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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 synthesis of amino acids

    NASA Astrophysics Data System (ADS)

    Marshall, William L.

    1994-05-01

    This study presents further evidence that amino acids can be synthesized rapidly in hydrothermal solutions from reactants that may have been present in primitive environments. Aqueous NH 4HCO 3 solutions were reacted with C 2H 2, H 2, and O 2 (formed in situ from CaC 2, Ca, and H 2O 2) at 200-275°C over 0.2-2 h periods to synthesize several amino acids and abundant amines. These amino acid and amine producing reactions were not observed to occur below 150°C. Amino acids and amines also were synthesized at 210°C from solutions of NH 4OH, HCHO, NaCN, and H 2. When NH 4OH was replaced by NH 4HCO 3, the syntheses predominantly confirmed the recent results of RENNET et al. (1992). Additionally, amino acids and amines were observed to form by reactions among NH 4OH, HCHO, and H 2 at hydrothermal conditions, essentially confirming the results of FOX and WINDSOR (1970). Inclusion of both carbonate and O 2 in these latter solutions greatly enhanced the production rate of amino acids. The amines synthesized hydrothermally could be significant if they are precursors in the amino acid syntheses either at hydrothermal or later at lower temperatures. These observations provide additional input to the current questions of synthesis, stability, and decomposition of amino acids at hydrothermal conditions, and their possible relevance to the origin of life.

  4. 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

  5. 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.

  6. 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.

  7. 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.

  8. 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

  9. 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.

  10. 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.

  11. Hydrothermal synthesis of bismuth germanium oxide

    DOEpatents

    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.

  12. 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.

  13. Hydrothermal Synthesis of Dicalcium Silicate Based Cement

    NASA Astrophysics Data System (ADS)

    Dutta, N.; Chatterjee, A.

    2017-06-01

    It is imperative to develop low energy alternative binders considering the large amounts of energy consumed as well as carbon dioxide emissions involved in the manufacturing of ordinary Portland cement. This study is on the synthesis of a dicalcium silicate based binder using a low temperature hydrothermal route.The process consists of synthesizing an intermediate product consisting of a calcium silicate hydrate phase with a Ca:Si ratio of 2:1 and further thermal treatment to produce the β-Ca2SiO4 (C2S) phase.Effect of various synthesis parameters like water to solid ratio, dwell time and temperature on the formation of the desired calcium silicate hydrate phase is reported along with effect of heating conditions for formation of the β-C2S phase. Around 77.45% of β-C2S phase was synthesized by thermal treatment of the intermediate phase at 820°C.

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. Hydrothermal synthesis of vanadium pentoxide nanowires

    SciTech Connect

    Kumar, J. Santhosh; Thangadurai, P. E-mail: thangadurai.p@gmail.com

    2016-05-23

    Nanowires of V{sub 2}O{sub 5} were prepared via hydrothermal route using NH{sub 4}VO{sub 3} as precursor in the presence of sulfuric acid at 120°C for 24 h. This synthesis process is free of any templates and reducing agents. Thermal analysis showed a phase change at 350°C and the samples were annealed at 500°C. The XRD analysis showed the monoclinic phase for the as-prepared and orthorhombic phase of V{sub 2}O{sub 5} when annealed at 500°C. Characteristic Raman peaks also expressed the same structural features. Microstructure analysis by SEM showed the nanowire structure of V{sub 2}O{sub 5} with thickness in the range of 20–50 nm and length in micrometers. The possible mechanisms of formation of the nanowires were schematically explained based on the layered structure of V{sub 2}O{sub 5}.

  20. 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.

  1. 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.

  2. Hydrothermal synthesis as a route to mineralogically-inspired structures.

    PubMed

    McMillen, Colin D; Kolis, Joseph W

    2016-02-21

    The use of high temperature hydrothermal reactions to prepare crystals having mineralogically-related structures is described. Complex naturally occurring minerals can have fascinating structures and exhibit important features like low dimensionality, noncentrosymmetry, or ion channels that can provide excellent guideposts for the designed synthesis of new materials. Actual minerals, even though they may have intriguing physical properties, are often unsuitable for study because of the persistent impurities inevitably present in natural samples. Hydrothermal fluids at relatively high temperatures provide access to large, high quality single crystals of structures with mineral-like structures. This enables the study of physical properties like ionic conduction, magnetic spin frustration and non-linear optical behavior. Some fundamental considerations of the hydrothermal technique are discussed in the context of synthesizing mineralogically-inspired materials. The metal vanadates provide a surprisingly rich and diversified range of compounds and are selected to illustrate many of the concepts described here. A series of low dimensional mineral analogs featuring isolated units, chains, and layers have been prepared in the laboratory as large single crystals using a high temperature hydrothermal synthetic methods, and their physical properties are under investigation. The metal silicates are also highlighted as another promising field of exploration, since their hydrothermal synthesis surprisingly lags behind the enormous literature of the natural silicate minerals. The introduction of heteroelements, such as boron to make borosilicates, appears to also open the door to additional new materials. Many of these new materials have direct equivalents in the mineral kingdom, while others have no known analogs but are reminiscent of minerals and can be classified in the same ways. From these initial results there appears to be a very rich vein of synthetic minerals waiting

  3. Zeolite synthesis from oil palm ash using hydrothermal treatment

    NASA Astrophysics Data System (ADS)

    Pa, Faizul Che; Chik, Abdullah

    2017-04-01

    The treated oil palm ash and kaolin powder are used as the starting material for the synthesis of zeolites materials. The method chose for the zeolites conversion is alkaline hydrothermal treatment. The chemical composition and crystalline phases of treated oil palm ash and as-synthesized samples were characterized and studied. From the analysis, the treated palm ash was a fertile source of silica and exists as quartz phase. The zeolite synthesis was carried out under hydrothermal conditions by activation with sodium hydroxide (NaOH) solution. The results indicated that the synthesized zeolite products obtained from 2 M NaOH concentrations contain zeolite gismondine as major constituent phase, whereas quartz was found as minor phase. The outcomes have significant motivation for the production of zeolites by using low cost material such as treated palm ash.

  4. Hydrothermal Synthesis of Metal Oxide Nanoparticles in Supercritical Water

    PubMed Central

    Hayashi, Hiromichi; Hakuta, Yukiya

    2010-01-01

    This paper summarizes specific features of supercritical hydrothermal synthesis of metal oxide particles. Supercritical water allows control of the crystal phase, morphology, and particle size since the solvent's properties, such as density of water, can be varied with temperature and pressure, both of which can affect the supersaturation and nucleation. In this review, we describe the advantages of fine particle formation using supercritical water and describe which future tasks need to be solved. PMID:28883312

  5. 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.

  6. 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

  7. 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.

  8. 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.

  9. 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.

  10. Monodispersed Ultrafine Zeolite Crystal Particles by Microwave Hydrothermal Synthesis

    SciTech Connect

    Hu, Michael Z.; Harris, Michael Tyrone; Khatri, Lubna

    2008-01-01

    Microwave hydrothermal synthesis of zeolites is reviewed. Monodispersed ultrafine crystal particles of zeolite (Silicalite-1) have been synthesized in batch reactor vessels by microwave irradiation heating of aqueous basic silicate precursor solutions with tetra propyl ammonium hydroxide as the templating molecule. The effects of major process parameters (such as synthesis temperature, microwave heating rate, volume ratio (i.e., the volume of the initial synthesis solution over the total volume of the reactor vessel), and synthesis time on the zeolite particle characteristics are studied using a computer-controlled microwave reactor system that allows real-time monitoring and control of reaction medium temperature. The changes in the morphology, size and crystal structure of the particles are investigated using scanning electron microscope, dynamic light scattering, X-ray diffraction, and BET surface analysis. We have found that the synthesis temperature, volume ratio, and heating rate play a significant role in controlling the particle size, uniformity, and morphology. Microwave processing has generated new morphologies of zeolite particles (i.e., uniform block-shaped particles that contain mixed gel-nanocrystallites and agglomerated crystal particles) that could not be made by a conventional hydrothermal process. At higher synthesis temperature and lower volume ratio, irregular block-shaped particles were produced, whereas increasing the volume ratio promoted the formation of monodispersed single-crystal particles with uniform shape. Our results clearly demonstrate that faster microwave heating is advantageous to enhance the zeolite crystallization kinetics and produces larger-size crystal particles in shorter time. In addition, zeolite crystallization mechanisms, depending on the microwave heating rate, were also discussed.

  11. Synthesis of KNbO3 nanorods by hydrothermal method.

    PubMed

    Wang, Guozhong; Yu, Yingda; Grande, Tor; Einarsrud, Mari-Ann

    2009-02-01

    Potassium niobate (KNbO3) nanorods were prepared from Nb2O5 powder by hydrothermal synthesis in KOH solution at 180 degrees C for 48 h using sodium dodecyl sulfate surfactant. The products were characterized by X-ray diffraction as well as scanning and transmission electron microscopy. The KNbO3 nanorods were shown to have orthorhombic crystal structure and were 100-300 nm in diameter and up to 5 microm long. The addition of surfactant changed the product morphology from agglomerated particles to nanorods. A possible mechanism for the formation of the KNbO3 nanorods is briefly discussed.

