4513(8) Å, c = 7.0867(3) Å, β = 90.808(3)°, V = 862.94(7) Å(3), Z = 2, R1 = 0.0269; compound 4: triclinic, P1, a = 7.7628(3) Å, b = 9.3324(4) Å, c = 11.9336(4) Å, α = 75.611(2)°, β = 73.136(2)°, γ = 86.329(2)°, V = 801.37(5) Å(3), Z = 1, R1 = 0.0336. The five compounds have layer structures consisting of uranyl square, pentagonal, and hexagonal bipyramids as well as AsO4 tetrahedra. Compound 1 contains chains of discrete uranyl square and pentagonal bipyramids, 2a contains three-polyhedron-wide ribbons of edge- and corner-sharing uranyl square and pentagonal bipyramids, 2b and 3 contain dimers of edge-shairing pentagonal bipyramids that share edges with hexagonal bipyramids to form chains, and 4 contains one-polyhedron-wide zigzag chains of edge-sharing uranyl polyhedra. The double sheet structure of 1 is new, but the chain topology has been observed in an organically templated uranyl sulfate. Compound 2b is a new geometrical isomer of the phosphuranylite group. The sheet anion topologies of 2a and 4 can be obtained by

  1. Synthesis of alpha'L-C2S cement from fly-ash using the hydrothermal method at low temperature and atmospheric pressure.

    PubMed

    Kacimi, Larbi; Cyr, Martin; Clastres, Pierre

    2010-09-15

    The objective of this study was the synthesis of alpha'(L)-C(2)S (Ca(2)SiO(4)) belite cement, starting from fly-ash of system CaO-SiO(2)-Al(2)O(3)-SO(3), and using the hydrothermal method in alkaline solution. The lime deficit in these ashes was compensated by the addition of slaked lime from lime bagging workshops. The hydrothermal treatment of the mixture was carried out in demineralized water, NaOH or KOH solution, continually stirred at a temperature below 100 degrees C and atmospheric pressure. The dehydration and calcination of the mixtures at temperatures between 800 and 1100 degrees C allowed alpha'(L)-C(2)S-rich cement to be obtained. The optimization of the synthesis parameters (temperature and time of stirring, pH of solution, temperature and duration of mixture burning) was also studied. The phase formation during various synthesis stages was studied by X-ray diffraction (XRD). Other techniques, such as SEM and EDX, were used to characterize the cement minerals. The results obtained showed that these ashes could form belite cement composed of only one dicalcium silicate phase (alpha'(L)-C(2)S).

  2. Hydrothermal synthesis of β-Co(OH)2 nanoplatelets: A novel catalyst for CO oxidation

    NASA Astrophysics Data System (ADS)

    Deng, Dongyang; Xing, Xinxin; Chen, Nan; Li, Yuxiu; Wang, Yude

    2017-01-01

    A facile, cost-effective, template-free chemical method was developed for the synthesis of β-Co(OH)2 nanoplatelets under the different preparation conditions. The morphology and microstructure of as-synthesized samples were examined by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectrum (XPS), respectively. The observations revealed the formation of a single phase of the hexagonal brucite-like β-Co(OH)2, which had an irregular hexagonal disk with angles of adjacent edges of 120°, edge lengths ranging from 200 to 300 nm, and thicknesses of 20-40 nm. When investigated as catalyst for CO oxidation, the β-Co(OH)2 nanoplatelets exhibited good catalytic activity for CO. Among β-Co(OH)2 nanoplatelets, the sample prepared at 100 °C for 8 h performed the best, giving the T100% (the temperature required for achieving a CO of 100%) of 120 °C for the oxidation of CO. There are good correlations of Co3+/Co2+, the absorbed Ox- ions and surface OH group with catalytic activity of the samples for CO oxidation.

  3. In situ synthesis of TiH{sub 2} layer on metallic titanium foil through gaseous hydrogen free acid-hydrothermal method

    SciTech Connect

    Ren, Na; Wang, Guancong; Liu, Hong; Ohachi, Tadashi

    2014-02-01

    Graphical abstract: The reaction mechanism for in situ synthesizing TiH{sub 2} layer on titanium foil by a gaseous hydrogen free acid-hydrothermal methodology. - Highlights: • A dense TiH{sub 2} layer is synthesized by a hydrogen free acid-hydrothermal method. • Hydrogen in a TiH{sub 2} layer synthesized can release at low temperature. • During the dehydrogenation process, there is no any intermediate phase forming. • We report a method of low-cost, low-risk and convenience toward productive TiH{sub 2}. - Abstract: A novel strategy for synthesis of TiH{sub 2} layer on surface of metallic titanium by using an acid-hydrothermal method was proposed. During the synthesis process, no any elemental hydrogen was involved. X-ray powder diffraction, energy-dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy and scanning electron microscopy results confirmed that a TiH{sub 2} layer of 20 μm thickness on a Ti foil surface can be formed in situ by an interface reaction of metallic titanium with sulfuric acid solution, hydrochloric acid, or phosphoric acid, which is a hydrogen self-storage process. By tuning reaction parameters, for example, concentration of acid, composition and morphology of TiH{sub 2}-Ti hybrid materials can be adjusted. The TiH{sub 2} layer on a metallic titanium surface can be decompounded completely heated below 400 °C. This convenient, safe and low-cost method is a promising gaseous hydrogen free approach for the synthesis of hydride-based hydrogen storage materials.

  4. Synthesis of large surface area nano-sized BiVO{sub 4} by an EDTA-modified hydrothermal process and its enhanced visible photocatalytic activity

    SciTech Connect

    Sun Wanting; Xie Mingzheng; Jing Liqiang; Luan Yunbo; Fu Honggang

    2011-11-15

    In this work, monoclinic scheelite-type BiVO{sub 4} nanoparticle with large surface area has been successfully synthesized, using Bi(NO{sub 3}){sub 3} and NH{sub 4}VO{sub 3} as raw materials, through a hydrothermal process in the presence of ethylene diamine tetraacetic acid (EDTA). It is demonstrated that the nanoparticle size of as-prepared BiVO{sub 4} becomes small by decreasing hydrothermal temperature, shortening hydrothermal reaction time and increasing EDTA amount used. The resulting BiVO{sub 4} nanoparticle with large surface area exhibits a good photocatalytic performance for degrading phenol solution as a model organic pollutant under visible illumination. The key of this method is the chelating role of EDTA group in the synthetic process that it can greatly control the concentration of Bi{sup 3+}, leading to the growth inhibition of BiVO{sub 4} crystallite. The work provides a route for the synthesis of Bi-containing nano-sized composite oxides with large surface area. - Graphical abstract: High visible active nano-sized BiVO{sub 4} photocatalyst with large surface area is successfully synthesized, which is attributed to the chelating role of EDTA group inhibiting the growth of BiVO{sub 4} crystallites. Highlights: > Monoclinic scheelite-type BiVO{sub 4} nanoparticle with large surface area has been synthesized by a hydrothermal process. > Key of this method is the chelating role of EDTA group inhibiting the growth of BiVO{sub 4} crystallites. > Resulting nano-sized BiVO{sub 4} exhibits a good photocatalytic activity for degrading phenol under visible illumination.

  5. Low-temperature hydrothermal synthesis of the three-layered sodium cobaltite P3-Na{sub x}CoO{sub 2} (x ∼ 0.60)

    SciTech Connect

    Miclau, M.; Bokinala, K.; Miclau, N.

    2014-06-01

    Highlights: • We report direct synthesis of the high temperature stable phase, P3-Na{sub 0.6}CoO{sub 2}. • The hydrothermal synthesis of P3-Na{sub 0.6}CoO{sub 2} involves one step and low temperature. • The yield diagram for Na–Co–H{sub 2}O system has been builded up to 250 °C. • We propose a formation mechanism of P3-Na{sub 0.6}CoO{sub 2} phase using the unit cell theory. • The thermal stability of P3-Na{sub 0.6}CoO{sub 2} has been investigated by means of HT-XRD. - Abstract: In order to obtain the layered sodium cobalt oxide materials by hydrothermal synthesis, the yield diagram for Na–Co–H{sub 2}O system has been built and studied. In the same time, the well-known data of Co–H{sub 2}O system have been extended at 250 °C in basic solution. We had first synthesized directly the high temperature stable phase, P3-Na{sub 0.6}CoO{sub 2} by a one-step low-temperature hydrothermal method. The rhombohedral structure of P3-Na{sub 0.6}CoO{sub 2} has been determined by X-ray diffraction (XRD) and the purity of phases has been confirmed by XPS. The thermal stability of P3-Na{sub 0.6}CoO{sub 2} has been investigated by means of high temperature X-ray diffraction in 298–873 K range and when the temperature has reached 723 K, the completely transformation of P3-Na{sub 0.6}CoO{sub 2} in the rhombohedral stable phase α-NaCoO{sub 2} (space group R-3m) was observed. Also, a formation mechanism of P3-Na{sub 0.6}CoO{sub 2} phase using the unit cell theory in the hydrothermal process was proposed.

  6. The Hydrothermal Synthesis and Electrochemistry of Oxyfluorides and Fluoro-bronzes for Lithium and Multivalent Battery Cathodes

    NASA Astrophysics Data System (ADS)

    Incorvati, Jared T.

    The next major breakthrough in multivalent batteries will come in the form of a cathode. To that end, the low temperature, phase-pure synthesis of both cubic and orthorhombic molybdenum fluoro-bronzes is presented. A study of temperature and fluoride concentration on reaction products proves to be critical, enabling control over formation of product phases. The orthorhombic fluoro-bronze appears as a solid solution with the formula MoO3-xF x and plausible end members (0.20≤x≤0.25). Microscopy of the cubic and orthorhombic molybdenum fluoro-bronzes reveal that the size and morphology of the products can largely be predicted from physical characteristics of alpha-MoO 3 reagent, suggesting the low temperature reaction may not follow a "traditional" hydrothermal mechanism. The cubic WO3-xF x can also be made at low temperatures; however, the low solubility of WO3 at these temperatures both enables and requires a different approach. Cathodes composed of orthorhombic molybdenum fluoro-bronze are found to reversibly intercalate magnesium. Fluoro-bronze cathodes have a higher capacity than isostructural alpha-MoO3 by an order of magnitude. Structural, spectroscopic, and modeling techniques indicate that the fluoro-bronze can accommodate the Mg2+ ion, without co-intercalation of anions, solvent imbibition, or the formation of conversion products such as MgO or MgF2. Fluorine's preference for bridging anion sites may account for the absence of fluoride abstraction. In lithium cells, electrochemical techniques indicate that cubic molybdenum fluoro-bronze discharges via a different mechanism than the orthorhombic fluoro-bronze. In addition, cubic fluoro-bronze has an irreversible two-phase plateau on its first discharge only, suggesting it undergoes a distinct break-in step compared to the orthorhombic fluoro-bronze. Both molybdenum fluoro-bronzes prove to have similar measured energy densities, approximately 350 Wh/Kg, though with distinct battery properties. In

  7. Carbon Isotope Characterization of Organic Intermediaries in Hydrothermal Hydrocarbon Synthesis by Pyrolysis-GC-MS-C-IRMS

    NASA Technical Reports Server (NTRS)

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

    2010-01-01

    We report results of experiments designed to characterize the carbon isotope composition of intermediate organic compounds produced as a result of mineral surface catalyzed reactions. The impetus for this work stems from recently reported detection of methane in the Martian atmosphere coupled with evidence showing extensive water-rock interaction during Martian history. Abiotic formation by Fischer-Tropsch-type (FTT) synthesis during serpentinization reactions may be one possible process responsible for methane generation on Mars, and measurement of carbon and hydrogen isotopes of intermediary organic compounds can help constrain the origin of this methane. Of particular interest within the context of this work is the isotopic composition of organic intermediaries produced on the surfaces of mineral catalysts (i.e. magnetite) during hydrothermal experiments, and the ability to make meaningful and reproducible isotope measurements. Our isotope measurements utilize a unique analytical technique combining Pyrolysis-Gas Chromatograph-Mass Spectrometry-Combustion-Isotope Ratio Mass Specrometry (Py-GC-MS-C-IRMS). Others have conducted similar pyrolysis-IRMS experiments on low molecular weight organic acids (Dias, et al, Organic Geochemistry, 33 [2002]). Our technique differs in that it carries a split of the pyrolyzed GC-separated product to a Thermo DSQ-II quadrupole mass spectrometer as a means of making qualitative and semi-quantitative compositional measurements of the organic compounds. A sample of carboxylic acid (mixture of C1 through C6) was pyrolyzed at 100 XC and passed through the GC-MS-C-IRMS (combusted at 940 XC). In order to test the reliability of our technique we compared the _13C composition of different molecular weight organic acids (from C1 through C6) extracted individually by the traditional sealed-tube cupric oxide combustion (940 XC) method with the _13C produced by our pyrolysis technique. Our data indicate that an average 4.3. +/-0.5. (V

  8. Synthesis of flower-like Boehmite (γ-AlOOH) via a one-step ionic liquid-assisted hydrothermal route

    SciTech Connect

    Tang, Zhe Liang, Jilei Li, Xuehui Li, Jingfeng Guo, Hailing; Liu, Yunqi Liu, Chenguang

    2013-06-01

    A simple and novel synthesis process, one-step ionic liquid-assisted hydrothermal synthesis route, has been developed in the work to synthesize Bohemithe (γ-AlOOH) with flower-like structure. The samples were characterized by X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) and Scanning Electron Microscope (SEM). Ionic liquid [Omim]{sup +}Cl{sup −}, as a template, plays an important role in the morphology and pore structure of the products due to its strong interactions with reaction particles. With the increase in the dosage of ionic liquid [Omim]{sup +}Cl{sup −}, the morphology of the γ-AlOOH was changed from initial bundles of nanosheets (without ionic liquid) into final well-developed monodispersed 3D flower-like architectures ([Omim]{sup +}Cl{sup −}=72 mmol). The pore structure was also altered gradually from initial disordered slit-like pore into final relatively ordered ink-bottle pore. Furthermore, the proposed formation mechanism and other influencing factors such as reaction temperature and urea on formation and morphology of the γ-AlOOH have also been investigated. - Graphical abstract: The flower-like γ-AlOOH architectures composed by nanosheets with narrow size distribution (1.6–2.2 μm) and uniform pore size (6.92 nm) have been synthesized via a one-step ionic liquid-assisted hydrothermal route. - Highlights: • The γ-AlOOH microflowers were synthesized via an ionic liquid-assisted hydrothermal route. • Ionic liquid plays an important role on the morphology and porous structure of the products. • Ionic liquid can be easily removed from the products and reused in recycling experiments. • A “aggregation–recrystallization–Ostwald Ripening“formation mechanism may occur.

  9. Microemulsion-mediated hydrothermal synthesis and characterization of zircon-type LaVO{sub 4} nanowires

    SciTech Connect

    Fan Weiliu Song Xinyu; Sun Sixiu Zhao Xian

    2007-01-15

    The zircon-type tetragonal (t-) LaVO{sub 4} nanowires were controlled synthesized by a new approach, a microemulsion-mediated hydrothermal method, in which the aqueous cores of sodium dodecyl sulfate (SDS)/cyclohexane/n-hexanol/water microemulsion were used as constrained microreactors for a controlled growth of t-LaVO{sub 4} nanocrystals under hydrothermal conditions. The microemulsion exists stably just at room temperature and not under hydrothermal conditions, in addition, the as-obtained nanowires are much larger than the microemulsion droplets, so that the microemulsion does not simply act as a template, but rather directs crystal growth into nanowires presumably by interacting with the surface of the growing crystal. A series of experimental results indicated that several experimental parameters, such as the SDS concentration, the species and content of the cosurfactant play important roles in the morphological control of the t-LaVO{sub 4} nanocrystals. Possible formation mechanism of t-LaVO{sub 4} nanowires is also discussed. - Graphical abstract: The zircon-type tetragonal (t-) LaVO{sub 4} nanowires were controlled synthesized by a microemulsion-mediated hydrothermal method, in which the aqueous cores of SDS/cyclohexane/n-hexanol/water microemulsion were used as constrained microreactors for a controlled growth of t-LaVO{sub 4} nanocrystals under hydrothermal conditions.

  10. Ultrasonically assisted hydrothermal synthesis of nanocrystalline ZrO2, TiO2, NiFe2O4 and Ni0.5Zn0.5Fe2O4 powders.

    PubMed

    Meskin, Pavel E; Ivanov, Vladimir K; Barantchikov, Alexander E; Churagulov, Bulat R; Tretyakov, Yury D

    2006-01-01

    Ultrasonic-hydrothermal and hydrothermal treatment was used for synthesis of nanocrystalline zirconia, titania, nickel and nickel-zinc ferrites powders from precipitated amorphous zirconyl, titanyl, binary nickel-iron and ternary nickel-zinc-iron hydroxides, respectively. Resulted nanopowders were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), nitrogen adsorption (BET), and magnetic susceptibility measurements. It was established that ultrasonically assisted hydrothermal treatment of amorphous zirconyl and titanyl gels results in significant rise of the rate of ZrO2 and TiO2 crystallization and promotes formation of thermodynamically stable monoclinic zirconia, but does not affect the microstructure and mean particles size of resulting nanopowders. Ultrasonic-hydrothermal processing of co-precipitated amorphous nickel, zinc and iron hydroxides favours formation of nanocrystalline ferrite powders with narrower particle size distribution.

  11. Ionic liquid-based hydrothermal synthesis of Lu2O3 and Lu2O3:Eu3+ microcrysals

    NASA Astrophysics Data System (ADS)

    Li, Yinyan; Xu, Shiqing

    2016-09-01

    Uniform and well-defined Lu2O3 and Lu2O3:Eu3+ microarchitectures have been successfully synthesized via a green and facile ionic liquid-based hydrothermal method followed by a subsequent calcination process. Novel 3D micro-rodbundles and 1D microrods of Lu2O3 and Lu2O3:Eu3+ were controllably obtained through this method. X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy and photoluminescence spectra were used to characterize the micromaterials. The proposed formation mechanisms have been investigated on the basis of a series of SEM studies of the products obtained at different hydrothermal durations. The results indicated that hydrothermal temperature and the ionic liquid-tetrabutylammonium hydroxide were two key factors for the formation as well as the morphology control of the Lu2O3 and Lu2O3:Eu3+ microarchitectures.

  12. Synthesis of SnO 2 micro-spheres, nano-rods and nano-flowers via simple hydrothermal route

    NASA Astrophysics Data System (ADS)

    Vuong, Dang Duc; Hien, Vu Xuan; Trung, Khuc Quang; Chien, Nguyen Duc

    2011-11-01

    SnO 2 micro-spheres (0.5-2 μm diameter), nano-flowers (petal size: 100-250 nm diameter; 500 nm-2 μm length) and nano-rods (3-6 nm diameter; 10-30 nm length) were synthesized by hydrothermal route. The samples were characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD). The influence of precursor, hydrothermal temperature and treatment time on the formation of SnO 2 multi-morphology was also investigated. Moreover, a possible formation mechanism and relationships among morphologies were discussed.

  13. Microwave assisted facile hydrothermal synthesis and characterization of zinc oxide flower grown on graphene oxide sheets for enhanced photodegradation of dyes

    NASA Astrophysics Data System (ADS)

    Kashinath, L.; Namratha, K.; Byrappa, K.

    2015-12-01

    Microwave assisted hydrothermal process of synthesis of ZnO-GO nanocomposite by using ZnCl2 and NaOH as precursors is being reported first time. In this investigation, a novel route to study on synthesis, interaction, kinetics and mechanism of hybrid zinc oxide-graphene oxide (ZnO-GO) nanocomposite using microwave assisted facile hydrothermal method has been reported. The results shows that the ZnO-GO nanocomposite exhibits an enhancement and acts as stable photo-response degradation performance of Brilliant Yellow under the UV light radiation better than pure GO and ZnO nanoparticles. The microwave exposure played a vital role in the synthesis process, it facilitates with well define crystalline structure, porosity and fine morphology of ZnO/GO nanocomposite. Different molar concentrations of ZnO precursors doped to GO sheets were been synthesized, characterized and their photodegradation performances were investigated. The optical studies by UV-vis and Photo Luminescence shows an increase in band gap of nanocomposite, which added an advantage in photodegradation performance. The in situ flower like ZnO nano particles are were densely decorated and anchored on the surfaces of graphene oxide sheets which aids in the enhancement of the surface area, adsorption, mass transfer of dyes and evolution of oxygen species. The nanocomposite having high surface area and micro/mesoporous in nature. This structure and morphology supports significantly in increasing photo catalytic performance legitimate to the efficient photosensitized electron injection and repressed electron recombination due to electron transfer process with GO as electron collector and transporter dependent on the proportion of GO in ZnO/GO composite.

  14. Facile synthesis of novel bowl-like hollow carbon spheres by the combination of hydrothermal carbonization and soft templating.

    PubMed

    Zhang, Zili; Qin, Mingli; Jia, Baorui; Zhang, Hongzhou; Wu, Haoyang; Qu, Xuanhui

    2017-03-07

    For the first time, bowl-like hollow carbon spheres (BHCSs) have been designed and fabricated by the combination of hydrothermal carbonization and soft templating. The obtained BHCSs exhibit well-defined shapes with the size ranging from 1 to 2 μm. As electrodes of electrochemical double layer capacitors they showed good performance.

  15. Hydrothermal Biogeochemistry

    NASA Astrophysics Data System (ADS)

    Shock, E.; Havig, J.; Windman, T.; Meyer-Dombard, D.; Michaud, A.; Hartnett, H.

    2006-12-01

    Life in hot spring ecosystems is confronted with diverse challenges, and the responses to those challenges have dynamic biogeochemical consequences over narrow spatial and temporal scales. Within meters along hot spring outflow channels at Yellowstone, temperatures drop from boiling, and the near-boiling conditions of hot chemolithotrophic communities, to those that permit photosynthesis and on down to conditions where nematodes and insects graze on the edges of photosynthetic mats. Many major and trace element concentrations change only mildly in the water that flows through the entire ecosystem, while concentrations of other dissolved constituents (oxygen, sulfide, ammonia, total organic carbon) increase or decrease dramatically. Concentrations of metals and micronutrients range from toxic to inadequate for enzyme synthesis depending on the choice of hot spring. Precipitation of minerals may provide continuous growth of microbial niches, while dissolution and turbulent flow sweeps them away. Consequently, microbial communities change at the meter scale, and even more abruptly at the photosynthetic fringe. Isotopic compositions of carbon and nitrogen in microbial biomass reflect dramatic and continuous changes in metabolic strategies throughout the system. Chemical energy sources that support chemolithotrophic communities can persist at abundant or useless levels, or change dramatically owing to microbial activity. The rate of temporal change depends on the selection of hot spring systems for study. Some have changed little since our studies began in 1999. Others have shifted by two or more units in pH over several years, with corresponding changes in other chemical constituents. Some go through daily or seasonal desiccation cycles, and still others exhibit pulses of changing temperature (up to 40°C) within minutes. Taken together, hydrothermal ecosystems provide highly manageable opportunities for testing how biogeochemical processes respond to the scale of

  16. Synthesis of Mg{sub 2}SiO{sub 4}:Dy{sup 3+} nanoparticles by hydrothermal method and investigation of their thermo and photo luminescence properties

    SciTech Connect

    Ghahari, M.; Mostafavi, K.

    2016-05-15

    Highlights: • Mg{sub 2}SiO{sub 4}:Dy{sup 3+} nanoparticles have been prepared by hydrothermal and combustion methods. • Thermo and photo luminescent behavior of Mg{sub 2}SiO{sub 4}:Dy{sup 3+} was studied. • The effect of synthesis method on TL properties of Mg{sub 2}SiO{sub 4}:Dy{sup 3+} was investigated. • The optimal dopant concentration for thermo-luminescent property was obtained. - Abstract: In this study, photo and thermo-luminescent properties of Nano crystalline Mg{sub 2}SiO{sub 4}:Dy{sup 3+} prepared by a hydrothermal method were studied and compared to those of nanoparticles prepared by combustion method. The synthesized sample was characterized by X-ray diffraction, transmission electron microscopy, scanning electron microscopy and photoluminescence spectroscopy. The effect of Dy concentration on photo and thermoluminescent intensities was studied. The X-ray diffraction (XRD) patterns of the samples revealed that forsterite was formed as a major phase for all the samples. The crystallite size was found to be in the range of 20–50 nm. The thermo luminescent glow curve indicated that the hydrothermal sample was more efficient than the combustion sample. Two prominent TL bands located at 200 nm and 320 nm were recorded. The prepared nanoparticles exhibited a roughly linear dose response to absorbed dose of 1000 Gy received from 60Co gamma source, suggesting that nanomaterial could be a good candidate for high dose dosimetry.

  17. Effect of the H2 plasma treatment of a seed layer on the synthesis of ZnO nanorods using a microwave hydrothermal method

    NASA Astrophysics Data System (ADS)

    Koo, Horng-Show; Lin, Ching-Cheng; Chen, Yao-Ju; Peng, Cheng-Hsiung; Chen, Mi

    2014-01-01

    The effect of H2 plasma treatment of a seed layer on the synthesis and characterization of zinc oxide (ZnO) nanorods is determined. Using an Al-doped ZnO (AZO) thin film as a seed layer, well-aligned ZnO nanorods are rapidly grown on an indium tin oxide (ITO)-coated glass substrate using a microwave hydrothermal method. The deposited AZO substrate was previously treated with H2 plasma. The effect of H2 plasma treatment of the seed layer on the alignment, growth rate, and crystallinity of the ZnO nanorods is determined. It is shown that the alignment and growth rate of the ZnO nanorods depend on the characteristics and roughness of the seed layer, which are improved by H2 plasma treatment. Various characterization methods such as X-ray diffraction (XRD), cathodoluminescence (CL), transmission electron microscopy (TEM), and X-ray photoemission spectroscopy (XPS) are used to determine the characteristic quality of the ZnO nanorods. A fundamental model of the effect of H2 plasma treatment on the seed layer and ZnO growth using a microwave hydrothermal process is also presented.

  18. Surfactant-free hydrothermal synthesis of hierarchically structured spherical CuBi2O4 as negative electrodes for Li-ion hybrid capacitors.

    PubMed

    Yuvaraj, Subramanian; Karthikeyan, Kaliyappan; Kalpana, Dharmalingam; Lee, Yun Sung; Selvan, Ramakrishnan Kalai

    2016-05-01

    Hierarchically structured spherical CuBi2O4 particles were prepared using a facile hydrothermal method without using a surfactant over various hydrothermal reaction periods. The prepared CuBi2O4 samples were examined via X-ray diffraction (XRD), which confirmed the formation of a tetragonal crystal structure. The morphological features were analyzed using field emission scanning electron microscopy (FESEM), which elucidated the construction of the hierarchical microspherical CuBi2O4 particles. The plausible growth mechanism of the hierarchical structure was explained in terms of a time-dependent synthesis process and its crystal structure. The uniform hierarchical CuBi2O4 microspheres were used to fabricate a Li-ion hybrid capacitor (Li-HC) along with activated carbon (AC), the generated device delivers a stable specific capacitance of 26.5 F g(-1) over 1500 cycles at a high current density of 1000 mA g(-1) and a capacity retention of ∼86%. The AC/CB2 Li-ion hybrid cell exhibits high energy density and power density values of 24 W h kg(-1) and 300 W kg(-1), respectively.

  19. Hydrothermal synthesis of doped lanthanum zirconate nanomaterials and the effect of V–Ge substitution on their structural, electrical and dielectric properties

    SciTech Connect

    Farid, Muhammad Asim; Asghar, Muhammad Adnan; Ashiq, Muhammad Naeem Ehsan, Muhammad Fahad; Athar, Muhammad

    2014-11-15

    Graphical abstract: Variation of dielectric constant with frequency for all the synthesized materials. - Highlights: • Hydrothermal method has been successfully employed to synthesize the zirconates. • XRD confirmed the formation of required phase. • Increased electrical resistivity makes these materials useful for microwave devices. • Dielectric parameters of zirconates decrease with increasing frequency. • Dielectric constant decreases with increasing substituents concentration. - Abstract: A hydrothermal method was successfully employed for the synthesis of a series of vanadium and germanium co-doped pyrochlore lanthanum zirconates with composition La{sub 2−x}V{sub x}Zr{sub 2−y}Ge{sub y}O{sub 7} (where x, y = 0.0, 0.25, 0.50, 0.75 and 1.0). The XRD and FTIR analyses confirmed the formation of single phase except vanadium and germanium substituted samples and the crystallite sizes are in the range of 7–31 nm for V{sup 3+}–Ge{sup 4+} substituted samples. The theoretical compositions are confirmed by the ED-XRF studies. The room temperature electrical resistivity increase with the substituents concentration which suggests that the synthesized materials can be used for microwave devices as such devices required highly resistive materials. Dielectric properties were measured in the frequency range of 6 kHz to 1 MHz. The dielectric parameters decrease with increase in frequency. The DC resistivity data is in good agreement with the dielectric data.

  20. Hydrothermal synthesis of MnO2/CNT nanocomposite with a CNT core/porous MnO2 sheath hierarchy architecture for supercapacitors

    PubMed Central

    2012-01-01

    MnO2/carbon nanotube [CNT] nanocomposites with a CNT core/porous MnO2 sheath hierarchy architecture are synthesized by a simple hydrothermal treatment. X-ray diffraction and Raman spectroscopy analyses reveal that birnessite-type MnO2 is produced through the hydrothermal synthesis. Morphological characterization reveals that three-dimensional hierarchy architecture is built with a highly porous layer consisting of interconnected MnO2 nanoflakes uniformly coated on the CNT surface. The nanocomposite with a composition of 72 wt.% (K0.2MnO2·0.33 H2O)/28 wt.% CNT has a large specific surface area of 237.8 m2/g. Electrochemical properties of the CNT, the pure MnO2, and the MnO2/CNT nanocomposite electrodes are investigated by cyclic voltammetry and electrochemical impedance spectroscopy measurements. The MnO2/CNT nanocomposite electrode exhibits much larger specific capacitance compared with both the CNT electrode and the pure MnO2 electrode and significantly improves rate capability compared to the pure MnO2 electrode. The superior supercapacitive performance of the MnO2/CNT nancomposite electrode is due to its high specific surface area and unique hierarchy architecture which facilitate fast electron and ion transport. PMID:24576342

  1. Synthesis and application of TiO2 single-crystal nanorod arrays grown by multicycle hydrothermal for dye-sensitized solar cells

    NASA Astrophysics Data System (ADS)

    Zhu, Jian-Jing; Zhao, Yu-Long; Zhu, Lei; Gu, Xiu-Quan; Qiang, Ying-Huai

    2014-04-01

    TiO2 is a wide band gap semiconductor with important applications in photovoltaic cells. Vertically aligned TiO2 nanorod arrays (NRs) are grown on the fluorine-doped tin oxide (FTO) substrates by a multicycle hydrothermal synthesis process. The samples are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), and selected-area electron diffraction (SAED). It is found that dye-sensitized solar cells (DSSCs) assembled by the as-prepared TiO2 single-crystal NRs exhibit different trends under the condition of different nucleation and growth concentrations. Optimum cell performance is obtained with high nucleation concentration and low growth cycle concentration. The efficiency enhancement is mainly attributed to the improved specific surface area of the nanorod.

  2. Magnesium phosphate pentahydrate nanosheets: Microwave-hydrothermal rapid synthesis using creatine phosphate as an organic phosphorus source and application in protein adsorption.

    PubMed

    Qi, Chao; Zhu, Ying-Jie; Wu, Cheng-Tie; Sun, Tuan-Wei; Chen, Feng; Wu, Jin

    2016-01-15

    Magnesium phosphate materials have aroused interest of researchers in recent years and are promising for biomedical applications due to their good biocompatibility and biodegradability. In this work, we report the microwave-hydrothermal rapid synthesis of magnesium phosphate pentahydrate nanosheets (MPHSs) using biocompatible creatine phosphate as an organic phosphorus source. This method is facile, rapid, surfactant-free and environmentally friendly. The as-prepared MPHSs have an obvious pH-dependent dissolution performance which can be used as an ideal pH-responsive nanocarrier for drug and gene delivery. Moreover, the MPHSs have a good cytocompatibility and a high ability to promote osteoblast MC-3T3 adhesion and spreading, as well as a relatively high protein adsorption ability using hemoglobin (Hb) as a model protein. Thus, the MPHSs are promising for the applications in biomedical fields such as protein adsorption and bone regeneration.

  3. One-pot hydrothermal synthesis of magnetically recoverable palladium/reduced graphene oxide nanocomposites and its catalytic applications in cross-coupling reactions.

    PubMed

    Fu, Wenzhi; Zhang, Zhuqing; Zhuang, Peiyuan; Shen, Jianfeng; Ye, Mingxin

    2017-07-01

    A facile, green, economical approach was designed to deposit palladium nanoparticles on magnetic reduced graphene oxide nanosheets (Pd-Fe3O4/rGO) via a one-pot hydrothermal synthesis method. The prepared Pd-Fe3O4/rGO nanocomposites were thoroughly characterized by Transmission electron microscopy, Scanning electron microscopy, Fourier-transform infrared spectroscopy, X-ray diffraction, and Raman spectroscopy. Importantly, the highly efficient catalytic property of the as-obtained Pd-Fe3O4/rGO catalyst was demonstrated for the Suzuki-Miyaura coupling reaction and Mizoroki-Heck coupling reaction. Significantly, the Suzuki-Miyaura coupling reactions could be efficiently performed in an environmentally friendly aqueous solution with no need for further additives. Besides, the nanocomposites could be conveniently separated from reaction system with an external permanent magnet for recycling and the inherent catalytic activity of the nanocomposites did not exacerbate after six repeated applications.

  4. Hydrothermal synthesis of flowerlike SnO{sub 2} nanorod bundles and their application for lithium ion battery

    SciTech Connect

    Wen, Zhigang; Zheng, Feng; Yu, Hongchun; Jiang, Ziran; Liu, Kanglian

    2013-02-15

    SnO{sub 2} nanorod bundles were synthesized by hydrothermal method. Field-emission scanning electron microscopy and transmission electron microscopy images showed that the as-prepared flowerlike SnO{sub 2} nanorod bundles consist of tetragonal nanorods with size readily tunable. Their electrochemical properties and application as anode for lithium-ion battery were evaluated by galvanostatic discharge–charge testing and cycle voltammetry. SnO{sub 2} nanorod flowers possess improved discharge capacity of 694 mA h g{sup −1} up to 40th cycle at 0.1 C. - Highlights: ► The flowerlike SnO{sub 2} nanorod bundles were synthesized by hydrothermal method. ► SnO{sub 2} nanorod bundles with tunable size by controlling concentration of SnCl{sub 4}. ► A probable formation mechanism of SnO{sub 2} nanorod bundles has been proposed.

  5. Hydrothermal synthesis and photoelectrochemical performance enhancement of TiO2/graphene composite in photo-generated cathodic protection

    NASA Astrophysics Data System (ADS)

    Zhang, Weiwei; Guo, Hanlin; Sun, Haiqing; Zeng, Rong-Chang

    2016-09-01

    TiO2/graphene composites were synthesized through one-step hydrothermal method. The composites show an enhancement in photo-generated cathodic protection as the time-dependent profiles of photocurrent responses has confirmed. XRD data show that a bicrystalline framework of anatase and brookite formed as graphene provided donor groups in the hydrothermal process. The transfer of photoinduced electrons in the biphasic TiO2 results in effective electron-hole separation. Moreover, graphene lead to a negative shift of the Fermi level as evidenced by Mott-Schottky analysis, which decreases the Schottky barrier formed in the TiO2 and 304 stainless steel interface and results in the enhancement of photo-generated cathodic protection.

  6. Comparative study of nanocrystalline titanium dioxide obtained through sol-gel and sol-gel-hydrothermal synthesis.

    PubMed

    Seck, E I; Doña-Rodríguez, J M; Pulido Melián, E; Fernández-Rodríguez, C; González-Díaz, O M; Portillo-Carrizo, D; Pérez-Peña, J

    2013-06-15

    TiO2 particles were prepared by sol-gel method alone and by sol-gel method combined with hydrothermal treatment. The structural and photocatalytic properties of the two series of photocatalysts were compared. XRD studies revealed that rutilization was faster in the series of photocatalysts, which had been additionally subjected to a hydrothermal process (SG-HT). The hydrothermally treated photocatalysts also displayed a higher specific surface area than those which had only been synthesized using the sol-gel process (SG) and subjected to low calcination temperatures of up to 873 K, while this tendency was inverted at higher temperatures. In accordance with the above observation, the hydrothermally treated series of photocatalysts had a lower particle size than the SG series calcined immediately after the sol-gel process up to 873 K, with this relation being inverted for the highest two temperatures which were studied (973 K and 1023 K) and which saw the commencement of rutilization. Increases in average particle size were observed for both series, with a polyhedral morphology seen as calcination temperature rose. FTIR studies highlighted the presence of the band at 2351 cm(-1) in the SG-HT photocatalysts, characteristic of surface-adsorbed CO2. This was not seen in the SG or P25 photocatalysts. In terms of photoreactivity, the best photocatalyst in the SG-HT series was that calcined at 923 K and in the SG series at 1023 K (SG-1023). Comparing these two photocatalysts and the commercial P25 photocatalyst, SG-1023 was found to be the most photoactive in both the photodegradation and the mineralization of phenol.

  7. Controlled synthesis of BiVO{sub 4} with multiple morphologies via an ethylenediamine-assisted hydrothermal method

    SciTech Connect

    Qi, Xuemei; Zhu, Xinyuan; Wu, Jiang; Wu, Qiang; Li, Xian; Gu, Miaoli

    2014-11-15

    Graphical abstract: BiVO{sub 4} samples with various morphologies were synthesized via a simple ethylenediamine (EN) assisted hydrothermal route. One of the mixed crystal phase with spherical and porous morphology showed excellent photocatalytic activity and about 90% Rhodamine B was degraded after 140 min visible light irradiation. - Highlights: • BiVO{sub 4} samples with various morphologies were synthesized by hydrothermal method. • Ethylenediamine mainly acts as alkaline source to adjust pH values of precursor. • BiVO{sub 4} with spherical morphology has excellent photocatalytic activity. - Abstract: In this work, BiVO{sub 4} particles with different crystal structures and morphologies including hexahedral, spherical porous and hyperbranched ones were fabricated in the presence of ethylenediamine by hydrothermal process. The as-fabricated samples were well characterized by X-ray diffraction, scanning electron microscopy, Fourier transform infrared spectroscopy, Raman spectroscopy and ultraviolet–visible absorption spectroscopy. The results showed that the morphology and crystal structure of BiVO{sub 4} particles could be well controlled by only changing the ethylenediamine content in the deionized water solution. Photocatalytic activity of the samples was evaluated by the degradation of Rhodamine B under visible-light irradiation. It was shown that BiVO{sub 4} sample with spherical porous morphology and mixed crystal phase exhibited the best photocatalytic performance after optimizing the ethylenediamine content. The best degradation ratio of Rhodamine B could reach about 87% after 140 min visible-light irradiation.

  8. Synthesis of bilayer MoS{sub 2} nanosheets by a facile hydrothermal method and their methyl orange adsorption capacity

    SciTech Connect

    Ye, Lijuan; Xu, Haiyan; Zhang, Dingke; Chen, Shijian

    2014-07-01

    Highlights: • Hexagonal phase of MoS{sub 2} nanosheets was synthesized by a facile hydrothermal method. • FE-SEM and TEM images show the sheets-like morphology of MoS{sub 2}. • Bilayer MoS{sub 2} can be grown under the optimized mole ratio of 2:1 of S:Mo at 180 °C for 50 h. • The MoS{sub 2} nanosheets possess high methyl orange adsorption capacity due to the large surface area. - Abstract: Molybdenum disulfide (MoS{sub 2}) nanosheets have received significant attention recently due to the potential applications for exciting physics and technology. Here we show that MoS{sub 2} nanosheets can be prepared by a facile hydrothermal method. The study of the properties of the MoS{sub 2} nanosheets prepared at different conditions suggests that the mole ratio of precursors and hydrothermal time significantly influences the purity, crystalline quality and thermal stability of MoS{sub 2}. X-ray diffraction, Raman spectra and transmission electron microscopy results indicate that bilayer MoS{sub 2} can be grown under an optimized mole ratio of 2:1 of S:Mo at 180 °C for 50 h. Moreover, such ultrathin nanosheets exhibit a prominent photoluminescence and possess high methyl orange adsorption capacity due to the large surface area, which can be potentially used in photodevice and photochemical catalyst.

  9. 1-Dodecane-sulfonic-acid-sodium-salt(LAS) assisted hydrothermal synthesis of Cd{sub x}Zn{sub 1-x}S solid solution as efficient photocatalysts under visible light irradiation

    SciTech Connect

    Jia, B.; Guo, L. J.

    2010-03-01

    With anionic surfactant LAS assisted, series of zinc cadmium sulfide semiconductor photocatalysts were synthesized by hydrothermal method. These products were characterized by X-ray diffraction (XRD), UV-Vis absorption spectra (UV-Vis) and scanning electron microscopy (FESEM). The photocatalytic activities of as-prepared samples were evaluated by photocatalytic hydrogen production from water under visible-light irradiation. The best synthesis parameters are: Composition 0.9:0.1 (Cd:Zn molar ratio), Temperature 160 deg. C, Hydrothermal Time 48 Hour, LAS Concentration 1.7 mmol/L, the maximum visible-light-catalytic hydrogen production rate is 161.25 {mu}mol/h (lambda>430 nm) which is higher than those of by coprecipitation method. The experiment results indicate that surfactant assisted hydrothermal method is an effective way to get highly active CdZnS solid solution photocatalyst.

  10. Global synthesis and analysis of deep-sea hydrothermal time-series data: Toward a characterization of the outflow dynamics

    NASA Astrophysics Data System (ADS)

    Barreyre, T.; Sohn, R. A.; Crone, T. J.

    2014-12-01

    Time-series records of mid-ocean ridge hydrothermal fluid properties and flow rates have the potential to help constrain the hydrogeology, subsurface circulation patterns, heat, mass, and chemical fluxes, and habitat conditions within young oceanic crust. This potential has motivated a concerted international effort to acquire such records from a variety of geologically distinct vent fields at numerous locations along the mid-ocean ridge system. However up until now, the global database has not been systematically explored. These records have only been analyzed in a piecemeal fashion, which is problematic because hydrothermal time-series records from individual sites typically exhibit enigmatic modes of episodic and periodic variability that are difficult to interpret in isolation. In this study, we conduct a systematic analysis of the extant set of hydrothermal time-series records from several mid-ocean ridge sites where observatory-style experiments have been conducted (including, LSHF, TAG, EPR 9°50'N and MEF). We show that most temperature records, regardless of location or geological setting, display systematic tide-related variability, with the strongest signal at the principal semidiurnal tidal periods (M2, S2, N2 and K2). Cross-spectral multi-taper methods applied to the temperature and bottom pressure records reveal robust phase relationships, particularly for the high-temperature, black-smoker records, as predicted by poroelastic theory. These results suggest that tidal pressures diffusely propagate through the formation, perturbing fluid velocities and temperatures, resulting in phase lags between the seafloor loading and the exit-fluid temperatures. Here, we use multi-layer analytical and numerical models to constrain the subseafloor permeability, skin depth, and Darcy velocities required to explain the phase lag observations.

  11. Hydrothermal synthesis of highly crystalline ZnO nanorod arrays: Dependence of morphology and alignment on growth conditions

    NASA Astrophysics Data System (ADS)

    Azzez, Shrook A.; Hassan, Z.; Hassan, J. J.; Alimanesh, M.; Rasheed, Hiba S.; Sabah, Fayroz A.; Abdulateef, Sinan A.

    2016-07-01

    Highly oriented zinc oxide nanorod were successfully grown on seeded p-type silicone substrate by hydrothermal methode. The morphology and the crystallinty of ZnO c-axis (002) arrays were systematically studied using field emission scanning electron microscopy (FESEM) and X-ray diffraction (XRD) methods. The effect of seed layer pre-annealing on nanorods properties was explained according to the nucleation site of ZnO nanoparticles on silicon substrate. In addition, the variation of the equal molarity of zinc nitrate hexahydrate and hexamine concentrations in the reaction vessel play a crucial role related to the ZnO nanorods.

  12. Microwave-Hydrothermal Synthesis of SnO2-CNTs Hybrid Nanocomposites with Visible Light Photocatalytic Activity

    PubMed Central

    Wu, Shuisheng; Dai, Weili

    2017-01-01

    SnO2 nanoparticles coated on carbon nanotubes (CNTs) were prepared via a simple microwave-hydrothermal route. The as-obtained SnO2-CNTs composites were characterized using X-ray powder diffraction, Raman spectroscopy, and transmission electron microscopy. The photocatalytic activity of as-prepared SnO2-CNTs for degradation of Rhodamine B under visible light irradiation was investigated. The results show that SnO2-CNTs nanocomposites have a higher photocatalytic activity than pure SnO2 due to the rapid transferring of electrons and the effective separation of holes and electrons on SnO2-CNTs. PMID:28336888

  13. Microwave-Hydrothermal Synthesis of SnO2-CNTs Hybrid Nanocomposites with Visible Light Photocatalytic Activity.

    PubMed

    Wu, Shuisheng; Dai, Weili

    2017-03-03

    SnO2 nanoparticles coated on carbon nanotubes (CNTs) were prepared via a simple microwave-hydrothermal route. The as-obtained SnO2-CNTs composites were characterized using X-ray powder diffraction, Raman spectroscopy, and transmission electron microscopy. The photocatalytic activity of as-prepared SnO2-CNTs for degradation of Rhodamine B under visible light irradiation was investigated. The results show that SnO2-CNTs nanocomposites have a higher photocatalytic activity than pure SnO2 due to the rapid transferring of electrons and the effective separation of holes and electrons on SnO2-CNTs.

  14. Tartaric acid assisted hydrothermal synthesis of different flower-like ZnO hierarchical architectures with tunable optical and oxygen vacancy-induced photocatalytic properties

    NASA Astrophysics Data System (ADS)

    Liu, Tingzhi; Li, Yangyang; Zhang, Hao; Wang, Min; Fei, Xiaoyan; Duo, Shuwang; Chen, Ying; Pan, Jian; Wang, Wei

    2015-12-01

    Different flower-like ZnO hierarchical architectures were prepared by tartaric acid assisted hydrothermal synthesis, especially four flower-like ZnO nanostructures were obtained simultaneously under the same reaction condition. The cauliflower-like ZnO is assembled by spherical shaped nanoparticles, and the chrysanthemum-like and other flower-like ZnO nanostructures are assembled by hexagonal rods/prisms with from planar to semi-pyramid, and to pyramid tips. TA acts as a capping agent and structure-directing agent during the synthesis. All ZnO possess the hexagonal wurtzite structure. The PL spectra can be tuned by changing TA concentration. XRD, PL and Raman spectra confirmed that oxygen vacancies mainly come from the ZnO surface. The flower-like samples of 1:4.5 and 1:3 with the largest aspect ratios have highest photocatalytic performance. They decompose 85% MB within 60 min. Combining PL Gaussian fitting with K, the higher content of oxygen vacancy is, the higher photocatalytic activity is. The enhanced photocatalytic performance is mainly induced by oxygen vacancy of ZnO. The possible formation mechanism, growth and change process of flower-like ZnO were proposed.

  15. Ethylenediamine-Assisted Hydrothermal Synthesis of NaCaSiO3OH: Controlled Morphology, Mechanism, and Luminescence Properties by Doping Eu(3+)/Tb(3).

    PubMed

    Chen, Mingyue; Xia, Zhiguo; Liu, Quanlin

    2016-11-07

    This paper demonstrates a facile hydrothermal method using ethylenediamine (EDA) as a "shape modifier" for the controlled synthesis of rod bunch, decanedron, spindle, flakiness, and flowerlike NaCaSiO3OH microarchitectures. The set of experimental conditions is important to obtain adjustable shape and size of NaCaSiO3OH particles, as the change in either the amount of EDA/H2O or reaction time, or the amount of NaOH. Accordingly, the crystal growth mechanism during the synthesis process is proposed, and it is found that the EDA, acting as the chelating agent and shape modifier, plays a crucial role in fine-tuning the NaCaSiO3OH morphology. Morphology evolution process of flowerlike NaCaSiO3OH as a function of NaOH is also explained in detail. Eu(3+)/Tb(3+) doped NaCaSiO3OH samples exhibit strong red and green emission under ultraviolet excitation, corresponding to the characteristic electronic transitions of Eu(3+) and Tb(3+). These results imply that the morphology-tunable NaCaSiO3OH:Eu(3+)/Tb(3+) microarchitectures with tunable luminescence properties are expected to have promising applications for micro/nano optical functional devices.

  16. Hydrothermal synthesis of Mn vanadate nanosheets and visible-light photocatalytic performance for the degradation of methyl blue

    SciTech Connect

    Pei, L.Z. Xie, Y.K.; Pei, Y.Q.; Jiang, Y.X.; Yu, H.Y.; Cai, Z.Y.

    2013-07-15

    Graphical abstract: - Highlights: • Mn vanadate nanosheets have been synthesized by simple hydrothermal process. • The formation of Mn vanadate nanosheets can be controlled by growth conditions. • Mn vanadate nanosheets exhibit good photocatalytic activities for methyl blue. - Abstract: Mn vanadate nanosheets have been synthesized via a facile hydrothermal route using ammonium metavanadate and Mn acetate as the raw materials, polyvinyl pyrrolidone (PVP) as the surfactant. X-ray diffraction (XRD) shows that the Mn vanadate nanosheets are composed of monoclinic MnV{sub 2}O{sub 6} phase. Scanning electron microscopy (SEM) observation indicates that the nanosheets have the average thickness of about 50 nm, length of 2–10 μm and width of 800 nm to 2 μm. The growth process of the Mn vanadate nanosheets has also been discussed based on the analysis of the roles of the growth conditions on the formation of the Mn vanadate nanosheets. The nanosheets show good photocatalytic activities for the degradation of methylene blue (MB) under visible light irradiation. About 72.96% MB can be degraded after visible light irradiation for 1 h over 10 mg Mn vanadate nanosheets in 10 mL MB solution with the concentration of 10 mg L{sup −1}.

  17. L-Cysteine-assisted hydrothermal synthesis of nickel disulfide/graphene composite with enhanced electrochemical performance for reversible lithium storage

    NASA Astrophysics Data System (ADS)

    Chen, Qiannan; Chen, Weixiang; Ye, Jianbo; Wang, Zhen; Lee, Jim Yang

    2015-10-01

    NiS2/graphene composite is synthesized by a facile hydrothermal reaction between NiCl2 and L-cysteine in the presence of graphene oxide sheets. L-Cysteine serves as both the sulfur source for NiS2 and reductant for reduction of graphene oxide sheets. The reduced graphene oxides can be used as a platform for growth of NiS2 particles and restrain NiS2 from agglomerating during hydrothermal process. The results of characterizations show that the sphere-like NiS2 particles exhibit smaller sizes and are well dispersed on the surface of reduced graphene sheets. The electrochemical measurements demonstrate that the NiS2/graphene composite delivers a reversible capacity as high as 1200 mAh g-1 at a current density of 100 mA g-1 and enhanced high-rate capability of 740 mAh g-1 at a high current density of 1000 mA g-1. After 1000 cycles, the NiS2/graphene still preserves the reversible capacity about 810 mAh g-1 at a current density of 500 mA g-1, indicating its excellent cyclic stability.

  18. Hydrothermal synthesis and characterization of Si and Sr co-substituted hydroxyapatite nanowires using strontium containing calcium silicate as precursors.

    PubMed

    Zhang, Na; Zhai, Dong; Chen, Lei; Zou, Zhaoyong; Lin, Kaili; Chang, Jiang

    2014-04-01

    In the absence of any organic surfactants and solvents, the silicon (Si) and strontium (Sr) co-substituted hydroxyapatite [Ca10(PO4)6(OH)2, Si/Sr-HAp] nanowires were synthesized via hydrothermal treatment of the Sr-containing calcium silicate (Sr-CS) powders as the precursors in trisodium phosphate (Na3PO4) aqueous solution. The morphology, phase, chemical compositions, lattice constants and the degradability of the products were characterized. The Si/Sr-HAp nanowires with diameter of about 60nm and up to 2μm in length were obtained after hydrothermal treatment of the Sr-CS precursors. The Sr and Si substitution amount of the HAp nanowires could be well regulated by facile tailoring the Sr substitution level of the precursors and the reaction ratio of the precursor/solution, respectively. The SiO4 tetrahedra and Sr(2+) ions occupied the crystal sites of the HAp, and the lattice constants increased apparently with the increase of the substitution amount. EDS mapping also suggested the uniform distribution of Si and Sr in the synthetic nanowires. Moreover, the Si/Sr-substitution apparently improved the degradability of the HAp materials. Our study suggested that the precursor transformation method provided a facile approach to synthesize the Si/Sr co-substituted HAp nanowires with controllable substitution amount, and the synthetic Si/Sr-HAp nanowires might be used as bioactive materials for hard tissue regeneration applications.

  19. Synthesis and photocatalytic activity for water-splitting reaction of nanocrystalline mesoporous titania prepared by hydrothermal method

    SciTech Connect

    Jitputti, Jaturong; Pavasupree, Sorapong; Suzuki, Yoshikazu; Yoshikawa, Susumu

    2007-05-15

    Nanocrystalline mesoporous TiO{sub 2} was synthesized by hydrothermal method using titanium butoxide as starting material. XRD, SEM, and TEM analyses revealed that the synthesized TiO{sub 2} had anatase structure with crystalline size of about 8 nm. Moreover, the synthesized titania possessed a narrow pore size distribution with average pore diameter and high specific surface area of 215 m{sup 2}/g. The photocatalytic activity of synthesized TiO{sub 2} was evaluated with photocatalytic H{sub 2} production from water-splitting reaction. The photocatalytic activity of synthesized TiO{sub 2} treated with appropriate calcination temperature was considerably higher than that of commercial TiO{sub 2} (Ishihara ST-01). The utilization of mesoporous TiO{sub 2} photocatalyst with high crystallinity of anatase phase promoted great H{sub 2} production. Furthermore, the reaction temperature significantly influences the water-splitting reaction. - Graphical abstract: Nanocrystalline mesoporous TiO{sub 2} was synthesized by hydrothermal method. The physical properties of the synthesized TiO{sub 2} were thoroughly studied in relation to its photocatalytic activity for H{sub 2} evolution from water-splitting reaction. It was found that the photocatalytic activity of synthesized TiO{sub 2} treated with appropriate calcination temperature was considerably higher than that of commercial TiO{sub 2} (Ishihara ST-01)

  20. A facile in-situ hydrothermal synthesis of SrTiO3/TiO2 microsphere composite

    NASA Astrophysics Data System (ADS)

    Wang, Hongxing; Zhao, Wei; Zhang, Yubo; Zhang, Shimeng; Wang, Zihao; Zhao, Dan

    2016-06-01

    TiO2 was successfully used as sacrificed template to synthesise SrTiO3/TiO2 microsphere composite via an in-situ hydrothermal process. The diameter of SrTiO3/TiO2 microsphere was about 700 nm with the same size of the template, and all of the microspheres were in good dispersity. The optimized reaction parameters for the phase and morphology of the as-synthesized samples were investigated. The results showed the SrTiO3/TiO2 microsphere can be synthesized at 170 °C when the concentration of sodium hydroxide was 0.1 M. Lower hydrothermal temperature hampered the formation of the SrTiO3/TiO2 composite, the higher alkali concentration, however, will destroy the morphology of products. The formation mechanism of SrTiO3/TiO2 microsphere composite was proposed and the photocatalytic properties of the samples were characterized using methylene blue solution as the pollutant under the UV light irradiation. The results indicated the proper OH- concentration will provide a channel for Sr2+ to react with Ti4+ located in the template and form the SrTiO3/TiO2 composite, and those with micro-scaled spherical morphology exhibited good photocatalytic activities.

  1. Synthesis of zinc aluminate with high surface area by microwave hydrothermal method applied in the transesterification of soybean oil (biodiesel)

    SciTech Connect

    Quirino, M.R.; Oliveira, M.J.C.; Keyson, D.; Lucena, G.L.; Oliveira, J.B.L.; Gama, L.

    2016-02-15

    Highlights: • ZnAl{sub 2}O{sub 4} spinel was synthesized by the microwave hydrothermal method in only 15 or 30 min. • The powders show high specific surface area. • ZAT{sub b}15 showed activity of 52.22% for the conversion of soybean oil into biodiesel. - Abstract: Zinc aluminate is a material with high thermal stability and high mechanical strength that, owing to these properties, is used as a catalyst or support. In this work, zinc aluminate spinel was synthesized by the microwave hydrothermal method in only 15 or 30 min at a low temperature (150 °C) without templates, using only Al(NO{sub 3}){sub 3}·9H{sub 2}O, Zn(NO{sub 3}){sub 2}·6H{sub 2}O, and urea as precursors and applied in the transesterification of soybean oil. X-ray diffraction analysis showed that ZnAl{sub 2}O{sub 4} had a cubic structure without secondary phases. The nitrogen adsorption measurements (BET) revealed a high surface area (266.57 m{sup 2} g{sup −1}) for the nanopowder synthesized in 15 min. This powder showed activity of 52.22% for the catalytic conversion of soybean oil into biodiesel by transesterification.

  2. One-step synthesis of intrinsically functionalized fluorescent carbon nanoparticles by hydrothermal carbonization from different carbon sources

    NASA Astrophysics Data System (ADS)

    Shen, Chen; Yao, Wei; Lu, Yun

    2013-10-01

    Highly functionalized carbon nanoparticles (F-CNPs) with average sizes of 5-30 nm were fabricated by hydrothermal carbonization of specific carbon sources at a mild temperature without usual strong acid treatment or surface modification. The morphology, structure, and fluorescent properties of the nanoparticles were characterized by transmission electron microscopy, dynamic light scattering, Fourier-transform infrared spectra, X-ray photoelectron spectroscopy, Raman spectra and fluorescent spectrophotometer. As a result, the abundant carboxylic, sulfonic, amine, or ethanamide groups were furnished on the surface of these carbon nanoparticles, offering the reaction sites for their possible further functionalization, and these functional groups also enhance the dispersion of carbon nanoparticles which are kept without precipitation for months. The hydrothermal treatment which is simple, green, and economical, also can endow the F-CNPs much more carboxyl groups, thus improving the quantum efficiency of as-prepared products. These functionalized carbon nanoparticles demonstrate the excitation wavelength-independent photoluminescence behavior, implying their potential applications in biological labeling, imaging, and chromatography.

  3. Hydrothermal synthesis and potential applicability of rhombohedral siderite as a high-capacity anode material for lithium ion batteries

    NASA Astrophysics Data System (ADS)

    Zhao, Shiqiang; Yu, Yue; Wei, Shanshan; Wang, Yuxi; Zhao, Chenhao; Liu, Rui; Shen, Qiang

    2014-05-01

    Natural siderite is a valuable iron mineral composed of ferrous carbonate (FeCO3), which is commonly found in hydrothermal veins and contains no sulfur or phosphorus. In this paper, micro-sized FeCO3 crystallites are synthesized via a facile hydrothermal route, and almost all of them possess a rhombohedral shape similar to that of natural products. When applied as an anode material for lithium ion batteries, the synthetic siderite can deliver an initial specific discharge capacity of ∼1587 mAh g-1 with a coulombic efficiency of 68% at 200 mA g-1, remaining a reversible value of 1018 mAh g-1 over 120 cycles. Even at a high current density of 1000 mA g-1, after 120 cycles the residual specific capacity (812 mAh g-1) is still higher than the theoretical capacity of FeCO3 (463 mAh g-1). Moreover, a novel reversible conversion mechanism accounts for the excellent electrochemical performances of rhombohedral FeCO3 to a great extent, implying the potential applicability of synthetic siderite as lithium ion battery anodes.

  4. Hydrothermal synthesis and characterization of hybrid Al/ZnO-GO composite for significant photodegrdation of dyes

    NASA Astrophysics Data System (ADS)

    Lellala, Kashinath; Namratha, K.; Sudhakar, K.; Byrappa, K.

    2016-05-01

    In the present work, undoped and doped Aluminum/Zinc Oxide - graphene oxide (Al/ZnO-GO) nanocomposite have been successfully synthesized by hydrothermal method from zinc acetate and aluminum nitrate solutions without using of any surfactant/stabilizing agents. The results show that the composites of GO nanosheets are decorated densely by Al/ZnO nanoparticles, which displays a good morphology and blend between GO and Al/ZnO. Hybrid composites exhibit an enhanced photocatalytic performance in reduction of dyes under UV-Vis radiation better than bare ZnO-GO and GO for methylene blue dye. The hydrothermal method leads to particles with a higher crystalline due to ambient temperature of the reaction and autogenously pressure conditions, which alters the phases and crystallizations of the nanocomposite. The optical band gap is narrowed to lower energy values due to controlled addition of aluminum and GO in the composite. The improved optical property in Al-doped ZnO flower decorated on GO can be attributed to the decrease in oxygen deficiency after Al doping. XRD, FTIR, UV-Vis spectroscopy, Raman, and Field Emission Scanning Electron Microscopy characterized the effects of Al doping on the structural characteristics and optical properties on the ZnO-GO.

  5. Hydrothermal synthesis of superparamagnetic Fe{sub 3}O{sub 4} nanoparticles with ionic liquids as stabilizer

    SciTech Connect

    Liu, Xiao-Di Chen, Hao; Liu, Shan-Shan; Ye, Li-Qun; Li, Yin-Ping

    2015-02-15

    Highlights: • Superparamagnetic Fe{sub 3}O{sub 4} nanoparticles with good dispersity have been synthesized via hydrothermal method. • Ionic liquid [C{sub 16}mim]Cl acts as stabilizer for the Fe{sub 3}O{sub 4} nanoparticles. • Fe{sub 3}O{sub 4} nanoparticles have a saturation magnetization of 67.69 emu/g at 300 K. - Abstract: Superparamagnetic Fe{sub 3}O{sub 4} nanoparticles have been successfully synthesized under hydrothermal condition with the assistant of ionic liquid 1-hexadecyl-3-methylimidazolium chloride ([C{sub 16}mim]Cl). The structure and morphology of the sample have been investigated by X-ray diffraction (XRD), X-ray photoelectron spectra (XPS), transmission electron microscopy (TEM), and high-resolution TEM (HRTEM), and the results indicate that the as-synthesized inverse spinel Fe{sub 3}O{sub 4} nanoparticles have an average diameter of about 10 nm and exhibit relatively good dispersity. More importantly, it is found that [C{sub 16}mim]Cl acts as stabilizer for the Fe{sub 3}O{sub 4} nanoparticles by adsorbing on the particles surfaces to prevent the agglomeration. In addition, the obtained superparamagnetic Fe{sub 3}O{sub 4} nanoparticles have a saturation magnetization of 67.69 emu/g at 300 K.

  6. Sonochemical assisted hydrothermal synthesis of pseudo-flower shaped Bismuth vanadate (BiVO4) and their solar-driven water splitting application.

    PubMed

    Khan, Ibrahim; Ali, Shahid; Mansha, Muhammad; Qurashi, Ahsanulhaq

    2017-05-01

    Bismuth vanadate (BiVO4) is a well-known photocatalyst due to its lower bandgap (Eg) and visible electromagnetic light absorption capacity. Herein, we reported the pulse ultra-sonochemical assisted hydrothermal approach to synthesize S-BiVO4. For the comparison purpose, H-BiVO4 is also synthesized via conventional hydrothermal approach. The surface morphology of S-BiVO4 through scanning electron microscope (SEM) indicates condensed microarrays (MAs) having pseudo-flower shapes. The energy dispersive X-rays (EDX) spectrum also confirmed the elemental percent composition of Bi, V and O in BiVO4. X-rays diffraction (XRD) pattern further confirmed the monoclinic scheelite phase of S-BiVO4. Fourier transformed infrared (FTIR) spectrum showed Bi-O and Bi-V-O vibrational bands at 1382 and 1630cm(-1), respectively. The diffuse reflectance spectroscopy (DRS) indicated absorption edge at ∼515nm, corresponds to bandgap value (Eg) of 2.41eV, which is suitable range for water splitting applications. The photocurrent density from water splitting under artificial 1 SUN visible light source found at 60 and 50μA/cm(2) for S-BiVO4 and H-BiVO4, respectively. The stability test through chronoamperometry showed that S-BiVO4 was more stable than H-BiVO4. It can be depicted from the growth mechanism that ultrasonication played a definite role in the overall synthesis of pseudo-flower shaped S-BiVO4 MAs.

  7. Hydrothermal synthesis of Li{sub 4}Ti{sub 5}O{sub 12}/C nanostructured composites: Morphology and electrochemical performance

    SciTech Connect

    Vujković, Milica; Stojković, Ivana; Mitrić, Miodrag; Mentus, Slavko; Cvjetićanin, Nikola

    2013-02-15

    Graphical abstract: Display Omitted Highlights: ► Nanostructured composite Li{sub 4}Ti{sub 5}O{sub 12}/C was obtained hydrothermally. ► The amount of carbon black influenced significantly the morphology of the composite. ► Rate capability of Li{sub 4}Ti{sub 5}O{sub 12} was improved by the synthesis in presence of carbon black. ► Coulombic capacity of 150 mAh g{sup −1} was obtained at a discharging rate of even 10 C. -- Abstract: Li{sub 4}Ti{sub 5}O{sub 12}/C composites with low (3 wt.%) and high (33 wt.%) carbon black content as well as carbon-free Li{sub 4}Ti{sub 5}O{sub 12} were prepared in two steps under identical conditions: hydrothermal reaction at 130 °C and post-calcination at 400 °C. The X-ray diffraction experiments confirmed the spinel structure of Li{sub 4}Ti{sub 5}O{sub 12} in all samples. The carbon content altered significantly the morphology of obtained micro/nanoparticles. The Li{sub 4}Ti{sub 5}O{sub 12}/C composite with the high carbon content showed the highest electrical conductivity (2.0 S cm{sup −1}), and displayed also extraordinary electrochemical performance: the cyclovoltammograms consisted of well defined reversible redox peaks at a scan rate as high as 10 mV s{sup −1}, while, by galvanostatic cycling, the coulombic capacity of 150 mAh g{sup −1} was evidenced at a discharging rate of 10 C.

  8. Hydrothermal synthesis attempts of dawsonite-type hydroxymetalocarbonate precursor compounds for catalytic Ho, Sm, and La oxides

    SciTech Connect

    Ali, Asma A.; Hasan, Muhammad A.; Zaki, Mohamed I.

    2008-01-08

    Chemical interactions in mixed, aqueous solutions of NH{sub 4}HCO{sub 3} and M(NO{sub 3}){sub 3}.9H{sub 2}O, where M stands for Ho, Sm, or La, were facilitated under various hydrothermal treatment conditions (pH 8-12 and temperature = 75-135 deg. C). The solution chemistry established did not make available necessary concentrations of soluble HCO{sub 3}{sup -} and MO(OH){sub 2}{sup -} species for the formation of dawsonite-type ammonium hydroxymetalocarbonates, NH{sub 4}M(CO{sub 3})(OH){sub 2}, but, alternatively, high concentrations of soluble CO{sub 3}{sup 2-}, and M(H{sub 2}O){sub n}{sup 3+} or M(H{sub 2}O){sub n-1}(OH){sup 2+} facilitating, respectively, precipitation of corresponding hydrated carbonate, M{sub 2}(CO{sub 3}){sub 2}.2H{sub 2}O, or carbonate hydroxide, MCO{sub 3}(OH). X-ray powder diffractometry, infrared spectroscopy, and thermal analyses proved alternative formation of Ho{sub 2}(CO{sub 3}){sub 3}.2H{sub 2}O or LaCO{sub 3}(OH) under the whole set of hydrothermal treatment conditions probed, and Sm{sub 2}(CO{sub 3}){sub 3}.2H{sub 2}O at pH < 10 or SmCO{sub 3}(OH) at pH {>=} 10, thus implying dependence of the composition of the product carbonate compound on the hydrolysability of the initial M(H{sub 2}O){sub n}{sup 3+} species and, hence, the metal ionic size (La > Sm > Ho). Calcination of the various hydrothermal treatment products at {>=}600 deg. C resulted in the thermal genesis of the corresponding sesqui-oxides (M{sub 2}O{sub 3}). Bulk and surface characterization studies of the product oxides, employing N{sub 2} sorptiometry and scanning electron microscopy, in addition to the above analytical techniques, revealed overall strong crystallinity, large average crystallite size, and well-defined particle morphology. They revealed, moreover, surfaces, though of limited accessibilities ({<=}13 m{sup 2}/g), exposing OH groups of various coordination symmetries and, hence, acid-base properties, thus furnishing promising surface catalytic attributes.

  9. Hydrothermal synthesis and luminescent properties of NaLa(MoO{sub 4}){sub 2}:Dy{sup 3+} phosphor

    SciTech Connect

    Li Linlin; Zi Wenwen; Li Guanghuan; Lan Shi; Ji Guijuan; Gan Shucai; Zou Haifeng; Xu Xuechun

    2012-07-15

    Pompon-like NaLa(MoO{sub 4}){sub 2}:Dy{sup 3+} phosphors have been successfully prepared via a hydrothermal method using ammonia as pH value regulator. The hydrothermal process was carried out under aqueous condition without the use of any organic solvent, surfactant, and catalyst. The experimental results demonstrate that the obtained NaLa(MoO{sub 4}){sub 2}:Dy{sup 3+} phosphor powders are single-phase scheelite structure with tetragonal symmetry. Moreover, the phosphor under the excitation of 390 and 456 nm exhibited blue emission (486 nm) and yellow emission (574 nm), corresponding to the {sup 4}F{sub 9/2}{yields}{sup 6}H{sub 15/2} transition and {sup 4}F{sub 9/2}{yields}{sup 6}H{sub 13/2} transition of Dy{sup 3+} ions, respectively. In addition, the yellow-to-blue emission intensity ratio (Y/B) can be changed with the doped concentration of Dy{sup 3+} ions. All chromaticity coordinates of the obtained NaLa(MoO{sub 4}){sub 2}:Dy{sup 3+} phosphors are located in the white-light region. The results indicate that this kind of phosphor may has potential applications in the fields of near UV-excited and blue-excited white LEDs. - Graphical abstract: It can be seen from the SEM images that a pompon-like shape was obtained with an average diameter of about 1 {mu}m, and it is composed of many nanoflakes. Highlights: Black-Right-Pointing-Pointer Pompon-like NaLa(MoO{sub 4}){sub 2}:Dy{sup 3+} phosphors have been successfully prepared via a hydrothermal method. Black-Right-Pointing-Pointer Blue emission at 486 nm and yellow emission at 574 nm were obtained from the samples. Black-Right-Pointing-Pointer The yellow-to-blue emission intensity ratio (Y/B) can be changed with the doped concentration of Dy{sup 3+} ions. Black-Right-Pointing-Pointer NaLa(MoO{sub 4}){sub 2}:Dy{sup 3+} can be efficiently excited by the blue light and the near ultraviolet light.

  10. Abiotic Synthesis of Methane Under Alkaline Hydrothermal Conditions: the Effect of pH in Heterogeneous Catalysis

    NASA Astrophysics Data System (ADS)

    Foustoukos, D. I.; Qi, F.; Seyfried, W. E.

    2004-12-01

    Abiotic formation of methane in hydrothermal reaction zones at mid-ocean ridges likely occurs by Fischer-Tropsch catalytic processes involving reaction of CO2-bearing fluids with mineral surfaces. The elevated concentrations of dissolved methane and low molecular weight hydrocarbons observed in high temperature vent fluids issuing from ultramafic-hosted hydrothermal systems, in particular, suggest that Fe and Cr-bearing mineral phases attribute as catalysts, enhancing abiotic production of alkanes. The chemi-adsorption of dissolved CO2 on the catalytic mineral surface, however, might be influenced by a pH dependent surface electron charge developed within the mineral-fluid interface. Thus, a series of experiments was conducted to evaluate the role of pH on rates of carbon reduction in fluids coexisting with Fe-oxides at 390 degree C and 400 bars. At two distinct pH conditions, acidic (pH = 5) and alkaline (pH = 8.8), the abiotic production of isotopically labelled CH4(aq) was monitored during FeO reaction with aqueous NaCl-NaHCO3-H2-bearing fluid (0.56 mol/kg NaCl, 0.03 mol/kg NaH13CO3). Despite the lower H2(aq) concentrations (120 mmol/kg) in the high pH system, concentrations of abiogenic methane attained values of 195 umol/kg and 120 umol/kg respectively, suggesting enhanced catalytic properties of mineral under moderately high pH. X-ray photoelectron spectroscopy (XPS), performed on unreacted and final solid products, reveal the significantly greater abundances of alkyl (C-C-) groups on the surface of FeO oxidized at elevated pH, in comparison with mineral reacted at low pH conditions. Thus, enhanced adsorption of dissolved CO2 and the resulting Fischer-Tropsch formation of alkyl groups likely contributes to methane production observed at alkaline conditions. Introducing the effect of pH in the Fischer-Tropsch mechanism of alkane formation has important implications for the recently discovered Lost City ultramafic-hosted hydrothermal system, where elevated p

  11. Hydrothermal synthesis of 3D hollow porous Fe3O4 microspheres towards catalytic removal of organic pollutants

    PubMed Central

    2014-01-01

    Three-dimensional hollow porous superparamagnetic Fe3O4 microspheres were synthesized via a facile hydrothermal process. A series of characterizations done with X-ray diffraction, Brunauer-Emmett-Teller method, Fourier transform infrared spectroscopy, scanning electron microscopy, and transmission electron microscopy indicated that the production of Fe3O4 microspheres possessed good monodispersity, uniform size distribution, hollow and porous structural characters, and strong superparamagnetic behavior. The obtained Fe3O4 microspheres have a diameter of ca. 300 nm, which is composed of many interconnected nanoparticles with a size of ca. 20 nm. The saturation magnetization is 80.6 emu·g-1. The as-prepared products had promising applications as novel catalysts to remove organic pollutants (methylene blue) from wastewater in the presence of H2O2 and ultrasound irradiation. PMID:25520596

  12. Surfactant free hydrothermal synthesis of SnO{sub 2} nanorods with their microstructure and Raman studies

    SciTech Connect

    Amutha, A.; Panigrahi, B. K.; Amirthapanian, S.; Thangadurai, P.

    2014-04-24

    SnO{sub 2} nanorods were prepared by hydrothermal method without any surfactant. Their microstructure was studied with X-ray diffraction, Raman scattering and transmission electron microscopy. The range of nanorods diameter size is ∼3 to 19 nm. The crystal structure was confirmed to be SnO{sub 2} rutile tetragonal structure. The nanorods were single crystalline in nature as confirmed by HRTEM. Electron energy loss studies were carried out. EELS analysis showed presence SnO{sub 2} phase and SnO phase was not observed. New Raman modes (352 and 579 cm{sup −1}) corresponding to small size effects were observed for the SnO{sub 2} nanorods.

  13. Effect of deposition parameters on the structural properties of ZnO nanopowders prepared by microwave-assisted hydrothermal synthesis.

    PubMed

    Caglar, Yasemin; Gorgun, Kamuran; Aksoy, Seval

    2015-03-05

    ZnO nanopowders were synthesized via microwave-assisted hydrothermal method at different deposition (microwave irradiation) times and pH values. The effects of pH and deposition (microwave irradiation) time on the crystalline structure and orientation of the ZnO nanopowders have been investigated by X-ray diffraction (XRD) study. XRD observations showed that the crystalline quality of ZnO nanopowders increased with increasing pH value. The crystallite size and texture coefficient values of ZnO nanopowders were calculated. The structural quality of ZnO nanopowder was improved by deposition parameters. Field emission scanning electron microscope (FESEM) was used to analyze the surface morphology of the ZnO nanopowders. Microwave irradiation time and pH value showed a significant effect on the surface morphology.

  14. 40% Efficiency enhancement in solar cells using ZnO nanorods as shell prepared via novel hydrothermal synthesis

    NASA Astrophysics Data System (ADS)

    Ebadi, Mohammad; Zarghami, Zabihullah; Motevalli, Kourosh

    2017-03-01

    Herein, rod-like ZnO nanostructures were synthesized via a novel hydrothermal route using Zn(OAc)2, ethylenediamine and hydrazine as a new set of starting reagents. The as-synthesized products were characterized by techniques including XRD, EDS, SEM, XPS, Pl and FTIR. The prepared ZnO nanostructures were utilized as shell on TiO2 film in DSSCs. Effect of precursor type, morphology and thickness of ZnO shell (number of electrophoresis cycle) on solar cells efficiency were well studied. Our results showed that ethylenediamine has crucial effect on morphology of synthesized ZnO nanostructures and using ZnO nanostructures leads to an increase in DSSCs efficiency compared to bare TiO2 from 4.66 to 7.13% ( 40% improvement). Moreover, highest amount of solar cell efficiency (7.13%) was obtained by using ZnO nanorods with two cycle of electrophoresis for deposition.