  12. 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.

  13. 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

  14. 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.

  15. Continuous Hydrothermal Synthesis of Inorganic Nanoparticles: Applications and Future Directions.

    PubMed

    Darr, Jawwad A; Zhang, Jingyi; Makwana, Neel M; Weng, Xiaole

    2017-09-13

    Nanomaterials are at the leading edge of the emerging field of nanotechnology. Their unique and tunable size-dependent properties (in the range 1-100 nm) make these materials indispensable in many modern technological applications. In this Review, we summarize the state-of-art in the manufacture and applications of inorganic nanoparticles made using continuous hydrothermal flow synthesis (CHFS) processes. First, we introduce ideal requirements of any flow process for nanoceramics production, outline different approaches to CHFS, and introduce the pertinent properties of supercritical water and issues around mixing in flow, to generate nanoparticles. This Review then gives comprehensive coverage of the current application space for CHFS-made nanomaterials including optical, healthcare, electronics (including sensors, information, and communication technologies), catalysis, devices (including energy harvesting/conversion/fuels), and energy storage applications. Thereafter, topics of precursor chemistry and products, as well as materials or structures, are discussed (surface-functionalized hybrids, nanocomposites, nanograined coatings and monoliths, and metal-organic frameworks). Later, this Review focuses on some of the key apparatus innovations in the field, such as in situ flow/rapid heating systems (to investigate kinetics and mechanisms), approaches to high throughput flow syntheses (for nanomaterials discovery), as well as recent developments in scale-up of hydrothermal flow processes. Finally, this Review covers environmental considerations, future directions and capabilities, along with the conclusions and outlook.

  16. 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.

  17. 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. Copyright © 2015 Elsevier Inc. All rights reserved.

  18. Performance improvement of miniaturized ZnO nanowire accelerometer fabricated by refresh hydrothermal synthesis.

    PubMed

    Song, Sangho; Kim, Hyun Chan; Kim, Jung Woong; Kim, Debora; Kim, Jaehwan

    2017-09-01

    Miniaturized accelerometers are necessary for evaluating the performance of small devices, such as haptics, robotics and simulators. In this study, we fabricated miniaturized accelerometers using well-aligned ZnO nanowires. The layer of ZnO nanowires is used for active piezoelectric layer of the accelerometer, and copper was chosen as a head mass. Seedless and refresh hydrothermal synthesis methods were conducted to grow ZnO nanowires on the copper substrate and the effect of ZnO nanowire length on the accelerometer performance was investigated. The refresh hydrothermal synthesis exhibits longer ZnO nanowires, 12 µm, than the seedless hydrothermal synthesis, 6 µm. Performance of the fabricated accelerometers was verified by comparing with a commercial accelerometer. The sensitivity of the fabricated accelerometer by the refresh hydrothermal synthesis is shown to be 37.7 pA g(-1), which is about 30 times larger than the previous result.

  19. 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.

  20. 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

  1. 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

  2. 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

  3. 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.

  4. Hydrothermal Synthesis of (K,Na)NbO3 Particles

    NASA Astrophysics Data System (ADS)

    Zhang, Fan; Han, Lu; Bai, Shan; Sun, Tiedong; Karaki, Tomoaki; Adachi, Masatoshi

    2008-09-01

    (K,Na)NbO3 (KNN) particles were successfully prepared by hydrothermal synthesis. The results showed that Na+ reacted more readily with Nb to form NaNbO3 than K+. For the purpose of obtaining KNN particles with K/Na=1, a mixed alkaline solution with K+/Na+ ratios ranging from 3.5/1 to 4/1 was required as a starting solution. The morphology and size of KNN particles synthesized strongly depended on K/Na ratio in the KNN particles. The KNN particles synthesized from the starting alkaline solution with K+/Na+=3.5/1 were the smallest with a pelletlike morphology affected by NaNbO3- and KNbO3-based particles. Surfactants such as sodium dodecylbenzenesulfonate (SDBS) and sodium hexametaphosphate (SH) were used to synthesize well dispersed and small KNN particles. Platelike KNN particles with 100 nm thickness and 1.5 µm width were obtained in this study.

  5. Synthesis of ultrafine layered double hydroxide (LDHs) nanoplates using a continuous-flow hydrothermal reactor.

    PubMed

    Wang, Qiang; Tang, Selina Vi Yu; Lester, Edward; O'Hare, Dermot

    2013-01-07

    We report a novel continuous-flow hydrothermal method for the synthesis of layered double hydroxide (LDH) nanoplates. The precursor solutions may be fed to the reactor so that the production of LDHs occurs in a continuous mode. By control of the synthesis temperature, pressure and contact time, the synthesis of LDH nanoplates can be tuned with constant and consistent product quality. This very general and simple approach shows high potential for commercial scale-up.

  6. Synthesis and characterization of nanosized MnZn ferrites via a modified hydrothermal method

    NASA Astrophysics Data System (ADS)

    Li, Mingling; Liu, Xiansong; Xu, Taotao; Nie, Yu; Li, Honglin; Zhang, Cong

    2017-10-01

    Nanosized MnZn ferrite particles, with narrow size distribution, regular morphology and high saturation magnetization have been synthesized via a modified hydrothermal method. This modified hydrothermal method involves a chemical co-precipitation of hydroxides under a vacuum condition using potassium hydroxide as precipitating agent, followed by a separate hydrothermal process. The microstructure and magnetic properties of the synthesized nanoparticles were investigated by X-ray diffraction (XRD), Raman spectroscopy, field emission scanning electron microscopy (FESEM), high resolution transmission electron microscopy (HRTEM) and vibrating sample magnetometer (VSM). The effects of different synthesis conditions (excess ratio of precipitating agent and hydrothermal reaction time) on the microstructure and magnetic properties of the as-synthesized nanoparticles were discussed. The magnetic measurements indicated that the obtained samples were superparamagnetic in nature at room temperature. Moreover, the MnZn ferrite nanoparticles with excellent magnetic performance could be synthesized at 180 °C for a short reaction time (3 h).

  7. 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.

  8. 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...

  9. Lipid Synthesis Under Hydrothermal Conditions by Fischer- Tropsch-Type Reactions

    NASA Astrophysics Data System (ADS)

    McCollom, Thomas M.; Ritter, Gilles; Simoneit, Bernd R. T.

    1999-03-01

    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 on 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 °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.

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

    PubMed

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

    1999-03-01

    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.

  11. 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...

  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. 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.

  14. The potential for prebiotic synthesis in hydrothermal systems. [Abstract only

    NASA Technical Reports Server (NTRS)

    Ferris, James P.

    1994-01-01

    Contemporary hydrothermal systems provide a reducing environment where organic compounds are formed and may react to generate the molecules used in the first living systems. The organic compounds percolate through mineral assemblages at a variety of temperatures so the proposed synthetic reactions are driven by heat and catalyzed by minerals (Ferris, 1992). Some examples of potential prebiotic reactions are discussed.

  15. 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.

  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. 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.

  18. 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.

  19. 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.

  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. Evaluating Experimental Artifacts in Hydrothermal Prebiotic Synthesis Experiments

    NASA Astrophysics Data System (ADS)

    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.

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. Hydrothermal synthesis of nanosize phases based on non-ferrous and noble metals

    SciTech Connect

    Tupikova, E. N. Platonov, I. A. Lykova, T. N.

    2016-04-13

    Research is devoted to reactions of binary complexes containing noble (platinum, palladium) and non-ferrous (cobalt, chrome) metals. Reactions proceed under hydrothermal conditions by the autoclave technique. Initials complexes and products of autoclave thermolysis were characterized by the FT-IR spectroscopy, the transmission electron microscopy (TEM) and the energy-dispersive X-ray spectroscopy (EDX). Comparative catalytic experiments in the test reaction were conducted. The obtained results can form the basis of new methods of nanosize multicomponent phases synthesis under hydrothermal conditions.

  7. Hydrothermal synthesis of nanosize phases based on non-ferrous and noble metals

    NASA Astrophysics Data System (ADS)

    Tupikova, E. N.; Platonov, I. A.; Lykova, T. N.

    2016-04-01

    Research is devoted to reactions of binary complexes containing noble (platinum, palladium) and non-ferrous (cobalt, chrome) metals. Reactions proceed under hydrothermal conditions by the autoclave technique. Initials complexes and products of autoclave thermolysis were characterized by the FT-IR spectroscopy, the transmission electron microscopy (TEM) and the energy-dispersive X-ray spectroscopy (EDX). Comparative catalytic experiments in the test reaction were conducted. The obtained results can form the basis of new methods of nanosize multicomponent phases synthesis under hydrothermal conditions.