  15. A facile hydrothermal synthesis, characterization and magnetic properties of mesoporous CoFe2O4 nanospheres

    NASA Astrophysics Data System (ADS)

    Reddy, M. Penchal; Mohamed, A. M. A.; Zhou, X. B.; Du, S.; Huang, Q.

    2015-08-01

    Mesoporous CoFe2O4 nanospheres with an average size of 180 nm were fabricated via a facile hydrothermal process using ethylene glycol as solvent and sodium acetate (NaAc) as electrostatic stabilizer. In this method, ethylene glycol plays a vital role in the formation of cobalt nanoospheres as a solvent and reducing agent. The structure and morphology of the prepared materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS). The nanospheres exhibited ferromagnetic properties with high saturation magnetization value of about 60.19 emu/g at room temperature. The BET surface area of the nanospheres was determined using the nitrogen absorption method. The porous CoFe2O4 nanospheres displayed good magnetic properties, which may provide a very promising candidate for their applications in target drug delivery.

  16. Hydrothermal synthesis and electrochemical properties of Li₃V₂(PO₄)₃/C-based composites for lithium-ion batteries.

    PubMed

    Sun, Chunwen; Rajasekhara, Shreyas; Dong, Youzhong; Goodenough, John B

    2011-09-01

    To improve performance at higher rates, we developed a hydrothermal method to prepare carbon-coated monoclinic lithium vanadium phosphate (Li(3)V(2)(PO(4))(3)) powder to be used as a cathode material for Li-ion batteries. The structural, morphological and electrochemical properties were characterized by X-ray diffraction (XRD), scanning and transmission electron microscopy (SEM and TEM), and galvanostatic charge-discharge cycling. A superior cycle and rate behavior are demonstrated for Li(3)V(1.85)Sc(0.15)(PO(4))(3)/C and Li(2.96)Ca(0.02)V(2)(PO(4))(3)/C electrodes at charge-discharge current rates above 5C.

  17. Hexagonal spherical Ln3+-doped NaGdF4: A facile double solvent hydrothermal synthesis and luminescent properties

    NASA Astrophysics Data System (ADS)

    Wu, Kelu; Huang, Zhuanzhuan; Yu, Qiao-He; Wang, Yi-Yan; Xia, Tian-Long

    2017-04-01

    Different sizes of hexagonal spherical NaGdF4:Eu3+ particles are synthesized via a facile hydrothermal method with the use of ethylene glycol (EG), propylene glycol (PG) or butylene glycol (BG) as another solvent. The particle size decreases with the addition of EG, PG or BG and the decreasing trend in BG/H2O system is significantly more than that in the other two systems. Meanwhile, results show that luminescent properties of NaGdF4:Eu3+ are enhanced along with the decrease of particle size. Besides, the energy transfer from Dy3+ to Eu3+ is directly observed in the PL spectra of NaGdF4:Eu3+/Dy3+.

  18. Solgel-hydrothermal synthesis of Tb/Tourmaline/TiO2 nano tubes and enhanced photocatalytic activity

    NASA Astrophysics Data System (ADS)

    Huang, Fengping; Guo, Yuyu; Wang, Shuai; Zhang, Shuang; Cui, Mengli

    2017-02-01

    In this study, we synthesized Tb/Tourmaline/TiO2 nano tubes (NTs) through a solgel-hydrothermal method. The as-prepared samples were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, Raman spectromicroscope, scanning electron microscopy, transmission electron microscopy and UV-vis diffuse reflectance spectroscopy. The resulting Tb/Tourmaline/TiO2 NTs exhibited higher photocatalytic activity than pure TiO2 and TiO2 nano particles (NPs) in the degradation of menthyl orange under UV-light. Results revealed that doping rare earth element Tb could narrow the wide band gap of TiO2 and tourmaline could trap the photogenerated electron of TiO2 to inhibit the recombination of photogenerated electron-hole pairs.

  19. Hydrothermal synthesis and crystal structure of a new lithium copper bismuth oxide, LiCuBiO4

    NASA Astrophysics Data System (ADS)

    Kumada, Nobuhiro; Nakamura, Ayumi; Miura, Akira; Takei, Takahiro; Azuma, Masaki; Yamamoto, Hajime; Magome, Eisuke; Moriyoshi, Chikako; Kuroiwa, Yoshihiro

    2017-01-01

    A new lithium copper bismuth oxide, LiCuBiO4 was prepared by hydrothermal reaction using NaBiO30.1*4H2O. The crystal structural model of this compound was refined by using synchrotron X-ray powder diffraction data. This bismuthate has the LiCuSbO4 related structure with the orthorhombic cell (Space group: Pnma) of a=10.9096(9), b=5.8113(5) and c=5.0073(4) Å, and the final R-factors were Rwp=4.84 and Rp=3.58%. This compound is the first example of a lithium copper bismuthate containing Bi5+. An antiferromagnetic ordering of Cu2+ moment was observed at 6 K.

  20. Hydrothermal synthesis of TiO2-ZnO-graphene nanocomposite towards photocatalytic and photovoltaic applications

    NASA Astrophysics Data System (ADS)

    Gayathri, S.; Jayabal, P.; Ramakrishnan, V.

    2015-06-01

    Titanium dioxide (TiO2) - Zinc oxide (ZnO) - Graphene (G) nanocomposite was successfully synthesized through facile hydrothermal method. The X-ray diffraction (XRD) pattern and the micro-Raman spectroscopic technique revealed the formation of TiO2-ZnO-Graphene (TZG) nanocomposite. The ZnO and TiO2 nanoparticles decorated graphene sheets were clearly noticeable in the Field Emission Scanning Electron Micrograph (FE-SEM). The UV-Visible absorption spectra clearly indicated that the formation of TZG nanocomposite enriched the absorption in the visible region. Hence, the prepared nanocomposite can be used as photocatalyst to remove organic dyes from water and as photoanode in the fabrication of dye sensitized solar cells (DSSCs).

  1. Effect of deposition parameters on the structural properties of ZnO nanopowders prepared by microwave-assisted hydrothermal synthesis

    NASA Astrophysics Data System (ADS)

    Caglar, Yasemin; Gorgun, Kamuran; Aksoy, Seval

    2015-03-01

    ZnO nanopowders were synthesized via microwave-assisted hydrothermal method at different deposition (microwave irradiation) times and pH values. The effects of pH and deposition (microwave irradiation) time on the crystalline structure and orientation of the ZnO nanopowders have been investigated by X-ray diffraction (XRD) study. XRD observations showed that the crystalline quality of ZnO nanopowders increased with increasing pH value. The crystallite size and texture coefficient values of ZnO nanopowders were calculated. The structural quality of ZnO nanopowder was improved by deposition parameters. Field emission scanning electron microscope (FESEM) was used to analyze the surface morphology of the ZnO nanopowders. Microwave irradiation time and pH value showed a significant effect on the surface morphology.

  2. Aloe vera plant-extracted solution hydrothermal synthesis and magnetic properties of magnetite (Fe3O4) nanoparticles

    NASA Astrophysics Data System (ADS)

    Phumying, Santi; Labuayai, Sarawuth; Thomas, Chunpen; Amornkitbamrung, Vittaya; Swatsitang, Ekaphan; Maensiri, Santi

    2013-06-01

    Magnetite (Fe3O4) nanoparticles have been successfully synthesized by a novel hydrothermal method using ferric acetylacetonate (Fe(C5H8O2)3) and aloe vera plant-extracted solution. The influences of different reaction temperatures and times on the structure and magnetic properties of the synthesized Fe3O4 nanoparticles were investigated. The synthesized nanoparticles are crystalline and have particle sizes of ˜6-30 nm, as revealed by transmission electron microscopy (TEM). The results of X-ray diffraction (XRD), High resolution TEM (HRTEM) and selected area electron diffraction (SAED) indicate that the synthesized Fe3O4 nanoparticles have the inverse cubic spinel structure without the presence of any other phase impurities. The hysteresis loops of the Fe3O4 nanoparticles at room temperature show superparamagnetic behavior and the saturation magnetization of the Fe3O4 samples increases with increasing reaction temperature and time.

  3. Hydrothermal synthesis of NiCo2O4 nanowires/nitrogen-doped graphene for high-performance supercapacitor

    NASA Astrophysics Data System (ADS)

    Yu, Mei; Chen, Jianpeng; Ma, Yuxiao; Zhang, Jingdan; Liu, Jianhua; Li, Songmei; An, Junwei

    2014-09-01

    NiCo2O4 nanowires/nitrogen-doped graphene (NCO/NG) composite materials were synthesized by hydrothermal treatment in a water-glycerol mixed solvent and subsequent thermal transformation. The obtained materials were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy and Raman spectroscopy. The electrochemical performance of the composites was evaluated by cyclic voltammetry, galvanostatic charge/discharge and electrochemical impedance spectrum techniques. NiCo2O4 nanowires are densely coated by nitrogen-doped graphene and the composite displays good electrochemical performance. The maximum specific capacitance of NCO/NG is 1273.13 F g-1 at 0.5 A g-1 in 6 M KOH aqueous solution, and it exhibits good capacity retention without noticeable degradation after 3000 cycles at 4 A g-1.

  4. Hydrothermal synthesis and the enhanced blue upconversion luminescence of NaYF 4:Nd 3+,Tm 3+,Yb 3+

    NASA Astrophysics Data System (ADS)

    Sun, Jiayue; Zhang, Weihang; Du, Haiyan; Yang, Zhiping

    2010-09-01

    Nd 3+, Tm 3+ and Yb 3+ co-doped NaYF 4 upconversion (UC) material was synthesized by the hydrothermal method. The structure of the sample was characterized by the X-ray diffraction, and its UC luminescence properties were investigated in detail. Under the 980 nm semiconductor laser excitation, its UC spectra exhibited distinct emission peaks at 451 nm, 475 nm and 646 nm respectively. On the basis of the comparison of UC spectra between NaYF 4:Nd 3+,Tm 3+,Yb 3+ and NaYF 4:Tm 3+,Yb 3+, it was indicated that the existence of Nd 3+ ion enhanced the blue emission intensity. The law of luminescence intensity versus pump power proved that the blue emission at 475 nm, and the red emission at 646 nm were the two-photon processes, while the blue emission at 451 nm was a three-photon process.

  5. Synthesis and enhanced photocatalytic property of feather-like Cd-doped CuO nanostructures by hydrothermal method

    NASA Astrophysics Data System (ADS)

    Wang, Yongqian; Jiang, Tingting; Meng, Dawei; Wang, Dagui; Yu, Meihua

    2015-11-01

    Feather-like Cd-doped CuO nanostructures were fabricated by a one-step hydrothermal method. X-ray diffraction pattern (XRD) and field emission scanning electron microscopy (FESEM) demonstrated that Cd2+ entered the crystal lattice of CuO and substituted Cu2+ without destroying crystal structures to form feather-like CuO nanostructures. The optical property of Cd-doped CuO was investigated by using UV-vis spectrophotometer. A slight blue-shift of optical band gap was observed because of quantum confinement effect. The doped samples exhibited obviously higher absorbance in UV light region and better photocatalytic activity for the photodegradation of methyl blue than the pure CuO nanosheets.

  6. Hydrothermal synthesis of TiO{sub 2}-ZnO-graphene nanocomposite towards photocatalytic and photovoltaic applications

    SciTech Connect

    Gayathri, S. Jayabal, P.; Ramakrishnan, V.

    2015-06-24

    Titanium dioxide (TiO{sub 2}) - Zinc oxide (ZnO) - Graphene (G) nanocomposite was successfully synthesized through facile hydrothermal method. The X-ray diffraction (XRD) pattern and the micro-Raman spectroscopic technique revealed the formation of TiO{sub 2}-ZnO-Graphene (TZG) nanocomposite. The ZnO and TiO{sub 2} nanoparticles decorated graphene sheets were clearly noticeable in the Field Emission Scanning Electron Micrograph (FE-SEM). The UV-Visible absorption spectra clearly indicated that the formation of TZG nanocomposite enriched the absorption in the visible region. Hence, the prepared nanocomposite can be used as photocatalyst to remove organic dyes from water and as photoanode in the fabrication of dye sensitized solar cells (DSSCs)

  7. Hydrothermal synthesis and photoelectric properties of BiVO 4 with different morphologies: An efficient visible-light photocatalyst

    NASA Astrophysics Data System (ADS)

    Fan, Haimei; Wang, Dejun; Wang, Lingling; Li, Haiyan; Wang, Ping; Jiang, Tengfei; Xie, Tengfeng

    2011-06-01

    Different morphologies of monoclinic BiVO 4 with smaller size were hydrothermal synthesized by simply adjusting the amount of surfactant (polyvinyl pyrrolidone PVP K30) added. The detailed field emission scanning electron microscope (FESEM) analysis revealed that the amount of PVP added could significantly affect the morphology and size of BiVO 4. Their photocatalytic activities were evaluated by the decolorization of methylene blue (MB) aqueous solution under visible-light irradiation ( λ > 400 nm), and the as-prepared sample with well-assembled flower-like morphology showed a much higher photocatalytic activity due to larger specific surface area and higher separation efficiency of photo-induced carriers. The relationship between the behavior of photo-induced carriers and photocatalytic activity was studied using the surface photovoltage spectroscopy (SPS) and corresponding phase spectra.

  8. SDS-assisted hydrothermal synthesis of NiO flake-flower architectures with enhanced gas-sensing properties

    NASA Astrophysics Data System (ADS)

    Miao, Ruiyang; Zeng, Wen; Gao, Qi

    2016-10-01

    A facile hydrothermal route was developed for the preparation of well-aligned hierarchical flower-like NiO nanostructure with the assistance of SDS that served as a structure-directing agent as well as a capping agent in the process of aggregation and assembly. Notably, the NiO sensors exhibit enhanced gas-sensing performance towards ethanol, which could be explained in association with the ultrathin nanosheets that are close to Debye length (LD) scale and thus get the majority carriers fully depleted due to the ionization of adsorbed oxygen, abundant effective gas diffusion paths as well as high surface-to-volume ratio to promote sufficient contact and reaction between the NiO sample and ethanol molecules, and numerous miniature reaction rooms assembled with nanosheets to make the test gas molecules stay long enough for completed gas-sensing reactions. Besides, a novel growth mechanism with the passage of reaction time was also proposed in detail.

  9. Hydrothermal synthesis of reduced graphene sheets/Fe2O3 nanorods composites and their enhanced electrochemical performance for supercapacitors

    NASA Astrophysics Data System (ADS)

    Yang, Wanlu; Gao, Zan; Wang, Jun; Wang, Bin; Liu, Lianhe

    2013-06-01

    Reduced graphene nanosheets/Fe2O3 nanorods (GNS/Fe2O3) composite has been fabricated by a hydrothermal route for supercapacitor electrode materials. The obtained GNS/Fe2O3 composite formed a uniform structure with the Fe2O3 nanorods grew on the graphene surface and/or filled between the graphene sheets. The electrochemical performances of the GNS/Fe2O3 hybrid supercapacitor were tested by cyclic voltammetry, electrochemical impedance spectroscopy, and galvanostatic charge-discharge tests in 6 M KOH electrolyte. Comparing with the pure Fe2O3 electrode, GNS/Fe2O3 composite electrode exhibits an enhanced specific capacitance of 320 F g-1 at 10 mA cm-2 and an excellent cycle-ability with capacity retention of about 97% after 500 cycles. The simple and cost-effective preparation technique of this composite with good capacitive behavior encourages its potential commercial application.

  10. One-step hydrothermal synthesis, characterization and magnetic properties of orthorhombic PrCrO{sub 3} cubic particles

    SciTech Connect

    Zhang, Youjin Yao, Chengpeng; Fan, Yun; Zhou, Maozhong

    2014-11-15

    Highlights: • Orthorhombic PrCrO{sub 3} cubic particles were prepared by a simple and facile one-step hydrothermal method. • The possible formation mechanism of PrCrO{sub 3} cubic particles was proposed. • The as-synthesized PrCrO{sub 3} exhibited behaviors of magnetic transition and negative magnetization. - Abstract: Orthorhombic PrCrO{sub 3} cubic particles were synthesized by a simple and facile one-step hydrothermal method of processing temperature 280 °C for 7 days. The products prepared in this paper have been characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and field-emission scanning electron microscopy (FESEM). The magnetic properties of the final sample are also studied. The XRD pattern shows the pure orthorhombic phase for PrCrO{sub 3} particles, the XPS and FTIR results further demonstrate the purity and composition of the product. FESEM images show cubic morphology for the PrCrO{sub 3} particles. The possible growth mechanism for PrCrO{sub 3} cubic particles is proposed. Through the investigation of magnetic properties, it can be seen that the orthorhombic PrCrO{sub 3} cubic particles exhibit behaviors of magnetic transition and negative magnetization. The Néel temperature is about 232 K and the magnetic hysteresis loop under 4 K shows that the coercivity (H{sub C}) and remanence (M{sub r}) is about 1728 Oe and 4.88 emu/g, respectively.

  11. Complexation of mercury(I) and mercury(II) by 18-crown-6: hydrothermal synthesis of the mercuric nitrite complex.

    PubMed

    Williams, Neil J; Hancock, Robert D; Riebenspies, Joseph H; Fernandes, Manuel; de Sousa, Alvaro S

    2009-12-21

    A dimercury(I) 18-crown-6 complex is isolated, and its possible role in the hydrothermal preparation of the mercuric nitrite complex is discussed. The reported structures are of [Hg(2)(18-crown-6)(2)(H(2)O)(2)](ClO(4))(2) (1), monoclinic, C2/c, a = 21.0345(9), b = 12.1565(5), c = 16.8010(7) A, beta = 113.2000(10) degrees , V = 3948.7(3) A(3), Z = 16, R = 0.0230; [Hg(18-crown-6)](NO(2))(2) (2), monoclinic, P2(1)/c, a = 8.027(5), b = 14.437(9), c = 7.827(5) A, beta = 95.165(11) degrees , V = 905.6(10) A(3), Z = 2, R = 0.0175. The complex cation in compound 1 consists of a mercurous dimer exhibiting a Hg-Hg bond length of 2.524(2) A. Non-bonding interactions between adjacent crown ether macrocycles across the Hg-Hg bond result in large variations in mercury to oxygen distances within equatorial coordination sites. At low pH compound 1 is proposed to be preferentially formed under hydrothermal conditions affording compound 2 upon disproportionation. Nitrite ions ligate via a unidentate nitrito (cis to metal) coordination mode as interpreted using vibrational (infrared) spectroscopy. The conformation adopted by 18-crown-6 in compounds 1 and 2 is closely related to a D(3d) conformation as evidenced by X-ray crystallography. Band splitting readily observed in vibrational spectra of the metal free crown ether, attributed to vibrational modes of oxyethylene fragments, is absent in spectra of 1 and 2 confirming a regular D(3d) macrocyclic orientation. Short Hg-O bonds observed for axially coordinated water molecules in 1 and coordinated nitrite ligands in 2, illustrate the prevalence of relativistic effects commonly observed in mercury complexes.

  12. Hydrothermal Processes

    NASA Astrophysics Data System (ADS)

    German, C. R.; von Damm, K. L.

    2003-12-01

    What is Hydrothermal Circulation?Hydrothermal circulation occurs when seawater percolates downward through fractured ocean crust along the volcanic mid-ocean ridge (MOR) system. The seawater is first heated and then undergoes chemical modification through reaction with the host rock as it continues downward, reaching maximum temperatures that can exceed 400 °C. At these temperatures the fluids become extremely buoyant and rise rapidly back to the seafloor where they are expelled into the overlying water column. Seafloor hydrothermal circulation plays a significant role in the cycling of energy and mass between the solid earth and the oceans; the first identification of submarine hydrothermal venting and their accompanying chemosynthetically based communities in the late 1970s remains one of the most exciting discoveries in modern science. The existence of some form of hydrothermal circulation had been predicted almost as soon as the significance of ridges themselves was first recognized, with the emergence of plate tectonic theory. Magma wells up from the Earth's interior along "spreading centers" or "MORs" to produce fresh ocean crust at a rate of ˜20 km3 yr-1, forming new seafloor at a rate of ˜3.3 km2 yr-1 (Parsons, 1981; White et al., 1992). The young oceanic lithosphere formed in this way cools as it moves away from the ridge crest. Although much of this cooling occurs by upward conduction of heat through the lithosphere, early heat-flow studies quickly established that a significant proportion of the total heat flux must also occur via some additional convective process (Figure 1), i.e., through circulation of cold seawater within the upper ocean crust (Anderson and Silbeck, 1981). (2K)Figure 1. Oceanic heat flow versus age of ocean crust. Data from the Pacific, Atlantic, and Indian oceans, averaged over 2 Ma intervals (circles) depart from the theoretical cooling curve (solid line) indicating convective cooling of young ocean crust by circulating seawater

  13. Hydrothermal Growth of Polyscale Crystals

    NASA Astrophysics Data System (ADS)

    Byrappa, Kullaiah

    In this chapter, the importance of the hydrothermal technique for growth of polyscale crystals is discussed with reference to its efficiency in synthesizing high-quality crystals of various sizes for modern technological applications. The historical development of the hydrothermal technique is briefly discussed, to show its evolution over time. Also some of the important types of apparatus used in routine hydrothermal research, including the continuous production of nanosize crystals, are discussed. The latest trends in the hydrothermal growth of crystals, such as thermodynamic modeling and understanding of the solution chemistry, are elucidated with appropriate examples. The growth of some selected bulk, fine, and nanosized crystals of current technological significance, such as quartz, aluminum and gallium berlinites, calcite, gemstones, rare-earth vanadates, electroceramic titanates, and carbon polymorphs, is discussed in detail. Future trends in the hydrothermal technique, required to meet the challenges of fast-growing demand for materials in various technological fields, are described. At the end of this chapter, an Appendix 18.A containing a more or less complete list of the characteristic families of crystals synthesized by the hydrothermal technique is given with the solvent and pressure-temperature (PT) conditions used in their synthesis.

  14. High-temperature, high-pressure hydrothermal synthesis, characterization, and structural relationships of mixed-alkali metals uranyl silicates

    SciTech Connect

    Chen, Yi-Hsin; Liu, Hsin-Kuan; Chang, Wen-Jung; Tzou, Der-Lii; Lii, Kwang-Hwa

    2016-04-15

    Three mixed-alkali metals uranyl silicates, Na{sub 3}K{sub 3}[(UO{sub 2}){sub 3}(Si{sub 2}O{sub 7}){sub 2}]·2H{sub 2}O (1), Na{sub 3}Rb{sub 3}[(UO{sub 2}){sub 3}(Si{sub 2}O{sub 7}){sub 2}] (2), and Na{sub 6}Rb{sub 4}[(UO{sub 2}){sub 4}Si{sub 12}O{sub 33}] (3), have been synthesized by high-temperature, high-pressure hydrothermal reactions at 550 °C and 1440 bar, and characterized by single-crystal X-ray diffraction, photoluminescence, and thermogravimetric analysis. Compound 1 and 2 are isostructural and contain layers of uranyl disilicate. The smaller cation, Na{sup +}, is located in the intralayer channels, whereas the larger cations, K{sup +} and Rb{sup +}, and water molecule are located in the interlayer region. The absence of lattice water in 2 can be understood according to the valence-matching principle. The structure is related to that of a previously reported mixed-valence uranium(V,VI) silicate. Compound 3 adopts a 3D framework structure and contains a unique unbranched dreier fourfold silicate chain with the structural formula {uB,4"1_∞}[{sup 3}Si{sub 12}O{sub 33}] formed of Q{sup 2}, Q{sup 3}, and Q{sup 4} Si. The connectivity of the Si atoms in the Si{sub 12}O{sub 33}{sup 18−} anion can be interpreted on the basis of Zintl–Klemm concept. Crystal data for compound 1: triclinic, P-1, a=5.7981(2) Å, b=7.5875(3) Å, c=12.8068(5) Å, α=103.593(2)°, β=102.879(2)°, γ=90.064(2)°, V=533.00(3) Å{sup 3}, Z=1, R1=0.0278; compound 2: triclinic, P-1, a=5.7993(3) Å, b=7.5745(3) Å, c=12.9369(6) Å, α=78.265(2)°, β=79.137(2)°, γ=89.936(2)°, V=546.02(4) Å{sup 3}, Z=1, R1=0.0287; compound 3: monoclinic, C2/m, a=23.748(1) Å, b=7.3301(3) Å, c=15.2556(7) Å, β=129.116(2)°, V=2060.4(2) Å{sup 3}, Z=2, R1=0.0304. - Graphical abstract: Three mixed-alkali metals uranyl silicates were synthesized under hydrothermal conditions at 550 °C and 1400 bar and structurally characterized by single-crystal X-ray diffraction. Two of them have a layer structure

  15. Hydrothermal synthesis and luminescence properties of octahedral LiYbF{sub 4}: Er{sup 3+} microcrystals

    SciTech Connect

    Lu, Chunhua; Huang, Wenjuan; Ni, Yaru; Xu, Zhongzi

    2011-02-15

    Graphical abstract: LiYbF{sub 4}: Er{sup 3+} octahedral microcrystals have been successfully prepared through a facile hydrothermal method assisted with EDTA. SEM, HRTEM, RD, PL spectra are used to characterize the samples. It can be seen from SEM data that the complexing agent EDTA made to hydrothermal synthetic procedures result in formation of LiYbF{sub 4} octahedral microparticles with smooth surface. From the HRTEM images, the distances between the lattice fringes were measured to be 2.99 A and 2.57 A which correspond to the d-spacing for (1 1 2) and (2 0 0) planes, respectively. From the XRD patterns for the LiYb{sub 0.99}Er{sub 0.01}F{sub 4} in the absence of chelating agent EDTA and in the presence of EDTA, it is evident that the diffraction peaks of both patterns are highly crystalline and all of the peaks could be readily indexed to the LiYbF{sub 4} phase (JCPDS 71-1211). No other impurity peaks were detected. Under 976 nm excitation, the upconversion (UC) luminescence emission spectra of LiYbF{sub 4}: Er{sup 3+} microcrystals show the characteristic Er{sup 3+} emissions. The results show that the infrared light emissions at 792 nm of {sup 4}I{sub 9/2} {yields} {sup 4}I{sub 15/2} are dominantly strong unusually, while the green emissions at 526 and 545 nm assigned to {sup 2}H{sub 11/2} {yields} {sup 4}I{sub 15/2} and {sup 4}S{sub 3/2} {yields} {sup 4}I{sub 15/2}, respectively, and the red emission at 667 nm of {sup 4}F{sub 9/2} {yields} {sup 4}I{sub 15/2} are relatively weaker. Research highlights: {yields} Monodisperse and regular octahedral microcrystals LiYbF{sub 4}: Er{sup 3+} with smooth surface has been prepared. {yields} The characteristic emissions of Er{sup 3+} ions are observed in LiYbF{sub 4} microcrystals. {yields} The content of EDTA will influence the fluorescence intensity. {yields} Luminescence intensity increases gradually at the beginning and then decreases gradually with increasing temperature. -- Abstract: LiYbF{sub 4}: Er{sup 3

  16. Hydrothermal synthesis and characterization of a two-dimensional piperazinium cobalt–zinc phosphate via a metastable one-dimensional phase

    SciTech Connect

    Torre-Fernández, Laura; Khainakova, Olena A.; Espina, Aránzazu; Amghouz, Zakariae; Khainakov, Sergei A.; Alfonso, Belén F.; Blanco, Jesús A.; García, José R.; García-Granda, Santiago

    2015-05-15

    A two-dimensional piperazinium cobalt–zinc phosphate, formulated as (C{sub 4}N{sub 2}H{sub 12}){sub 1.5}(Co{sub 0.6}Zn{sub 0.4}){sub 2}(HPO{sub 4}){sub 2}(PO{sub 4})·H{sub 2}O (2D), was synthesized under hydrothermal conditions. The crystal structure was determined using single-crystal X-ray diffraction data (monoclinic P2{sub 1}/c, a=8.1165(3) Å, b=26.2301(10) Å, c=8.3595(4) Å, and β=110.930(5)°) and the hydrogen atom positions were optimized by DFT calculations. A single-crystal corresponding to one-dimensional metastable phase, (C{sub 4}N{sub 2}H{sub 12})Co{sub 0.3}Zn{sub 0.7}(HPO{sub 4}){sub 2}·H{sub 2}O (1D), was also isolated and the crystal structure was determined (monoclinic P2{sub 1}/c, a=8.9120(6) Å, b=14.0290(1) Å, c=12.2494(5) Å, and β=130.884(6)°). The bulk was characterized by chemical (C–H–N) analysis, powder X-ray diffraction (PXRD), powder X-ray thermodiffractometry (HT-XRD), transmission electron microscopy (STEM(DF)-EDX and EFTEM), and thermal analysis (TG/SDTA-MS), including activation energy data of its thermal decomposition. The magnetic susceptibility and magnetization measurements show no magnetic ordering down to 4 K. - Graphical abstract: Hydrothermal synthesis and structural characterization of a two-dimensional piperazinium cobalt–zinc phosphate, (C{sub 4}N{sub 2}H{sub 12}){sub 1.5}(Co{sub 0.6}Zn{sub 0.4}){sub 2}(HPO{sub 4}){sub 2}(PO{sub 4})·H{sub 2}O (2D), have been reported. The crystal structure of a one-dimensional piperazinium cobalt–zinc phosphate, (C{sub 4}N{sub 2}H{sub 12})Co{sub 0.3}Zn{sub 0.7}(HPO{sub 4}){sub 2}·H{sub 2}O (1D) a metastable phase during the hydrothermal synthesis, was also determined. The thermal behavior of 2D compound is strongly dependent on the selected heating rate and the magnetic susceptibility and magnetization measurements show no magnetic ordering down to 4 K. - Highlights: • A 2D piperazinium cobalt–zinc phosphate has been synthesized and characterized. • Crystal

  17. Four divalent transition metal carboxyarylphosphonate compounds: Hydrothermal synthesis, structural chemistry and generalized 2D FTIR correlation spectroscopy studies

    SciTech Connect

    Lei Ran; Chai Xiaochuan; Mei Hongxin; Zhang Hanhui; Chen Yiping; Sun Yanqiong

    2010-07-15

    Four divalent transition metal carboxyarylphosphonates, [Ni(4,4'-bipy)H{sub 2}L{sup 1}(HL{sup 1}){sub 2}(H{sub 2}O){sub 2}].2H{sub 2}O 1, [Ni{sub 2}(4,4'-bipy)(L{sup 2})(OH)(H{sub 2}O){sub 2}].3H{sub 2}O 2, Mn(phen){sub 2}(H{sub 2}L{sup 1}){sub 2}3 and Mn(phen)(HL{sup 2}) 4 (H{sub 3}L{sup 1}=p-H{sub 2}O{sub 3}PCH{sub 2}-C{sub 6}H{sub 4}-COOH, H{sub 3}L{sup 2}=m-H{sub 2}O{sub 3}PCH{sub 2}-C{sub 6}H{sub 4}-COOH, 4,4'-bipy=4,4'-bipyridine, phen=1,10-phenanthroline) were synthesized under hydrothermal conditions. 1 features 1D linear chains built from Ni(II) ions bridging 4,4'-bipy. In 2, neighboring Ni{sub 4} cluster units are connected by pairs of H{sub 3}L{sup 2} ligands to form 1D double-crankshaft chains, which are interconnected by pairs of 4,4'-bipy into 2D sheets. 3 exhibits 2D supramolecular layers via the R{sub 2}{sup 2}(8) ringed hydrogen bonding units. 4 has 1D ladderlike chains, in which the 4-membered rings are cross-linked by the organic moieties of the H{sub 3}L{sup 2} ligands. Additionally, 2D FTIR correlation analysis is applied with thermal and magnetic perturbation to clarify the structural changes of functional groups from H{sub 3}L{sup 1} and H{sub 3}L{sup 2} ligands in the compounds more efficiently. - Graphical abstract: A series of divalent transition metal carboxyarylphosphonate compounds were synthesized under hydrothermal conditions. The figure displays 2D sheet structure with large windows in compound 2.

  18. Hydrothermal synthesis of high-quality type-II CdTe/CdSe quantum dots with near-infrared fluorescence.

    PubMed

    Wang, Jing; Han, Heyou

    2010-11-01

    A simple hydrothermal method is developed for the synthesis of high-quality, water-soluble, and near-infrared (NIR)-emitting type-II core/shell CdTe/CdSe quantum dots (QDs) by employing thiol-capped CdTe QDs as core templates and CdCl(2) and Na(2)SeO(3) as shell precursors. Compared with the original CdTe core QDs, the core/shell CdTe/CdSe QDs exhibit an obvious red-shifted emission, whose color can be tuned between visible and NIR regions (620-740 nm) by controlling the thickness of the CdSe shell. The photoluminescence quantum yield (PL QY) of CdTe/CdSe QDs with an optimized thickness of the CdSe shell can reach up to 44.2% without any post-preparative treatment. Through a thorough study of the core/shell structure by high-resolution transmission electron microscopy (HRTEM), ultraviolet-visible (UV-vis) absorption spectra, fluorescence spectra, X-ray powder diffraction (XRD) and X-ray photoelectron spectroscopy (XPS), the as-prepared CdTe/CdSe QDs demonstrate good monodispersity, hardened lattice structure and excellent photostability, offering a great potential for biological application.

  19. Hydrothermal synthesis of 3D hierarchical flower-like MoSe2 microspheres and their adsorption performances for methyl orange

    NASA Astrophysics Data System (ADS)

    Tang, Hua; Huang, Hong; Wang, Xiaoshuai; Wu, Kongqiang; Tang, Guogang; Li, Changsheng

    2016-08-01

    In this paper, we report a facile and versatile modified hydrothermal method for synthesis of three-dimensional (3D) hierarchical flower-like MoSe2 microspheres using selenium powders and sodium molybdate as raw materials. The as-prepared MoSe2 was investigated for application as an adsorbent for the removal of dye contaminants from water. Power X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscope (XPS) and N2 adsorption-desorption analysis were carried out to study the microstructure of the as-synthesized product. A possible growth mechanism of MoSe2 flower-like microspheres was preliminarily proposed on the basis of observation of a time-dependent morphology evolution process. Moreover, the MoSe2 sample exhibited good adsorption properties, with maximum adsorption capacity of 36.91 mg/g for methyl orange. The adsorption process of methyl orange on 3D hierarchical flower-like MoSe2 microspheres was systematically investigated, which was found to obey the pseudo-second-order rate equation and Langmuir adsorption model.

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

    NASA Astrophysics Data System (ADS)

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

    2017-04-01

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

  1. Microwave assisted hydrothermal synthesis and magnetocaloric properties of La0.67Sr0.33MnO3 manganite.

    PubMed

    Anwar, M S; Kumar, Shalendra; Ahmed, Faheem; Kim, G W; Koo, Bon Heun

    2012-07-01

    We report microwave assisted hydrothermal synthesis and magnetocaloric properties of La0.67Sr0.33MnO3 manganite. The synthesized La0.67Sr0.33MnO3 nanoparticles was characterized using X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDS) and magnetization measurements. The XRD results indicated that La0.67Sr0.33MnO3 nanoparticles have polycrystalline nature with monoclinic structure. FE-SEM results suggested that La0.67Sr0.33MnO3 nanoparticles are assembled into rod like morphology. Magnetization measurements show that La0.67Sr0.33MnO3 nanoparticles exhibit transition temperature (Tc) above room temperature. The maximum magnetic entropy change (deltaS(M))max was found to be 0.52 J/kg K near Tc approximately 325 K at applied magnetc field of 20 kOe. This compound may considered as potential material for magnetic refrigeration near room temperature.

  2. High-throughput continuous hydrothermal flow synthesis of Zn-Ce oxides: unprecedented solubility of Zn in the nanoparticle fluorite lattice.

    PubMed

    Kellici, Suela; Gong, Kenan; Lin, Tian; Brown, Sonal; Clark, Robin J H; Vickers, Martin; Cockcroft, Jeremy K; Middelkoop, Vesna; Barnes, Paul; Perkins, James M; Tighe, Christopher J; Darr, Jawwad A

    2010-09-28

    High-throughput continuous hydrothermal flow synthesis has been used as a rapid and efficient synthetic route to produce a range of crystalline nanopowders in the Ce-Zn oxide binary system. High-resolution powder X-ray diffraction data were obtained for both as-prepared and heat-treated (850 degrees C for 10 h in air) samples using the new robotic beamline I11, located at Diamond Light Source. The influence of the sample composition on the crystal structure and on the optical and physical properties was studied. All the nanomaterials were characterized using Raman spectroscopy, UV-visible spectrophotometry, Brunauer-Emmett-Teller surface area and elemental analysis (via energy-dispersive X-ray spectroscopy). Initially, for 'as-prepared' Ce(1-x)Zn(x)O(y), a phase-pure cerium oxide (fluorite) structure was obtained for nominal values of x=0.1 and 0.2. Biphasic mixtures were obtained for nominal values of x in the range of 0.3-0.9 (inclusive). High-resolution transmission electron microscopy images revealed that the phase-pure nano-CeO(2) (x=0) consisted of ca 3.7 nm well-defined nanoparticles. The nanomaterials produced herein generally had high surface areas (greater than 150 m(2) g(-1)) and possessed combinations of particle properties (e.g. bandgap, crystallinity, size, etc.) that were unobtainable or difficult to achieve by other more conventional synthetic methods.

  3. PEG-assisted hydrothermal synthesis of CoFe2O4 nanoparticles with enhanced selective adsorption properties for different dyes

    NASA Astrophysics Data System (ADS)

    Wu, Xiaofei; Wang, Wei; Li, Feng; Khaimanov, Spartak; Tsidaeva, Natalia; Lahoubi, Mahieddine

    2016-12-01

    Cobalt ferrite nanoparticles (CFO NPs) are synthesized by a facile and polyethylene glycol (PEG) assisted hydrothermal method. In the synthesis of cobalt ferrites, PEG is used as a surfactant. The formation of single-phase spinel structure in the samples is confirmed by XRD patterns. TEM images show that the addition of PEG results in the decrease in the size of the CFO NPs. When the amount of PEG is lower than 2.4 g, the particle sizes decrease, then, further increasing the concentration of PEG in the solution, the particle sizes begin to increase, for much more PEG will cover onto the surface of the nanoparticles. Here, the existence of PEG on the surface of CFO NPs is confirmed from the characteristic bands of PEG in FTIR spectra. All the samples are ferromagnetic, and their saturation magnetization (Ms) decreases with the increase in PEG concentration. The as-synthesized samples show highly selective adsorption characteristics for organic dyes. Compared with methyl orange (MO) and methyl blue (MB) dyes, good adsorption performance of the PEG/CoFe2O4 nanocomposites for Congo red (CR) dye is presented. Moreover, the addition of PEG greatly enhances their adsorption capacity (qe) for CR. The corresponding adsorption behavior fits well with the pseudo-second-order kinetic model and the Langmuir model. And the adsorption mechanism is investigated. This study suggests that the as-prepared products can be regarded as an excellent selective adsorbent to remove dyes from the wastewater.

  4. Microwave-assisted hydrothermal synthesis of Ag₂(W(1-x)Mox)O₄ heterostructures: Nucleation of Ag, morphology, and photoluminescence properties.

    PubMed

    Silva, M D P; Gonçalves, R F; Nogueira, I C; Longo, V M; Mondoni, L; Moron, M G; Santana, Y V; Longo, E

    2016-01-15

    Ag2W(1-x)MoxO4 (x=0.0 and 0.50) powders were synthesized by the co-precipitation (drop-by-drop) method and processed using a microwave-assisted hydrothermal method. We report the real-time in situ formation and growth of Ag filaments on the Ag2W(1-x)MoxO4 crystals using an accelerated electron beam under high vacuum. Various techniques were used to evaluate the influence of the network-former substitution on the structural and optical properties, including photoluminescence (PL) emission, of these materials. X-ray diffraction results confirmed the phases obtained by the synthesis methods. Raman spectroscopy revealed significant changes in local order-disorder as a function of the network-former substitution. Field-emission scanning electron microscopy was used to determine the shape as well as dimensions of the Ag2W(1-x)MoxO4 heterostructures. The PL spectra showed that the PL-emission intensities of Ag2W(1-x)MoxO4 were greater than those of pure Ag2WO4, probably because of the increase of intermediary energy levels within the band gap of the Ag2W(1-x)MoxO4 heterostructures, as evidenced by the decrease in the band-gap values measured by ultraviolet-visible spectroscopy.

  5. Hydrothermal synthesis, characterization and composition-dependent magnetic properties of LaFe 1- xCr xO 3 system (0≤ x≤1)

    NASA Astrophysics Data System (ADS)

    Hu, Weiwei; Chen, Yan; Yuan, Hongming; Zhang, Ganghua; Li, Guanghua; Pang, Guangsheng; Feng, Shouhua

    2010-07-01

    Hydrothermal synthesis, characterization and magnetic properties of a series of ABO 3-perovskites LaFe 1- xCr xO 3 (0≤ x≤1) are reported. The alkalinity in initial reaction mixtures plays a critical role in controlling the designed stoichiometry of the final compositions. Their magnetic properties are strongly dependent on the compositions and a maximum magnetic moment is found for the sample at x=0.5. Weak ferromagnetic interaction observed for the samples from x=0 to 0.9 arises from the presence of Fe-O-Fe antisymmetric exchange and Fe-O-Cr superexchange interaction. The weak ferromagnetism as well as the linear variation of the lattice parameters implies the possible random distribution of Fe and Cr ions in B sites of the perovskites. The evolution of magnetic ordering transition temperatures has a close relationship with substituent ratios, for the competition of antiferromagnetism and ferromagnetism. The saturated magnetic moment shows a great improvement compared with that for the samples synthesized by solid state method.

  6. Microwave assisted hydrothermal synthesis of Ag/AgCl/WO{sub 3} photocatalyst and its photocatalytic activity under simulated solar light

    SciTech Connect

    Adhikari, Rajesh; Gyawali, Gobinda; Sekino, Tohru; Wohn Lee, Soo

    2013-01-15

    Simulated solar light responsive Ag/AgCl/WO{sub 3} composite photocatalyst was synthesized by microwave assisted hydrothermal process. The synthesized powders were characterized by X-Ray Diffraction (XRD) spectroscopy, X-Ray Photoelectron Spectroscopy (XPS), Transmission Electron Microscopy (TEM), Diffuse Reflectance Spectroscopy (UV-Vis DRS), and BET surface area analyzer to investigate the crystal structure, morphology, chemical composition, optical properties and surface area of the composite photocatalyst. This photocatalyst exhibited higher photocatalytic activity for the degradation of rhodamine B under simulated solar light irradiation. Dye degradation efficiency of composite photocatalyst was found to be increased significantly as compared to that of the commercial WO{sub 3} nanopowder. Increase in photocatalytic activity of the photocatalyst was explained on the basis of surface plasmon resonance (SPR) effect caused by the silver nanoparticles present in the composite photocatalyst. Highlights: Black-Right-Pointing-Pointer Successful synthesis of Ag/AgCl/WO{sub 3} nanocomposite. Black-Right-Pointing-Pointer Photocatalytic experiment was performed under simulated solar light. Black-Right-Pointing-Pointer Nanocomposite photocatalyst was very active as compared to WO{sub 3} commercial powder. Black-Right-Pointing-Pointer SPR effect due to Ag nanoparticles enhanced the photocatalytic activity.

  7. Hydrothermal synthesis of a crystalline rutile TiO2 nanorod based network for efficient dye-sensitized solar cells.

    PubMed

    Yu, Hua; Pan, Jian; Bai, Yang; Zong, Xu; Li, Xinyong; Wang, Lianzhou

    2013-09-27

    One-dimensional (1D) TiO2 nanostructures are desirable as photoanodes in dye-sensitized solar cells (DSSCs) due to their superior electron-transport capability. However, making use of the DSSC performance of 1D rutile TiO2 photoanodes remains challenging, mainly due to the small surface area and consequently low dye loading. Herein, a new type of photoanode with a three-dimensional (3D) rutile-nanorod-based network structure directly grown on fluorine-doped tin oxide (FTO) substrates was developed by using a facile two-step hydrothermal process. The resultant photoanode possesses oriented rutile nanorod arrays for fast electron transport as the bottom layer and radially packed rutile head-caps with an improved large surface area for efficient dye adsorption. The diffuse reflectance spectra showed that with the radially packed top layer, the light-harvesting efficiency was increased due to an enhanced light-scattering effect. A combination of electrochemical impedance spectroscopy (EIS), dark current, and open-circuit voltage decay (OCVD) analyses confirmed that the electron-recombiantion rate was reduced on formation of the nanorod-based 3D network for fast electron transport. As a resut, a light-to-electricity conversion efficiency of 6.31% was achieved with this photoanode in DSSCs, which is comparable to the best DSSC efficiencies that have been reported to date for 1D rutile TiO2 .

  8. Hydrothermal synthesis and structural and spectroscopic properties of the new triclinic form of GdBO3:Eu3+ nanocrystals.

    PubMed

    Szczeszak, Agata; Grzyb, Tomasz; Barszcz, Bolesław; Nagirnyi, Vitali; Kotlov, Aleksei; Lis, Stefan

    2013-05-06

    Triclinic Gd1-xEuxBO3 nanophosphors have been prepared by a hydrothermal method without using additional coreagents and prior precipitation of precursor (in situ). The formation of the borate nanorods and their crystal structure was refined on the basis of X-ray diffraction patterns (XRD) and well confirmed using various techniques such as infrared spectroscopy (IR), Raman spectroscopy, transmission electron microscopy (TEM), and energy-dispersive X-ray spectroscopy (EDX). The new triclinic crystal structure (space group P1) for the GdBO3 nanocrystals and detailed structure parameters were determined with the help of the Rietveld analysis. The spectroscopic characteristics of the synthesized nanomaterials with different concentrations of Eu(3+) ions were defined with the use of luminescence excitation spectra as well as emission spectra and decay kinetics. The Judd-Ofelt parameters (Ω2, Ω4) and quantum efficiency, η, were also calculated for the more detailed analysis of Eu(3+) spectra in the GdBO3 host.

  9. Hydrothermal synthesis of In2S3/g-C3N4 heterojunctions with enhanced photocatalytic activity.

    PubMed

    Xing, Chaosheng; Wu, Zhudong; Jiang, Deli; Chen, Min

    2014-11-01

    Graphitic carbon nitride (g-C3N4) was hybridized by In2S3 to form a novel In2S3/g-C3N4 heterojunction photocatalyst via a hydrothermal method. TEM and HRTEM results reveal that In2S3 nanoparticles and g-C3N4 closely contact with each other to form an intimate interface. The as-obtained In2S3/g-C3N4 heterojunctions exhibit higher photocatalytic activity than those of pure g-C3N4 and In2S3 for the photodegradation of rhodamine B (RhB) under visible light irradiation. The enhanced photocatalytic performance of In2S3/g-C3N4 heterojunctions could be attributed to its wide absorption in the visible region and efficient electron-hole separation. On the basis of radical scavenger experiments, superoxide radicals and holes are suggested to play a critical role in RhB degradation over In2S3/g-C3N4 heterojunctions.

  10. Synthesis and characterization of monoclinic BiVO 4 nanorods and nanoplates via microemulsion-mediated hydrothermal method

    NASA Astrophysics Data System (ADS)

    Li, Haibin; Liu, Guocong; Chen, Shuguang; Liu, Qicheng; Lu, Weiming

    2011-05-01

    Monoclinic BiVO 4 nanorods and nanoplates were synthesized via the CTAB/water/n-butanol/n-octane microemulsion-mediated hydrothermal process. The physical and photophysical properties of the as-prepared samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman spectroscopy, and UV-vis diffuse reflectance spectroscopy (UV-vis). It was found that the ratio of H 2O to CTAB in microemulsion played a key role in the morphology evolution of the products. The possible formation mechanism of BiVO 4 nanostructure with various morphologies was briefly discussed. The Raman results indicated that the symmetry distortions in the local structure of the synthesized BiVO 4 were affected by the morphology of the products. The bandgaps ( Eg) of BiVO 4 nanorods and nanoplates are 2.45 and 2.38 eV, respectively. The synthesized BiVO 4 nanoplates showed superior photocatalytic activity compared with BiVO 4 nanorods due to their higher degree of structural distortion, larger surface area, and thinness.

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

    SciTech Connect

    Guan, Lei; Wang, Ying

    2015-08-15

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

  12. Ultrafast hydrothermal synthesis of high quality magnetic core phenol-formaldehyde shell composite microspheres using the microwave method.

    PubMed

    You, Li-Jun; Xu, Shuai; Ma, Wan-Fu; Li, Dian; Zhang, Yu-Ting; Guo, Jia; Hu, Jack J; Wang, Chang-Chun

    2012-07-17

    An ultrafast, facile, and efficient microwave hydrothermal approach was designed to fabricate magnetic Fe(3)O(4)/phenol-formaldehyde (PF) core-shell microspheres for the first time. The structure of the Fe(3)O(4)/PF core-shell microspheres could be well controlled by the in situ polycondensation of phenol and formaldehyde with magnetic Fe(3)O(4) clusters as the seeds in an aqueous solution without any surfactants. The effect of synthetic parameters, such as the feeding amounts of phenol, the dosages of formaldehyde, the reaction temperatures, and the microwave heating time, on the morphologies and sizes of the Fe(3)O(4)/PF microspheres were investigated in details. The phenol-formaldehyde shell is found to be evenly coated on Fe(3)O(4) clusters within 10 min of the irradiation. The as-prepared microspheres were highly uniform in morphology, and the method was found to allow the shell thickness to be finely controlled in the range of 10-200 nm. The properties of the composite microspheres were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), thermogravimetic analysis (TGA), Fourier transform infrared (FT-IR) spectra, X-ray diffraction (XRD), and vibrating sample magnetometer (VSM). The as-prepared Fe(3)O(4)/PF microspheres were monodisperse and highly dispersible in water, ethanol, N,N-dimethyformamide, and acetone, a beneficial quality for the further functionalization and applications of the Fe(3)O(4)/PF microspheres.

  13. Synthesis and crystallographic study of Pb-Sr hydroxyapatite solid solutions by high temperature mixing method under hydrothermal conditions

    SciTech Connect

    Zhu Kongjun; Yanagisawa, Kazumichi; Shimanouchi, Rie; Onda, Ayumu; Kajiyoshi, Koji; Qiu Jinhao

    2009-06-03

    The solid solutions in the system of Pb and Sr hydroxyapatite, Sr{sub 10-x}Pb{sub x}HAp (x = 0-10), were successfully synthesized by high-temperature mixing method (HTMM) at 160 deg. C for 12 h under hydrothermal conditions. The samples were characterized by X-ray diffraction, chemical analysis and electron microscopic observation, and the site of the metal ions in the solid solutions was analyzed with the Rietveld method. The lattice constants, both a and c, of the solid solutions varied linearly with Pb content. It was found that Pb ions in the solid solutions preferentially occupied the M(2) site in the apatite structure. HTMM gives Sr-Pb HAp solid solutions much better crystallization. However, due to the formation of intermediate compound of Pb{sub 3}O{sub 2}(OH){sub 2} in the Pb(NO{sub 3}){sub 2}.4H{sub 2}O solution before mixing with (NH{sub 4}){sub 2}HPO{sub 4} solution at 160 deg. C, HTMM causes the decrease of crystallization of the samples with high Pb content.

  14. Hydrothermal synthesis of fluorinated anatase TiO2/reduced graphene oxide nanocomposites and their photocatalytic degradation of bisphenol A

    NASA Astrophysics Data System (ADS)

    Luo, Lijun; Yang, Ye; Zhang, Ali; Wang, Min; Liu, Yongjun; Bian, Longchun; Jiang, Fengzhi; Pan, Xuejun

    2015-10-01

    The surface fluorinated TiO2/reduced graphene oxide nanocomposites (denoted as F-TiO2-RGO) were synthesized via hydrothermal method. The as-prepared materials were characterized by transmission electron microscopy (TEM), X-ray diffractometer (XRD), Raman spectroscopy, Fourier Transform Infrared spectra (FTIR), X-ray photoelectron spectroscopy (XPS) and X-ray fluorescence (XRF). The results showed that pure anatase TiO2 particles were anchored on the surface of reduced graphene oxide. And the HF added during the preparation process can not only prevent phase transformation from anatase to rutile, but also the F- ion adsorbed on the surface of TiO2-RGO surface can enhance photocatalytic activity of F-TiO2-RGO. The photocatalytic activities of F-TiO2-RGO nanocomposites were evaluated by decomposing bisphenol A under UV light illumination. Under optimal degradation condition, the degradation rate constant of BPA over F-TiO2-10RGO (0.01501 min-1) was 3.41 times than that over P25 (0.00440 min-1). The result indicated that the enhanced photocatalytic activity of F-TiO2-10RGO was ascribed to the adsorbed F ion and RGO in F-TiO2-RGO composite, which can reduce the recombination rate of the photo-generated electrons and holes synergistically.

  15. Sodium dodecyl sulfate-assisted hydrothermal synthesis of mesoporous nickel cobaltite nanoparticles with enhanced catalytic activity for methanol electrooxidation

    NASA Astrophysics Data System (ADS)

    Ding, Rui; Qi, Li; Jia, Mingjun; Wang, Hongyu

    2014-04-01

    Mesoporous nickel cobaltite (NiCo2O4) nanoparticles have been synthesized via a facile hydrothermal strategy with the assistance of sodium dodecyl sulfate (SDS) soft template (ST). Their physicochemical properties have been characterized via X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy-dispersive X-ray spectra (EDS), transmission electron microscopy (TEM), X-ray photoelectron spectra (XPS) and nitrogen sorption measurements. Their electrocatalytic performances have been examined by cyclic voltammetry (CV), linear sweep voltammetry (LSV), chronoamperometry (CA) and electrochemical impedance spectroscopy (EIS) tests. The obtained NiCo2O4 materials exhibit a typical nanoscale crystalline hexagonal morphology with specific surface area (SSA) and mesopore volume of 88.63 m2 g-1 and 0.298 cm3 g-1. Impressively, the SDS-assisted NiCo2O4 electrode shows a catalytic current density of 125 mA cm-2 and 72% retention for consecutive 1000 s at 0.6 V in 1 M KOH and 0.5 M CH3OH electrolytes towards methanol (CH3OH) electrooxidation, which is better than the one without SDS assistance. The pronounced electrocatalytic activity is largely ascribed to their higher surface intensities of Co and Ni species and superior mesoporous nanostructures, which provide the richer electroactive sites and faster electrochemical kinetics, leading to the enhanced electrocatalytic activity.

  16. Controllable synthesis of magnetic Fe3O4 particles with different morphology by one-step hydrothermal route

    NASA Astrophysics Data System (ADS)

    Chen, Zhongtao; Du, Yi; Li, Zhongfu; Yang, Kai; Lv, Xingjie

    2017-03-01

    Well-defined Fe3O4 particles were successfully fabricated by a facile triethanolamine (TEA)-assisted method under mild hydrothermal conditions. Hydrated ferric salt was employed as the single iron precursor. TEA was used as the complexing agent and/or alkaline source. The crystalline phases of the as-obtained samples were characterized by X-ray diffraction (XRD). Furthermore, the morphology as well as the compositions of the samples were investigated by scanning electron microscopy (SEM) equipped with an energy dispersion spectroscopy (EDS). The results indicated that the products were Fe3O4 crystal phase, and the morphology and powder size of the particles were varied with adding different amount of NaOAc and keeping the content of TEA unchanged. On the basis of these results, the possible formation mechanism of Fe3O4 was discussed. It was observed that TEA and NaOAc affected the growth rate of crystal planes and nucleation. Besides, the magnetic property tested by a vibrating sample magnetometer (VSM) showed that the products exhibited a ferromagnetic behavior and possessed the excellent saturation magnetization (Ms) at room temperature.

  17. Synthesis of nano-Se/bamboo charcoal composites via hydrothermal method and their application on remaining fresh of cutting roses.

    PubMed

    Tang, Ping; Yu, Weiping; Jiang, Kunpeng; Liao, Lei; Qin, Aimiao

    2013-02-01

    Nano-Se/bamboo charcoal (BC) composites were prepared successfully by hydrothermal method. The composites were characterized by SEM, XRD, Atomic Absorption Spectroscopy (AAS) and Atomic fluorescence spectroscopy (AFS) analysis. The effects of the synthesized conditions on the morphologies of Se particles on BC were investigated. The results showed that the reaction time, the adding order of reagents and the concentration of hydrazine have much influence on the formation of nano-Se/BC composites. The application of composites on the keeping fresh of cutting rose flowers was also studied, the experiment results indicate that Nano-Se/BC composites have better effect on the keeping fresh of cutting rose flowers than single BC, Nano-Se, distilled water and commercial "flower food" nutrient solution, the florescence of cutting rose flowers is distinctly extend by Nano-Se/BC composites up to 48 and 24 days in winter and summer respectively. "Synergy effects" and "Delayed release capsule effects" were used to explain the mechanism of Nano-Se/BC composites on the keeping fresh of cutting rose flowers.

  18. Facile Hydrothermal Synthesis of Fe3O4/C Core-Shell Nanorings for Efficient Low-Frequency Microwave Absorption.

    PubMed

    Wu, Tong; Liu, Yun; Zeng, Xiang; Cui, Tingting; Zhao, Yanting; Li, Yana; Tong, Guoxiu

    2016-03-23

    Using elliptical iron glycolate nanosheets as precursors, elliptical Fe3O4/C core-shell nanorings (NRs) [25 ± 10 nm in wall thickness, 150 ± 40 nm in length, and 1.6 ± 0.3 in long/short axis ratio] are synthesized via a one-pot hydrothermal route. The surface-poly(vinylpyrrolidone) (PVP)-protected-glucose reduction/carbonization/Ostwald ripening mechanism is responsible for Fe3O4/C NR formation. Increasing the glucose/precursor molar ratio can enhance carbon contents, causing a linear decrease in saturation magnetization (Ms) and coercivity (Hc). The Fe3O4/C NRs reveal enhanced low-frequency microwave absorption because of improvements to their permittivity and impedance matching. A maximum RL value of -55.68 dB at 3.44 GHz is achieved by Fe3O4/C NRs with 11.95 wt % C content at a volume fraction of 17 vol %. Reflection loss (RL) values (≤-20 dB) are observed at 2.11-10.99 and 16.5-17.26 GHz. Our research provides insights into the microwave absorption mechanism of elliptical Fe3O4/C core-shell NRs. Findings indicate that ring-like and core-shell nanostructures are promising structures for devising new and effective microwave absorbers.

  19. Synthesis and performances of bio-sourced nanostructured carbon membranes elaborated by hydrothermal conversion of beer industry wastes.

    PubMed

    El Korhani, Oula; Zaouk, Doumit; Cerneaux, Sophie; Khoury, Randa; Khoury, Antonio; Cornu, David

    2013-03-07

    Hydrothermal carbonization (HTC) process of beer wastes (Almaza Brewery) yields a biochar and homogeneous carbon-based nanoparticles (NPs). The NPs have been used to prepare carbon membrane on commercial alumina support. Water filtration experiments evidenced the quasi-dense behavior of the membrane with no measurable water flux below an applied nitrogen pressure of 6 bar. Gas permeation tests were conducted and gave remarkable results, namely (1) the existence of a limit temperature of utilization of the membrane, which was below 100°C in our experimental conditions, (2) an evolution of the microstructure of the carbon membrane with the operating temperature that yielded to improved performances in gas separation, (3) the temperature-dependent gas permeance should follow a Knudsen diffusion mechanism, and (4) He permeance was increasing with the applied pressure, whereas N2 and CO2 permeances remained stable in the same conditions. These results yielded an enhancement of both the He/N2 and He/CO2 permselectivities with the applied pressure. These promising results made biomass-sourced HTC-processed carbon membranes encouraging candidates as ultralow-cost and sustainable membranes for gas separation applications.

  20. Hydro-thermal synthesis and crystal structure of a new lanthanum(III) coordination polymer with fumaric acid.

    PubMed

    Anana, Hayet; Trifa, Chahrazed; Bouacida, Sofiane; Boudaren, Chaouki; Merazig, Hocine

    2015-05-01

    The title compound, poly[di-aqua-tris-(μ4-but-2-enedioato)(μ2-but-2-enedioic acid)dilanthanum(III)], [La2(C4H2O4)3(C4H4O4)(H2O)2] n , was synthesized by the reaction of lanthanum chloride penta-hydrate with fumaric acid under hydro-thermal conditions. The asymmetric unit comprises an La(III) cation, one and a half fumarate dianions (L (2-)), one a half-mol-ecule of fumaric acid (H2 L) and one coordinated water mol-ecule. Each La(III) cation has the same nine-coordinate environment and is surrounded by eight O atoms from seven distinct fumarate moieties, including one proton-ated fumarate unit and one water mol-ecule in a distorted tricapped trigonal-prismatic environment. The LaO8(H2O) polyhedra centres are edge-shared through three carboxyl-ate bridges of the fumarate ligand, forming chains in three dimensions to construct the MOF. The crystal structure is stabilized by O-H⋯O hydrogen-bond inter-actions between the coordin-ated water mol-ecule and the carboxyl-ate O atoms, and also between oxygen atoms of fumaric acid.

  1. Facile hydrothermal synthesis of TiO2-Bi2WO6 hollow superstructures with excellent photocatalysis and recycle properties.

    PubMed

    Hou, Ya-Fei; Liu, Shu-Juan; Zhang, Jing-huai; Cheng, Xiao; Wang, You

    2014-01-21

    One-dimensional mesoporous TiO2-Bi2WO6 hollow superstructures are prepared using a hydrothermal method and their photocatalysis and recycle properties are investigated. Experimental results indicate that anatase TiO2 nanoparticles are coupled with hierarchical Bi2WO6 hollow tubes on their surfaces. The TiO2-Bi2WO6 structure has a mesoporous wall and the pores in the wall are on average 21 nm. The hierarchical TiO2-Bi2WO6 heterostructures exhibit the highest photocatalytic activity in comparison with P25, pure Bi2WO6 hollow tube and mechanical mixture of Bi2WO6 tube and TiO2 nanoparticle in the degradation of rhodamine B (RhB) under simulated sunlight irradiation. The as-prepared TiO2-Bi2WO6 heterostructures can be easily recycled through sedimentation and they retains their high photocatalytic activity during the cycling use in the simulated sunlight-driving photodegradation process of RhB. The prepared mesoporous TiO2-Bi2WO6 with hollow superstructure is therefore a promising candidate material for water decontamination use.

  2. One-Pot Hydrothermal Synthesis of Magnetite Prussian Blue Nano-Composites and Their Application to Fabricate Glucose Biosensor

    PubMed Central

    Jomma, Ezzaldeen Younes; Ding, Shou-Nian

    2016-01-01

    In this work, we presented a simple method to synthesize magnetite Prussian blue nano-composites (Fe3O4-PB) through one-pot hydrothermal process. Subsequently, the obtained nano-composites were used to fabricate a facile and effective glucose biosensor. The obtained nanoparticles were characterized using transmission electron microscopy, scanning electron microscopy, Fourier-transform infrared spectroscopy, UV-vis absorbance spectroscopy, cyclic voltammetry and chronoamperometry. The resultant Fe3O4-PB nanocomposites have magnetic properties which could easily controlled by an external magnetic field and the electro-catalysis of hydrogen peroxide. Thus, a glucose biosensor based on Fe3O4-PB was successfully fabricated. The biosensor showed super-electrochemical properties toward glucose detection exhibiting fast response time within 3 to 4 s, low detection limit of 0.5 µM and wide linear range from 5 µM to 1.2 mM with sensitivity of 32 µA∙mM−1∙cm−2 and good long-term stability. PMID:26901204

  3. Aloe vera mediated hydrothermal synthesis of reduced graphene oxide decorated ZnO nanocomposite: Luminescence and antioxidant properties

    NASA Astrophysics Data System (ADS)

    Kavyashree, D.; Nagabhushana, H.; Ananda Kumari, R.; Basavaraj, R. B.; Suresh, D.; Daruka Prasad, B.; Sharma, S. C.

    2016-05-01

    A zinc oxide/reduced graphene oxide (ZnO/rGO) nanocomposite was fabricated by facile hydrothermal route using Aloe vera gel as surfactant. The PL emission spectrum of the ZnO/rGO composite consists of four peaks at around 380, 394, 449 and 465nm. The PL intensity is found to diminish in ZnO-rGO composites rather than in pure ZnO, which was attributed to electron transfer from ZnO to rGO. A single intense glow curve was recorded in rGo-ZnO for a dose range of 1-8kGy. The TL response curve of rGO-ZnO is found to be a simple glow curve structure, linear dependence over a dose range of 1-8kGy. The obtained ZnO/rGO composite could provide a facile and eco-friendly method for the development of graphene-based nanocomposites with promising applications in radiation dosimetry and antioxidant activities.

  4. Hydrothermal synthesis of Yb3+, Tm3+ co-doped Gd6MoO12 and its upconversion properties

    NASA Astrophysics Data System (ADS)

    Di, Qiu-Mei; Sun, Yu-Mei; Xu, Qi-Guang; Han, Liu; Xue, Bing; Sun, Jia-Yue

    2015-06-01

    Yb3+, Tm3+ co-doped Gd6MoO12 phosphors with different morphologies are prepared by the hydrothermal method. The dendrites present different morphologies (including hexagonal prisms, spindles, and spheres) after changing the pH value and edetate disodium (EDTA) usage. It is found that each of the two factors plays a crucial role in forming different morphologies. The up-conversion (UC) luminescence is studied. Under 980-nm semiconductor laser excitation, relatively strong blue emission and weak red emission are observed. Finally, the effect of pumping power on the UC luminescence properties and the level diagram mechanism of Gd6MoO12:Yb3+/Tm3+ phosphor are also discussed. Project supported by the National Natural Science Foundation of China (Grant No. 20976002), the Beijing Natural Science Foundation, China (Grant No. 2122012), the Key Projects for Science and Technology of Beijing Education Commission, China (Grant No. KZ201310011013), and the Education and Research Fund of Guangdong Province, China (Grant No. 2011B090400100).

  5. Hydrothermal synthesis and tunable luminescence of persimmon-like sodium lanthanum tungstate:Tb3+, Eu3+ hierarchical microarchitectures.

    PubMed

    Tian, Yue; Chen, Baojiu; Tian, Bining; Yu, Naisen; Sun, Jiashi; Li, Xiangping; Zhang, Jinsu; Cheng, Lihong; Zhong, Haiyang; Meng, Qingyu; Hua, Ruinian

    2013-03-01

    Persimmon-like NaLa(WO(4))(2) microarchitectures were prepared via hydrothermal process with using trisodium citrate (Na(3)Cit) as chelated reagent and characterized by X-ray diffraction (XRD), field emission scanning electron microscope (FE-SEM), photoluminescence (PL), and fluorescent dynamics. The influences of Na(3)Cit concentration, organic additivities, and reaction time on the morphologies of NaLa(WO(4))(2) phosphor were studied. The results revealed that Na(3)Cit species had double functions of strong ligand and structure-directing reagent that could efficiently control the formation of persimmon-like NaLa(WO(4))(2) microarchitectures. The possible mechanism for the growth of persimmon-like NaLa(WO(4))(2) microarchitectures was attributed to the Ostwald ripening mechanism. The energy transfer from Tb(3+) to Eu(3+) in the persimmon-like NaLa(WO(4))(2) phosphors was observed. The energy transfer efficiencies and emission colors can be tuned by changing the concentration of Eu(3+). Finally, it was deduced that the electric dipole-dipole interaction (D-D) is the main mechanism for energy transfer between Tb(3+) and Eu(3+) in the persimmon-like NaLa(WO(4))(2) phosphor.

  6. Template-directed hydrothermal synthesis of hydroxyapatite as a drug delivery system for the poorly water-soluble drug carvedilol

    NASA Astrophysics Data System (ADS)

    Zhao, Qinfu; Wang, Tianyi; Wang, Jing; Zheng, Li; Jiang, Tongying; Cheng, Gang; Wang, Siling

    2011-09-01

    In order to improve the dissolution rate and increase the bioavailability of a poorly water-soluble drug, intended to be administered orally, the biocompatible and bioactive mesoporous hydroxyapatite (HA) was successfully synthesized. In the present study, mesoporous HA nanoparticles were produced using Pluronic block co-polymer F127 and cetyltrimethylammonium bromide (CTAB) as templates by the hydrothermal method. The obtained mesoporous HA was employed as a drug delivery carrier to investigate the drug storage/release properties using carvedilol (CAR) as a model drug. Characterizations of the raw CAR powder, mesoporous HA and CAR-loaded HA were carried out by the scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray powder diffraction (XRPD), differential scanning calorimetry (DSC), Fourier transform infrared (FT-IR) spectroscopy, N2 adsorption/desorption, thermogravimetric analysis (TGA), and UV-VIS spectrophotometry. The results demonstrated that CAR was successfully incorporated into the mesoporous HA host. In vitro drug release studies showed that mesoporous HA had a high drug load efficiency and provided immediate release of CAR compared with micronized raw drug in simulated gastric fluid (pH 1.2) and intestinal fluid (pH 6.8). Consequently, mesoporous HA is a good candidate as a drug carrier for the oral delivery of poorly water-soluble drugs.

  7. Synthesis and characterization of ZnO microstructures via a cationic surfactant-assisted hydrothermal microemulsion process

    SciTech Connect

    Liu Yumin Lv Hua; Li Shuangqing; Xi Guoxi; Xing Xinyan

    2011-05-15

    Hexagonal cylinder-like ZnO with a regular twinning microstructure was successfully synthesized via a cationic surfactant-assisted hydrothermal microemulsion route. X-ray diffraction, scanning electron microscopy and Ultraviolet and Visible absorption spectroscopy were employed to characterize the structure, morphologies and properties of the as-prepared samples. The results showed that the reaction temperature, reaction time and molar ratio (w) between water and CTAB exhibited obvious influences on the morphologies and sizes of the products. The Ultraviolet and Visible absorption spectra revealed a strong and broad absorption band from ultraviolet to visible region and the maximum absorption peak appeared at 376 nm. Moreover, the possible growth mechanism for the ZnO microstructures was also discussed in this study. - Research Highlights: {yields} Hexagonal cylinder-like ZnO with twinning microstructure was prepared. {yields} Water/surfactant ratio exhibits obvious influence on the morphology and size of ZnO. {yields} An aggregation mechanism of the ZnO microstructures has been proposed.

  8. Synthesis and performances of bio-sourced nanostructured carbon membranes elaborated by hydrothermal conversion of beer industry wastes

    PubMed Central

    2013-01-01

    Hydrothermal carbonization (HTC) process of beer wastes (Almaza Brewery) yields a biochar and homogeneous carbon-based nanoparticles (NPs). The NPs have been used to prepare carbon membrane on commercial alumina support. Water filtration experiments evidenced the quasi-dense behavior of the membrane with no measurable water flux below an applied nitrogen pressure of 6 bar. Gas permeation tests were conducted and gave remarkable results, namely (1) the existence of a limit temperature of utilization of the membrane, which was below 100°C in our experimental conditions, (2) an evolution of the microstructure of the carbon membrane with the operating temperature that yielded to improved performances in gas separation, (3) the temperature-dependent gas permeance should follow a Knudsen diffusion mechanism, and (4) He permeance was increasing with the applied pressure, whereas N2 and CO2 permeances remained stable in the same conditions. These results yielded an enhancement of both the He/N2 and He/CO2 permselectivities with the applied pressure. These promising results made biomass-sourced HTC-processed carbon membranes encouraging candidates as ultralow-cost and sustainable membranes for gas separation applications. PMID:23497215

  9. Synthesis and performances of bio-sourced nanostructured carbon membranes elaborated by hydrothermal conversion of beer industry wastes

    NASA Astrophysics Data System (ADS)

    El Korhani, Oula; Zaouk, Doumit; Cerneaux, Sophie; Khoury, Randa; Khoury, Antonio; Cornu, David

    2013-03-01

    Hydrothermal carbonization (HTC) process of beer wastes (Almaza Brewery) yields a biochar and homogeneous carbon-based nanoparticles (NPs). The NPs have been used to prepare carbon membrane on commercial alumina support. Water filtration experiments evidenced the quasi-dense behavior of the membrane with no measurable water flux below an applied nitrogen pressure of 6 bar. Gas permeation tests were conducted and gave remarkable results, namely (1) the existence of a limit temperature of utilization of the membrane, which was below 100°C in our experimental conditions, (2) an evolution of the microstructure of the carbon membrane with the operating temperature that yielded to improved performances in gas separation, (3) the temperature-dependent gas permeance should follow a Knudsen diffusion mechanism, and (4) He permeance was increasing with the applied pressure, whereas N2 and CO2 permeances remained stable in the same conditions. These results yielded an enhancement of both the He/N2 and He/CO2 permselectivities with the applied pressure. These promising results made biomass-sourced HTC-processed carbon membranes encouraging candidates as ultralow-cost and sustainable membranes for gas separation applications.

  10. Biomolecule-assisted hydrothermal synthesis and self-assembly of Bi2Te3 nanostring-cluster hierarchical structure.

    PubMed

    Mi, Jian-Li; Lock, Nina; Sun, Ting; Christensen, Mogens; Søndergaard, Martin; Hald, Peter; Hng, Huey H; Ma, Jan; Iversen, Bo B

    2010-05-25

    A simple biomolecule-assisted hydrothermal approach has been developed for the fabrication of Bi(2)Te(3) thermoelectric nanomaterials. The product has a nanostring-cluster hierarchical structure which is composed of ordered and aligned platelet-like crystals. The platelets are approximately 100 nm in diameter and only approximately 10 nm thick even though a high reaction temperature of 220 degrees C and a long reaction time of 24 h were applied to prepare the sample. The growth of the Bi(2)Te(3) hierarchical structure appears to be a self-assembly process. Initially, Te nanorods are formed using alginic acid as both reductant and template. Subsequently, Bi(2)Te(3) grows in a certain direction on the surface of the Te rods, resulting in the nanostring structure. The nanostrings further recombine side-by-side with each other to achieve the ordered nanostring clusters. The particle size and morphology can be controlled by adjusting the concentration of NaOH, which plays a crucial role on the formation mechanism of Bi(2)Te(3). An even smaller polycrystalline Bi(2)Te(3) superstructure composed of polycrystalline nanorods with some nanoplatelets attached to the nanorods is achieved at lower NaOH concentration. The room temperature thermoelectric properties have been evaluated with an average Seebeck coefficient of -172 microV K(-1), an electrical resistivity of 1.97 x 10(-3) Omegam, and a thermal conductivity of 0.29 W m(-1) K(-1).

  11. Synthesis of TiO2 nanorods from titania and titanyl sulfate produced from ilmenite dissolution by hydrothermal method

    NASA Astrophysics Data System (ADS)

    Wahyuningsih, S.; Ramelan, A. H.; Munifa, R. M. I.; Saputri, L. N. M. Z.; Chasanah, U.

    2016-11-01

    TiO2 powder has been synthesized through hydrolysis-condensation of titanyl sulfate solution to a starting material of TiO2 nanorods formation. This processing was conducted by the solid separation of TiO2 from ilmenite by roasting ilmenite, acidic leaching (hydrolysis), and co-precipitation (condensation). Roasting of ilmenite was carried out by the addition of Na2S at a temperature of 800°C. While the acidic leaching process was conducted by sulfuric acid at a various concentrations of 3, 3.5, 4.5, 6, and 9 M. The result shown that the solubility optimum occurs in H2SO4 6 M condition. Separation of Fe impurities of TiO2 gel from titanyl sulfate (TiOSO4) solution was done through complexation using KCNS addition. The characteristic of TiO2 obtained using X-Ray Fluorescence (XRF) and X-Ray Diffraction (XRD) showed good crystallinity and purity. Further treatment of the TiO2 is the formation of one-dimensional nano-size (1-D nanorods) through a hydrothermal method under basic condition NaOH 12M solution. TiO2 nanorods were confirmed by Transmission Electron Microscope (TEM) which indicated that the diameter of TiO2 nanorods was about 7.02 nm in size.

  12. Hydrothermal Synthesis of Hematite-Rich Spherules: Implications for Diagenesis and Hematite Spherule Formation in Outcrops at Meridiani Planum, Mars

    NASA Technical Reports Server (NTRS)

    Golden, D. C.; Ming, D. W.; Morris, R. V.; Graff, T. G.

    2007-01-01

    The Athena science payload onboard the Opportunity rover identified hematite-rich spherules (mean diameter of 4.2 +/- 0.8 mm) embedded in outcrops and occurring as lag deposits at Meridiani Planum. They have formed as diagenetic concretions from the rapid breakdown of pre-existing jarosite and other iron sulfates when chemically distinct groundwater passed through the sediments. Diagenetic, Fe-cemented concretions found in the Jurassic Navajo Formation, Utah and hematite-rich spherules found within sulfate-rich volcanic breccia on Mauna Kea volcano, Hawaii are possible terrestrial analogues for Meridiani spherules. The Navajo Formation concretions form in porous quartz arenite from the dissolution of iron oxides by reducing fluids and subsequent Fe precipitation to form spherical Fe- and Si-rich concretions. The Mauna Kea spherules form by hydrothermal, acid-sulfate alteration of basaltic tephra. The formation of hematite-rich spherules with similar chemical, mineralogical, and morphological properties to the Meridiani spherules is rare on Earth, so little is known about their formation conditions. In this study, we have synthesized in the laboratory hematite-rich spherules that are analogous in nearly all respects to the Meridiani spherules.