  8. Hydrothermal synthesis and morphology of Ga-bearing tourmaline

    NASA Astrophysics Data System (ADS)

    Setkova, T. V.; Balitsky, V. S.; Vereschagin, O. S.; Shapovalov, Yu. B.

    2017-04-01

    Ga-bearing tourmaline was originally synthesized in boron, boron-alkaline, and boron-fluorine hydrothermal solutions at a temperature of 600-650°C and pressure of 100 MPa as crystals of spontaneous growth and on seeds. The maximal concentration of Ga2O3 in synthetic crystals reaches 24.5 wt %. In addition to Ga-bearing tourmaline, Ga-bearing topaz crystallizes in boron-fluorine solution. Ga-bearing albite crystallizes in boron-alkaline solutions, whereas no additional phases are formed in pure boron solutions.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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

  14. 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.

  15. 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.

  16. The rapid size- and shape-controlled continuous hydrothermal synthesis of metal sulphide nanomaterials

    NASA Astrophysics Data System (ADS)

    Dunne, Peter W.; Starkey, Chris L.; Gimeno-Fabra, Miquel; Lester, Edward H.

    2014-01-01

    Continuous flow hydrothermal synthesis offers a cheap, green and highly scalable route for the preparation of inorganic nanomaterials which has predominantly been applied to metal oxide based materials. In this work we report the first continuous flow hydrothermal synthesis of metal sulphide nanomaterials. A wide range of binary metal sulphides, ZnS, CdS, PbS, CuS, Fe(1-x)S and Bi2S3, have been synthesised. By varying the reaction conditions two different mechanisms may be invoked; a growth dominated route which permits the formation of nanostructured sulphide materials, and a nucleation driven process which produces nanoparticles with temperature dependent size control. This offers a new and industrially viable route to a wide range of metal sulphide nanoparticles with facile size and shape control.Continuous flow hydrothermal synthesis offers a cheap, green and highly scalable route for the preparation of inorganic nanomaterials which has predominantly been applied to metal oxide based materials. In this work we report the first continuous flow hydrothermal synthesis of metal sulphide nanomaterials. A wide range of binary metal sulphides, ZnS, CdS, PbS, CuS, Fe(1-x)S and Bi2S3, have been synthesised. By varying the reaction conditions two different mechanisms may be invoked; a growth dominated route which permits the formation of nanostructured sulphide materials, and a nucleation driven process which produces nanoparticles with temperature dependent size control. This offers a new and industrially viable route to a wide range of metal sulphide nanoparticles with facile size and shape control. Electronic supplementary information (ESI) available: Experimental details, refinement procedure, fluorescence spectra of ZnS samples. See DOI: 10.1039/c3nr05749f

  17. 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.

  18. 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 +}.

  19. Short-time hydrothermal synthesis and delamination of ion exchangeable Mg/Ga layered double hydroxides

    SciTech Connect

    Unal, Ugur

    2007-09-15

    The hydrothermal synthesis of magnesium-gallium layered double hydroxides (Mg/Ga LDHs) was studied under static and agitated conditions. Not only well-crystallized and large-sized Mg/Ga LDHs having hexagonal morphology were obtained but also the reaction time was comparatively decreased from 24 to 2 h by means of agitation during hydrothermal synthesis. In static conditions, mainly GaOOH and magnesite phases were formed. The elemental analysis results show that the final Mg/Ga ratio is significantly different from the initial ratio. The reason was attributed to the difference in the hydrolytic behavior of Mg{sup 2+} and Ga{sup 3+}. Furthermore, the anion exchange studies with glycine, dodecyl sulfate, ferrocyanide and ferricyanide were performed to investigate the intercalation behavior of the anions into Mg/Ga LDHs. In addition, delamination of Mg/Ga LDHs was performed in formamide for the glycine exchanged forms. Large size of nanosheets thus obtained can be utilized in the fabrication of functional thin films. - Graphical abstract: Hydrothermal synthesis under agitation resulted in highly crystalline Mg/Ga LDHs slabs in a short time. The LDHs slabs were delaminated into two-dimensional nanosize sheets.

  20. 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.

  1. Hydrothermal synthesis of siderite nano-particles and characterizations

    NASA Astrophysics Data System (ADS)

    Oza, Mahatta; Joshi, M. J.

    2017-05-01

    Siderite is an iron ore in the form of ferrous carbonate (FeCO3). It finds applications in ceramics, in pig iron production, pigments in paints and in petroleum drilling fluids as a scavenger for H2S. An attempt was made to synthesize FeCO3 nano-particles by hydrothermal treatment of aqueous solution of iron sulphate, ascorbic acid, and ammonium carbonate with a molar ratio of 1:1:3, respectively, at 140˚C for 1.5 h. The synthesized powder was further characterized by different characterization techniques like powder XRD, FT-IR and TGA. The powder XRD analysis suggested the nano-crystalline nature of the sample with Hexagonal crystal system having unit cell parameters as: a = 4.691Ǻ, b = 4.691 Ǻ and c = 15.37Ǻ. The average crystallite size was found to be ̴ 10.70 nm from Scherrer's formula. FT-IR spectrum confirmed the presence of O-H, and C-O functional groups. The TGA results suggested that the material started decomposing from the beginning and showed weight loss of 32.4% at 358°C temperature. Thereafter, the sample very slowly decomposed and at the end of process sample showed weight loss of 39.5% at 900°C after giving up carbon dioxide.

  2. Hydrothermal Synthesis and Structure of Neptunium(V) Oxide

    SciTech Connect

    Forbes, Tori Z.; Burns, Peter C.; Soderholm, L. |; Skanthakumar, S.

    2007-07-01

    Single crystals of Np{sub 2}O{sub 5} have been synthesized by low-temperature hydrothermal reaction of a (NpO{sub 2}){sup +} stock solution with natural calcite crystals. The structure of Np{sub 2}O{sub 5} was solved by direct methods and refined on the basis of F{sup 2} for all unique data collected on a Bruker X-ray diffractometer equipped with an APEX II CCD detector. Np{sub 2}O{sub 5} is monoclinic, space group P2/c, with a = 8.168(2) A, b = 6.584(1) A, c = 9.3130(2) A, {beta} = 116.01(1) deg., V = 449.8(2) A{sup 3}, and Z = 1. The structure contains chains of edge-sharing neptunyl pentagonal bi-pyramids linked into sheets through cation-cation interactions with distorted neptunyl square bi-pyramids. Additional cation-cation interactions connect the sheets into a three-dimensional framework. The formation of Np{sub 2}O{sub 5} on the surface of calcite crystals has important implications for the precipitation of isolated neptunyl phases in natural aqueous systems. (authors)

  3. 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.

  4. 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

  5. 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.

  6. 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.

  7. Effect of ultrasound pretreatment on the hydrothermal synthesis of SSZ-13 zeolite.

    PubMed

    Mu, Yanyan; Zhang, Yu; Fan, Jiangyang; Guo, Cuili

    2017-09-01

    SSZ-13 zeolite has been identified as effective material for catalysts and membranes for years because of its structure, but the long crystallization time is the main obstacle for the industry application. The sonochemical-assisted method was identified as one of the potential pre-treatment methods which could reduce the formation duration of zeolites as well as other microporous and mesoporous materials. In this work, zeolite SSZ-13 was prepared by ultrasound pretreatment prior to hydrothermal crystallization. For comparison, samples by the conventional pretreatment and hydrothermal method were also prepared. The synthesized powders were characterized by XRD, SEM, BET, FTIR, NMR and TGA. The results showed that the complete crystallization of SSZ-13 synthesized by the ultrasound-assisted hydrothermal method was achieved within 72h, and much faster than conventional hydrothermal synthesis (120h). Furthermore, the ultrasound pretreatment showed very little effect on the structure properties of the final product compared with the conventional aging method. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. Hydrothermal synthesis and structure of the ordered modification of Pb 7F 12Br 2

    NASA Astrophysics Data System (ADS)

    Kubel, F.; Völlenkle, H.

    2000-05-01

    We recently discovered a disordered and ordered modification of a compound with composition Ba 7F 12Cl 2. Both modifications of the lead compound, Pb 7F 12Cl 2, can be obtained from a flux (disordered, space group (P6 3/m) or by hydrothermal growth (ordered, space group P overline6)). Needle shaped crystals of the title compound, Pb 7F 12Br 2, were found to form during hydrothermal synthesis. The structure was refined in the hexagonal space group P overline6 to R=0.028 for 829 reflections and 45 parameters. Lattice parameters are a= b=1035.6(2) pm and c=402.24(8) pm with Z=1.

  15. 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.

  16. 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)

  17. 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

  18. 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.

  19. 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.

  20. 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

  1. Precursor-induced template free hydrothermal synthesis of faujasite and its application in catalytic pyrolysis

    NASA Astrophysics Data System (ADS)

    Rahman, Mati ur; Ullah Wazir, Hameed; Khan, Matiullah; Nosheen, Shaneela; Rahman, Sami Ur; Ullah, Asad

    2017-05-01

    This paper reports the fabrication of Faujasite type zeolite by template free hydrothermal method without using structural directing agent (SDA) and seed source. The effect of various modifiers during synthesis process such as mineralization source and solvent is investigated. The as-prepared materials are characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR) and thermo gravimetric analysis (TGA). It is found that microwave process, solvent, and mineralization source significantly impact the morphology, pore structure, crystallization behavior and nature of resulting zeolites.

  2. Hydrothermal Synthesis of BaBe2Si2O7

    NASA Astrophysics Data System (ADS)

    Maeda, Masaki; Uehara, Toshio; Sato, Hidetaka; Ikeda, Takuro

    1991-09-01

    The growth conditions of BaBe2Si2O7 crystals in the hydrothermal synthesis method were investigated. Experiments were carried out to determine P-T phase diagrams and reaction phase diagrams. The optimum conditions in the present experiments were 1) pressure: 500 bar, 2) temperature: 385°C, 3) temperature gradient: 15°C, 4) KOH concentration in water: 3 mol/1, 5) baffle-opening-area ratio: 15%, and 6) growth time: 60 h. Under these growth conditions, transparent single crystals of platelet shape (0.2 mm in edge) were obtained on the ceramic seeds.

  3. 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.

  4. 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.

  5. 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.

  6. Hydrothermal synthesis of highly nitrogen-doped few-layer graphene via solid–gas reaction

    SciTech Connect

    Liang, Xianqing; Zhong, Jun; Shi, Yalin; Guo, Jin; Huang, Guolong; Hong, Caihao; Zhao, Yidong

    2015-01-15

    Highlights: • A novel approach to synthesis of N-doped few-layer graphene has been developed. • The high doping levels of N in products are achieved. • XPS and XANES results reveal a thermal transformation of N bonding configurations. • The developed method is cost-effective and eco-friendly. - Abstract: Nitrogen-doped (N-doped) graphene sheets with high doping concentration were facilely synthesized through solid–gas reaction of graphene oxide (GO) with ammonia vapor in a self-designed hydrothermal system. The morphology, surface chemistry and electronic structure of N-doped graphene sheets were investigated by TEM, AFM, XRD, XPS, XANES and Raman characterizations. Upon hydrothermal treatment, up to 13.22 at% of nitrogen could be introduced into the crumpled few-layer graphene sheets. Both XPS and XANES analysis reveal that the reaction between oxygen functional groups in GO and ammonia vapor produces amide and amine species in hydrothermally treated GO (HTGO). Subsequent thermal annealing of the resultant HTGO introduces a gradual transformation of nitrogen bonding configurations in graphene sheets from amine N to pyridinic and graphitic N with the increase of annealing temperature. This study provides a simple but cost-effective and eco-friendly method to prepare N-doped graphene materials in large-scale for potential applications.

  7. Confined-pyrolysis as an experimental method for hydrothermal organic synthesis

    NASA Astrophysics Data System (ADS)

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

    1995-10-01

    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 compounds 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.

  8. Hydrothermal Synthesis of Yttria-Stabilized Zirconia Nanocrystals with Controlled Yttria Content.

    PubMed

    Sato, Kazuyoshi; Horiguchi, Kazuya; Nishikawa, Taku; Yagishita, Sadahiro; Kuruma, Kazuo; Murakami, Takeshi; Abe, Hiroya

    2015-08-17

    In this study, we demonstrate for the first time the hydrothermal synthesis of yttria-stabilized zirconia (YSZ) nanocrystals with controlled yttria content (x = 3-12 mol %; xYSZ) with negligible aggregation from aqueous solution. The nanocrystals were grown via the hydrothermal treatment of basic Zr(IV) and Y(III) carbonate complex aqueous solutions in the presence of a cationic ligand, N(CH3)4(+). The nanocrystals were characterized in detail by dynamic light scattering, ζ-potential measurement, X-ray diffraction, specific surface area measurement based on the Brunauer-Emmett-Teller theory, transmission electron microscopy, energy dispersive X-ray spectroscopy, and Raman spectroscopy. Shorter reaction times and higher Y2O3 content produce aqueous solutions with higher transparencies containing nanocrystals with sizes of 10 nm or less. Nanocrystals with the target composition were obtained by hydrothermal reaction for longer than 3 h, regardless of the Y2O3 content. The main phase is tetragonal for (3-6)YSZ and cubic with disordered oxygen vacancies for (8-12)YSZ. The characteristics of the nanocrystalline material synthesized are consistent with those of bulk YSZ crystals, indicating the growth of high-quality nanocrystals.

  9. 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.

  10. 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.

  11. 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.

  12. Confined-pyrolysis as an experimental method for hydrothermal organic synthesis.

    PubMed

    Leif, R N; Simoneit, B R

    1995-10-01

    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 compounds and 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. 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.

  14. 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.

  15. 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.

  16. Synthesis and Geochemical Indicators of Abiogenic Hydrocarbons Produced Under Hydrothermal Conditions

    NASA Astrophysics Data System (ADS)

    Morrill, P. L.; Weinberger, D. S.; Sherwood Lollar, B.; Fogel, M. L.; Cody, G. D.

    2009-05-01

    Determining the geologically relevant conditions for, and geochemical indicators of, abiogenic hydrocarbon production in hydrothermal systems will aid in the identification of abiogenic and biogenic hydrocarbons, and carbon cycling in hydrothermal systems. In this study, abiogenic gaseous hydrocarbons were synthesized in hydrothermal experiments at 250C and 500 bar using a native Fe powder catalyst over short time periods (1 to 20 hr) to observe the product distribution and kinetic isotope effects associated with abiogenic organic synthesis of gaseous alkane hydrocarbons. The composition as well as the carbon and hydrogen isotope values (delta13C and delta2H respectively) of the gaseous hydrocarbons were measured to determine the mechanisms of formation and to determine if the abiogenic gases produced shared otherwise unique geochemical indicators for microbial and thermogenic hydrocarbon gases. Methane was the dominant hydrocarbon in all the experiments. Higher molecular weight gaseous alkanes decreased in concentration with increasing carbon number, which was well described by Anderson Schultz Flory probability of propagation factors (with an average of -0.31 ±0.15). At low percentage of carbon converted, the carbon isotopic separation between CO2 and CH4 (51.0 permil) was similar in magnitude to the carbon isotopic separation associated with microbial CO2 reduction. However, as the percentage of carbon converted increased, the carbon isotopic separation between CO2 and CH4 became progressively smaller (24.4 ±1.8 permil) overlapping with ranges for thermogenic hydrocarbons and thermophilic methanogens. The inability to distinguish abiogenic products, CO2 and CH4, from thermogenic and microbial methanogens products suggests that carbon isotope values alone of CO2 and CH4 are not enough to differentiate between alternative sources of CH4. In this study, ratios of C1/C2+ differentiated hydrocarbons produced by abiogenic synthesis from microbial gases.

  17. 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.

  18. Synthesis of kalsilite from microcline powder by an alkali-hydrothermal process

    NASA Astrophysics Data System (ADS)

    Su, Shuang-qing; Ma, Hong-wen; Yang, Jing; Zhang, Pan; Luo, Zheng

    2014-08-01

    The properties of aluminosilicate kalsilite have attracted the interest of researchers in chemical synthesis, ceramic industry, biofuels, etc. In this study, kalsilite was hydrothermally synthesized from microcline powder in a KOH solution. The microcline powder, rich in potassium, aluminum, and silicon, was collected from Mountain Changling in Northwestern China. The effects of temperature, time, and KOH concentration on the decomposition of microcline were investigated. The kalsilite and intermediate products were characterized by means of wet chemistry analysis, X-ray Diffraction (XRD), infrared spectrometry (IR), 29Si magic angle spinning nuclear magnetic resonance (29Si MAS NMR), 27Al MAS NMR, and scanning electron microscope (SEM). With increasing temperature, the microcline powder transforms into a metastable KAlSiO4 polymorph before transforming further into pure kalsilite. A mixture of both kalsilite and metastable KAlSiO4 polymorph is obtained when the hydrothermal reaction is carried out within 2 h; but after 2 h, kalsilite is the predominant product. The concentration of KOH, which needs to be larger than 4.3 M, is an important parameter influencing the synthesis of kalsilite.