  13. Hydrothermal synthesis of layer-controlled MoS2/graphene composite aerogels for lithium-ion battery anode materials

    NASA Astrophysics Data System (ADS)

    Zhao, Bing; Wang, Zhixuan; Gao, Yang; Chen, Lu; Lu, Mengna; Jiao, Zheng; Jiang, Yong; Ding, Yuanzhang; Cheng, Lingli

    2016-12-01

    Layer-controlled MoS2/graphene aerogels (MoS2/GA) composites are synthesized by a facile hydrothermal route, in which few-layer (5-15 layers) MoS2 nanosheets with high crystalline are decorated on the surface of graphene nanosheets homogeneously and tightly. The number of the MoS2 layers can be easily controlled through adjusting the amount of molybdenum source in the reaction system. Moreover, the growth mechanism of the lay-controlled MoS2/GA composites is proposed. The three-dimensional MoS2/GA with macroporous micro-structure not only shortens the transportation length of electrons and ions, but also restrains the re-stacking of MoS2 effectively, stabilizing the electrode structure during repeated charging/discharging processes. Electrochemical tests demonstrate that this few-layer MoS2/GA composite exhibits a high reversible capacity of 1085.0 mAh g-1 at current density of 100 mA g-1, as well as extraordinarily high cycling stability and rate capability.

  14. Hydrothermal synthesis, structure, heterogeneous catalytic activity and photoluminescent properties of a novel homoleptic Sm(III)-organic framework

    NASA Astrophysics Data System (ADS)

    Ay, Burak; Yildiz, Emel; Felts, Ashley C.; Abboud, Khalil A.

    2016-12-01

    A novel metal-organic framework, (H2pip)n[Sm2(pydc)4(H2O)2]n (1) (H2pydc=2,6-pyridinedicarboxylic acid, H2pip=piperazine) has been synthesized under hydrothermal conditions and characterized by the elemental analysis, inductively coupled plasma (ICP) spectrometer, fourier transform infrared (FT-IR) spectra, thermogravimetric analysis (TGA), single crystal X-ray diffraction analysis and powder X-ray diffraction (PXRD). The structure of 1 was determined to be three-dimensional, linked along Sm-O-Sm chains. The asymmetric unit consisted of one singly anionic fragment consisting of Sm(III) coordinated to two H2pydc ligands and one water, and one half of a protonated H2pip, which sits on an inversion center. 1 exhibited luminescence emission bands at 534 nm at room temperature when excited at 440 nm. Its thermal behavior and catalytic performance were investigated and the selectivity was measured as 100% for the oxidation of thymol to thymoquinone.

  15. Part III: lithium metasilicate (Li2SiO3)—mild condition hydrothermal synthesis, characterization and optical properties

    NASA Astrophysics Data System (ADS)

    Alemi, Abdolali; Khademinia, Shahin; Sertkol, Murat

    2015-02-01

    Li2SiO3 nanopowders were synthesized via a non-stoichiometric 2:3 (S1), 1:3 (S2), 1:4 (S3) and 1:5 (S4) Li/Si molar ratios via hydrothermal reaction for 72 h at 180 °C in an aqua solution using Li2CO3 and H2SiO3 as raw materials. The synthesized materials were characterized by powder X-ray diffraction (PXRD) technique and Fourier transform infrared spectroscopy. PXRD data showed that the crystal structure of the obtained materials is orthorhombic with the space group of Cmc21. Also, to investigate the effect of the Li/Si molar ratio on the morphology of the obtained materials, the morphologies of the synthesized materials were studied by field emission scanning electron microscopy. The technique showed that with changing the Li/Si molar ratio from S1 to S4, the morphology of as-prepared samples changed from flower structures to microrod-microsphere and then to a non-homogenous layer-like structure. Ultraviolet-visible spectra showed that the nanostructure lithium silicate powders had good light absorption properties in the ultraviolet light region. It showed that with changing the Li/Si molar ratio from S1 to S4, the calculated band gap was decreased. Also, cell parameter refinement showed that with changing the Li/Si molar ratio from S1 to S4 the cell parameters decreased. Photoluminescence analysis of the obtained materials was studied at the excitation wavelength of 247 nm. It showed that the emission spectra of the obtained materials had a blue shift from S1 to S4.

  16. The simple hydrothermal synthesis of Ag-ZnO-SnO2 nanochain and its multiple applications.

    PubMed

    Balachandran, Subramanian; Selvam, Kaliyamoorthy; Babu, Balraj; Swaminathan, Meenakshisundaram

    2013-12-14

    In this article, we report the fabrication of a stable Ag-ZnO-SnO2 nanochain by template free hydrothermal method and its photocatalytic activity for the first time. This composite material represents a potential new class of photocatalysts with enhanced light absorption, hydrophobic and electronic properties of ZnO. This catalyst has been characterized by X-ray diffraction (XRD), high resolution scanning electron microscopy (HRSEM), field emission scanning electron microscopy (FESEM), elemental mapping, energy dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), UV-Vis diffuse reflectance spectroscopy (DRS) and photoluminescence spectroscopy (PL). XRD and elemental mapping reveal the presence of SnO2 and Ag in the catalyst. Ag-ZnO-SnO2 has increased absorption in the visible region when compared to ZnO. This three component nano junction system exhibits enhanced photocatalytic activity for the degradation of azo dyes, Acid Black 1 (AB 1) and Acid Violet 7 (AV 7) under UV light (365 nm), far exceeding those of the single and two component systems. Ag-ZnO-SnO2 is found to be reusable without appreciable loss of catalytic activity up to four runs. Based on the band gap energies of ZnO and SnO2, a mechanism is proposed for the photodegradation of dyes. Hydrophobicity and photoconductivity of Ag-ZnO-SnO2 have been evaluated. Nanochain exhibiting higher positive photoconductivity can be useful for soliton wave communication as well as solar cell applications. Our results provide some new insights on the fabrication of Ag-ZnO-SnO2 and its performance as an active photocatalyst, self cleaning and conducting material.

  17. Hydrothermal synthesis and characterization under dynamic conditions of cobalt oxide nanoparticles supported over magnesium oxide nano-plates.

    PubMed

    Alayoglu, Selim; Rosenberg, Daniel J; Ahmed, Musahid

    2016-06-14

    A nano-catalyst comprised of oxidized Co NPs supported on MgO nano-plates was synthesized via a hydrothermal co-precipitation strategy and calcination in O2 and subsequently in H2 at 250 °C. Spectro-microscopy characterization was performed by scanning transmission electron microscopy, electron energy loss spectroscopy and scanning X-ray transmission microscopy. Surface measurements under H2 and H2 + CO atmospheres were obtained by ambient pressure X-ray photoelectron spectroscopy and in situ X-ray absorption spectroscopy in the 225-480 °C range. These measurements at the atomic and microscopic levels demonstrated that the oxidized Co nanoparticles uniformly decorated the MgO nano-plates. The surfaces are enriched with Co, and with a mixture of Co(OH)2 and CoO under H2 and H2 + CO atmospheres. Under a H2 atmosphere, the outermost surfaces were composed of (lattice) O(2-), CO3(2-) and OH(-). No inorganic carbonates were observed in the bulk. Chemisorbed CO, likely on the oxidized Co surfaces, was observed at the expense of O(2-) under 300 mTorr H2 + CO (2 : 1) at 225 °C. Gas phase CO2 was detected under 32 Torr H2 + CO (2 : 1) at 225 °C upon prolonged reaction time, and was attributed to a surface chemical reaction between O(2-) and chemisorbed CO. Furthermore, sp(3) like carbon species were detected on the otherwise carbon free surface in H2 + CO, which remained on the surface under the subsequent reaction conditions. The formation of sp(3) like hydrocarbons was ascribed to a surface catalytic reaction between the chemisorbed CO and OH(-) as the apparent hydrogen source.

  18. [Study on the Hydrothermal Synthesis and Fluorescence of LaF3 : Tb3+, Ce3+ Nanocrystals].

    PubMed

    Xu, Shi-hua; Huang, Zhong-jing; Liu, Guo-cong; Wei, Qing-min

    2016-03-01

    LaF3 : Tba3+, Ce3+ nanocrystals were prepared with hydrothermal method with the help of cetyltrimethyl ammonium bromide (CTAB). The effects of pH values of the solution, Ce3+/Tb+ ratio value and reaction time on the luminescent properties were investigated. XRD analysis shows that the as-prepared samples possess hexagonal phase and their main diffraction peaks of samples are similar to the standard card (JCPDS 32-0483). Compared with pure LaF3, the main diffraction peaks of the doped samples have a slight shift, showing existing isomorphous substitution between La3+ and the doped rare earth ions in parent lattice of LaF3. It is found from TEM results that the as-prepared samples have good crystallinity and their average grain sizes change in the range of 20-50 nm. The excitation spectra indicate that the stronger excitation spectrum peaks exist at 250 nm, which is assigned to the transition of 4f --> 5d from Ce3+. When activated at 250 nm, all LaF3 : Tb3+, Ce3+ nanocrystals possess weak blue emission at 490 nm (electric dipole transition, 5D4 --> 7F6) and good green emission at 543 nm (magnetic dipole transition, 5D4 -->7F5). As the Ce3+/Tb+ ratio increases, the fluorescence intensities increase at first and then weaken, and reach the strongest green emission at n(Ce)3+ /n(Tb)3+ = 4. The pH values have some influence on the colors and intensities of the LaF3 : Tb3+, Ce3+ nanocrystals. The sample prepared at pH 9 presents the best color, while the one at pH 7 exhibits the strongest green emission. Besides, increasing reaction time is helpful to improve color purity of sample and enhance its green emission.

  19. Rare earth doped LiYbF{sub 4} phosphors with controlled morphologies: Hydrothermal synthesis and luminescent properties

    SciTech Connect

    Huang, Wenjuan; Lu, Chunhua; Jiang, Chenfei; Jin, Junyang; Ding, Mingye; Ni, Yaru; Xu, Zhongzi

    2012-06-15

    Highlights: ► LiYbF{sub 4} microparticles as an excellent upconverting materials. ► High temperature and long time can favor high crystalline LiYbF{sub 4} microparticles. ► The shape of LiYbF{sub 4} microparticles can be tuned by the molar ratio of EDTA to Yb{sup 3+}. ► Bright green emission can be obtained by changing the doping concentration of Er{sup 3+}. -- Abstract: High quality monodisperse LiYbF{sub 4} microparticles with shape of octahedron had been prepared via a facile hydrothermal route. The crystalline phase, size, morphology and luminescence properties were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), photoluminescence (PL) spectra and Commission Internationale de L’Eclairage (CIE 1931) chromaticity coordinates, respectively. The influences of reaction temperature, reaction time and the molar ratio of EDTA to Yb{sup 3+} on the crystal phases and shapes of as-prepared products had been investigated in detail. The upconversion (UC) luminescence properties of LiYb{sub 1−x}F{sub 4}:xEr{sup 3+} (x =0.1, 0.2, 0.5, 1, 2, 5 and 10 mol%) particles with octahedral microstructures were studied under 976 nm excitation. The results showed that the luminescence colors of the corresponding products could be tuned to bright green by changing the doping concentration of Er{sup 3+} ion. The luminescence mechanisms for the doped Er{sup 3+} ion were thoroughly analyzed, showing great potential in applications such as biolabels, displays and other optical technologies.

  20. Rapid synthesis of Ti-MCM-41 by microwave-assisted hydrothermal method towards photocatalytic degradation of oxytetracycline.

    PubMed

    Chen, Hanlin; Peng, Yen-Ping; Chen, Ku-Fan; Lai, Chia-Hsiang; Lin, Yung-Chang

    2016-06-01

    This study employed microwave-assisted hydrothermal method to synthesize Ti-MCM-41, which are mesoporous materials with a high surface area and excellent photocatalytic ability. Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), and ultraviolet-visible spectroscopy (UV-Vis) were employed. The XRD findings showed that Ti-MCM-41 exhibited a peak at 2θ of 2.2°, which was attributed to the hexagonal MCM-41 structure. The BET (Brunauer-Emmett-Teller) results agreed with the TEM findings that Ti-MCM-41 has a pore size of about 3-5nm and a high surface area of 883m(2)/g. FTIR results illustrated the existence of Si-O-Si and Si-O-Ti bonds in Ti-MCM-41. The appearance of Ti 2p peaks in the XPS results confirmed the FTIR findings that the Ti was successfully doped into the MCM-41 structure. Zeta (ζ)-potential results indicated that the iso-electric point (IEP) of Ti-MCM-41 was at about pH3.02. In this study, the photocatalytic degradation of oxytetracycline (OTC) at different pH was investigated under Hg lamp irradiation (wavelength 365nm). The rate constant (K'obs) for OTC degradation was 0.012min(-1) at pH3. Furthermore, TOC (total organic carbon) and high resolution LC-MS (liquid chromatography-mass spectrometry) analyses were conducted to elucidate the possible intermediate products and degradation pathway for OTC. The TOC removal efficiency of OTC degradation was 87.0%, 74.4% and 50.9% at pH3, 7 and 10, respectively. LC-MS analysis results showed that the degradation products from OTC resulted from the removal of functional groups from the OTC ring.

  1. Synthesis, characterization, and magnetic properties of monodisperse CeO2 nanospheres prepared by PVP-assisted hydrothermal method

    PubMed Central

    2012-01-01

    Ferromagnetism was observed at room temperature in monodisperse CeO2 nanospheres synthesized by hydrothermal treatment of Ce(NO3)3·6H2O using polyvinylpyrrolidone as a surfactant. The structure and morphology of the products were characterized by X-ray diffraction (XRD), Raman spectroscopy, transmission electron microscopy, high-resolution transmission electron microscopy, and field-emission scanning electron microscopy (FE-SEM). The optical properties of the nanospheres were determined using UV and visible spectroscopy and photoluminescence (PL). The valence states of Ce ions were also determined using X-ray absorption near edge spectroscopy. The XRD results indicated that the synthesized samples had a cubic structure with a crystallite size in the range of approximately 9 to 19 nm. FE-SEM micrographs showed that the samples had a spherical morphology with a particle size in the range of approximately 100 to 250 nm. The samples also showed a strong UV absorption and room temperature PL. The emission might be due to charge transfer transitions from the 4f band to the valence band of the oxide. The magnetic properties of the samples were studied using a vibrating sample magnetometer. The samples exhibited room temperature ferromagnetism with a small magnetization of approximately 0.0026 to 0.016 emu/g at 10 kOe. Our results indicate that oxygen vacancies could be involved in the ferromagnetic exchange, and the possible mechanism of formation was discussed based on the experimental results. PMID:22849756

  2. Hydrothermal synthesis of coral-like Au/ZnO catalyst and photocatalytic degradation of Orange II dye

    SciTech Connect

    Chen, P.K.; Lee, G.J.; Davies, S.H.; Masten, S.J.; Amutha, R.; Wu, J.J.

    2013-06-01

    Highlights: ► Coral-like Au/ZnO was successfully prepared using green synthetic method. ► Gold nanoparticles were deposited on the ZnO structure using NaBH{sub 4} and β-D-glucose. ► Coral-like Au/ZnO exhibited superior photocatalytic activity to degrade Orange II. - Abstract: A porous coral-like zinc oxide (c-ZnO) photocatalyst was synthesized by the hydrothermal method. The coral-like structure was obtained by precipitating Zn{sub 4}(CO{sub 3})(OH){sub 6}·H{sub 2}O (ZnCH), which forms nanosheets that aggregate together to form microspheres with the coral-like structure. X-ray diffraction (XRD) studies indicate that after heating at 550 °C the ZnCH microspheres can be converted to ZnO microspheres with a morphology similar to that of ZnCH microspheres. Thermogravimetric analysis (TGA) shows this conversion takes place at approximately 260 °C. A simple electrostatic self-assembly method has been employed to uniformly disperse Au nanoparticles (1 wt.%) on the ZnO surface. In this procedure β-D-glucose was used to stabilize the Au nanoparticles. Scanning electron microscope images indicate that the diameter of coral-like ZnO microspheres (c-ZnO) is about 8 μm. X-ray diffraction reveals that the ZnO is highly crystalline with a wurtzite structure and the Au metallic particles have an average size of about 13 nm. X-ray photoelectron spectroscopic (XPS) studies have confirmed the presence of ZnO and also showed that the Au is present in the metallic state. The photocatalytic degradation of Orange II dye, with either ultraviolet or visible light, is faster on Au/c-ZnO than on c-ZnO.

  3. High-temperature, high-pressure hydrothermal synthesis, characterization, and structural relationships of mixed-alkali metals uranyl silicates

    NASA Astrophysics Data System (ADS)

    Chen, Yi-Hsin; Liu, Hsin-Kuan; Chang, Wen-Jung; Tzou, Der-Lii; Lii, Kwang-Hwa

    2016-04-01

    Three mixed-alkali metals uranyl silicates, Na3K3[(UO2)3(Si2O7)2]·2H2O (1), Na3Rb3[(UO2)3(Si2O7)2] (2), and Na6Rb4[(UO2)4Si12O33] (3), have been synthesized by high-temperature, high-pressure hydrothermal reactions at 550 °C and 1440 bar, and characterized by single-crystal X-ray diffraction, photoluminescence, and thermogravimetric analysis. Compound 1 and 2 are isostructural and contain layers of uranyl disilicate. The smaller cation, Na+, is located in the intralayer channels, whereas the larger cations, K+ and Rb+, and water molecule are located in the interlayer region. The absence of lattice water in 2 can be understood according to the valence-matching principle. The structure is related to that of a previously reported mixed-valence uranium(V,VI) silicate. Compound 3 adopts a 3D framework structure and contains a unique unbranched dreier fourfold silicate chain with the structural formula {uB,41∞}[3Si12O33] formed of Q2, Q3, and Q4 Si. The connectivity of the Si atoms in the Si12O3318- anion can be interpreted on the basis of Zintl-Klemm concept. Crystal data for compound 1: triclinic, P-1, a=5.7981(2) Å, b=7.5875(3) Å, c=12.8068(5) Å, α=103.593(2)°, β=102.879(2)°, γ=90.064(2)°, V=533.00(3) Å3, Z=1, R1=0.0278; compound 2: triclinic, P-1, a=5.7993(3) Å, b=7.5745(3) Å, c=12.9369(6) Å, α=78.265(2)°, β=79.137(2)°, γ=89.936(2)°, V=546.02(4) Å3, Z=1, R1=0.0287; compound 3: monoclinic, C2/m, a=23.748(1) Å, b=7.3301(3) Å, c=15.2556(7) Å, β=129.116(2)°, V=2060.4(2) Å3, Z=2, R1=0.0304.

  4. Hydrothermal synthesis, structure, Raman spectroscopy, and self-irradiation studies of {sup 248}Cm(IO{sub 3}){sub 3}

    SciTech Connect

    Sykora, Richard E.; Assefa, Zerihun; Haire, Richard G. . E-mail: hairerg@ornl.gov; Albrecht-Schmitt, Thomas E. . E-mail: albreth@auburn.edu

    2004-12-01

    The study of curium iodate, Cm(IO{sub 3}){sub 3}, was undertaken as part of a systematic investigation of the 4f- and 5f-elements' iodates. The reaction of {sup 248}CmCl{sub 3} with aqueous H{sub 5}IO{sub 6} under mild hydrothermal conditions results in the reduction of IO{sub 6}{sup 5-} to IO{sub 3}{sup -} anions, and the subsequent formation of Cm(IO{sub 3}){sub 3} single crystals. Crystallographic data are: (193K, MoK{alpha}, {lambda}=0.71073A): monoclinic, space group P2{sub 1}/c, a=7.2014(7)A, b=8.5062(9)A, c=13.4622(14)A, {beta}=100.142(2){sup o}, V=811.76(14), Z=4, R(F)=2.11%, Rw(Fo2)=4.43% for 119 parameters with 1917 reflections with I>2{sigma}(I). The structure consists of Cm{sup 3+} cations bound by iodate anions to form [Cm(IO{sub 3}){sub 8}] units, where the local coordination environment around the curium centers can be described as a distorted dodecahedron. There are three crystallographically unique iodate anions within the structure; two iodates bridge between three Cm centers, and one iodate bridges between two Cm centers and has a terminal oxygen atom. The bridging of the curium centers by the iodate anions creates a three-dimensional structure. Three strong Raman bands with comparable intensities were observed at 846, 804, and 760cm{sup -1} and correspond to the I-O symmetric stretching of the three crystallographically distinct iodate ions. The Raman profile suggests a lack of inter-ionic vibrational coupling of the I-O stretching, while intra-ionic coupling provides symmetric and asymmetric components that correspond to each iodate site. Repeated collection of X-ray diffraction data for a crystal of Cm(IO{sub 3}){sub 3} over a period of time revealed a gradual expansion of the unit cell from self-irradiation. After 71 days, the new parameters were: a=7.2132(7)A, b=8.5310(8)A, c=13.505(1)A, {beta}=100.021(2){sup o}, V=818.3(2)

  5. Hydrothermal synthesis of titanium dioxide nanoparticles: mosquitocidal potential and anticancer activity on human breast cancer cells (MCF-7).

    PubMed

    Murugan, Kadarkarai; Dinesh, Devakumar; Kavithaa, Krishnamoorthy; Paulpandi, Manickam; Ponraj, Thondhi; Alsalhi, Mohamad Saleh; Devanesan, Sandhanasamy; Subramaniam, Jayapal; Rajaganesh, Rajapandian; Wei, Hui; Kumar, Suresh; Nicoletti, Marcello; Benelli, Giovanni

    2016-03-01

    Mosquito vectors (Diptera: Culicidae) are responsible for transmission of serious diseases worldwide. Mosquito control is being enhanced in many areas, but there are significant challenges, including increasing resistance to insecticides and lack of alternative, cost-effective, and eco-friendly products. To deal with these crucial issues, recent emphasis has been placed on plant materials with mosquitocidal properties. Furthermore, cancers figure among the leading causes of morbidity and mortality worldwide, with approximately 14 million new cases and 8.2 million cancer-related deaths in 2012. It is expected that annual cancer cases will rise from 14 million in 2012 to 22 million within the next two decades. Nanotechnology is a promising field of research and is expected to give major innovation impulses in a variety of industrial sectors. In this study, we synthesized titanium dioxide (TiO2) nanoparticles using the hydrothermal method. Nanoparticles were subjected to different analysis including UV-Vis spectrophotometry, Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), zeta potential, and energy-dispersive spectrometric (EDX). The synthesized TiO2 nanoparticles exhibited dose-dependent cytotoxicity against human breast cancer cells (MCF-7) and normal breast epithelial cells (HBL-100). After 24-h incubation, the inhibitory concentrations (IC50) were found to be 60 and 80 μg/mL on MCF-7 and normal HBL-100 cells, respectively. Induction of apoptosis was evidenced by Acridine Orange (AO)/ethidium bromide (EtBr) and 4',6-diamidino-2-phenylindole dihydrochloride (DAPI) staining. In larvicidal and pupicidal experiments conducted against the primary dengue mosquito Aedes aegypti, LC50 values of nanoparticles were 4.02 ppm (larva I), 4.962 ppm (larva II), 5.671 ppm (larva III), 6.485 ppm (larva IV), and 7.527 ppm (pupa). Overall, our results suggested that TiO2 nanoparticles may be considered as

  6. Photovoltaic performance of dye-sensitized solar cells using TiO2 nanotubes aggregates produced by hydrothermal synthesis

    NASA Astrophysics Data System (ADS)

    Chen, Qiufan; Sun, Xiaonan; Liu, Anping; Zhang, Qifeng; Cao, Guozhong; Zhou, Xiaoyuan

    2015-09-01

    This paper reports the synthesis, detailed structural characterization of aggregated TiO2 nanotubes and the application of such aggregated TiO2 nanotubes as photoelectrodes in solar cells (dye sensitized DSCs). A maximum overall conversion efficiency of 7.9% has been achieved, which use conventional dyes without any additional chemical treatments under circumstances of an open-circuit voltage of 710 mV, a short-circuit current density of 16.8mA/cm2, and a fill factor of 66%. This impressive performance is believed to attribute to the micron-sized aggregate structure which may be favorable for light harvesting, the desired high specific surface area and pure anatase phase for dye absorption. This significant improvement in the conversion efficiency indicates that DSCs based on aggregated TiO2 nanotubes are a promising alternative to semiconductor-based solar cells.

  7. Microwave-hydrothermal synthesis and characterization of nanostructured copper substituted ZnM2O4 (M = Al, Ga) spinels as precursors for thermally stable Cu catalysts.

    PubMed

    Conrad, Franziska; Massue, Cyriac; Kühl, Stefanie; Kunkes, Edward; Girgsdies, Frank; Kasatkin, Igor; Zhang, Bingsen; Friedrich, Matthias; Luo, Yuan; Armbrüster, Marc; Patzke, Greta R; Behrens, Malte

    2012-03-21

    Nanostructured Cu(x)Zn(1-x)Al(2)O(4) with a Cu:Zn ratio of ¼:¾ has been prepared by a microwave-assisted hydrothermal synthesis at 150 °C and used as a precursor for Cu/ZnO/Al(2)O(3)-based catalysts. The spinel nanoparticles exhibit an average size of approximately 5 nm and a high specific surface area (above 250 m(2) g(-1)). Cu nanoparticles of an average size of 3.3 nm can be formed by reduction of the spinel precursor in hydrogen and the accessible metallic Cu(0) surface area of the reduced catalyst was 8 m(2) g(-1). The catalytic performance of the material in CO(2) hydrogenation and methanol steam reforming was compared with conventionally prepared Cu/ZnO/Al(2)O(3) reference catalysts. The observed lower performance of the spinel-based samples is attributed to a lack of synergetic interaction of the Cu nanoparticles with ZnO due to the incorporation of Zn(2+) in the stable spinel lattice. Despite its lower performance, however, the nanostructured nature of the spinel catalyst was stable after thermal treatment up to 500 °C in contrast to other Cu-based catalysts. Furthermore, a large fraction of the re-oxidized copper migrates back into the spinel upon calcination of the reduced catalyst, thereby enabling a regeneration of sintered catalysts after prolonged usage at high temperatures. Similarly prepared samples with Ga instead of Al exhibit a more crystalline catalyst with a spinel particle size around 20 nm. The slightly decreased Cu(0) surface area of 3.2 m(2) g(-1) due to less copper incorporation is not a significant drawback for the methanol steam reforming.

  8. Carbonated hydroxyapatite starting from calcite and different orthophosphates under moderate hydrothermal conditions: Synthesis and surface reactivity in simulated body fluid

    SciTech Connect

    Pham Minh, Doan Nzihou, Ange; Sharrock, Patrick

    2014-12-15

    Highlights: • Carbonated apatite (CAP) could be easily obtained from CaCO{sub 3} and orthophosphates. • Highest CaCO{sub 3} dissolution and apatitic carbonate content were obtained with H{sub 3}PO{sub 4}. • A-B-type CAP was formed. • The synthesized CAP was thermally stable up to 1000 °C. • This CAP showed high biomineralization activity before and after thermal treatment. - Abstract: The one-step synthesis of carbonated hydroxyapatite (CAP) using calcite and different orthophosphates was investigated in a closed batch reactor. Only orthophosphoric acid could lead to the complete decomposition of calcite particles, when the reaction temperature was set at 80 °C. On the other hand, the reaction time and the dilution of the initial calcite suspension had no significant influence on the formation of the solid products. CAP was formed as the main crystalline calcium phosphate with the carbonate content in the range of 4.2–4.6 wt.%. The thermal decarbonation of the synthesized CAP started at 750 °C but it was only significant at 1000 °C under air atmosphere. This thermal decarbonation was total at 1200 °C or above. All CAP samples and products following thermal treatments were found bioactive in the test using simulated body fluid (SBF) solution.

  9. Hydrothermal Conditions and the Origin of Cellular Life.

    PubMed

    Deamer, David W; Georgiou, Christos D

    2015-12-01

    The conditions and properties of hydrothermal vents and hydrothermal fields are compared in terms of their ability to support processes related to the origin of life. The two sites can be considered as alternative hypotheses, and from this comparison we propose a series of experimental tests to distinguish between them, focusing on those that involve concentration of solutes, self-assembly of membranous compartments, and synthesis of polymers. Key Word: Hydrothermal systems.

  10. Controlled synthesis of La{sub 1−x}Sr{sub x}CrO{sub 3} nanoparticles by hydrothermal method with nonionic surfactant and their ORR activity in alkaline medium

    SciTech Connect

    Choi, Bo Hyun; Park, Shin-Ae; Park, Bong Kyu; Chun, Ho Hwan; Kim, Yong-Tae

    2013-10-15

    Graphical abstract: We demonstrate that Sr-doped LaCrO{sub 3} nanoparticles were successfully prepared by the hydrothermal synthesis method using the nonionic surfactant Triton X-100 and the applicability of La{sub 1−x}Sr{sub x}CrO{sub 3} to oxygen reduction reaction (ORR) electrocatalysis in an alkaline medium. Compared with the nanoparticles synthesized by the coprecipitation method, they showed enhanced ORR activity. - Highlights: • Sr-doped LaCrO{sub 3} nanoparticles were successfully prepared by the hydrothermal method using the nonionic surfactant. • Homogeneously shaped and sized Sr-doped LaCrO{sub 3} nanoparticles were readily obtained. • Compared with the nanoparticles synthesized by the coprecipitation method, they showed an enhanced ORR activity. • The main origin was revealed to be the decreased particle size due to the nonionic surfactant. - Abstract: Sr-doped LaCrO{sub 3} nanoparticles were prepared by the hydrothermal method with the nonionic surfactant Triton X-100 followed by heat treatment at 1000 °C for 10 h. The obtained perovskite nanoparticles had smaller particle size (about 100 nm) and more uniform size distribution than those synthesized by the conventional coprecipitation method. On the other hand, it was identified with the material simulation that the electronic structure change by Sr doping was negligible, because the initially unfilled e{sub g}-band was not affected by the p-type doping. Finally, the perovskite nanoparticles synthesized by hydrothermal method showed much higher ORR activity by over 200% at 0.8 V vs. RHE than those by coprecipitation method.

  11. Hierarchical macro-mesoporous structures in the system TiO{sub 2}-Al{sub 2}O{sub 3}, obtained by hydrothermal synthesis using Tween-20 as a directing agent

    SciTech Connect

    Garcia-Benjume, M.L.; Espitia-Cabrera, M.I.; Contreras-Garcia, M.E.

    2009-12-15

    Macro-mesoporous powders of titania, alumina, and mixed titania-20%alumina systems were obtained by hydrothermal synthesis employing surfactant Tween-20 as structural directing agent in order to promote the textural properties of titania. The effect of the alumina in the titania phase and on textural properties was analyzed. The obtained powders presented a macroporous channel structure that was characterized by X-ray diffractometry, scanning and transmission electron microscopy, N{sub 2} adsorption-desorption analysis, pore size distribution, Fourier transform infrared spectrometry, and thermogravimetric analysis. It was found that alumina content retarded the anatase phase crystallization and increased the Brunauer-Emmet-Teller surface area from 136 to 210 m{sup 2}/g. The powders calcined at 400 deg. C are thermally stable and possess an interconnected macro-mesoporous hierarchical structure; the results indicate that this synthesis can be employed to prepare mixed titania-alumina with good textural properties.

  12. Preparation of highly photocatalytic active CdS/TiO{sub 2} nanocomposites by combining chemical bath deposition and microwave-assisted hydrothermal synthesis

    SciTech Connect

    Li, Li; Wang, Lili; Hu, Tianyu; Zhang, Wenzhi; Zhang, Xiuli; Chen, Xi

    2014-10-15

    CdS/TiO{sub 2} nanocomposites were prepared from Cd and Ti (1:1 M ratio) using cetyltrimethylammonium bromide by a two-step chemical bath deposition (CBD) and microwave-assisted hydrothermal synthesis (MAHS) method. A series of nanocomposites with different morphologies and activities were prepared by varying the reaction time in the MAHS (2, 4, and 6 h). The crystal structure, morphology, and surface physicochemical properties of the nanocomposites were characterized by X-ray diffraction, UV–visible diffuse reflectance spectroscopy, X-ray photoelectron spectroscopy, scanning electron microscopy, and N{sub 2} adsorption–desorption measurements. The results show that the CdS/TiO{sub 2} nanocomposites were composed of anatase TiO{sub 2} and hexagonal CdS phases with strong absorption in the visible region. The surface morphologies changed slightly with increasing microwave irradiation time, while the Brunauer–Emmett–Teller surface area increased remarkably. The photocatalytic degradation of methyl orange (MO) was investigated under UV light and simulated sunlight irradiation. The photocatalytic activity of the CdS/TiO{sub 2} (6 h) composites prepared by the MAHS method was higher than those of CdS, P25, and other CdS/TiO{sub 2} nanocomposites. The CdS/TiO{sub 2} (6 h) nanocomposites significantly affected the UV and microwave-assisted photocatalytic degradation of different dyes. To elucidate the photocatalytic reaction mechanism for the CdS/TiO{sub 2} nanocomposites, controlled experiments were performed by adding different radical scavengers. - Graphical abstract: CdS/TiO{sub 2} nanocomposites were prepared using CTAB by CBD combined with MAHS method. In addition, with increasing microwave irradiation time, the morphology of CdS/TiO{sub 2} changed from popcorn-like to wedge-like structure. - Highlights: • The CdS/TiO{sub 2} was prepared by CBD combined with MAHS two-step method under CTAB. • The morphologies of as-samples were different with the time of

  13. Hydrothermal synthesis of potassium molybdenum oxide bronzes: structure-inheriting solid-state route to blue bronze and dissolution/deposition route to red bronze

    SciTech Connect

    Eda, Kazuo . E-mail: eda@kobe-u.ac.jp; Chin, Kin; Sotani, Noriyuki; Stanley Whittingham, M.

    2005-01-15

    The hydrothermal syntheses of the alkali metal molybdenum bronzes from starting solids (H{sub x}MoO{sub 3}) with structural affinities to the desired products were investigated. Single-phase potassium blue and red bronzes were prepared by the hydrothermal treatments at around 430K, and characterized by powder X-ray diffraction, IR spectroscopy, and SEM. The formation processes of these two bronzes during the hydrothermal treatments were found to differ. The blue bronze was formed by a structure-inheriting solid-state route from H{sub x}MoO{sub 3} with x<0.3, whereas the red bronze was formed for x>0.3 through a solution dissolution/deposition route via the formation of MoO{sub 3}+MoO{sub 2}.

  14. Ultrasonic waves induce rapid zeolite synthesis in a seawater solution.

    PubMed

    Belviso, Claudia; Cavalcante, Francesco; Fiore, Saverio

    2013-01-01

    The synthesis of zeolites from fly ash was performed through a low-temperature hydrothermal process with seawater. Compared with the results obtained using the same hydrothermal method but in the absence of sonication, the application of an ultrasonic pre-treatment to the conventional hydrothermal process with seawater reduces the crystallization temperature below that observed when hydrothermal synthesis is performed using distilled water.

  15. Synthesis of lead-free piezoelectric powders by ultrasonic-assisted hydrothermal method and properties of sintered (K0.48Na0.52)NBO3 ceramics.

    PubMed

    Isobe, Gaku; Maeda, Takafumi; Bornmann, Peter; Hemsel, Tobias; Morita, Takeshi

    2014-02-01

    (K,Na)NbO3 ceramics have attracted much attention as lead-free piezoelectric materials with high piezoelectric properties. High-quality (K,Na)NbO3 ceramics can be sintered using KNbO3 and NaNbO3 powders synthesized by a hydrothermal method. In this study, to enhance the quality factor of the ceramics, high-power ultrasonic irradiation was employed during the hydrothermal method, which led to a reduction in the particle size of the resultant powders.

  16. Chemical environments of submarine hydrothermal systems. [supporting abiogenetic theory

    NASA Technical Reports Server (NTRS)

    Shock, Everett L.

    1992-01-01

    The paper synthesizes diverse information about the inorganic geochemistry of submarine hydrothermal systems, provides a description of the fundamental physical and chemical properties of these systems, and examines the implications of high-temperature, fluid-driven processes for organic synthesis. Emphasis is on a few general features, i.e., pressure, temperature, oxidation states, fluid composition, and mineral alteration, because these features will control whether organic synthesis can occur in hydrothermal systems.

  17. Hydrothermal systems and the emergence of life

    NASA Technical Reports Server (NTRS)

    Shock, E. L.

    1994-01-01

    The author reviews current thought about life originating in hyperthermophilic microorganisms. Hyperthermophiles obtain food from chemosynthesis of sulfur and have an RNA nucleotide sequence different from bacteria and eucarya. It is postulated that a hyperthermophile may be the common ancestor of all life. Current research efforts focus on the synthesis of organic compounds in hydrothermal systems.

  18. In situ synthesis and hydrothermal crystallization of nanoanatase TiO2 -SiO2 coating on aramid fabric (HTiSiAF) for UV protection.

    PubMed

    Deng, Hui; Zhang, Hongda

    2015-10-01

    TiO2 -SiO2 thin film was prepared by sol-gel method and coated on the aramid fabric to prepare functional textiles. The aramid fabric was dipped and withdrawn in TiO2 -SiO2 gel and hydrothermal crystallization at 80(°) C, then its UV protection functionality was evaluated. The crystalline phase and the surface morphology of TiO2 -SiO2 thin film were characterized using SEM, XRD, and AFM respectively. SEM showed hydrothermal crystallization led to a homogeneous dispersion of anatase nonocrystal in TiO2 -SiO2 film, and XRD suggested the mean particle size of the formed anatase TiO2 was less than 30 nm. AFM indicated that hydrothermal treatment enhanced the crystallization of TiO2 . UV protection analysis suggested that the hydrothermally treated coated textile had a better screening property in comparison with TiO2 -SiO2 gel and native aramid fabric.

  19. Chemical environments of submarine hydrothermal systems

    NASA Technical Reports Server (NTRS)

    Shock, Everett L.

    1992-01-01

    Perhaps because black-smoker chimneys make tremendous subjects for magazine covers, the proposal that submarine hydrothermal systems were involved in the origin of life has caused many investigators to focus on the eye-catching hydrothermal vents. In much the same way that tourists rush to watch the spectacular eruptions of Old Faithful geyser with little regard for the hydrology of the Yellowstone basin, attention is focused on the spectacular, high-temperature hydrothermal vents to the near exclusion of the enormous underlying hydrothermal systems. Nevertheless, the magnitude and complexity of geologic structures, heat flow, and hydrologic parameters which characterize the geyser basins at Yellowstone also characterize submarine hydrothermal systems. However, in the submarine systems the scale can be considerably more vast. Like Old Faithful, submarine hydrothermal vents have a spectacular quality, but they are only one fascinating aspect of enormous geologic systems operating at seafloor spreading centers throughout all of the ocean basins. A critical study of the possible role of hydrothermal processes in the origin of life should include the full spectrum of probable environments. The goals of this chapter are to synthesize diverse information about the inorganic geochemistry of submarine hydrothermal systems, assemble a description of the fundamental physical and chemical attributes of these systems, and consider the implications of high-temperature, fluid-driven processes for organic synthesis. Information about submarine hydrothermal systems comes from many directions. Measurements made directly on venting fluids provide useful, but remarkably limited, clues about processes operating at depth. The oceanic crust has been drilled to approximately 2.0 km depth providing many other pieces of information, but drilling technology has not allowed the bore holes and core samples to reach the maximum depths to which aqueous fluids circulate in oceanic crust. Such

  20. Controllable hydrothermal synthesis of rutile TiO{sub 2} hollow nanorod arrays on TiCl{sub 4} pretreated Ti foil for DSSC application

    SciTech Connect

    Xi, Min; Zhang, Yulan; Long, Lizhen; Li, Xinjun

    2014-11-15

    Rutile TiO{sub 2} nanorod arrays (TNRs) were achieved by hydrothermal process on TiCl{sub 4} pretreated Ti foil. Subsequently, TNRs were hydrothermally etched in HCl solution to form hollow TiO{sub 2} nanorod arrays (H-TNRs). The TiCl{sub 4} pretreatment plays key roles in enhancement of Ti foil corrosion resistance ability and crystal nucleation introduction for TNRs growth. TNRs with desired morphology can be obtained by controlling TiCl{sub 4} concentration and the amount of tetrabutyl titanate (TTB) accordingly. TNRs with the length of ∼1.5 μm and diameter of ∼200 nm, obtained on 0.15 M TiCl{sub 4} pretreated Ti foil with 0.6 mL TTB, exhibits relatively higher photocurrent. The increased pore volume of the H-TNRs has contributed to the increased surface area which is benefit for Dye-Sensitized Solar Cells (DSSC) application. And the 180 °C-H-TNRs photoanode obtained from the 0.15-TiCl{sub 4}-TNRs sample demonstrated 128.9% enhancement of photoelectric efficiency of DSSC compared to that of the original TNR photoanode. - Graphical abstract: Rutile hollow TiO{sub 2} nanorod array photoanode obtained from original TiO{sub 2} nanorod array photoanode by hydrothermal etching demonstrates enhanced photoelectric efficiency of DSSC. - Highlights: • TiO{sub 2} nanorods are prepared via hydrothermal process on TiCl{sub 4}-pretreated Ti foil. • Hollow TiO{sub 2} nanorods are obtained by hydrothermal etching of TiO{sub 2} nanorods. • TiCl{sub 4} pretreatment plays a key role in protecting Ti foil from chemical corrosion. • Hollow TiO{sub 2} nanorods photoanode shows enhanced photoelectric efficiency for DSSC.

  1. Synthesis of ZnO nanorod–nanosheet composite via facile hydrothermal method and their photocatalytic activities under visible-light irradiation

    SciTech Connect

    Tan, Wai Kian; Abdul Razak, Khairunisak; Lockman, Zainovia; Kawamura, Go; Muto, Hiroyuki; Matsuda, Atsunori

    2014-03-15

    ZnO composite films consisting of ZnO nanorods and nanosheets were prepared by low-temperature hydrothermal processing at 80 °C on seeded glass substrates. The seed layer was coated on glass substrates by sol–gel dip-coating and pre-heated at 300 °C for 10 min prior to hydrothermal growth. The size of the grain formed after pre-heat treatment was ∼40 nm. A preferred orientation seed layer at the c-axis was obtained, which promoted vertical growth of the ZnO nanorod arrays and formation of the ZnO nanosheets. X-ray diffraction patterns and high-resolution transmission electron microscope (HR-TEM) images confirmed that the ZnO nanorods and nanosheets consist of single crystalline and polycrystalline structures, respectively. Room temperature photoluminescence spectra of the ZnO nanorod–nanosheet composite films exhibited band-edge ultraviolet (UV) and visible emission (blue and green) indicating the formation of ZnO crystals with good crystallinity and are supported by Raman scattering results. The formation of one-dimensional (1D) ZnO nanorod arrays and two-dimensional (2D) ZnO nanosheet films using seeded substrates in a single low-temperature hydrothermal step would be beneficial for realization of device applications that utilize substrates with limited temperature stability. The ZnO nanorods and nanosheets composite structure demonstrated higher photocatalytic activity during degradation of aqueous methylene blue under visible-light irradiation. -- Graphical abstract: Schematic illustration of ZnO nanorod–nanosheet composite structure formation by hydrothermal at low-temperature of 80 °C against time. Highlights: • Novel simultaneous formation of ZnO nanorods and nanosheets composite structure. • Facile single hydrothermal step formation at low-temperature. • Photoluminescence showed ultraviolet and visible emission. • Feasible application on substrates with low temperature stability. • Improved photocatalytic activity under visible

  2. Hydrothermal synthesis and characterization of the first mixed alkali borate-nitrate K{sub 3}Na[B{sub 6}O{sub 9}(OH){sub 3}]NO{sub 3}

    SciTech Connect

    Ortner, Teresa S.; Wurst, Klaus; Perfler, Lukas; Tribus, Martina; Huppertz, Hubert

    2015-01-15

    The first mixed alkali borate-nitrate K{sub 3}Na[B{sub 6}O{sub 9}(OH){sub 3}]NO{sub 3} was synthesized under hydrothermal conditions from Na{sub 2}B{sub 4}O{sub 7}·10H{sub 2}O and K{sub 2}B{sub 4}O{sub 7}·4H{sub 2}O using KNO{sub 3} as a nitrate source. The compound crystallizes in the space group Pnnm (no. 58) with the lattice parameters a=1320.8(3), b=910.7(2), and c=1232.5(3) pm (Z=4). Isolated Sechserrings formed by BO{sub 4} and BO{sub 3} groups are linked through hydrogen bridges to form a three-dimensional network. - Graphical abstract: The first mixed alkali borate-nitrate K{sub 3}Na[B{sub 6}O{sub 9}(OH){sub 3}]NO{sub 3} was synthesized under hydrothermal conditions from Na{sub 2}B{sub 4}O{sub 7}·10H{sub 2}O and K{sub 2}B{sub 4}O{sub 7}·4H{sub 2}O using KNO{sub 3} as a nitrate source. - Highlights: • The first mixed alkali borate-nitrate K{sub 3}Na[B{sub 6}O{sub 9}(OH){sub 3}]NO{sub 3} is reported. • Hydrothermal conditions (240 °C, 3d) were used for the synthesis of K{sub 3}Na[B{sub 6}O{sub 9}(OH){sub 3}]NO{sub 3}. • Borate Sechserrings are interconnected through hydrogen-bonding.

  3. Size-controlled synthesis of NiFe2O4 nanospheres via a PEG assisted hydrothermal route and their catalytic properties in oxidation of alcohols by periodic acid

    NASA Astrophysics Data System (ADS)

    Paul, Bappi; Purkayastha, Debraj Dhar; Dhar, Siddhartha Sankar

    2016-05-01

    A novel and facile approach for synthesis of spinel nickel ferrites (NiFe2O4) nanoparticles (NPs) employing homogeneous chemical precipitation followed by hydrothermal heating is reported. The synthesis involves use of tributylamine (TBA) as a hydroxylating agent in synthesis of nickel ferrites. Polyethylene glycol (PEG) 4000 was used as surfactant. As-synthesized NiFe2O4 NPs were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), N2 adsorption-desorption isotherm (BET) and vibrating sample magnetometry (VSM). The XRD pattern revealed formation of cubic face-centered NiFe2O4 and TEM image showed spherical particles of sizes 2-10 nm. These NiFe2O4 NPs were used as magnetically recoverable catalyst in oxidation of cyclic alcohols to their corresponding aldehydes by periodic acid. This eco-friendly procedure affords products in very high yield and selectivity. The reusability of the catalyst is proved to be noteworthy as the material exhibits no significant changes in its catalytic activity even after five cycles of reuse.

  4. Hydrothermal synthesis of CuO micro-/nanostructures and their applications in the oxidative degradation of methylene blue and non-enzymatic sensing of glucose/H2O2.

    PubMed

    Prathap, M U Anu; Kaur, Balwinder; Srivastava, Rajendra

    2012-03-15

    In this paper, we report on the amino acids-/citric acid-/tartaric acid-assisted morphologically controlled hydrothermal synthesis of micro-/nanostructured crystalline copper oxides (CuO). These oxides were characterized by means of X-ray diffraction, nitrogen sorption, scanning electron microscopy, Fourier transform infrared, and UV-visible spectroscopy. The surface area of metal oxides depends on the amino acid used in the synthesis. The formation mechanisms were proposed based on the experimental results, which show that amino acid/citric acid/tartaric acid and hydrothermal time play an important role in tuning the morphology and structure of CuO. The catalytic activity of as-synthesized CuO was demonstrated by catalytic oxidation of methylene blue in the presence of hydrogen peroxide (H(2)O(2)). CuO synthesized using tyrosine was found to be the best catalyst compared to a variety of CuO synthesized in this study. CuO (synthesized in this study)-modified electrodes were used for the construction of non-enzymatic sensors, which displayed excellent electrocatalytic response for the detection of H(2)O(2) and glucose compared to conventional CuO. The high electrocatalytic response observed for the CuO synthesized using tyrosine can be correlated with the large surface area, which enhances the accessibility of H(2)O(2)/glucose molecule to the active site that results in high observed current. The methodology adopted in the present study provides a new platform for the fabrication of CuO-based high-performance glucose and other biosensors.

  5. Elucidating some issues regarding the synthesis of superparamagnetic-like single crystalline micrometric Fe3O4 during the hydrothermal process

    NASA Astrophysics Data System (ADS)

    Kiss, Mihaela Luminita; Chirita, Marius; Mihaila, Alexandru Ionut Chirita; Beljung, Corina Ana; Niznansky, Daniel; Savii, Cecilia

    2015-12-01

    By hydrothermal decomposition of the Fe-EDTA complex, at 230°C, after 38 h of high -pressure treatment time, magnetite octahedrons with micrometric dimensions (15-45 µm) were obtained. Unusual and notable for these crystallites is the very small hysteresis surface, indicating a superparamagnetic-like behavior at micrometer scale, which means that the agglomeration of these crystallites is avoided after the removal of the magnetic field. This behavior can be correlated with a low level of imperfections in magnetite octahedrons, involving a low level of internal stresses, which leads to coercivity decreasing. The large dispersion in the crystallite axes is consistent with low remanence. We assumed that these attributes are related to the hydrothermal crystal growth process. To elucidate some issues regarding the magnetite crystallites development during the hydrothermal process, a careful observation of occurring intermediate phases by optical and SEM microscopy has been performed. Also the purity of the ferrous carbonate/magnetite mixture was analyzed by FTIR and Mössbauer spectroscopy

  6. Surfactant-assisted hydrothermal synthesis of Eu(3+)-doped white light hydroxyl sodium yttrium tungstate microspheres and their conversion to NaY(WO(4))(2).

    PubMed

    Lei, Fang; Yan, Bing; Chen, Hao Hong; Zhao, Jing Tai

    2009-08-17

    In this work, large-scale three-dimensional "flake-ball" microarchitectures of Eu(3+) doped white light hydroxyl sodium yttrium tungstate were prepared by the well-known hydrothermal approach at 180 degrees C for 48 h in the presence of triblock-copolymer poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol) (P123). NaY(WO(4))(2):Eu(3+) phosphor was formed by annealing the hydrothermal product at approximately 630 degrees C for 2 h. A time-dependent microstructure evolution study was performed under hydrothermal reaction. The evolution process is the self-assembly process of P123, and the effects of other reaction parameters, such as influence of the concentration of P123 on morphology, and the influence of temperature on PL. The mechanism by which the "flake-ball" particles are formed is discussed in detail. The PL spectra of Eu(3+)-doped hydroxyl sodium yttrium tungstate phosphor contain two parts: the broad blue-green band and the (5)D(0)-->(7)F(J) (J = 1, and 2) characteristic transition of Eu(3+). This approach provides a facile route for the production of high-quality hydroxyl sodium yttrium tungstate microstructures with an interesting optical property.

  7. Template-free synthesis of ZnWO{sub 4} powders via hydrothermal process in a wide pH range

    SciTech Connect

    Hojamberdiev, Mirabbos; Zhu, Gangqiang; Xu, Yunhua

    2010-12-15

    ZnWO{sub 4} powders with different morphologies were fabricated through a template-free hydrothermal method at 180 {sup o}C for 8 h in a wide pH range. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-visible and luminescence spectrophotometers were applied to study the effects of pH values on crystallinity, morphology, optical and luminescence properties. The XRD results showed that the WO{sub 3} + ZnWO{sub 4}, ZnWO{sub 4}, and ZnO phases could form after hydrothermal processing at 180 {sup o}C for 8 h with the pH values of 1, 3-11, and 13, respectively. The SEM and TEM observation revealed that the morphological transformation of ZnWO{sub 4} powders occurred with an increase in pH values as follows: star anise-, peony-, and desert rose-like microstructures and soya bean- and rod-like nanostructures. The highest luminescence intensity was found to be in sample consisting of star anise-like crystallites among all the samples due to the presence of larger particles with high crystallinity resulted from the favorable pH under the current hydrothermal conditions.

  8. Hydrothermal systems as environments for the emergence of life.

    PubMed

    Shock, E L

    1996-01-01

    Analysis of the chemical disequilibrium provided by the mixing of hydrothermal fluids and seawater in present-day systems indicates that organic synthesis from CO2 or carbonic acid is thermodynamically favoured in the conditions in which hyperthermophilic microorganisms are known to live. These organisms lower the Gibbs free energy of the chemical mixture by synthesizing many of the components of their cells. Primary productivity is enormous in hydrothermal systems because it depends only on catalysis of thermodynamically favourable, exergonic reactions. It follows that hydrothermal systems may be the most favourable environments for life on Earth. This fact makes hydrothermal systems logical candidates for the location of the emergence of life, a speculation that is supported by genetic evidence that modern hyperthermophilic organisms are closer to a common ancestor than any other forms of life. The presence of hydrothermal systems on the early Earth would correspond to the presence of liquid water. Evidence that hydrothermal systems existed early in the history of Mars raises the possibility that life may have emerged on Mars as well. Redox reactions between water and rock establish the potential for organic synthesis in and around hydrothermal systems. Therefore, the single most important parameter for modelling the geochemical emergence of life on the early Earth or Mars is the composition of the rock which hosts the hydrothermal system.

  9. Hydrothermal systems as environments for the emergence of life

    NASA Technical Reports Server (NTRS)

    Shock, E. L.

    1996-01-01

    Analysis of the chemical disequilibrium provided by the mixing of hydrothermal fluids and seawater in present-day systems indicates that organic synthesis from CO2 or carbonic acid is thermodynamically favoured in the conditions in which hyperthermophilic microorganisms are known to live. These organisms lower the Gibbs free energy of the chemical mixture by synthesizing many of the components of their cells. Primary productivity is enormous in hydrothermal systems because it depends only on catalysis of thermodynamically favourable, exergonic reactions. It follows that hydrothermal systems may be the most favourable environments for life on Earth. This fact makes hydrothermal systems logical candidates for the location of the emergence of life, a speculation that is supported by genetic evidence that modern hyperthermophilic organisms are closer to a common ancestor than any other forms of life. The presence of hydrothermal systems on the early Earth would correspond to the presence of liquid water. Evidence that hydrothermal systems existed early in the history of Mars raises the possibility that life may have emerged on Mars as well. Redox reactions between water and rock establish the potential for organic synthesis in and around hydrothermal systems. Therefore, the single most important parameter for modelling the geochemical emergence of life on the early Earth or Mars is the composition of the rock which hosts the hydrothermal system.

  10. METEORIC-HYDROTHERMAL SYSTEMS.

    USGS Publications Warehouse

    Criss, Robert E.; Taylor, Hugh P.

    1986-01-01

    This paper summarizes the salient characteristics of meteoric-hydrothermal systems, emphasing the isotopic systematics. Discussions of permeable-medium fluid dynamics and the geology and geochemistry of modern geothermal systems are also provided, because they are essential to any understanding of hydrothermal circulation. The main focus of the paper is on regions of ancient meteoric-hydrothermal activity, which give us information about the presently inaccessible, deep-level parts of modern geothermal systems. It is shown oxygen and hydrogen isotopes provide a powerful method to discover and map fossil hydrothermal systems and to investigate diverse associated aspects of rock alteration and ore deposition.

  11. Hierarchical Na-doped cubic ZrO{sub 2} synthesis by a simple hydrothermal route and its application in biodiesel production

    SciTech Connect

    Lara-García, Hugo A.; Romero-Ibarra, Issis C.; Pfeiffer, Heriberto

    2014-10-15

    Hierarchical growth of cubic ZrO{sub 2} phase was successfully synthesized via a simple hydrothermal process in the presence of different surfactants (cationic, non-ionic and anionic) and sodium hydroxide. The structural and microstructural characterizations of different ZrO{sub 2} powders were performed using various techniques, such as X-ray diffraction, transmission electron microscopy, N{sub 2} adsorption–desorption, scanning electron microscopy and infrared. Results indicated that sodium addition stabilized the cubic ZrO{sub 2} phase by a Na-doping process, independently of the surfactant used. In contrast, microstructural characteristics varied as a function of the surfactant and sodium presence. In addition, water vapor (H{sub 2}O) and carbon dioxide (CO{sub 2}) sorption properties were evaluated on ZrO{sub 2} samples. Results evidenced that sample surface reactivity changed as a function of the sodium content. Finally, this surface reactivity was evaluated on the biodiesel transesterification reaction using the different synthesized samples, obtaining yields of 93%. - Graphical abstract: Hierarchical growth of cubic Na-ZrO{sub 2} phase was synthesized by hydrothermal processes in the presence of surfactants and sodium. Sodium addition stabilized the cubic phase by a Na-doping process, while the microstructural characteristics varied with surfactants. Finally, this surface reactivity was evaluated on the biodiesel transesterification reaction. - Highlights: • Cubic-ZrO{sub 2} phase was synthesized via a simple hydrothermal process. • ZrO{sub 2} structure and microstructures changed as a function of the surfactant. • Cubic-ZrO{sub 2} phase was evaluated on the biodiesel transesterification reaction.

  12. A facile one-pot hydrothermal synthesis of β-MnO{sub 2} nanopincers and their catalytic degradation of methylene blue

    SciTech Connect

    Cheng, Gao; Yu, Lin Lin, Ting; Yang, Runnong; Sun, Ming; Lan, Bang; Yang, Lili; Deng, Fangze

    2014-09-15

    Branched β-MnO{sub 2} bipods with novel nanopincer morphology were prepared by a facile one-pot hydrothermal method via a redox reaction between NaClO{sub 3} and MnSO{sub 4} in sulfuric acid solution without using any surfactants or templates. The products were characterized in detail by various techniques including X-ray powder diffraction, Raman spectroscopy, X-ray photoelectron spectroscopy, surface area analyzer, field emission scanning electron microscopy and transmission electron microscopy. Results show that the obtained β-MnO{sub 2} nanopincers consist of two sharp nanorods with a diameter of 100–200 nm and a length of 1–2 μm. The concentration of H{sub 2}SO{sub 4} solution plays an important role in controlling the crystal phase and morphology of the final product. A possible formation mechanism for the β-MnO{sub 2} nanopincers was proposed. Moreover, these β-MnO{sub 2} nanostructures exhibited better catalytic performance than the commercial MnO{sub 2} particles to decompose methyl blue (MB) in the presence of H{sub 2}O{sub 2}. - Graphical abstract: Branched β-MnO{sub 2} bipods with novel nanopincer morphology were prepared by a facile one-pot hydrothermal method through oxidizing MnSO{sub 4} with NaClO{sub 3} in H2SO{sub 4} condition without using any surfactants or templates. - Highlights: {sup •} Branched β-MnO{sub 2} nanopincers were prepared by a facile one-pot hydrothermal method. {sup •} Morphology and crystal phase of MnO{sub 2} were controlled by the H{sub 2}SO{sub 4} concentration. {sup •} A possible formation mechanism for the obtained β-MnO{sub 2} nanopincers was proposed. {sup •} The products showed great catalytic performance in degradation of methylene blue.

  13. Controllable synthesis, shape evolution, and luminescence properties of uniform and well-dispersed NaEuF{sub 4} microcrystals through hydrothermal route

    SciTech Connect

    Xu, Zhenhe Zhao, Qian; Ding, Fu; Sun, Yaguang

    2013-08-01

    Graphical abstract: Sodium europium fluorides NaEuF{sub 4} microcrystals have been prepared via a facile hydrothermal route. The possible growth mechanism and the luminescent properties of the as-prepared microcrystals have been discussed. - Highlights: • Sodium europium fluorides NaEuF{sub 4} microspheres were prepared by a facile hydrothermal route. • The as-prepared samples NaEuF{sub 4} and EuF{sub 3} exhibit respective red or orange-red emissions. • These finding may find potential applications in the fields of color display, UV laser and biomedicine. - Abstract: Sodium europium fluorides NaEuF{sub 4} microcrystals with uniform and well-dispersed shapes and dimensions have been prepared via a facile hydrothermal route using Na{sub 3}Cit as the chelating ligand and shape modifier. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected-area electron diffraction (SAED), energy-dispersive X-ray (EDX) and photoluminescence spectra (PL) were taken to characterize the samples. A series of controlled experiments reveal that the trisodium citrate (Na{sub 3}Cit) content, pH value of the initial solution, and reaction time have an indispensable role on the phase, size, and morphology of the as-prepared microcrystals. Based on the experimental results, the possible growth mechanism of the microcrystals prepared under different conditions was proposed. Moreover, we systematically investigated the luminescent properties of the as-prepared microcrystals with different morphologies obtained under different amounts of Na{sub 3}Cit, which have potential application in the fields of color display, UV laser and biomedicine.

  14. Synthesis and in-depth analysis of highly ordered yttrium doped hydroxyapatite nanorods prepared by hydrothermal method and its mechanical analysis

    SciTech Connect

    Nathanael, A. Joseph; Mangalaraj, D.; Hong, S.I.; Masuda, Y.

    2011-12-15

    In this study, undoped and yttrium (Y) doped nanocrystalline hydroxyapatite crystals were synthesized by the hydrothermal method at 180 Degree-Sign C for 24 h. Highly ordered and oriented hydroxyapatite (HAp) nanorods were prepared by yttrium doping and their nanostructure and physical properties were compared with those of undoped HAp rods. FESEM images showed that the doping with Y ions reduced the diameter (from 25 nm to 15 nm) and increased the length (from 95 nm to 115 nm) of the synthesized rods. The aspect ratio of the undoped and Y-doped nanorods were calculated to be 4.303 (SD = 0.0959) and 7.61 (SD = 0.0355), respectively. Specific surface area (SSA) analysis showed that SSA also increased from 66.74 m{sup 2}/g to 68.57 m{sup 2}/g with the addition of yttrium. Y-doped HAp nanorod reinforced HMWPE composites displayed the better mechanical performance than those reinforced with pure HAp nanorods. The possible strengthening of nanorods and the increase of SSA due to the reduction in the size of nanorods in the presence of yttrium may have contributed to the strengthening of Y-doped HAp/HMWPE composites. - Graphical Abstract: Highly ordered and oriented yttrium doped hydroxyapatite (HAp) nanorods were prepared by hydrothermal method. For undoped HAp the average length of the nanorod is 95 nm with mean diameter of 24 nm and for a Y doped nanorod the average length is {approx} 115 nm and the mean diameter is 15 nm. Mechanical analysis was carried out by polymer/nanoparticle composite method. Highlights: Black-Right-Pointing-Pointer Yttrium doped hydroxyapatite nanorods were prepared by hydrothermal method. Black-Right-Pointing-Pointer The nanorods have highly uniform size distribution. Black-Right-Pointing-Pointer Yttrium substitution and nanostructure formation was confirmed by careful analysis. Black-Right-Pointing-Pointer Mechanical strength was analyzed by polymer nanoparticle reinforcement method.

  15. Synthesis of flower-like Al doped ZnO microstructures by hydrothermal process and analysis of their gas sensing properties

    NASA Astrophysics Data System (ADS)

    Li, Zan; Qin, Wei; Zhao, Wenjie; Wu, Xiaohong

    2014-04-01

    Al-doped ZnO (AZO) powders with flower-like microstructures were successfully synthesized through a simple and efficient hydrothermal approach, and were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy diffraction spectrum (EDS). All the samples presented high crystallinity with a hexagonal wurtzite structure. The heater gas sensors based on AZO were fabricated and investigation of gas sensing properties was conducted. The sensors showed high response values and reproducible response-recovery for 50-1800 ppm ethanol at 332°C, comparing with NH3, SO2, CO, and HCHO. The underlying mechanism was discussed.

  16. Hydrothermal synthesis and luminescent properties of SrF2 and SrF2:Ln3+ (Ln = Eu, Ce, Tb) nano-assembly with controllable morphology.

    PubMed

    Sun, Yuanping; Jia, Peiyun

    2014-05-01

    SrF2 and SrF2:Ln3+ (Ln = Eu, Ce, Tb) nano-assemblies with controllable size and morphology have been successfully prepared via a facile hydrothermal process. X-ray diffraction, scanning electron microscopy, and photoluminescence spectrum were used to characterize the samples. The experimental results indicate that chelating reagent and acidity play important roles in the formation of micro-crystals with uniform size and peculiar morphology. As-obtained SrF2:Eu3+ and SrF2:Ce3+, SrF2:Tb3+ samples show red, ultraviolet and green emission under the irradiation of ultraviolet.

  17. Hydrothermal Synthesis of Unique Hollow Hexagonal Prismatic Pencils of Co3 V2 O8 ⋅n H2 O: A New Anode Material for Lithium-Ion Batteries.

    PubMed

    Wu, Fangfang; Xiong, Shenglin; Qian, Yitai; Yu, Shu-Hong

    2015-09-07

    Hollow structures of transition-metal oxides, particularly mixed-metal oxides, could be promising for various applications such as lithium-ion batteries (LIBs). Compared to the synthesis of metal oxide hollow spheres by the template method, non-spherical metal oxide hollow hexagonal polyhedra have not been developed to date. Herein, we report the controlled hydrothermal synthesis of a new phase of Co3 V2 O8 ⋅n H2 O hollow hexagonal prismatic pencils (HHPPs), which is composed of uniform structural units. By varying the amount of NaOH in the presence of NH4 (+) and without any template or organic surfactant, the hexagonal prismatic pencils gradually transform from solid into hollow structures, with sizes varying from 5 to 20 μm. The structure of pencils can be preserved only in a limited range of the molar ratio of OH(-) /NH4 (+) . As a new anode material for LIBs, such hollow pencils exhibit impressive lithium storage properties with high capacity, good cycling stability, and superior rate capability.

  18. Morphology-controlled synthesis of Co{sub 3}O{sub 4} by one step template-free hydrothermal method

    SciTech Connect

    Zhou, Keqing; Liu, Jiajia; Wen, Panyue; Hu, Yuan Gui, Zhou

    2015-07-15

    Highlights: • Co{sub 3}O{sub 4} crystals had been synthesized by one step template-free hydrothermal method. • The H{sub 2}O{sub 2} plays a crucial role in morphological control of Co{sub 3}O{sub 4} nanostructures. • The morphology has significant effect on the optical property of Co{sub 3}O{sub 4}. - Abstract: We had developed a facile synthetic route of Co{sub 3}O{sub 4} crystals with different morphologies via one step template-free hydrothermal method. The phase and composition of the Co{sub 3}O{sub 4} were investigated by X-ray powder diffraction and Raman spectrum. The morphology and structure of the synthesized samples were characterized by scanning electron microscopy and transmission electron microscopy. The H{sub 2}O{sub 2} played a crucial role in morphological control of Co{sub 3}O{sub 4} nanostructures. It only obtained Co-based precursor in the absence of H{sub 2}O{sub 2}. On the contrary, the Co{sub 3}O{sub 4} with different morphologies including nanoparticles, nano-discs and well-defined octahedral nanostructures were synthesized in the presence of H{sub 2}O{sub 2}. In addition, the optical property of the obtained Co{sub 3}O{sub 4} samples was investigated by UV–vis spectra.

  19. Synthesis and characterization of K(Ta(x)Nb(1_x))O3 particles by high temperature mixing method under hydrothermal and solvothermal conditions.

    PubMed

    Gu, Honghui; Zhu, Kongjun; Qiu, Jinhao; Ji, Hongli; Cao, Yang; Jin, Jiamei

    2013-02-01

    KTa(x)Nb(1_x)O3 (KTN) particles with an orthorhombic perovskite structure were synthesized via a high temperature mixing method (HTMM) under hydrothermal and solvothermal conditions. The obtained products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and high-resolution transmission electron microcopy (HRTEM). The influences of alkaline concentration and Ta doping amounts on the phase structure and morphology of the obtained powders were investigated. The results showed that KTN powders could be solvothermally prepared when the KOH concentration is as low as 0.5 M. In comparison with the hydrothermal process, supercritical isopropanol plays an important role in synthesizing KTN particles under milder conditions. The KTa(0.4)Nb(0.6)O3 particles solvothermally synthesized in isopropanol are made of well crystallized and single crystalline particles with a size of about 100-200 nm. Room temperature PL studies excited at different wavelengths reveal five emission bands centered at about 421 nm, 446 nm, 468 nm, 488 nm, and 498 nm, respectively. The supercritical process proposed here provides a new potential route for synthesizing other perovskite-type materials.

  20. Facile one-step hydrothermal synthesis toward strongly coupled TiO2/graphene quantum dots photocatalysts for efficient hydrogen evolution

    NASA Astrophysics Data System (ADS)

    Min, Shixiong; Hou, Jianhua; Lei, Yonggang; Ma, Xiaohua; Lu, Gongxuan

    2017-02-01

    The coupling of semiconductor photocatalysts with graphene quantum dots (GQDs) has been proven to be an effective strategy to enhance the photocatalytic and photoelectrical conversion performances of the resulted composites; however, the preparation of semiconductor/GQDs composites usually involves several time-inefficient and tedious post-treatment steps. Herein, we present a facile one-step hydrothermal route for the preparation of GQDs coupled TiO2 (TiO2/GQDs) photocatalysts using 1,3,6-trinitropyrene (TNP) as the sole precursor of GQDs. During the hydrothermal process, TNP molecules undergo an intramolecular fusion to form GQDs, which simultaneously decorate on the surface of TiO2 nanoparticles, leading to a strong surface interaction between the two components. The effective coupling of GQDs on TiO2 can effectively extend the light absorption of the TiO2 to visible region and enhance the charge separation efficiency of TiO2/GQDs composites as a result of GQDs acting as a photosensitizer and an excellent electron acceptor. These key advances make the TiO2/GQDs photocatalyst highly active towards the H2 evolution reaction, resulting in 7 and 3 times higher H2 evolution rate and photocurrent response at optimal GQDs content than TiO2 alone, respectively. This study provides a new methodology for the development of high-performance GQDs modified semiconductor photocatalysts for energy conversion applications.

  1. Hydrothermal synthesis and properties of NiFe2O4@BaTiO3 composites with well-matched interface

    PubMed Central

    Zhou, Jian-Ping; Lv, Li; Liu, Qian; Zhang, Yu-Xiang; Liu, Peng

    2012-01-01

    NiFe2O4@BaTiO3 multiferroic composite particles were produced by a simple hydrothermal method in two steps: preparing NiFe2O4 nanoparticles and then synthesizing core-shell nanocomposites. Multiferroic composite ceramics were sintered from these powders. X-ray diffraction, Raman scattering and energy dispersive x-ray analyses indicated that the core-shell composites with a NiFe2O4 core and BaTiO3 shell were formed in the hydrothermal environment. Different types of sharp interfaces were self-assembled owing to the minimization of direct elastic energy. The saturation magnetization of the composites linearly increased with the NiFe2O4 content while the dielectric constant decreased. A dielectric peak appeared at around 460 °C because of the oxygen vacancies in the BaTiO3 ceramics. It resulted in an enhancement of magnetic permeability in the composites, indicating magnetoelectric coupling that was also observed by direct magnetoelectric measurements. PMID:27877501

  2. Hydrothermal synthesis of urchin-like Co3O4 nanostructures and their electrochemical sensing performance of H2O2

    NASA Astrophysics Data System (ADS)

    Barkaoui, Sami; Haddaoui, Marwa; Dhaouadi, Hassouna; Raouafi, Noureddine; Touati, Fathi

    2015-08-01

    Nanostructured tricobalt tetraoxide, Co3O4, was hydrothermally synthesized starting from cobalt dichloride hexahydrate (CoCl2·6H2O) and urea (H2NCONH2) as precursor and polyethylene glycol-400 (PEG-400) as a structure-directing agent. Uniform urchin-like nanostructures were hydrothermally obtained at 150 °C for 16 h, and the Co3O4 morphology did not collapse after a subsequent calcination at 300 °C for 2 h. XRD measurements indicated that the average sizes of Co3O4 particles prior and after heating at 300 °C are 64 and 44 nm, respectively. This material has been successfully used for the nanostructuration of screen-printed carbon electrodes (SPCEs) which were used for the sensitive electrochemical detection of hydrogen peroxide (H2O2). The sensor is endowed with a large dynamic range (0.1 to 50 μM) and a limit of detection of 0.145 μM. The as obtained results show that the Co3O4 nanomaterial could be a candidate to be used as sensors for the detection of analytes.

  3. Synthesis of BiFeO3 thin films on single-terminated Nb : SrTiO3 (111) substrates by intermittent microwave assisted hydrothermal method

    NASA Astrophysics Data System (ADS)

    Velasco-Davalos, Ivan; Ambriz-Vargas, Fabian; Kolhatkar, Gitanjali; Thomas, Reji; Ruediger, Andreas

    2016-06-01

    We report on a simple and fast procedure to create arrays of atomically flat terraces on single crystal SrTiO3 (111) substrates and the deposition of ferroelectric BiFeO3 thin films on such single-terminated surfaces. A microwave-assisted hydrothermal method in deionized water and ammonia solution selectively removes either (SrO3)4- or Ti4+ layers to ensure the same chemical termination on all terraces. Measured step heights of 0.225 nm (d111) and uniform contrast in the phase image of the terraces confirm the single termination in pure and Nb doped SrTiO3 single crystal substrates. Multiferroic BiFeO3 thin films were then deposited by the same microwave assisted hydrothermal process on Nb : SrTiO3 (111) substrates. Bi(NO3)3 and Fe(NO3)3 along with KOH served as the precursors solution. Ferroelectric behavior of the BiFeO3 films on Nb : SrTiO3 (100) substrates was verified by piezoresponse force microscopy.

  4. Hydrothermal Synthesis of Mn x Co y Ni1- x- y (OH)2 as a Novel Anode Material for the Lithium-Ion Battery

    NASA Astrophysics Data System (ADS)

    Jiang, Qiang; Yin, Shengyu; Feng, Chuanqi; Guo, Zaiping

    2015-08-01

    Three-dimensional (3D) Mn x Co y Ni1- x- y (OH)2 microspheres were synthesized using a simple hydrothermal method. The structure and morphology of the samples were characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results showed that the Mn x Co y Ni1- x- y (OH)2 compound has the same structure as that of Ni(OH)2 and takes on the morphology of microspheres. The electrochemical properties of the Mn x Co y Ni1- x- y (OH)2 compound were also investigated. It exhibited both high reversible capacity and good cycling performance when cycled at room temperature in a 3.0-0.01 V potential window (versus Li+/Li) at current density of 100 mA g-1. The Mn x Co y Ni1- x- y (OH)2 compound retained a discharge capacity of 575 mAh g-1 after 140 cycles, which suggests that the Mn x Co y Ni1- x- y (OH)2 synthesized by the hydrothermal method can be used as an anode material for the lithium-ion battery.

  5. Hydrothermal synthesis and photoluminescence of novel green-emitting phosphor Y{sub 1-x}BO{sub 3}:xTb{sup 3+}

    SciTech Connect

    Wang Yuhua . E-mail: wyh@lzu.edu.cn; Wu Chunfang; Zhang Jiachi

    2006-08-10

    Y{sub 1-x}BO{sub 3}:xTb{sup 3+} phosphors were first synthesized by hydrothermal reaction, and the samples were characterized by X-ray powder diffractometry, infrared absorption, nuclear magnetic resonance, scanning electron microscopy and photoluminescence. The results show that single phase is obtained with Tb concentration up to 0.28 and all the samples exhibit flake-like morphology. The sample was determined to be vaterite-type orthoborate and the boron is both four-coordinated (chief) and three-coordinated (few). The Y{sub 1-x}BO{sub 3}:xTb{sup 3+} phosphors showed intense green emission at 550 nm and the intensity of the emission increases with Tb{sup 3+} substitution up to 0.22 and then decreases for higher Tb{sup 3+} content. In the phosphors prepared by the hydrothermal method the concentration quenching is higher than in the phosphors prepared by solid-state reaction; the intensity of emission is stronger in the former than that of the latter. Y{sub 1-x}BO{sub 3}:xTb3{sup +} is a promising phosphor for plasma display panels and hydrargyrum-free lamps.

  6. ZnS/Ni{sub 2}P core/shell composites: Simple hydrothermal synthesis, characterization and its photocatalytic degradation of pyronine B

    SciTech Connect

    Liu, Shuling; Ma, Lanbing; Zhang, Hongzhe; Ma, Chenlu

    2016-05-15

    Highlights: • ZnS/Ni{sub 2}P composites have been firstly synthesized via a gentle hydrothermal route. • The composites have been characterized by XRD, SEM and TEM. • ZnS/Ni{sub 2}P showed enhanced photocatalytic degradation activity for pyronine B. • The reason for the enhanced photocatalytic activity has been discussed. - Abstract: ZnS/Ni{sub 2}P core/shell composites were successfully synthesized using a hydrothermal method. The composites have been characterized by XRD, SEM, TEM and the corresponding results showed that the composites were composed of the cubic ZnS microspheres, which were made up of ZnS nanoparticles, and Ni{sub 2}P nanoparticles coated on the surfaces of ZnS microspheres. Compared with ZnS microspheres, ZnS/Ni{sub 2}P core/shell composites showed enhanced photocatalytic degradation activity for pyronine B under UV irradiation. This may be related to the effective separation of photogenerated electron–hole pairs in ZnS/Ni{sub 2}P composites which can greatly reduce the chance of their recombination. Furthermore, superoxide ions and hydroxyl radical can be more easily produced through ZnS/Ni{sub 2}P composites, which is also beneficial for the degradation of pyronine B.