  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. Hydrothermal synthesis of zeolites with three dimensionally ordered mesoporous-imprinted (3DOm-i) structure

    SciTech Connect

    Chen, Huiyong; Wydra, James; Zhang, Xueyi; Lee, Pyung-Soo; Wang, Zhuopeng; Fan, Wei; Tsapatsis, Michael

    2011-08-17

    Zeolites are microporous materials with pores and channels of molecular dimensions that find numerous applications in catalysis, separations, ion exchange, etc. However, whereas uniformity of micropore size is a most desirable and enabling characteristic for many of their uses, in certain cases, for example in reactions involving bulky molecules, it is a limitation. For this reason, synthesis of hierarchical zeolites with micro- and mesoporosity is of considerable interest as a way to control molecular traffic for improved catalytic and separation performance. Herein, we report a general synthesis route for the confined synthesis of zeolites within three-dimensionally ordered mesoporous carbon templates by conventional hydrothermal synthesis. Various zeolites, including BEA, LTA, FAU, and LTL, with three-dimensionally ordered mesoporous-imprinted structure have been synthesized by this approach. It is expected that these hierarchical zeolite materials will provide building blocks for thin-film and other syntheses and may provide a basis for quantitatively studying the mass-transfer limitation on the catalytic performance of zeolite catalysts.

  1. Hydrothermal synthesis of zeolites with three-dimensionally ordered mesoporous-imprinted structure.

    PubMed

    Chen, Huiyong; Wydra, James; Zhang, Xueyi; Lee, Pyung-Soo; Wang, Zhuopeng; Fan, Wei; Tsapatsis, Michael

    2011-08-17

    Zeolites are microporous materials with pores and channels of molecular dimensions that find numerous applications in catalysis, separations, ion exchange, etc. However, whereas uniformity of micropore size is a most desirable and enabling characteristic for many of their uses, in certain cases, for example in reactions involving bulky molecules, it is a limitation. For this reason, synthesis of hierarchical zeolites with micro- and mesoporosity is of considerable interest as a way to control molecular traffic for improved catalytic and separation performance. Herein, we report a general synthesis route for the confined synthesis of zeolites within three-dimensionally ordered mesoporous carbon templates by conventional hydrothermal synthesis. Various zeolites, including BEA, LTA, FAU, and LTL, with three-dimensionally ordered mesoporous-imprinted structure have been synthesized by this approach. It is expected that these hierarchical zeolite materials will provide building blocks for thin-film and other syntheses and may provide a basis for quantitatively studying the mass-transfer limitation on the catalytic performance of zeolite catalysts.

  2. 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

  3. 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

  4. 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.

  5. 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.

  6. Controlled Hydrothermal Synthesis and Photoluminescence of Nanocrystalline ZnGa2O4:Cr3+ Monospheres

    NASA Astrophysics Data System (ADS)

    Luan, Tian; Liu, Jinhan; Yuan, Xiaoxue; Li, Ji-Guang

    2017-03-01

    The hydrothermal synthesis of nanocrystalline ZnGa2O4:Cr3+ (ZGC) red phosphor monospheres was accomplished in this work, and the effects of system pH, reactant content, reaction time, and citrate anions (Cit3-) on the phase and morphology evolution of the product were systematically studied. Under the optimized conditions of Cit3-/ M = 1.0 molar ratio ( M = total cations), pH = 5.0, and 0.2 mmol of Zn2+, well-dispersed ZGC monospheres with an average diameter of 454 ± 56 nm (average crystallite size 15 nm) were successfully obtained via hydrothermal reaction at 180 °C for 18 h. Cit3+ ions were demonstrated to be crucial to the formation of monospheres and substantially affect the pathway of phase formation. The ZGC monospheres calcined at 800 °C (average diameter 353 ± 59 nm; average crystallite size 30 nm) have an intensity 6 times that of the original phosphor for the 700 nm red emission of Cr3+ (the 2E → 4A2 transition) under excitation with the O2- → Ga3+ charge transfer band at 250 nm. Fluorescence decay analysis found that the 700 nm emission has lifetime values of 5 ms for the ZGC phosphors.

  7. 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.

  8. 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).

  9. Hydrothermal synthesis of pollucite, analcime and their solid solutions and analysis of their properties

    NASA Astrophysics Data System (ADS)

    Jing, Zhenzi; Cai, Kunchuan; Li, Yan; Fan, Junjie; Zhang, Yi; Miao, Jiajun; Chen, Yuqian; Jin, Fangming

    2017-05-01

    Pollucite, as a perfect long-term potential host for radioactive Cs immobilization, barely exists in pure form naturally but in an isomorphism form between pollucite and analcime due to coexistence of Cs and Na. Pollucite could be hydrothermally synthesized with Cs-polluted soil or clay minerals which contain Cs and Na, and it is necessary to study the properties of the synthesis if Cs and Na contained. Pure pollucite, analcime and their solid solutions were hydrothermally synthesized with chemicals, and it was found that the most formed pollucite analcime solid solutions with Cs/(Cs + Na) ratios of 2/6-5/6 had very similar properties in mineral composition, morphology and size, structural water (Cs cations) and coordination environment to pollucite. This also suggests that even coexistence of Cs and Na in nature, pollucite favors to form due to site preference for Cs over Na, which leads to the property and the structure of the most solid solutions similar to that of pollucite.

  10. Hydrothermal synthesis of high surface area ZIF-8 with minimal use of TEA

    NASA Astrophysics Data System (ADS)

    Butova, V. V.; Budnyk, A. P.; Bulanova, E. A.; Lamberti, C.; Soldatov, A. V.

    2017-07-01

    In this paper we present, for the first time, a simple hydrothermal recipe for the synthesis of ZIF-8 Metal-Organic Framework (MOF) with a large specific surface area (1340 m2/g by BET). An important feature of the method is that the product forms in aqueous medium under standard hydrothermal conditions without DMF and great excess of linker with the use of TEA as structure directing agent. The ZIF-8 crystal phase of the product was confirmed by XRD; this technique has been also exploited to check the crystallinity and to follow the changes in the MOF structure induced by heating. TGA and temperature dependent XRD testify the high thermal stability of the material (470 °C in N2 and at 400 °C in air). The IR spectral profile of the material provides a complete picture of vibrations assigned to the linker and the metal center. The systematic investigation of the products obtained by increasing the TEA amount in the reacting medium from 0 to 25.5 mol equivalent Zn2+, allowed us to understand its role and to find 2.6 mol equivalent Zn2+ as the minimum amount needed to obtain a single phase ZIF-8 material with the high standard reported above. The stability of the material under severe basic conditions makes it a promising candidate in heterogeneous catalysis. The material has shown high capacity in I2 uptake, making it interesting also for selective molecular adsorption.

  11. 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).

  12. 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.

  13. 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.

  14. 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).

  15. 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.

  16. 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.

  17. 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.

  18. Hydrothermal synthesis of TiO2/WO3 compositions and their photocatalytic activity

    NASA Astrophysics Data System (ADS)

    Pyachin, Sergey A.; Karpovich, Natalia F.; Zaitsev, Alexey V.; Makarevich, Konstantin S.; Burkov, Alexander A.; Ustinov, Alexander Yu.

    2016-11-01

    Photocatalytic activity, optical properties, thermal stability, phase patterns and morphology of nano-size TiO2/WO3 compositions obtained from organic precursors through hydrothermal synthesis have been studied. It has been shown that doping of anatase nanoparticles with tungsten W+6 results in particle diameter reduction from 35 to 10 nm; decrease in width of the band gap from 3.15 eV to 2.91 eV and increase in temperature of phase transition of anatase to rutile up to 980oC. Catalytic activity of TiO2/WO3 (4 mol.%) composition under photochemical methylene blue (MB) oxidation by simulated solar light exceeds that of undoped anatase (obtained in the same way) 6-fold.

  19. 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.

  20. 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.

  1. 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. Copyright © 2014 Elsevier B.V. All rights reserved.

  2. 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

  3. 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

  4. 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.

  5. 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

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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

  11. 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

  12. 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.

  13. Abiotic Condensation Synthesis of Glyceride Lipids and Wax Esters Under Simulated Hydrothermal Conditions

    NASA Astrophysics Data System (ADS)

    Rushdi, Ahmed I.; Simoneit, Bernd R. T.

    2006-04-01

    Precursor compounds for abiotic proto cellular membranes are necessary for the origin of life. Amphipathic compounds such as fatty acids and acyl glycerols are important candidates for micelle/bilayer/vesicle formation. Two sets of experiments were conducted to study dehydration reactions of model lipid precursors in aqueous media to form acyl polyols and wax esters, and to evaluate the stability and reactions of the products at elevated temperatures. In the first set, mixtures of n-nonadecanoic acid and ethylene glycol in water, with and without oxalic acid, were heated at discrete temperatures from 150 ∘C to 300 ∘C for 72 h. The products were typically alkyl alkanoates, ethylene glycolyl alkanoates, ethylene glycolyl bis-alkanoates and alkanols. The condensation products had maximum yields between 150 ∘C and 250 ∘C, and were detectable and thus stable under hydrothermal conditions to temperatures < 300 ∘C. In the second set of experiments, mixtures of n-heptanoic acid and glycerol were heated using the same experimental conditions, with and without oxalic acid, between 100 ∘C and 250 ∘C. The main condensation products were two isomers each of monoacylglycerols and diacylglycerols at all temperatures, as well as minor amounts of the fatty acid anhydride and methyl ester. The yield of glyceryl monoheptanoates generally increased with increasing temperature and glyceryl diheptanoates decreased noticeably with increasing temperature. The results indicate that condensation reactions and abiotic synthesis of organic lipid compounds under hydrothermal conditions occur easily, provided precursor concentrations are sufficiently high.

  14. 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

  15. 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.

  16. 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.

  17. Ultra-Fast Supercritical Hydrothermal Synthesis of Tobermorite under Thermodynamically Metastable Conditions.

    PubMed

    Diez-Garcia, Marta; Gaitero, Juan J; Dolado, Jorge S; Aymonier, Cyril

    2017-03-13

    Tobermorite is a fibrillar mineral of the family of calcium silicates. In spite of not being abundant in nature, its structure and properties are reasonably well known because of its interest in the construction industry. Currently, tobermorite is synthesized by hydrothermal methods at mild temperatures. The problem is that such processes are very slow (>5 h) and temperature cannot be increased to speed them up because tobermorite is metastable over 130 °C. Furthermore the product obtained is generally foil-like and not very crystalline. Herein we propose an alternative synthesis method based on the use of a continuous flow reactor and supercritical water. In spite of the high temperature, the transformation of tobermorite to more stable phases can be prevented by accurately controlling the reaction time. As a result, highly crystalline fibrillar tobermorite can be obtained in just a few seconds under thermodynamically metastable conditions. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. 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).

  19. Magnetic properties of hematite (α-Fe2O3) nanoparticles prepared by hydrothermal synthesis method

    NASA Astrophysics Data System (ADS)

    Tadic, Marin; Panjan, Matjaz; Damnjanovic, Vesna; Milosevic, Irena

    2014-11-01

    Hematite (α-Fe2O3) nanoparticles are successfully synthesized by using the hydrothermal synthesis method. An X-ray powder diffraction (XRPD) of the sample shows formation of the nanocrystalline α-Fe2O3 phase. A transmission electron microscopy (TEM) measurements show spherical morphology of the hematite nanoparticles and narrow size distribution. An average hematite nanoparticle size is estimated to be about 8 nm by TEM and XRD. Magnetic properties were measured using a superconducting quantum interference device (SQUID) magnetometry. Investigation of the magnetic properties of hematite nanoparticles showed a divergence between field-cooled (FC) and zero-field-cooled (ZFC) magnetization curves below Tirr = 103 K (irreversibility temperature). The ZFC magnetization curve showed maximum at TB = 52 K (blocking temperature). The sample did not exhibit the Morin transition. The M(H) (magnetization versus magnetic field) dependence at 300 K showed properties of superparamagnetic iron oxide nanoparticles (SPION). The M(H) data were successfully fitted by the Langevin function and magnetic moment μp = 657 μB and diameter d = 8.1 nm were determined. Furthermore, magnetic measurements showed high magnetization at room temperature (MS = 3.98 emu/g), which is desirable for application in spintronics and biomedicine. Core-shell structure of the nanoparticles was used to describe high magnetization of the hematite nanoparticles.

  20. Face-selective electrostatic control of hydrothermal zinc oxide nanowire synthesis.

    PubMed

    Joo, Jaebum; Chow, Brian Y; Prakash, Manu; Boyden, Edward S; Jacobson, Joseph M

    2011-07-10

    Rational control over the morphology and the functional properties of inorganic nanostructures has been a long-standing goal in the development of bottom-up device fabrication processes. We report that the geometry of hydrothermally grown zinc oxide nanowires can be tuned from platelets to needles, covering more than three orders of magnitude in aspect ratio (~0.1-100). We introduce a classical thermodynamics-based model to explain the underlying growth inhibition mechanism by means of the competitive and face-selective electrostatic adsorption of non-zinc complex ions at alkaline conditions. The performance of these nanowires rivals that of vapour-phase-grown nanostructures, and their low-temperature synthesis (<60 °C) is favourable to the integration and in situ fabrication of complex and polymer-supported devices. We illustrate this capability by fabricating an all-inorganic light-emitting diode in a polymeric microfluidic manifold. Our findings indicate that electrostatic interactions in aqueous crystal growth may be systematically manipulated to synthesize nanostructures and devices with enhanced structural control.

  1. 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}.

  2. 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.

  3. Preparation of PBO/ZnO fibers by hydrothermal synthesis method and its properties

    NASA Astrophysics Data System (ADS)

    Ma, Qi; Wang, Bin; Lv, Junwei; Li, Yuntao; Li, Hui; Zhao, Chunxia

    2017-08-01

    In this article, zinc oxide (ZnO) nanoparticles were synthesized and deposited on the surface of PBO fibers through hydrothermal synthesis method. The structures and properties of PBO/ZnO fibers and PBO fibers were characterized by scanning electron microscopy (SEM), energy dispersive spectrometer (EDS), x-ray diffraction (XRD), Fourier transform infrared spectrum (FTIR), Thermogravimetric analysis (TG), and tensile testing. The results revealed that the PBO/ZnO fibers have good mechanical properties and high thermal stability. Moreover, the fibers exhibited excellent UV-blocking properties by putting them under UV irradiation of 313 nm. Specifically, ZnO coated fibers will lose only 18.93% of tensile strength after 50 h irradiation, and then will keep over 65% of tensile strength after 100 h UV irradiation. Additionally the interface shear strength is increased significantly, and the results also showed modified PBO fibers exhibited excellent hydrophobic quality. So the functional materials have great potentials in future engineering applications.

  4. 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.

  5. 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.

  6. 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.

  7. 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).

  8. 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. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. A Facile Hydrothermal Synthesis of Iron Oxide Nanoparticles with Tunable Magnetic Properties

    PubMed Central

    Ge, Song; Shi, Xiangyang; Sun, Kai; Li, Changpeng; Baker, James R.; Banaszak Holl, Mark M.; Orr, Bradford G.

    2009-01-01

    We report a facile one-step hydrothermal approach to the synthesis of iron oxide (Fe3O4) nanoparticles (NPs) with controllable diameters, narrow size distribution, and tunable magnetic properties. In this approach, the iron oxide NPs were fabricated by oxidation of FeCl2·4H2O in basic aqueous solution under an elevated temperature and pressure. Transmission electron microscopy (TEM) and X-ray diffraction (XRD) studies reveal that the particles are highly crystalline and that the diameters of the particles can be tuned from 15 nm to 31 nm through the variation of the reaction conditions. The NPs exhibit high saturation magnetization in the range of 53.3 ~ 97.4 emu/g and their magnetic behavior can be either ferromagnetic or superparamagnetic depending on the particle size. A superconducting quantum interference device magnetorelaxometry (SQUID-MRX) study shows that the size of the NPs significantly affects the detection sensitivity. The investigated iron oxide NPs may find many potential biological applications in cancer diagnosis and treatment. PMID:20174618

  10. Hydrothermal Synthesis and Photocatalytic Property of β-Ga2O3 Nanorods.

    PubMed

    Reddy, L Sivananda; Ko, Yeong Hwan; Yu, Jae Su

    2015-12-01

    Gallium oxide (Ga2O3) nanorods were facilely prepared by a simple hydrothermal synthesis, and their morphology and photocatalytic property were studied. The gallium oxide hydroxide (GaOOH) nanorods were formed in aqueous growth solution containing gallium nitrate and ammonium hydroxide at 95 °C of growth temperature. Through the calcination treatment at 500 and 1000 °C for 3 h, the GaOOH nanorods were converted into single crystalline α-Ga2O3 and β-Ga2O3 phases. From X-ray diffraction analysis, it could be confirmed that a high crystalline quality of β-Ga2O3 nanorods was achieved by calcinating at 1000 °C. The thermal behavior of the Ga2O3 nanorods was also investigated by differential thermal analysis, and their vibrational bands were identified by Fourier transform infrared spectroscopy. In order to examine the photocatalytic activity of samples, the photodegradation of Rhodamine B solution was observed under UV light irradiation. As a result, the α-Ga2O3 and β-Ga2O3 nanorods exhibited high photodegeneration efficiencies of 62 and 79 %, respectively, for 180 min of UV irradiation time.

  11. Preparation of Bi2Fe4O9 particles by hydrothermal synthesis and functional properties

    NASA Astrophysics Data System (ADS)

    Gheorghiu, Felicia; Tanasa, Radu; Buscaglia, Maria Teresa; Buscaglia, Vincenzo; Pastravanu, Cristina G.; Popovici, Eveline; Mitoseriu, Liliana

    2013-07-01

    In the present study, particles with different Bi2Fe4O9 micro/nanostructures with a few particular morphologies (flower-like nanoplatelets, hierarchical microstructures, perfectly square platelets single crystals, etc.) obtained under specific hydrothermal synthesis conditions were investigated. The role of the processing parameters (such as NaOH concentration, reaction temperature, and reaction duration time) on the phase formation mechanism and on the microstructural characteristics was investigated. All the Bi2Fe4O9 morphologies showed orthorhombic symmetry with space group Pbam. The photocatalytic properties and magnetic behavior as a function of the micro/nanostructural characteristics of various Bi2Fe4O9 powders were determined. In the presence of Bi2Fe4O9, a degradation rate of Rose Bengal in the range of 52-61% was determined after 180 min under UV light irradiation (λ = 254 nm). Magnetic activity with antiferromagnetic behavior and a transition at ∼240 K slightly dependent on the microstructures was found. The role of Bi2Fe4O9 microstructures in the photocatalytic activity and magnetic properties was discussed.