  7. Preparation and characterization of LaMnO3 and LaNiO3 perovskite type oxides by the hydrothermal synthesis method

    NASA Astrophysics Data System (ADS)

    Özbay, N.; Şahin, R. Z. Yarbay

    2017-02-01

    Perovskites which both naturally occurring and synthetically produced with important technological applications are a large class of minerals. Physical properties of interest to materials science through perovskites include superconductivity, magnetoresistance, ionic conductivity, and a multitude of dielectric properties, which are of great importance in microelectronics and telecommunication. Recently interest has arisen in perovskite-type oxides as catalysts due to high thermal and hydrothermal stability as well as high mechanical strength among other properties. In the present work, LaMnO3 and LaNiO3 perovskite type oxide catalysts are developed for the purpose of pyrolysis of biomass, and they are studied in terms of structure. The crystal structures of catalysts were determined via X-Ray Diffraction (XRD), morphology of the samples were analyzed by Scanning Electron Microscope (SEM), and the specific surface area of the samples were determined by N2 adsorption desorption isotherms (BET) measurements.

  8. Alkaline earth metal-based metal-organic framework: hydrothermal synthesis, X-ray structure and heterogeneously catalyzed Claisen-Schmidt reaction.

    PubMed

    Saha, Debraj; Maity, Tanmoy; Koner, Subratanath

    2014-09-14

    Two alkaline earth metal-based carboxylate systems, [Mg(HL)(H2O)2]n (1) and [Ca(H2L)2]n (2) (H3L = chelidamic acid) have been hydrothermally synthesized, and characterized by single-crystal X-ray diffraction, IR, elemental analysis, and thermo-gravimetric analysis. Compound 1 has a 2D structure incorporating two water molecules. The dehydrated species, 1a, generated from 1 by removal of the coordinated water, has been characterized by thermo-gravimetric analysis, IR, elemental analysis and variable temperature powder X-ray diffraction. Both 1 and its dehydrated species 1a catalyze the Claisen-Schmidt reaction under heterogeneous conditions, but 1a is a more effective catalyst under environmentally friendly conditions. The catalyst can readily be recovered and reused in successive cycles without detectable loss of activity. Compound 2 has a 3D structure and is thermally stable up to 540 °C, but is inactive catalytically.

  9. Template-free synthesis of CdS hollow nanospheres based on an ionic liquid assisted hydrothermal process and their application in photocatalysis

    SciTech Connect

    Li Xinping; Gao Yanan; Yu Li; Zheng Liqiang

    2010-06-15

    Polycrystalline CdS hollow nanospheres with diameter of about 130 nm have been successfully synthesized in high yield by an ionic liquid (IL) assisted template-free hydrothermal method for the first time. Both the molar ratios of Cd/S precursor in the solution and the reaction temperature play important roles in the formation of the CdS hollow nanospheres. The concentrations of capping agent hexamethylenetetramine (HMT) and polyvinylpyrrolidone (PVP) are also crucial for the morphology and size of the final product. IL was found to be a key component in the formation of CdS hollow structures, because solid spheres were obtained in the absence of IL. A subsequent growth mechanism of hollow interior by localized Ostwald ripening process has been further discussed. Such hollow structures show high photocatalytic ability in the photodegradation of methylene blue. - Graphical abstract: TEM images of typical as-prepared CdS hollow nanospheres.

  10. Rapid synthesis of an aluminum-rich MSE-type zeolite by the hydrothermal conversion of an FAU-type zeolite.

    PubMed

    Inagaki, Satoshi; Tsuboi, Yasuyuki; Nishita, Yuji; Syahylah, Tuan; Wakihara, Toru; Kubota, Yoshihiro

    2013-06-10

    An aluminum-rich MSE-type zeolite (Si/Al is as small as 7) has been successfully synthesized in a remarkably short crystallization period of only 3 days by the hydrothermal conversion of an FAU-type zeolite, presumably by the assembly of four-membered-ring (4-R) aluminosilicate oligomers supplied by the double 6-R (D6R) components of the FAU framework with the aid of the structure-directing agents and seed crystals. The dealuminated version of the aluminum-rich MSE-type zeolite showed a high level of coke durability in addition to a significant yield of propylene, which indicates that this novel zeolitic material is suitable for industrial applications as a highly selective and long-lived catalyst.

  11. Synthesis of an attapulgite clay@carbon nanocomposite adsorbent by a hydrothermal carbonization process and their application in the removal of toxic metal ions from water.

    PubMed

    Chen, Li-Feng; Liang, Hai-Wei; Lu, Yang; Cui, Chun-Hua; Yu, Shu-Hong

    2011-07-19

    A new kind of attapulgite clay@carbon (ATP@C) nanocomposite adsorbent has been synthesized by a one-pot hydrothermal carbonization process under mild conditions using two cheap, ecofriendly materials (i.e., attapulgite clay (ATP), which is a magnesium aluminum silicate that is abundant in nature, and glucose, which is a green chemical obtained from biomass). Compared to carbon-based materials, this new ATP@C nanocomposite exhibits a high adsorption ability for Cr(VI) and Pb(II) ions with maximum adsorption capacities of 177.74 and 263.83 mg·g(-1), respectively. The results demonstrate that this nanocomposite is an exceptionally promising candidate as a low-cost, sustainable, and effective adsorbent for the removal of toxic ions from water.

  12. Hydrothermal synthesis of Bismuth(III) coordination polymer and its transformation to nano α-Bi2O3 for photocatalytic degradation

    NASA Astrophysics Data System (ADS)

    Huang, Ya-Jing; Zheng, Yue-Qing; Zhu, Hong-Lin; Wang, Jin-Jian

    2016-07-01

    A new Bi(III) coordination polymer Bi2(Hpdc)2(pdc)2·2H2O (H2pdc=pyridine-2,6-dicarboxylic acid) was synthesized by hydrothermal method. Solid state thermal decomposition of this complex under 500 °C for 1 h led to the foliated Bi2O3 nanoparticles, which were then characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Comparative study on their photocatalytic activity toward the degradation of rhodamine B (RhB), methylene blue (MB) and methyl orange (MO) in polluted water was explored, and the mechanism of these photocatalytic degradation was discussed. These results provided some interesting insights into their photocatalytic applications.

  13. Synthesis of High-Density Poinsettia-Like Microstructure of CuO by the Hydrothermal Method and Its Ethanol Sensing Properties

    NASA Astrophysics Data System (ADS)

    Hien, Vu Xuan; Minh, Vu Duy; Phuoc, Luong Huu; Vuong, Dang Duc; Heo, Young-Woo; Chien, Nguyen Duc

    2017-03-01

    Highly uniform and dense poinsettia-like microstructures of CuO were synthesized by a facile hydrothermal method. The effect of the treatment time on the growth of the CuO microstructures was investigated. The CuO microflowers with diameters in the range 3-5 μm were composed of many interconnected nanoleaves (1-2 μm in diameter and 20-30 nm in thickness). A plausible growth mechanism for the formation of the CuO microstructures has been proposed and discussed. In addition, the ethanol sensing properties of the CuO microflowers were characterized at 150-350°C. The poinsettia-like microstructures of CuO exhibited better response to ethanol when compared to the sensing properties of the CuO nanoleaves. The sensing mechanism based on the models of carrier transport and leaf-to-leaf contact has been proposed and discussed.

  14. Hydrothermal synthesis and photocatalytic performance of hierarchical Bi2MoO6 microspheres using BiOI microspheres as self-sacrificing templates

    NASA Astrophysics Data System (ADS)

    Xu, Ming; Zhang, Wei-De

    2015-07-01

    Bi2MoO6 hierarchical microspheres were successfully prepared through phase transformation from BiOI microspheres with the assistance of sodium citrate under hydrothermal condition. The possible formation mechanism for the conversion of BiOI to Bi2MoO6 is discussed here. After being annealed at 300 °C for 2 h, the obtained Bi2MoO6 microspheres exhibited remarkably enhanced photocatalytic activity towards the degradation of rhodamine B and phenol. The superior catalytic performance can be attributed to its larger surface area and higher crystallinity. In addition, Bi2MoO6 microspheres are stable during the degradation reaction and can be used repeatedly.

  15. Hydrothermal synthesis of nitrogen-doped carbon dots with real-time live-cell imaging and blood-brain barrier penetration capabilities.

    PubMed

    Lu, Shousi; Guo, Shanshan; Xu, Pingxiang; Li, Xiaorong; Zhao, Yuming; Gu, Wei; Xue, Ming

    Nitrogen-doped carbon dots (N-CDs) were synthesized using a one-pot hydrothermal treatment with citric acid in the presence of polyethylenimine. Transmission electron microscopy analysis revealed that the N-CDs were monodispersed and quasi-spherical with an average size of ~2.6 nm. Under ultraviolet irradiation the N-CDs emitted a strong blue luminescence with a quantum yield as high as 51%. Moreover, the N-CDs exhibited a negligible cytotoxicity and could be applied as efficient nanoprobes for real-time imaging of live cells. In addition, the ability of the N-CDs to cross the blood-brain barrier (BBB) in a concentration-dependent manner was demonstrated using an in vitro BBB model. Therefore, these PEI-passivated N-CDs with real-time live-cell imaging and BBB-penetration capabilities hold promise for traceable drug delivery to the brain.

  16. An experimental design approach for hydrothermal synthesis of NaYF4: Yb3+, Tm3+ upconversion microcrystal: UV emission optimization

    NASA Astrophysics Data System (ADS)

    Kaviani Darani, Masoume; Bastani, Saeed; Ghahari, Mehdi; Kardar, Pooneh

    2015-11-01

    Ultraviolet (UV) emissions of hydrothermally synthesized NaYF4: Yb3+, Tm3+ upconversion crystals were optimized using the response surface methodology experimental design. In these experimental designs, 9 runs, two factors namely (1) Tm3+ ion concentration, and (2) pH value were investigated using 3 different ligands. Introducing UV upconversion emissions as responses, their intensity were separately maximized. Analytical methods such as XRD, SEM, and FTIR could be used to study crystal structure, morphology, and fluorescent spectroscopy in order to obtain luminescence properties. From the photo-luminescence spectra, emissions centered at 347, 364, 452, 478, 648 and 803 nm were observed. Some results show that increasing each DOE factor up to an optimum value resulted in an increase in emission intensity, followed by reduction. To optimize UV emission, as a final result to the UV emission optimization, each design had a suggestion.

  17. Hydrothermal synthesis of nitrogen-doped carbon dots with real-time live-cell imaging and blood–brain barrier penetration capabilities

    PubMed Central

    Lu, Shousi; Guo, Shanshan; Xu, Pingxiang; Li, Xiaorong; Zhao, Yuming; Gu, Wei; Xue, Ming

    2016-01-01

    Nitrogen-doped carbon dots (N-CDs) were synthesized using a one-pot hydrothermal treatment with citric acid in the presence of polyethylenimine. Transmission electron microscopy analysis revealed that the N-CDs were monodispersed and quasi-spherical with an average size of ~2.6 nm. Under ultraviolet irradiation the N-CDs emitted a strong blue luminescence with a quantum yield as high as 51%. Moreover, the N-CDs exhibited a negligible cytotoxicity and could be applied as efficient nanoprobes for real-time imaging of live cells. In addition, the ability of the N-CDs to cross the blood–brain barrier (BBB) in a concentration-dependent manner was demonstrated using an in vitro BBB model. Therefore, these PEI-passivated N-CDs with real-time live-cell imaging and BBB-penetration capabilities hold promise for traceable drug delivery to the brain. PMID:27932880

  18. Synthesis of single-crystal PbS nanorods via a simple hydrothermal process using PEO-PPO-PEO triblock copolymer as a structure-directing agent

    NASA Astrophysics Data System (ADS)

    Bu, Junfu; Nie, Chageng; Liang, Jinxia; Sun, Lan; Xie, Zhaoxiong; Wu, Qi; Lin, Changjian

    2011-03-01

    Single-crystal PbS nanorods were successfully synthesized through a simple hydrothermal route using PEO-PPO-PEO triblock copolymer (P123) as a structure-directing agent. The XRD pattern indicates that the crystal structure of the nanorods is face-centre-cubic rocksalt. A SEM image shows that the nanorods have a diameter of 40-70 nm and a length of 200-600 nm, and both tips exhibit taper-like structures. HRTEM and SAED images reveal the single-crystalline nature of the nanorods with the growth along the lang111rang direction. The experimental results indicated that the P123 concentration and reaction temperature played important roles in controlling the morphology of the PbS nanostructures. The optical property of PbS nanorods was investigated by UV-Vis absorption spectroscopy and the band structure was calculated by the B3LYP hybrid density functional theory.

  19. Hierarchical Na-doped cubic ZrO2 synthesis by a simple hydrothermal route and its application in biodiesel production

    NASA Astrophysics Data System (ADS)

    Lara-García, Hugo A.; Romero-Ibarra, Issis C.; Pfeiffer, Heriberto

    2014-10-01

    Hierarchical growth of cubic ZrO2 phase was successfully synthesized via a simple hydrothermal process in the presence of different surfactants (cationic, non-ionic and anionic) and sodium hydroxide. The structural and microstructural characterizations of different ZrO2 powders were performed using various techniques, such as X-ray diffraction, transmission electron microscopy, N2 adsorption-desorption, scanning electron microscopy and infrared. Results indicated that sodium addition stabilized the cubic ZrO2 phase by a Na-doping process, independently of the surfactant used. In contrast, microstructural characteristics varied as a function of the surfactant and sodium presence. In addition, water vapor (H2O) and carbon dioxide (CO2) sorption properties were evaluated on ZrO2 samples. Results evidenced that sample surface reactivity changed as a function of the sodium content. Finally, this surface reactivity was evaluated on the biodiesel transesterification reaction using the different synthesized samples, obtaining yields of 93%.

  20. Flower-like nanostructure MNb{sub 2}O{sub 6} (M = Mn, Zn) with high surface area: Hydrothermal synthesis and enhanced photocatalytic performance

    SciTech Connect

    Huang, Xue; Jing, Yan; Yang, Jia; Ju, Jing; Cong, Rihong; Gao, Wenliang; Yang, Tao

    2014-03-01

    Graphical abstract: - Highlights: • MNb{sub 2}O{sub 6} was prepared by a mild two-step hydrothermal method. • Their flower-like nanostructure morphology was studied by SEM and TEM. • High BET surface areas for MnNb{sub 2}O{sub 6} (∼50 m{sup 2}/g) and ZnNb{sub 2}O{sub 6} (∼100 m{sup 2}/g). • Band gap energies were estimated by UV–vis diffuse reflectance spectra. • Photocatalytic activities were evaluated under UV-light irradiation. - Abstract: Nano-scaled MNb{sub 2}O{sub 6} (M = Mn, Zn) was successfully synthesized via a two-step hydrothermal method. It is important to control the exact pH of the reaction solution in order to obtain pure products. The as-prepared samples both crystallize in the columbite structure. Interestingly, the products possess a flower-like morphology in a pseudo-six-fold symmetry, which is in fact arrayed by two-dimensional nanosheets. Their surface areas (51 m{sup 2}/g for MnNb{sub 2}O{sub 6} and 103 m{sup 2}/g for ZnNb{sub 2}O{sub 6}) are about 25–50 times of those prepared by solid state reaction. UV–vis diffuse reflectance spectra show the nano-scaled sample has a stronger absorption and a narrower band gap than its bulk form. The estimated band gap energies are 2.70 eV (MnNb{sub 2}O{sub 6}) and 3.77 eV (ZnNb{sub 2}O{sub 6}), respectively. The nano-scaled ZnNb{sub 2}O{sub 6} exhibits a double enhancement of photocatalytic activity in the decolorization of methylene blue than bulk ZnNb{sub 2}O{sub 6}.

  1. Hydrothermal synthesis and photocatalytic activities of Bi{sub 4}Ti{sub 3}O{sub 12}/SrTiO{sub 3} composite micro-platelets

    SciTech Connect

    Zhao, Wei Wang, Hongxing; Feng, Xiangning; Jiang, Wangyang; Zhao, Dan; Li, Jiyuan

    2015-10-15

    Highlights: • Bi{sub 4}Ti{sub 3}O{sub 12}/SrTiO{sub 3} composite was fabricated by combining hydrothermal reaction and molten salt method. • Bi{sub 4}Ti{sub 3}O{sub 12}/SrTiO{sub 3} exhibits higher photocatalytic activity than pure Bi{sub 4}Ti{sub 3}O{sub 12}. • The absorption light of Bi{sub 4}Ti{sub 3}O{sub 12}/SrTiO{sub 3} has been broadened to visible light. - Abstract: In this study, Bi{sub 4}Ti{sub 3}O{sub 12}/SrTiO{sub 3} micro-platelets were successfully synthesized by using hydrothermal and molten salt methods, and the morphology and photocatalytic degradation performance of Bi{sub 4}Ti{sub 3}O{sub 12}/SrTiO{sub 3} was characterized. The results indicated a much higher degradation rate of methylene blue and methylene orange, reaching more than 90% and 65%, respectively, within 3 h under visible-light irradiation. Compared with pure Bi{sub 4}Ti{sub 3}O{sub 12}, the photocatalytic activity of Bi{sub 4}Ti{sub 3}O{sub 12}/SrTiO{sub 3} was significantly better, due to the micron–submicron heterojunction with SrTiO{sub 3} reducing the band gap of Bi{sub 4}Ti{sub 3}O{sub 12}. In addition, the perovskite structure layer facilitates the mobility of the photogenerated carriers and hampers their recombination, which were affected the photocatalytic properties.

  2. (Zn, Mg)2GeO4:Mn2+ submicrorods as promising green phosphors for field emission displays: hydrothermal synthesis and luminescence properties.

    PubMed

    Shang, Mengmeng; Li, Guogang; Yang, Dongmei; Kang, Xiaojiao; Peng, Chong; Cheng, Ziyong; Lin, Jun

    2011-10-07

    (Zn(1-x-y)Mg(y))(2)GeO(4): xMn(2+) (y = 0-0.30; x = 0-0.035) phosphors with uniform submicrorod morphology were synthesized through a facile hydrothermal process. X-Ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), photoluminescence (PL), and cathodoluminescence (CL) spectroscopy were utilized to characterize the samples. SEM and TEM images indicate that Zn(2)GeO(4):Mn(2+) samples consist of submicrorods with lengths around 1-2 μm and diameters around 200-250 nm, respectively. The possible formation mechanism for Zn(2)GeO(4) submicrorods has been presented. PL and CL spectroscopic characterizations show that pure Zn(2)GeO(4) sample shows a blue emission due to defects, while Zn(2)GeO(4):Mn(2+) phosphors exhibit a green emission corresponding to the characteristic transition of Mn(2+) ((4)T(1)→(6)A(1)) under the excitation of UV and low-voltage electron beam. Compared with Zn(2)GeO(4):Mn(2+) sample prepared by solid-state reaction, Zn(2)GeO(4):Mn(2+) phosphors obtained by hydrothermal process followed by high temperature annealing show better luminescence properties. In addition, codoping Mg(2+) ions into the lattice to substitute for Zn(2+) ions can enhance both the PL and CL intensity of Zn(2)GeO(4):Mn(2+) phosphors. Furthermore, Zn(2)GeO(4):Mn(2+) phosphors exhibit more saturated green emission than the commercial FEDs phosphor ZnO:Zn, and it is expected that these phosphors are promising for application in field-emission displays.

  3. Synthesis and characterization of hybrid nanostructures produced in the presence of the titanium dioxide and bioactive organic substances by hydrothermal method

    SciTech Connect

    Zima, Tatyana; Baklanova, Natalya; Bataev, Ivan

    2013-02-15

    Hybrid nanostructures produced by hydrothermal treatment of TiO{sub 2} in the presence of bioactive organic substances such as chitosan, aminoterephthalic acid and their mixture have been investigated. Sodium polytitanates as one-dimensional elongated structures with lengths of several hundred of nanometers were obtained in the presence of chitosan and aminoterephthalic acid. With chitosan the elongated nanostructures are formed by successive superposition of structural fragments-nanostrips with well-ordered multilayered morphology and increased distance between successive layers to 1.2 nm. Quite different amorphous products as agglomerates with roundest and rhomboid morphology are formed when the mixture of chitosan and aminoterephthalic acid is added to the reaction system. One can propose that main reason of such behavior is a low rate of diffusion of dissolved Ti(IV) ions in the high viscous mixed chitosan-aminoterephthalic system. An effect of organic substances on the formation, morphology and transformation of various titanates is discussed. - Graphical abstract: The typical images of hybrid nanostructures produced by hydrothermal treatment of TiO{sub 2} in the presence chitosan and mixed chitosan with aminoterephthalic acid. Highlights: Black-Right-Pointing-Pointer Various shapes of TiO{sub 2} based structures can be produced in the presence of organic. Black-Right-Pointing-Pointer An addition of chitosan results in the formation of the elongated nanostructures. Black-Right-Pointing-Pointer These structures have multilayered morphology and increased distance between layers. Black-Right-Pointing-Pointer Different agglomerates are formed when chitosan and aminoterephthalic acid are mixed.

  4. Hydrothermal synthesis of 3D urchin-like Ag/TiO2/reduced graphene oxide composites and its enhanced photocatalytic performance

    NASA Astrophysics Data System (ADS)

    Liu, Yuhuan; Zhou, Yi; Yang, Luyue; Wang, Yutang; Wu, Yiwei; Li, Chaocheng; Lu, Jun

    2016-09-01

    Innovative 3D urchin-like ternary TiO2 composites, which combine Ag nanoparticles with graphene, have been successfully synthesized through a simple hydrothermal method. This process employed nontoxic and mild dihydrate sodium citrate as a reducing agent. During the hydrothermal process, graphene oxide and AgNO3 were reduced to reduced graphene oxide (RGO) and Ag, respectively. Subsequently, they were grown on the surface of rutile TiO2 with a 3D urchin-like microsphere (1.5 μm). The as-prepared 3D urchin-like composites were characterized by X-ray diffraction, SEM and TEM. These techniques were also employed to ensure the morphology of urchin-like and rutile phase of TiO2. FT-IR, Raman spectroscopy and XPS characterization demonstrated the successful reduction in AgNO3 and graphite oxide to metallic Ag and RGO. The UV-visible spectrum of the ternary composite displayed strong absorption in the visible light region, which was attributed to the efficient electron transport of well-dispersed Ag nanoparticles (20-40 nm) and the formation of Ti-O-C bond between graphene and titania. The synthesized urchin-like ternary composite exhibited enhanced photocatalytic activity (98.7 %) for Rhodamine B degradation. This work provides a very convenient chemical route to the scalable production of Ag/TiO2/RGO ternary composite photocatalyst for potential applications in solving the environmental problems and energy issues. Also, the proposed mechanism underlying the photocatalytic degradation of Rhodamine B dyes was discussed.

  5. Hydrothermal synthesis of Ca{sub 3}Bi{sub 8}O{sub 15} rods and their visible light photocatalytic properties

    SciTech Connect

    Li, Wenjuan; Kong, Desheng; Cui, Xiaoli; Du, Dandan; Yan, Tingjiang; You, Jinmao

    2014-03-01

    Graphical abstract: The novel Ca{sub 3}Bi{sub 8}O{sub 15} rods can utilize the sunlight efficiently with the small band-gap. Using methyl orange (MO) as a model organic pollutant, the photocatalysts exhibited good photocatalytic activity, with the photodegradation conversion ratio of MO being up to 90% after 2 h of visible light (420 nm < λ < 800 nm) irradiation. - Highlights: • Ca{sub 3}Bi{sub 8}O{sub 15} rods were synthesized by a hydrothermal method. • They can utilize the sunlight efficiently with the small band-gap. • They showed good photocatalytic activities in the degradation of MO, RhB and 4-CP. • The conversion ratio of MO was up to 90% after 2 h of visible light irradiation. - Abstract: High efficient visible light Ca{sub 3}Bi{sub 8}O{sub 15} photocatalysts were synthesized by a hydrothermal method. Characterized by X-ray diffractometer, transmission electron microscopy, and the UV–vis diffuse reflectance spectroscopy, the results showed that the novel Ca{sub 3}Bi{sub 8}O{sub 15} rods can utilize the sunlight efficiently with the small band-gap. Using methyl orange (MO) as a model organic pollutant, the photocatalysts exhibited good photocatalytic activity, with the photodegradation conversion ratio of MO being up to 90% after 2 h of visible light (420 nm < λ < 800 nm) irradiation. Furthermore, they also showed good photocatalytic activities in the degradation of rhodamine B and p-chlorophenol. Through the investigation of the degraded mechanism, the main active species played important roles in the degradation process were holes, O{sub 2}·{sup −} and ·OH.

  6. Hydrothermal synthesis of Bismuth(III) coordination polymer and its transformation to nano α-Bi{sub 2}O{sub 3} for photocatalytic degradation

    SciTech Connect

    Huang, Ya-Jing; Zheng, Yue-Qing Zhu, Hong-Lin; Wang, Jin-Jian

    2016-07-15

    A new Bi(III) coordination polymer Bi{sub 2}(Hpdc){sub 2}(pdc){sub 2}·2H{sub 2}O (H{sub 2}pdc=pyridine-2,6-dicarboxylic acid) was synthesized by hydrothermal method. Solid state thermal decomposition of this complex under 500 °C for 1 h led to the foliated Bi{sub 2}O{sub 3} nanoparticles, which were then characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Comparative study on their photocatalytic activity toward the degradation of rhodamine B (RhB), methylene blue (MB) and methyl orange (MO) in polluted water was explored, and the mechanism of these photocatalytic degradation was discussed. These results provided some interesting insights into their photocatalytic applications. - Graphical abstract: We regard Bi{sub 2}(Hpdc){sub 2}(pdc){sub 2}·2H{sub 2}O with 1D chain structures as the precursor, then calcinate the complex to prepare nano-powder α-Bi{sub 2}O{sub 3}. The photochemical experiment indicates that Bi{sub 2}(Hpdc){sub 2}(pdc){sub 2}·2H{sub 2}O can be used as an efficient photocatalyst for the degradation of RhB and MB. Interestingly, nano α-Bi{sub 2}O{sub 3} shows higher activity than the commercial Bi{sub 2}O{sub 3} for the degradation of RhB, MB or MO. Display Omitted - Highlights: • A novel dinuclear Bi(III) coordination polymer is hydrothermally synthesized. • Calcinating the precursor Bi-CP will result in the nano Bi{sub 2}O{sub 3} with foliated morphology. • Nano Bi{sub 2}O{sub 3} shows higher activity than the commercial Bi{sub 2}O{sub 3} for the degradation of dyes.

  7. Hydrothermal synthesis of Y{sub 2}O{sub 3} coated Y{sub 2}O{sub 3}:Eu{sup 3+} nanotubes for enhanced photoluminescence properties

    SciTech Connect

    Gao, Linhui; Wang, Guangfa; Zhu, Hongliang; Zhou, Weijie; Ou, Guofu

    2015-10-15

    Highlights: • Eu{sup 3+} doped Y{sub 2}O{sub 3} nanotubes. • Hydrothermal synthesis of Y{sub 2}O{sub 3} coated Y{sub 2}O{sub 3}:Eu{sup 3+} nanostructures assissted with a further heat treatment. • Tunable coating ratios of Y{sub 2}O{sub 3} coated Y{sub 2}O{sub 3}:Eu{sup 3+} nanophosphor. • Enhanced photoluminescence intensity of Y{sub 2}O{sub 3}:Eu{sup 3+} more than 60% by Y{sub 2}O{sub 3} surface coating. - Abstract: Novel Y{sub 2}O{sub 3} coated Y{sub 2}O{sub 3}:Eu{sup 3+} nanotubes with different coating ratios were synthesized successfully by a facile two-step process, including hydrothermal synthesis of Y(OH){sub 3} coated Y(OH){sub 3}:Eu{sup 3+} as precursors and then calcination of them at 1000 °C for 2 h. X-ray diffraction patterns and field emission scanning electron microscope images indicated these Y{sub 2}O{sub 3} coated Y{sub 2}O{sub 3}:Eu{sup 3+} phosphors possess tubular nanostructures. The photoluminescence properties of Y{sub 2}O{sub 3} coated Y{sub 2}O{sub 3}:Eu{sup 3+} were systematically investigated by photoluminescence spectra, and photoluminescence enhancement was observed after proper coating. In other words, the coating ratio played a crucial role in photoluminescence efficiency. When it was 1/9, the photoluminescence intensity of {sup 5}D{sub 0} → {sup 7}F{sub 2} emission (about 613 nm) was 60% higher than that of Y{sub 2}O{sub 3}: Eu{sup 3+} phosphors under 255 nm excitation. Therefore, surface coating may be an alternative route for enhanced photoluminescence properties of the Y{sub 2}O{sub 3}:Eu{sup 3+} red-emitting phosphor.

  8. Hydrothermal synthesis of zinc(II)-phosphonate coordination polymers with different dimensionality (0D, 2D, 3D) and dimensionality change in the solid phase (0D→3D) induced by temperature

    SciTech Connect

    Fernández-Zapico, Eva; Montejo-Bernardo, Jose; Fernández-González, Alfonso; García, José R. García-Granda, Santiago

    2015-05-15

    Three new zinc(II) coordination polymers, [Zn(HO{sub 3}PCH{sub 2}CH{sub 2}COO)(C{sub 12}H{sub 8}N{sub 2})(H{sub 2}O)] (1), [Zn{sub 3}(O{sub 3}PCH{sub 2}CH{sub 2}COO){sub 2}(C{sub 12}H{sub 8}N{sub 2})](H{sub 2}O){sub 3.40} (2) and [Zn{sub 5}(HO{sub 3}PCH{sub 2}CH{sub 2}COO){sub 2}(O{sub 3}PCH{sub 2}CH{sub 2}COO){sub 2}(C{sub 12}H{sub 8}N{sub 2}){sub 4}](H{sub 2}O){sub 0.32} (3), with different structural dimensionality (0D, 2D and 3D, respectively) have been prepared by hydrothermal synthesis, and their structures were determined by single-crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic system (P2{sub 1}/c) forming discrete dimeric units bonded through H-bonds, while compounds 2 and 3 crystallize in the triclinic (P−1) and the monoclinic (C2/c) systems, respectively. Compound 3, showing three different coordination numbers (4, 5 and 6) for the zinc atoms, has also been obtained by thermal treatment of 1 (probed by high-temperature XRPD experiments). The crystalline features of these compounds, related to the coordination environments for the zinc atoms in each structure, provoke the increase of the relative fluorescence for 2 and 3, compared to the free phenanthroline. Thermal analysis (TG and DSC) and XPS studies have been also carried out for all compounds. - Graphical abstract: Three new coordination compounds of zinc with 2-carboxyethylphosphonic acid (H{sub 2}PPA) and phenanthroline have been obtained by hydrothermal synthesis. The crystalline structure depends on the different coordination environments of the zinc atoms (see two comparative Zn{sub 6}-moieties). The influence of the different coordination modes of H{sub 2}PPA with the central atom in all structures have been studied, being found new coordination modes for this ligand. Several compounds show a significant increase in relative fluorescence with respect to the free phenanthroline. - Highlights: • Compounds have been obtained modifying the reaction time and the rate of

  9. Hydrothermal synthesis of highly crystalline RuS{sub 2} nanoparticles as cathodic catalysts in the methanol fuel cell and hydrochloric acid electrolysis

    SciTech Connect

    Li, Yanjuan; Li, Nan; Yanagisawa, Kazumichi; Li, Xiaotian; Yan, Xiao

    2015-05-15

    Highlights: • Highly crystalline RuS{sub 2} nanoparticles have been first synthesized by a “one-step” hydrothermal method. • The product presents a pure cubic phase of stoichiometric ratio RuS{sub 2} with average particle size of 14.8 nm. • RuS{sub 2} nanoparticles were used as cathodic catalysts in methanol fuel cell and hydrochloric acid electrolysis. • The catalyst outperforms commercial Pt/C in methanol tolerance and stability towards Cl{sup −}. - Abstract: Highly crystalline ruthenium sulfide (RuS{sub 2}) nanoparticles have been first synthesized by a “one-step” hydrothermal method at 400 °C, using ruthenium chloride and thiourea as reactants. The products were characterized by powder X-ray diffraction (XRD), scanning electron microscopy/energy disperse spectroscopy (SEM/EDS), thermo gravimetric-differential thermal analyze (TG-DTA), transmission electron microscopy equipped with selected area electron diffraction (TEM/SAED). Fourier transform infrared spectra (IR), and X-ray photoelectron spectroscopy (XPS). XRD result illustrates that the highly crystalline product presents a pure cubic phase of stoichiometric ratio RuS{sub 2} and the average particle size is 14.8 nm. SEM and TEM images display the products have irregular shape of 6–25 nm. XPS analyst indicates that the sulfur exists in the form of S{sub 2}{sup 2−}. Cyclic voltammetry (CV), rotating disk electrode (RDE), chronoamperometry (CA) and electrochemical impedance spectroscopy (EIS) measurements are conducted to evaluate the electrocatalytic activity and stability of the highly crystalline RuS{sub 2} nanoparticles in oxygen reduction reaction (ORR) for methanol fuel cell and hydrochloric acid electrolysis. The results illustrate that RuS{sub 2} is active towards oxygen reduction reaction. Although the activity of RuS{sub 2} is lower than that of Pt/C, the RuS{sub 2} catalyst outperforms commercial Pt/C in methanol tolerance and stability towards Cl{sup −}.

  10. One-step hydrothermal synthesis of N-doped TiO2/C nanocomposites with high visible light photocatalytic activity.

    PubMed

    Wang, Dong-Hong; Jia, Li; Wu, Xi-Lin; Lu, Li-Qiang; Xu, An-Wu

    2012-01-21

    N-doped TiO(2) nanoparticles modified with carbon (denoted N-TiO(2)/C) were successfully prepared by a facile one-pot hydrothermal treatment in the presence of L-lysine, which acts as a ligand to control the nanocrystal growth and as a source of nitrogen and carbon. As-prepared nanocomposites were characterized by thermogravimetric analysis (TGA), X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), Raman spectroscopy, ultraviolet-visible (UV-vis) diffuse reflectance spectroscopy, X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR), electron paramagnetic resonance (EPR) spectra, and N(2) adsorption-desorption analysis. The photocatalytic activities of the as-prepared photocatalysts were measured by the degradation of methyl orange (MO) under visible light irradiation at λ≥ 400 nm. The results show that N-TiO(2)/C nanocomposites increase absorption in the visible light region and exhibit a higher photocatalytic activity than pure TiO(2), commercial P25 and previously reported N-doped TiO(2) photocatalysts. We have demonstrated that the nitrogen was doped into the lattice and the carbon species were modified on the surface of the photocatalysts. N-doping narrows the band gap and C-modification enhances the visible light harvesting and accelerates the separation of the photo-generated electrons and holes. As a consequence, the photocatalytic activity is significantly improved. The molar ratio of L-lysine/TiCl(4) and the pH of the hydrothermal reaction solution are important factors affecting the photocatalytic activity of the N-TiO(2)/C; the optimum molar ratio of L-lysine/TiCl(4) is 8 and the optimum pH is ca. 4, at which the catalyst exhibits the highest reactivity. Our findings demonstrate that the as-obtained N-TiO(2)/C photocatalyst is a better and more promising candidate than well studied N-doped TiO(2) alternatives as visible light photocatalysts for

  11. Zinc(II) and lead(II) metal-organic networks driven by a multifunctional pyridine-carboxylate building block: Hydrothermal synthesis, structural and topological features, and luminescence properties

    NASA Astrophysics Data System (ADS)

    Yang, Ling; Li, Yu; You, Ao; Jiang, Juan; Zou, Xun-Zhong; Chen, Jin-Wei; Gu, Jin-Zhong; Kirillov, Alexander M.

    2016-09-01

    4-(5-Carboxypyridin-2-yl)isophthalic acid (H3L) was applied as a flexible, multifunctional N,O-building block for the hydrothermal self-assembly synthesis of two novel coordination compounds, namely 2D [Zn(μ3-HL)(H2O)]n·nH2O (1) and 3D [Pb2(μ5-HL)(μ6-HL)]n (2) coordination polymers (CPs). These compounds were obtained in aqueous medium from a mixture containing zinc(II) or lead(II) nitrate, H3L, and sodium hydroxide. The products were isolated as stable crystalline solids and were characterized by IR spectroscopy, elemental, thermogravimetric (TGA), powder (PXRD) and single-crystal X-ray diffraction analyses. Compound 1 possesses a 2D metal-organic layer with the fes topology, which is further extended into a 3D supramolecular framework via hydrogen bonds. In contrast, compound 2 features a very complex network structure, which was topologically classified as a binodal 5,6-connected net with the unique topology defined by the point symbol of (47.63)(49.66). Compounds 1 and 2 disclose an intense blue or green luminescent emission at room temperature.

  12. ZnIO3(OH): a new layered noncentrosymmetric polar iodate--hydrothermal synthesis, crystal structure, and second-harmonic generating (SHG) properties.

    PubMed

    Lee, Dong Woo; Kim, Saet Byeol; Ok, Kang Min

    2012-07-21

    A new noncentrosymmetric polar iodate material, ZnIO(3)(OH), has been hydrothermally synthesized as crystals and pure powders by using ZnO (or Zn(CH(3)CO(2))(2)·2H(2)O), HIO(3), and water. Single crystal X-ray diffraction was used to determine the crystal structure of the reported material. ZnIO(3)(OH) exhibits a layered structure that is composed of ZnO(6) and IO(3) polyhedra. Powder nonlinear optical (NLO) properties measurements on ZnIO(3)(OH) using 1064 nm radiation indicate the material has a second-harmonic generating (SHG) efficiency of approximately 20 times that of α-SiO(2). Additional SHG measurements reveal that the material is not phase-matchable (type 1). Infrared spectroscopy, elemental analysis, and thermogravimetric analysis for the reported compound are also presented. Crystal data: ZnIO(3)(OH), monoclinic, space group Cc (no. 9) with a = 4.67670(10) Å, b = 11.2392(4) Å, c = 6.3308(2) Å, β = 90.019(2)°, and Z = 4.