  12. Hydrothermal synthesis of leucite nanoparticles using anionic surfactant: Structural evaluation and catalytic properties

    NASA Astrophysics Data System (ADS)

    Farrukh, Muhammad Akhyar; Naseem, Fizza; Imtiaz, Ayesha; Khaleeq-ur-Rahman, Muhammad; Martins, Tatiana Duque; Zia, Khalid Mahmood

    2016-06-01

    Surfactant-assisted synthesis of leucite (KAlSi2O6) nanoparticles was carried out by a hydrothermal method using an anionic surfactant at variable temperatures and surfactant concentrations. The newly synthesized leucite nanoparticles were characterized by FTIR, TGA, XRD, FESEM, and TEM. These nanoparticles have a wide and direct band gap at their smallest particle size ( E g = 3.30 eV), showing a significant quantum confinement effect. Samples of leucite were prepared at 180°C with different SDS concentrations 0.006, 0.007, 0.008, 0.009, and 0.01 M and were used to degrade methylene blue under ultraviolet radiations. These samples degraded methylene blue to 18.5, 31.7, 45.81, 31.61, 30.1%, respectively. The most effective catalyst is the one which was synthesized at 200°C and the CMC value of the surfactant (sodium dodecyl sulfate) having the percentage degradation of 49.1%.

  13. Morphology control of lithium iron phosphate nanoparticles by soluble starch-assisted hydrothermal synthesis

    NASA Astrophysics Data System (ADS)

    Chen, Zhaoyong; Xu, Ming; Du, Binglin; Zhu, Huali; Xie, Tian; Wang, Wenhua

    2014-12-01

    Lithium iron phosphate (LiFePO4) is a potentially high efficiency cathode material for lithium ion batteries, but the low electronic conductivity and one-dimensional diffusion channel for lithium ions require small particle size and shape control during the synthesis. In this paper, well-crystallized and morphology-controlled LiFePO4 cathode material for lithium-ion batteries is successfully synthesized via a soluble starch-assisted hydrothermal method at 180 °C for 5 h, followed by calcining with phenolic resin at 750 °C for 6 h. In this study, we investigate the effect of five different concentrations of starch solution on controlling morphology of LiFePO4. Interestingly, the nano-sized LiFePO4 particles obtained in 0.075 mol L-1 starch solution exhibit a spheroidal microstructure, while the platelet shape LiFePO4 particles are synthesized in lower or higher concentration of starch solution. The mechanism and process of forming such spheroidal microstructure is discussed. These unique structural and morphological properties of LiFePO4 lead to high specific capacity and stable cycling performance. Analysis of the electrochemical impedance spectroscopy reveals that nano-sized carbon/polyacene coated LiFePO4 cathode materials play an critical role in achieving excellent electrochemical performance.

  14. 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.

  15. 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.

  16. An evaluation of the critical parameters for abiotic peptide synthesis in submarine hydrothermal systems.

    PubMed

    Cleaves, H J; Aubrey, A D; Bada, J L

    2009-04-01

    It has been proposed that oligopeptides may be formed in submarine hydrothermal systems (SHSs). Oligopeptides have been synthesized previously under simulated SHS conditions which are likely geochemically implausible. We have herein investigated the oligomerization of glycine under SHS-like conditions with respect to the limitations imposed by starting amino acid concentration, heating time, and temperature. When 10(-1) M glycine solutions were heated at 250 degrees C for < 20 min glycine oligomers up to tetramers and diketopiperazine (DKP) were detectable. At 200 degrees C, less oligomerization was noted. Peptides beyond glycylglycine (gly2) and DKP were not detected below 150 degrees C. At 10(-2) M initial glycine concentration and below, only gly2, DKP, and gly3 were detected, and then only above 200 degrees C at < 20 min reaction time. Gly3 was undetectable at longer reaction times. The major parameters limiting peptide synthesis in SHSs appear to be concentration, time, and temperature. Given the expected low concentrations of amino acids, the long residence times and range of temperatures in SHSs, it is unlikely that SHS environments were robust sources of even simple peptides. Possible unexplored solutions to the problems presented here are also discussed.

  17. 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

  18. 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)…

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

    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)…

  20. 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.

  1. 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.

  2. Low-temperature hydrothermal synthesis of BiFeO{sub 3} microcrystals and their visible-light photocatalytic activity

    SciTech Connect

    Wei, Jie; Zhang, Chao; Xu, Zhuo

    2012-11-15

    Highlights: ► Urea-assisted hydrothermal synthesis of pure BiFeO{sub 3} at 120 °C was reported. ► Possible formation mechanism of pure phase BiFeO{sub 3} at low temperature was illuminated. ► BiFeO{sub 3} microcrystals exhibited efficient visible-light photocatalytic activity. -- Abstract: Pure BiFeO{sub 3} (BFO) microcrystals were synthesized at the temperature as low as 120 °C via a urea-assisted hydrothermal process. The crystal structure, morphology and photocatalytic property of BFO microcrystals were investigated. The analysis reveals that the hydrolysis of urea in the hydrothermal process plays a key role in the synthesis of pure phase BFO microcrystals. FE-SEM and TEM results show that these BFO microcrystals present a nearly spherical microstructure, and specially exhibit superstructures consisting of large amounts of small particles with the size of 100–150 nm by further observation. Moreover, these BFO microcrystals exhibit efficient photocatalytic activity under visible-light irradiation, suggesting their promising applications as photocatalysts and related fields.

  3. Sol-gel (template) synthesis of macroporous Mo-based catalysts for hydrothermal oxidation of radionuclide-organic complexes

    NASA Astrophysics Data System (ADS)

    Papynov, E. K.; Palamarchuk, M. S.; Mayorov, V. Yu; Modin, E. B.; Portnyagin, A. S.; Sokol'nitskaya, T. A.; Belov, A. A.; Tananaev, I. G.; Avramenko, V. A.

    2017-07-01

    Molybdenum compounds are industrially demanding as heterogeneous catalysts for oxidation of various organic substances. Highly porous structure of molybdenum-containing catalysts avoids surface's colmatation and prevents blocking catalytic sites that makes these materials play a key role in processes of hydrothermal oxidation of radionuclide organic complexes. The study presents an original way of sol-gel synthesis of new macroporous molybdenum compounds using ;core-shell; colloid template (polymer latex) as poreforming agent. We have described three individual routs of template removal via thermal decomposition to obtain porous materials based on molybdenum compounds. Thermal treatment conditions (temperature, gaseous atmosphere) have been studied with respect to their influence on composition, structure and catalytic properties of synthesized molybdenum systems. The optimal way to synthesis of crystal molybdenum (VI) oxide with ordered porous structure (mean pore size 100-160 nm) has been suggested. Catalytic properties of macroporous molybdenum materials have been investigated in the process of liquid phase and hydrothermal oxidation of such organic substances thiazine and stable Co-EDTA complex. It was shown that macroporous molybdenum oxides could be applied as prospective catalysts for hydrothermal oxidation of organic radionuclide complexes during the processing of radioactive waste.

  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. High-Throughput Continuous Hydrothermal Synthesis of Transparent Conducting Aluminum and Gallium Co-doped Zinc Oxides.

    PubMed

    Howard, Dougal P; Marchand, Peter; McCafferty, Liam; Carmalt, Claire J; Parkin, Ivan P; Darr, Jawwad A

    2017-04-10

    High-throughput continuous hydrothermal flow synthesis was used to generate a library of aluminum and gallium-codoped zinc oxide nanoparticles of specific atomic ratios. Resistivities of the materials were determined by Hall Effect measurements on heat-treated pressed discs and the results collated into a conductivity-composition map. Optimal resistivities of ∼9 × 10(-3) Ω cm were reproducibly achieved for several samples, for example, codoped ZnO with 2 at% Ga and 1 at% Al. The optimum sample on balance of performance and cost was deemed to be ZnO codoped with 3 at% Al and 1 at% Ga.

  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-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.

  12. 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

  13. 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

  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. Controlled synthesis of α-Al2O3 via the hydrothermal-pyrolysis method

    NASA Astrophysics Data System (ADS)

    Li, Zhao; Wu, Kunyao; Cao, Jing; Wang, Yongfeng

    2017-06-01

    Taking aluminum sulfate and urea as the raw materials produce α-Al2O3 by employing the hydrothermal-pyrolysis method. The study analyzes the characterization of the products by XRD and SEM, The results indicate as follows: after 6 hours’ hydrothermal reaction in the 120°C water, with the aluminum sulfate and urea as the raw materials, spherical α-Al2O3 can be obtained through calcination at 1200°C.