  13. Alkali-dependent synthesis of flower-like ZnO structures with enhanced photocatalytic activity via a facile hydrothermal method

    NASA Astrophysics Data System (ADS)

    Sun, Lin; Shao, Rong; Chen, Zhidong; Tang, Lanqin; Dai, Yong; Ding, Jianfei

    2012-05-01

    Flower-like ZnO structures with high photocatalytic performance were successfully synthesized via a facile hydrothermal method. Alkaline environment played a critical role during the morphological transformation. When the molar ratio of Zn(CH3COO)2·2H2O to NaOH was set as 1:8 in the presence of triethanolamine (TEA), and the molar ratio of Zn2+ to TEA was 1:9, the flower-like ZnO product was produced. The hexagonal sphere-like, oblate-like, and hexagonal biprism-like samples were also obtained by adjusting the molar ratio of Zn2+ to NaOH as 1:2, 1:5 and 1:12 with the presence of invariable amount of TEA, respectively. The prepared ZnO products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) surface area. Photodegradation experiments of the samples were carried out by choosing Methylene Blue (MB) as a model target under UV irradiation with homemade photocatalytic apparatus. Among these products, flower-shaped samples exhibited the highest photocatalytic activity.

  14. Hydrothermal synthesis of high-quality type-II CdTe/CdSe core/shell quantum dots with dark red emission.

    PubMed

    Liu, Ning; Yang, Ping

    2014-08-01

    A hydrothermal method was used to synthesize type-II CdTe/CdSe core/shell quantum dots (QDs) using the thilglycolic acid (TGA) capped CdTe QDs as cores, which show a number of advantages. Because of the spatial separation of carriers the low excited states of CdTe/CdSe QDs, they exhibit many novel properties that are fundamentally different from the type-I QDs. On the other hand, our experiment results show that the wave function of the hole of the exciton in the CdTe core extends well into the CdSe shell. The results also reveal that a thick shell can confine the electrons inside the particles and thereby improve the PL efficiency and prolong the lifetime of the core/shell QDs. We use the UV-vis absorption and fluorescence spectrum measurements on growing particles in detail. We found that the fluorescence of the CdTe/CdSe QDs was strongly dependent on the thick of the shell and size of the core as well as the unique type-II heterostructure, which make the type-II core/shell QDs more suitable in photovoltaic or photoconduction applications.

  15. Acid-assisted hydrothermal synthesis of nanocrystalline TiO2 from titanate nanotubes: influence of acids on the photodegradation of gaseous toluene.

    PubMed

    Chen, Kunyang; Zhu, Lizhong; Yang, Kun

    2015-01-01

    In order to efficiently remove volatile organic compounds (VOCs) from indoor air, one-dimensional titanate nanotubes (TiNTs) were hydrothermally treated to prepare TiO2 nanocrystals with different crystalline phases, shapes and sizes. The influences of various acids such as CH3COOH, HNO3, HCl, HF and H2SO4 used in the treatment were separately compared to optimize the performance of the TiO2 nanocrystals. Compared with the strong and corrosive inorganic acids, CH3COOH was not only safer and more environmentally friendly, but also more efficient in promoting the photocatalytic activity of the obtained TiO2. It was observed that the anatase TiO2 synthesized in 15 mol/L CH3COOH solution exhibited the highest photodegradation rate of gaseous toluene (94%), exceeding that of P25 (44%) by a factor of more than two. The improved photocatalytic activity was attributed to the small crystallite size and surface modification by CH3COOH. The influence of relative humidity (20%-80%) on the performance of TiO2 nanocrystals was also studied. The anatase TiO2 synthesized in 15 mol/L CH3COOH solution was more tolerant to moisture than the other TiO2 nanocrystals and P25.

  16. One-pot hydrothermal synthesis of CuBi co-doped mesoporous zeolite Beta for the removal of NOx by selective catalytic reduction with ammonia

    NASA Astrophysics Data System (ADS)

    Xie, Zhiguo; Zhou, Xiaoxia; Wu, Huixia; Chen, Lisong; Zhao, Han; Liu, Yan; Pan, Linyu; Chen, Hangrong

    2016-07-01

    A series of CuBi co-doped mesoporous zeolite Beta (CuxBiy-mBeta) were prepared by a facile one-pot hydrothermal treatment approach and were characterized by XRD, N2 adsorption-desorption, TEM/SEM, XPS, H2-TPR, NH3-TPD and in situ DRIFTS. The catalysts CuxBiy-mBeta were applied to the removal of NOx by selective catalytic reduction with ammonia (NH3-SCR), especially the optimized Cu1Bi1-mBeta achieved the high efficiency for the removal of NOx and N2 selectivity, superior water and sulfur resistance as well as good durability. The excellent catalytic performance could be attributed to the acid sites of the support and the synergistic effect between copper and bismuth species. Moreover, in situ DRIFTS results showed that amides NH2 and NH4+ generated from NH3 adsorption could be responsible for the high selective catalytic reduction of NOx to N2. In addition, a possible catalytic reaction mechanism on Cu1Bi1-mBeta for the removal of NOx by NH3-SCR was proposed for explaining this catalytic process.

  17. Hydrothermal synthesis of Ag@TiO2-Fe3O4 nanocomposites using sonochemically activated precursors: magnetic, photocatalytic and antibacterial properties

    NASA Astrophysics Data System (ADS)

    Bokare, Anuja; Singh, Hema; Pai, Mrinal; Nair, Roopa; Sabharwal, Sushma; Athawale, Anjali A.

    2014-12-01

    Fe3O4-TiO2 nanocomposites have been synthesized by hydrothermal method using sonochemically activated precursors. X-ray diffraction analysis of the samples reveals the formation of pure phase composites. The optical properties of the composites are superior to TiO2 as noted from the red shift in the diffused reflectance spectra of the composites. The presence of nanocubes of Fe3O4, nanospheres of TiO2 and heterojunctions of the two in the composite samples have been observed in transmission electron micrographs. The magnetic properties of the samples were determined with the help of vibrating sample magnetometry (VSM) and magnetic force microscopy (MFM). The photocatalytic activity of the samples was investigated in terms of degradation of methyl orange (MO) dye. The composites could be easily separated from the reaction mixture after photocatalysis due to their magnetic behaviour. However, the photocatalytic activity of the composites was observed to be lower compared to bare TiO2. The composite (15% Fe3O4-TiO2) when modified by coating it with Ag showed enhanced photocatalytic activity. Further, the antibacterial activities of the samples were also examined using E. coli as a model organism. Positive results were obtained only for the Ag coated composite with lower MIC (minimum inhibition concentration) values.

  18. Hydrothermal synthesis and characterization of a new layered gallophosphate JGP-L1 with a Ga/P ratio of non-unity

    NASA Astrophysics Data System (ADS)

    Yang, Yulin; Liu, Yunling; Mu, Zhongcheng; Ye, Ling; Hu, Tao; Chen, Chao; Pang, Wenqin

    2004-03-01

    A new compound, Ga 6(OH) 4(HPO 4) 2(PO 4) 5·C 8H 28N 5·3H 2O (denoted JGP-L1), with a gallophosphate layer and a Ga/P ratio of 6/7 has been synthesized hydrothermally by using tetraethylenepentamine as template. It is characterized by powder X-ray diffraction (XRD), elemental analysis, inductively coupled plasma, and TGA analysis and structurally determined by single-crystal XRD analysis. JGP-L1 crystallizes in the orthorhombic, space group Pna2 1 (no. 33), with a=16.422(3), b=11.898(2), c=18.730(4) Å, V=3659.6(13) Å 3 and Z=4. The structure of JGP-L1 is built up by alternating of Ga(OH) 2O 4 octahedra, Ga(OH)O 4 trigonal bipyramids and PO 4 (or HPO 4) tetrahedra to form inorganic sheets. It is noteworthy that JGP-L1 was synthesized with extremely low reactant concentration, where the reaction mixture exhibits a H 2O:Ga 2O 3 molar ratio of 2220:1.

  19. Hydrothermal synthesis, crystal structure, conductivity, and thermal decomposition of [Cu(4,4'-bipy)(H2O)(Mo3O10)].H2O.

    PubMed

    Kong, Zuping; Weng, Linhong; Tan, Dejun; He, Heyong; Zhang, Biao; Kong, Jilie; Yue, Bin

    2004-09-06

    The hydrothermal reaction of (NH(4))(6)Mo(7)O(24).4H(2)O, CuCl(2).2H(2)O, and 4,4'-bipyridine yields bipyridine-ligated copper-trimolybdate monohydrate [Cu(4,4'-bipy)(H(2)O)(Mo(3)O(10))].H(2)O in the monoclinic system with space group of C(2/c) and cell parameters of a = 15.335(2) A, b = 15.535(2) A, c = 15.106(2) A, beta = 101.162(2) degrees, V = 3530.7(9) A(3), and Z = 8. Its structure consists of one-dimensional infinite ([Mo3O10]2-)( infinity ) chains linked through [Cu2(H2O)2(4,4'-bipy)] units. The Mo-O chain contains distorted [MoO(6)] octahedra connected through corner-sharing oxygen atoms into infinite chains along the c direction and each chain is located in the channel formed by four adjacent crossing chains of [Cu(4,4'-bipy)(H2O)](n)(2n+). The crystal shows weak conductivity through Mo-O chain along the c direction and insulating property along either a or b direction. Furthermore, a crystalline bimetallic oxide, CuMo3O10, forms when the title compound undergoes thermal treatment in N(2) atmosphere after the complete removal of the ligands.

  20. Hydrothermal synthesis of NaLuF4:153Sm,Yb,Tm nanoparticles and their application in dual-modality upconversion luminescence and SPECT bioimaging.

    PubMed

    Yang, Yang; Sun, Yun; Cao, Tianye; Peng, Juanjuan; Liu, Ying; Wu, Yongquan; Feng, Wei; Zhang, Yingjian; Li, Fuyou

    2013-01-01

    Upconversion luminescence (UCL) properties and radioactivity have been integrated into NaLuF(4):(153)Sm,Yb,Tm nanoparticles by a facile one-step hydrothermal method, making these nanoparticles potential candidates for UCL and single-photon emission computed tomography (SPECT) dual-modal bioimaging in vivo. The introduction of small amount of radioactive (153)Sm(3+) can hardly vary the upconversion luminescence properties of the nanoparticles. The as-designed nanoparticles showed very low cytotoxicity, no obvious tissue damage in 7 days, and excellent in vitro and in vivo performances in dual-modal bioimaging. By means of a combination of UCL and SPECT imaging in vivo, the distribution of the nanoparticles in living animals has been studied, and the results indicated that these particles were mainly accumulated in the liver and spleen. Therefore, the concept of (153)Sm(3+)/Yb(3+)/Tm(3+) co-doped NaLuF(4) nanoparticles for UCL and SPECT dual-modality imaging in vivo of whole-body animals may serve as a platform for next-generation probes for ultra-sensitive molecular imaging from the cellular scale to whole-body evaluation. It also introduces an easy methodology to quantify in vivo biodistribution of nanomaterials which still needs further understanding as a community.

  1. Single red upconversion and near-infrared downconversion luminescence properties of cubic ZrO2:Y3+-Yb3+-Er3+ nanophosphors via microwave hydrothermal synthesis

    NASA Astrophysics Data System (ADS)

    Liao, Jinsheng; Wang, Qi; Nie, Liling; You, Weixiong; Chen, Jinglin

    2016-12-01

    The Yb3+-Er3+-Y3+ tri-doped cubic ZrO2 (brief as YSZ:Yb, Er) nanophosphors with different Yb3+ (Er3+) doping concentrations have been prepared by microwave hydrothermal method followed by further calcining treatment. X-ray diffraction (XRD), transmission electron microscope (TEM), and photoluminescence spectra were used to characterize the properties of YSZ:Yb, Er nanophosphors. Under the 980 nm excitation, the sample gives a set of upconversion light: very strong red emissions near 655 and 679 nm (4F9/2 → 4I15/2), very weak green (525 nm 2H11/2 → 4I15/2, 544 nm and 557 nm 4S3/2 → 4I15/2). Moreover, the sample gives near-infrared downconversion emission (1530 nm 4I13/2 → 4I15/2). Concentration dependent studies revealed that the optimal composition was realized for the 15 at% Yb3+ and 1 at% Er3+-doping concentration with a strong pure red emission. All the results indicate that YSZ:Yb, Er nanophosphors could be a promising biological labeling materials.

  2. Hydrothermal synthesis of meso/macroporous BiVO4 hierarchical particles and their photocatalytic degradation properties under visible light irradiation.

    PubMed

    Madhusudan, Puttaswamy; Kumar, Malahalli Vijaya; Ishigaki, Tadashi; Toda, Kenji; Uematsu, Kazuyoshi; Sato, Mineo

    2013-09-01

    An ordered hierarchical meso/macroporous monoclinic bismuth vanadate (BiVO4) particle was fabricated for the first time by a simple two-step melamine template hydrothermal method followed by calcination. The physiochemical parameters of as-prepared porous materials were characterized by means of X-ray diffraction, scanning electron microscopy, high-resolution transmission electron microscopy, Raman, Barrett-Emmett-Teller, and UV-vis techniques. The nitrogen adsorption-desorption measurement and pore size distribution curve suggest that meso/macropores exist in these hierarchical microarchitectures. Further, it is found that melamine plays a significant role in the formation of porous BiVO4 particles, and when a known amount of melamine was added, the surface area and pore size of such porous BiVO4 particles were increased. The photocatalytic activities of the as-prepared hierarchical BiVO4 samples were measured for the photodegradation of Congo red aqueous dye solution under visible light irradiation. Surprisingly, the porous BiVO4 particles showed outstanding photocatalytic activities than polycrystalline BiVO4 sample. The possible enhancement of such catalytic performance has also been further discussed.

  3. Hydrothermal synthesis of graphitic carbon nitride-BiVO4 composites with enhanced visible light photocatalytic activities and the mechanism study

    NASA Astrophysics Data System (ADS)

    Guo, Feng; Shi, Weilong; Lin, Xue; Che, Guangbo

    2014-11-01

    Novel graphitic carbon nitride (C3N4) and bismuth vanadate (BiVO4) composite photocatalysts were successfully synthesized by a facile hydrothermal method. The scanning electron microscopy (SEM) revealed that an intimate interface between C3N4 and BiVO4 formed in the composites. Compared with the pure C3N4 and BiVO4, the C3N4-BiVO4 photocatalysts showed remarkably the higher photocatalytic activities in degrading rhodamine B (Rh B). The best active heterojunction proportion was 0.5C3N4-0.5BiVO4. Over this catalyst, the 100% degradation of Rh B (0.002 mmol L-1) was obtained under visible light irradiation (λ>420 nm) for 40 min. The active species in Rh B degradation were examined by adding a series of scavengers. The study on photocatalytic mechanism revealed that the electrons injected directly from the conduction band of C3N4 to that of BiVO4, resulting in the production of superoxide radical (O2•-) and hydroxyl radical (OH•) in the conduction band of BiVO4. Simultaneously, the rich holes in the valence band of g-C3N4 oxidized Rh B directly to promote the photocatalytic degradation reaction.

  4. Supercritical hydrothermal synthesis of Cu{sub 2}O(SeO{sub 3}): Structural characterization, thermal, spectroscopic and magnetic studies

    SciTech Connect

    Larranaga, Aitor

    2009-01-08

    Cu{sub 2}O(SeO{sub 3}) has been synthesized in supercritical hydrothermal conditions, using an externally heated steel reactor with coupled hydraulic pump for the application of high pressure. The compound crystallizes in the P2{sub 1}3 cubic space group. The unit cell parameter is a = 9.930(1) A with Z = 12. The crystal structure has been refined by the Rietveld method. The limit of thermal stability is, approximately, 490 deg. C. Above this temperature the compound decomposes to SeO{sub 2}(g) and CuO(s). The IR spectrum shows the characteristic bands of the (SeO{sub 3}){sup 2-} oxoanion. In the diffuse reflectance spectrum two intense absorptions characteristic of the Cu(II) cations in five-coordination are observed. The ESR spectra are isotropic from room temperature to 5 K, with g = 2.11(2). The thermal evolution of the intensity and line width of the signals suggest a ferromagnetic transition in the 50-45 K range. Magnetic measurements, at low temperatures, confirm the existence of a ferromagnetic transition with a critical temperature of 55 K.

  5. One-pot hydrothermal synthesis of CuBi co-doped mesoporous zeolite Beta for the removal of NOx by selective catalytic reduction with ammonia

    PubMed Central

    Xie, Zhiguo; Zhou, Xiaoxia; Wu, Huixia; Chen, Lisong; Zhao, Han; Liu, Yan; Pan, Linyu; Chen, Hangrong

    2016-01-01

    A series of CuBi co-doped mesoporous zeolite Beta (CuxBiy-mBeta) were prepared by a facile one-pot hydrothermal treatment approach and were characterized by XRD, N2 adsorption-desorption, TEM/SEM, XPS, H2-TPR, NH3-TPD and in situ DRIFTS. The catalysts CuxBiy-mBeta were applied to the removal of NOx by selective catalytic reduction with ammonia (NH3-SCR), especially the optimized Cu1Bi1-mBeta achieved the high efficiency for the removal of NOx and N2 selectivity, superior water and sulfur resistance as well as good durability. The excellent catalytic performance could be attributed to the acid sites of the support and the synergistic effect between copper and bismuth species. Moreover, in situ DRIFTS results showed that amides NH2 and NH4+ generated from NH3 adsorption could be responsible for the high selective catalytic reduction of NOx to N2. In addition, a possible catalytic reaction mechanism on Cu1Bi1-mBeta for the removal of NOx by NH3-SCR was proposed for explaining this catalytic process. PMID:27445009

  6. Hydrothermal synthesis of (C6N2H14)2(UVI2UIVO4F12), a mixed-valent one-dimensional uranium oxyfluoride.

    PubMed

    Allen, S; Barlow, S; Halasyamani, P S; Mosselmans, J F; O'Hare, D; Walker, S M; Walton, R I

    2000-08-21

    A new hybrid organic-inorganic mixed-valent uranium oxyfluoride, (C6N2H14)2(U3O4F12), UFO-17, has been synthesized under hydrothermal conditions using uranium dioxide as the uranium source, hydrofluoric acid as mineralizer, and 1,4-diazabicyclo[2.2.2]octane as template. The single-crystal X-ray structure was determined. Crystals of UFO-17 belonged to the orthorhombic space group Cmcm (no. 63), with a = 14.2660(15) A, b = 24.5130(10) A, c = 7.201(2) A, and Z = 4. The structure reveals parallel uranium-containing chains of two types: one type is composed of edge-sharing UO2F5 units; the other has a backbone of edge-sharing UF8 units, each sharing an edge with a pendant UO2F5 unit. Bond-valence calculations suggest the UF8 groups contain UIV, while the UO2F5 groups contain UVI. EXAFS data give results consistent with the single-crystal X-ray structure determination, while comparison of the uranium LIII-edge XANES of UFO-17 with that of related UIV and UVI compounds supports the oxidation-state assignment. Variable-temperature magnetic susceptibility measurements on UFO-17 and a range of related hybrid organic-inorganic uranium(IV) and uranium(VI) fluorides and oxyfluorides further support the formulation of UFO-17 as a mixed-valent UIV/UVI compound.

  7. Hydrothermal Synthesis of TiO2@SnO2 Hybrid Nanoparticles in a Continuous-Flow Dual-Stage Reactor.

    PubMed

    Hellstern, Henrik L; Bremholm, Martin; Mamakhel, Aref; Becker, Jacob; Iversen, Bo B

    2016-03-08

    TiO2@SnO2 hybrid nanocomposites were successfully prepared in gram scale using a dual-stage hydrothermal continuous-flow reactor. Temperature and pH in the secondary reactor were found to selectively direct nucleation and growth of the secondary material into either heterogeneous nanocomposites or separate intermixed nanoparticles. At low pH, 2 nm rutile SnO2 nanoparticles were deposited on 9 nm anatase TiO2 particles; the presence of TiO2 was found to suppress formation of larger SnO2 particles. At high pH SnO2 formed separate particles and no deposition on TiO2 was observed. Ball-milling of TiO2 and SnO2 produced no TiO2@SnO2 composites. This verifies that the composite particles must be formed by nucleation and growth of the secondary precursor on the TiO2 . High concentration of secondary precursor led to formation of TiO2 particles embedded in aggregates of SnO2 nanoparticles. The results demonstrate how nanocomposites may be produced in high yield by green chemistry.

  8. AlOOH-reduced graphene oxide nanocomposites: one-pot hydrothermal synthesis and their enhanced electrochemical activity for heavy metal ions.

    PubMed

    Gao, Chao; Yu, Xin-Yao; Xu, Ren-Xia; Liu, Jin-Huai; Huang, Xing-Jiu

    2012-09-26

    This work described the preparation, characterization, and electrochemical behavior toward heavy metal ions of the AlOOH-reduced graphene oxide nanocomposites. This new material was synthesized through a green one-pot hydrothermal method. The morphologic and structure of the nanocomposites were characterized using atomic force microscopy, X-ray diffraction, Raman spectroscopy, X-ray photoemission spectroscopy, Fourier transform-infrared spectroscopy, and transmission electron microscopy. Electrochemical properties were characterized by cyclic voltammetry and electrochemical impedance spectroscopy. The chemical and electrochemical parameters that have influence on deposition and stripping of metal ions, such as pH value, deposition potential, and deposition time, were also studied. Due to the strong affinity of AlOOH to heavy metal ions and the fast electron-transfer kinetics of graphene, the combination of solid-phase extraction and stripping voltammetric analysis allowed fast and sensitive determination of Cd(II) and Pb(II) in drinking water, making these new nanocomposites promising candidates for practical applications in the fields of detecting heavy metal ions. Most importantly, these new nanocomposites may possess many unknown properties waiting to be explored.

  9. Metal-organic and supramolecular networks driven by 5-chloronicotinic acid: Hydrothermal self-assembly synthesis, structural diversity, luminescent and magnetic properties

    NASA Astrophysics Data System (ADS)

    Gao, Zhu-Qing; Li, Hong-Jin; Gu, Jin-Zhong; Zhang, Qing-Hua; Kirillov, Alexander M.

    2016-09-01

    Four new crystalline solids, namely [Co2(μ2-5-Clnic)2(μ3-5-Clnic)2(μ2-H2O)]n (1), [Co(5-Clnic)2(H2O)4]·2(5-ClnicH) (2), [Pb(μ2-5-Clnic)2(phen)]n (3), and [Cd(5-Clnic)2(phen)2]·3H2O (4) were generated by hydrothermal self-assembly methods from the corresponding metal(II) chlorides, 5-chloronicotinic acid (5-ClnicH) as a principal building block, and 1,10-phenanthroline (phen) as an ancillary ligand (optional). All the products 1-4 were characterized by IR spectroscopy, elemental analysis, thermogravimetric (TGA), powder X-ray diffraction (PXRD) and single-crystal X-ray diffraction. Their structures range from an intricate 3D metal-organic network 1 with the 3,6T7 topology to a ladder-like 1D coordination polymer 3 with the 2C1 topology, whereas compounds 2 and 4 are the discrete 0D monomers. The structures of 2 and 4 are further extended (0D→2D or 0D→3D) by hydrogen bonds, generating supramolecular networks with the 3,8L18 and ins topologies, respectively. Synthetic aspects, structural features, thermal stability, magnetic (for 1) and luminescent (for 3 and 4) properties were also investigated and discussed.

  10. Rapid microwave hydrothermal synthesis of ZnGa2O4 with high photocatalytic activity toward aromatic compounds in air and dyes in liquid water

    NASA Astrophysics Data System (ADS)

    Sun, Meng; Li, Danzhen; Zhang, Wenjuan; Chen, Zhixin; Huang, Hanjie; Li, Wenjuan; He, Yunhui; Fu, Xianzhi

    2012-06-01

    ZnGa2O4 was synthesized from Ga(NO3)3 and ZnCl2 via a rapid and facile microwave-assisted hydrothermal method. The photocatalytic properties of the as-prepared ZnGa2O4 were evaluated by the degradation of pollutants in air and aqueous solution under ultraviolet (UV) light illumination. The results demonstrated that ZnGa2O4 had exhibited efficient photocatalytic activities higher than that of commercial P25 (Degussa Co.) in the degradation of benzene, toluene, and ethylbenzene, respectively. In the liquid phase degradation of dyes (methyl orange, Rhodamine B, and methylene blue), ZnGa2O4 has also exhibited remarkable activities higher than that of P25. After 32 min of UV light irradiation, the decomposition ratio of methyl orange (10 ppm, 150 mL) over ZnGa2O4 (0.06 g) was up to 99%. The TOC tests revealed that the mineralization ratio of MO (10 ppm, 150 mL) was 88.1% after 90 min of reaction. A possible mechanism of the photocatalysis over ZnGa2O4 was also proposed.

  11. A facile one-pot hydrothermal synthesis of β-MnO2 nanopincers and their catalytic degradation of methylene blue

    NASA Astrophysics Data System (ADS)

    Cheng, Gao; Yu, Lin; Lin, Ting; Yang, Runnong; Sun, Ming; Lan, Bang; Yang, Lili; Deng, Fangze

    2014-09-01

    Branched β-MnO2 bipods with novel nanopincer morphology were prepared by a facile one-pot hydrothermal method via a redox reaction between NaClO3 and MnSO4 in sulfuric acid solution without using any surfactants or templates. The products were characterized in detail by various techniques including X-ray powder diffraction, Raman spectroscopy, X-ray photoelectron spectroscopy, surface area analyzer, field emission scanning electron microscopy and transmission electron microscopy. Results show that the obtained β-MnO2 nanopincers consist of two sharp nanorods with a diameter of 100-200 nm and a length of 1-2 μm. The concentration of H2SO4 solution plays an important role in controlling the crystal phase and morphology of the final product. A possible formation mechanism for the β-MnO2 nanopincers was proposed. Moreover, these β-MnO2 nanostructures exhibited better catalytic performance than the commercial MnO2 particles to decompose methyl blue (MB) in the presence of H2O2.

  12. Hydrothermal Synthesis of TiO2 Porous Hollow Nanospheres for Coating on the Photoelectrode of Dye-Sensitized Solar Cells

    NASA Astrophysics Data System (ADS)

    Madhu Mohan, Varishetty; Murakami, Kenji

    2012-02-01

    Various sizes of TiO2 hollow nanosphers were synthesized by a hydrolysis followed by the hydrothermal treatment using different water content and titanium isopropoxide (TTIP) while the remaining components such as methylamine, ethanol and acetonitrile were kept as a constant. We synthesized the various sizes of spheres, 150, 250, 400, 450, and 600 nm in diameter; those are represented as SP150, SP250, SP400, SP450, and SP600. The prepared spheres diameters were confirmed by scanning electron microscopy (SEM). These spheres were coated by using a simple spray technique with the TiO2 colloidal solution as a scattering layer for the TiO2 photoelectrode of dye-sensitized solar cells. Optical absorption measurements did not find a difference in the dye adsorption amount with and without the scattering layer. The scattering effect was observed by incident photon to current conversion efficiency (IPCE) measurements especially in the wavelength region of 550-700 nm. The current-voltage (I-V) measurements show that the scattering layer with 450 nm spheres coated on the photoelectrode gave the improved photovoltaic performances compared to other diameters of the spheres. In the present study, the best energy conversion efficiency of 9.56% was obtained for the photoelectrode with the scattering layer, while the pure photoelectrode without the layer gave 8.4%.

  13. Synthesis of LiFePO4/Li2SiO3/reduced Graphene Oxide (rGO) Composite via Hydrothermal Method

    NASA Astrophysics Data System (ADS)

    Arifin, M.; Iskandar, F.; Aimon, A. H.; Munir, M. M.; Nuryadin, B. W.

    2016-08-01

    LiFePO4 is a type of cathode active material used for lithium ion batteries. It has a high electrochemical performance. However, it suffers from certain disadvantages such as a very low intrinsic electronic conductivity and low ionic diffusion. This study was conducted to increase the conductivity of LiFePO4. We have investigated the addition of Li2SiO3 and reduced graphene oxide (rGO) to LiFePO4. The objective of this research was to synthesize LiFePO4/Li2SiO3/rGO via hydrothermal method. Fourier transform infrared spectroscopy (FTIR) measurement showed that the peaks corresponded to the vibration of LiFePO4/Li2SiO3. Further, X-ray diffraction (XRD) measurement confirmed a single phase of LiFePO4. Finally, scanning electron microscopy (SEM) images showed that rGO was distributed on the LiFePO4/Li2SiO3 structure.

  14. Hydrothermal Synthesis g-C3N4/Nano-InVO4 Nanocomposites and Enhanced Photocatalytic Activity for Hydrogen Production under Visible Light Irradiation.

    PubMed

    Hu, Bo; Cai, Fanpeng; Chen, Tianjun; Fan, Mingshan; Song, Chengjie; Yan, Xu; Shi, Weidong

    2015-08-26

    We synthesized g-C3N4/nano-InVO4 heterojunction-type photocatalyts by in situ growth of InVO4 nanoparticles onto the surface of g-C3N4 sheets via a hydrothermal process. The results of SEM and TEM showed that the obtained InVO4 nanoparticles 20 nm in size dispersed uniformly on the surface of g-C3N4 sheets, which revealed that g-C3N4 sheets was probably a promising support for in situ growth of nanosize materials. The achieved intimate interface promoted the charge transfer and inhibited the recombination rate of photogenerated electron-hole pairs, which significantly improved the photocatalytic activity. A possible growth process of g-C3N4/nano-InVO4 nanocomposites was proposed based on different mass fraction of g-C3N4 content. The obtained g-C3N4/nano-InVO4 nanocomposites could achieve effective separation of charge-hole pairs and stronger reducing power, which caused enhanced H2 evolution from water-splitting compared with bare g-C3N4 sheets and g-C3N4/micro-InVO4 composites, respectively. As a result, the g-C3N4/nano-InVO4 nanocomposite with a mass ratio of 80:20 possessed the maximum photocatalytic activity for hydrogen production under visible-light irradiation.

  15. Facile hydrothermal synthesis and characterization of Co2GeO4/r-GO@C ternary nanocomposite as negative electrode for Li-ion batteries.

    PubMed

    Subramanian, Yuvaraj; Kaliyappan, Karthikeyan; Ramakrishnan, Kalai Selvan

    2017-03-02

    Ternary nanocomposite of Co2GeO4/r-GO@C is synthesized by single step hydrothermal method followed by calcination. The XRD analysis reveals the formation of cubic structured Co2GeO4 and their corresponding functional groups identified through Raman analysis. The TEM analysis assures that uniform distribution of Co2GeO4 nanoparticles on the r-GO layers. The Galvanostatic charge-discharge (GCD) curve demonstrates that the initial discharge capacity of pristine Co2GeO4, Co2GeO4/r-GO and Co2GeO4/r-GO@C composite is 1400, 1284 and 1594mAhg(-1) at 50mAg(-1), respectively. The cycling stability curve shows the specific capacity of 609, 970 and 1180mAhg(-1) for pristine, Co2GeO4/r-GO and Co2GeO4/r-GO@C composite, respectively over 15 cycles. The ternary composite of Co2GeO4/r-GO@C delivers the discharge capacity of 323mAhg(-1) at high current density of 1Ag(-1) over 500 cycles with capacity retention of 71%. The rate capability curve indicates that Co2GeO4/r-GO@C composite shows the better rate capability.

  16. Hydrothermal synthesis and characterization of a two-dimensional piperazinium cobalt-zinc phosphate via a metastable one-dimensional phase

    NASA Astrophysics Data System (ADS)

    Torre-Fernández, Laura; Khainakova, Olena A.; Espina, Aránzazu; Amghouz, Zakariae; Khainakov, Sergei A.; Alfonso, Belén F.; Blanco, Jesús A.; García, José R.; García-Granda, Santiago

    2015-05-01

    A two-dimensional piperazinium cobalt-zinc phosphate, formulated as (C4N2H12)1.5(Co0.6Zn0.4)2(HPO4)2(PO4)·H2O (2D), was synthesized under hydrothermal conditions. The crystal structure was determined using single-crystal X-ray diffraction data (monoclinic P21/c, a=8.1165(3) Å, b=26.2301(10) Å, c=8.3595(4) Å, and β=110.930(5)°) and the hydrogen atom positions were optimized by DFT calculations. A single-crystal corresponding to one-dimensional metastable phase, (C4N2H12)Co0.3Zn0.7(HPO4)2·H2O (1D), was also isolated and the crystal structure was determined (monoclinic P21/c, a=8.9120(6) Å, b=14.0290(1) Å, c=12.2494(5) Å, and β=130.884(6)°). The bulk was characterized by chemical (C-H-N) analysis, powder X-ray diffraction (PXRD), powder X-ray thermodiffractometry (HT-XRD), transmission electron microscopy (STEM(DF)-EDX and EFTEM), and thermal analysis (TG/SDTA-MS), including activation energy data of its thermal decomposition. The magnetic susceptibility and magnetization measurements show no magnetic ordering down to 4 K.

  17. Ionic liquid-assisted hydrothermal synthesis of dendrite-like NaY(MoO4)2:Tb3+ phosphor

    NASA Astrophysics Data System (ADS)

    Tian, Yue; Chen, Baojiu; Tian, Bining; Sun, Jiashi; Li, Xiangping; Zhang, Jinsu; Cheng, Lihong; Zhong, Haiyang; Zhong, Hua; Meng, Qingyu; Hua, Ruinian

    2012-07-01

    Micro-sized NaY(MoO4)2:Tb3+ phosphors with dendritic morphology was synthesized by a ionic liquid-assisted hydrothermal process. X-ray diffraction (XRD) indicated that the as-prepared product is pure tetragonal phase of NaY(MoO4)2. Field emission scanning electron microscopy (FE-SEM) images showed that the as-prepared NaY(MoO4)2:Tb3+ phosphors have dendritic morphology. The photoluminescent (PL) spectra displayed that the as-prepared NaY(MoO4)2:Tb3+ phosphors show a stronger green emission with main emission wavelength 545 nm corresponding to the 5D4→7F5 transition of Tb3+ ion, and the optimal Tb3+ doping concentration for obtaining maximum emission intensity was confirmed to be 10 mol%. Based on Van Uitert's and Dexter's models the electric dipole-dipole (D-D) interaction was confirmed to be responsible for the concentration quenching of 5D4 fluorescence of Tb3+ in the NaY(MoO4)2:Tb3+ phosphors. The intrinsic radiative transition lifetime of 5D4 level is found to be 0.703 ms.

  18. Hydrothermal synthesis and photocatalytic performance of hierarchical Bi{sub 2}MoO{sub 6} microspheres using BiOI microspheres as self-sacrificing templates

    SciTech Connect

    Xu, Ming; Zhang, Wei-De

    2015-07-15

    Bi{sub 2}MoO{sub 6} hierarchical microspheres were successfully prepared through phase transformation from BiOI microspheres with the assistance of sodium citrate under hydrothermal condition. The possible formation mechanism for the conversion of BiOI to Bi{sub 2}MoO{sub 6} is discussed here. After being annealed at 300 °C for 2 h, the obtained Bi{sub 2}MoO{sub 6} microspheres exhibited remarkably enhanced photocatalytic activity towards the degradation of rhodamine B and phenol. The superior catalytic performance can be attributed to its larger surface area and higher crystallinity. In addition, Bi{sub 2}MoO{sub 6} microspheres are stable during the degradation reaction and can be used repeatedly. - Graphical abstract: Bi{sub 2}MoO{sub 6} hierarchical microspheres were successfully prepared through a facile partial anion exchange strategy using BiOI microspheres as self-sacrificing templates. The Bi{sub 2}MoO{sub 6} microspheres show high visible light photocatalytic activity. - Highlights: • Bi{sub 2}MoO{sub 6} microspheres were prepared via self-sacrificing template anion exchange. • Sodium citrate-assisted anion exchange for preparation of Bi{sub 2}MoO{sub 6} photocatalyst. • Bi{sub 2}MoO{sub 6} catalysts show high visible light photocatalytic activity.

  19. One-pot synthesis of carbon-coated SnO2 nano-composite using hydrothermal method for lithium ion battery application.

    PubMed

    Lee, Hye Rim; Kim, Hwan Jin; Park, Jong Hyeok; Yoon, Dae Ho

    2013-06-01

    Carbon-coated SnO2 nano-composite was synthesized by using a hydrothermal method in a one step process with sizes of 1 to 3 microm. The carbon-coated SnO2 nano-composite was easily obtained by changing firing atmosphere from air to argon (600 degrees C for 3 hours). The carbon-coating thickness and size of the SnO2 nanoparticles in carbon-coated SnO2 nano-composite were confirmed through a high-resolution transmission electron microscopy (HRTEM) as 40 and 5 nm, respectively. Carbon-coating and particle size affect to the capacity retention property. Carbon-coated and non carbon-coated samples were investigated as anode materials. It was confirmed that the non carbon-coated SnO2 nano-composite had a 718 mA h/g initial charge capacity, 91% reached to theoretical value of SnO2 (790 mA h/g), while the carbon-coated SnO2 nano-composite had an excellent capacity retention of 89.6% after 70 cycles (10.88% for non carbon-coated SnO2 nano-composite).

  20. Biomolecule-controlled hydrothermal synthesis of C-N-S-tridoped TiO2 nanocrystalline photocatalysts for NO removal under simulated solar light irradiation.

    PubMed

    Wang, Yawen; Huang, Yu; Ho, Wingkei; Zhang, Lizhi; Zou, Zhigang; Lee, Shuncheng

    2009-09-30

    In this study, C-N-S-tridoped titanium dioxide (TiO(2)) nanocrystals were synthesized by using a facile hydrothermal method in the presence of a biomolecule l-cysteine. This biomolecule could not only serve as the common source for the carbon, sulfur and nitrogen tridoping, but also could control the final crystal phases and morphology. The resulting materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), nitrogen adsorption and UV-vis diffuse reflectance spectroscopy. XPS analysis revealed that S was incorporated into the lattice of TiO(2) through substituting oxygen atoms, N might coexist in the forms of N-Ti-O and Ti-O-N in tridoped TiO(2) and most C could form a mixed layer of carbonate species deposited on the surface of TiO(2) nanoparticles. The photocatalytic activities of the samples were tested on the removal of NO at typical indoor air level in a flow system under simulated solar light irradiation. The tridoped TiO(2) samples showed much higher removal efficiency than commercial P25 and the undoped counterpart photocatalyst. The enhanced visible light photocatalytic activity of C-N-S-tridoped TiO(2) nanocrystals was explained on the basis of characterizations. The possible formation process of the monodispersed C-N-S-tridoped anatase TiO(2) nanocrystals was also proposed. This study provides a new method to prepare visible light active TiO(2) photocatalyst.