  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. 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

  20. 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.

  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. 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.

  4. Hydrothermal Synthesis of VO2 Polymorphs: Advantages, Challenges and Prospects for the Application of Energy Efficient Smart Windows.

    PubMed

    Li, Ming; Magdassi, Shlomo; Gao, Yanfeng; Long, Yi

    2017-09-01

    Vanadium dioxide (VO2 ) is a widely studied inorganic phase change material, which has a reversible phase transition from semiconducting monoclinic to metallic rutile phase at a critical temperature of τc ≈ 68 °C. The abrupt decrease of infrared transmittance in the metallic phase makes VO2 a potential candidate for thermochromic energy efficient windows to cut down building energy consumption. However, there are three long-standing issues that hindered its application in energy efficient windows: high τc , low luminous transmittance (Tlum ), and undesirable solar modulation ability (ΔTsol ). Many approaches, including nano-thermochromism, porous films, biomimetic surface reconstruction, gridded structures, antireflective overcoatings, etc, have been proposed to tackle these issues. The first approach-nano-thermochromism-which is to integrate VO2 nanoparticles in a transparent matrix, outperforms the rest; while the thermochromic performance is determined by particle size, stoichiometry, and crystallinity. A hydrothermal method is the most common method to fabricate high-quality VO2 nanoparticles, and has its own advantages of large-scale synthesis and precise phase control of VO2 . This Review focuses on hydrothermal synthesis, physical properties of VO2 polymorphs, and their transformation to thermochromic VO2 (M), and discusses the advantages, challenges, and prospects of VO2 (M) in energy-efficient smart windows application. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. High-temperature synthesis of highly hydrothermal stable mesoporous silica and Fe-SiO{sub 2} using ionic liquid as a template

    SciTech Connect

    Liu, Hong; Wang, Mengyang; Hu, Hongjiu; Liang, Yuguang; Wang, Yong; Cao, Weiran; Wang, Xiaohong

    2011-03-15

    Mesoporous silicas and Fe-SiO{sub 2} with worm-like structures have been synthesized using a room temperature ionic liquid, 1-hexadecane-3-methylimidazolium bromide, as a template at a high aging temperature (150-190 {sup o}C) with the assistance of NaF. The hydrothermal stability of mesoporous silica was effectively improved by increasing the aging temperature and adding NaF to the synthesis gel. High hydrothermally stable mesoporous silica was obtained after being aged at 190 {sup o}C in the presence of NaF, which endured the hydrothermal treatment in boiling water at least for 10 d or steam treatment at 600 {sup o}C for 6 h. The ultra hydrothermal stability could be attributed to its high degree of polymerization of silicate. Furthermore, highly hydrothermal stable mesoporous Fe-SiO{sub 2} has been synthesized, which still remained its mesostructure after being hydrothermally treated at 100 {sup o}C for 12 d or steam-treated at 600 {sup o}C for 6 h. -- Graphical abstract: Worm-like mesoporous silica and Fe-SiO{sub 2} with high hydrothermal stability have been synthesized using ionic liquid 1-hexadecane-3-methylimidazolium bromide as a template under the assistance of NaF at high temperature. Display Omitted Research highlights: {yields} Increasing aging temperature improved the hydrothermal stability of materials. {yields}Addition of NaF enhanced the polymerization degree of silicates. {yields} Mesoporous SiO{sub 2} and Fe-SiO{sub 2} obtained have remarkable hydrothermal stability.

  13. 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...

  14. 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...

  15. 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.

  16. Hydrothermal Synthesis of Hydroxyapatite Nanorods for Rapid Formation of Bone-Like Mineralization

    NASA Astrophysics Data System (ADS)

    Hoai, Tran Thanh; Nga, Nguyen Kim; Giang, Luu Truong; Huy, Tran Quang; Tuan, Phan Nguyen Minh; Binh, Bui Thi Thanh

    2017-08-01

    Hydroxyapatite (HAp) is an excellent biomaterial for bone repair and regeneration. The biological functions of HAp particles, such as biomineralization, cell adhesion, and cell proliferation, can be enhanced when their size is reduced to the nanoscale. In this work, HAp nanoparticles were synthesized by the hydrothermal technique with addition of cetyltrimethylammonium bromide (CTAB). These particles were also characterized, and their size controlled by modifying the CTAB concentration and hydrothermal duration. The results show that most HAp nanoparticles were rod-like in shape, exhibiting the most uniform and smallest size (mean diameter and length of 39 nm and 125 nm, respectively) at optimal conditions of 0.64 g CTAB and hydrothermal duration of 12 h. Moreover, good biomineralization capability of the HAp nanorods was confirmed through in vitro tests in simulated body fluid. A bone-like mineral layer of synthesized HAp nanorods formed rapidly after 7 days. This study shows that highly bioactive HAp nanorods can be easily prepared by the hydrothermal method, being a potential nanomaterial for bone regeneration.

  17. 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.

  18. Synthesis and electrochemical properties of Co3O4 nanoparticles by hydrothermal method at different temperatures

    NASA Astrophysics Data System (ADS)

    Duan, Qiuyan; Chen, Haiyan

    2017-06-01

    In this work, Co3O4 nanoparticles were synthesized by hydrothermal method at different temperatures. The synthesized Co3O4 nanoparticles were characterized using transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectrometer (XPS) and nitrogen adsorption-desorption. The Co3O4 nanoparticles prepared at the hydrothermal temperature of 140 °C and at the annealing temperature of 350 °C have a shorter crystal spacing distance associated to the (220) crystal planes, larger BET surface area and more bivalent cobalt on the surface than these of Co3O4 nanoparticles prepared at higher hydrothermal temperature or higher annealing temperature. The supercapacitor performances of synthesized Co3O4 nanoparticles were analysed by cyclic voltammograms (CVs), Galvano static charge/discharge (GCD) and the electrochemical impedance spectroscopy (EIS) in 6 M KOH aqueous electrolyte solution. The Co3O4 nanoparticles produced at lower temperatures exhibit good pseudo capacitance behaviour. Also, owning to the low hydrothermal temperature and the annealing temperature of Co3O4 nanoparticles, they can be relatively low cost in favour of a promising candidate for electrochemical supercapacitors.

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. Hydrothermal Synthesis of Lanthanum Vanadates: Synthesis and Crystal Structures of Zircon-Type LaVO 4 and a New Compound LaV 3O 9

    NASA Astrophysics Data System (ADS)

    Oka, Yoshio; Yao, Takeshi; Yamamoto, Naoichi

    2000-07-01

    In the course of hydrothermal synthesis of lanthanum vanadates, zircon-type LaVO4 and LaV3O9 have been obtained and structurally characterized. The former is a metastable phase, and the latter is a new compound. Single-crystal X-ray diffractometry confirmed the zircon-type structure for LaVO4: I41/amd with a=7.4578(7) Å, c=6.5417(9) Å, and Z=4; R=0.020 and Rw=0.025 for 276 reflections with I>3σ(I). The structure consists of isolated VO4 tetrahedra which surround the La atom to form a LaO8 dodecahedron. LaV3O9 adopts the monoclinic system: P21/m with a=4.949(2) Å, b=9.547(3) Å, c=7.411(2) Å, β=100.76(2)°, and Z=2; R=0.035 and Rw=0.042 for 1868 reflections with I>3σ(I). The structure adopts a chain-type one consisting of a V3O9 chain along [010] which is made up of edge-sharing VO5 trigonal-bipyramid pairs and VO4 tetrahedra. The La atom residues between the V3O9 chains and is coordinated with ten oxygens. The present study demonstrates the applicability of hydrothermal method to the synthesis of new and/or metastable lanthanide vanadates.

  4. 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

  5. CTAB-assisted hydrothermal synthesis of YVO 4:Eu 3+ powders in a wide pH range

    NASA Astrophysics Data System (ADS)

    Wang, Juan; Hojamberdiev, Mirabbos; Xu, Yunhua

    2012-01-01

    Rhombus-, rod-, soya bean- and aggregated soya bean-like YVO 4:Eu 3+ micro- and nanostructures were synthesized by a cetyltrimethylammonium bromide (CTAB)-assisted hydrothermal method at 180 °C for 24 h in a wide pH range. The as-synthesized powders were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and photoluminescence spectroscopy (PL). The XRD results confirmed the formation of phase-pure YVO 4:Eu 3+ powders with tetragonal structure under hydrothermal process in a wide pH range. Electron microscopic observations evidenced the morphological transformation of YVO 4:Eu 3+ powders from rhombus-like microstructure to rod-, soya bean, and aggregated soya bean-like nanostructures with an increase in the pH of the synthesis solution. The results from the PL measurements revealed that the intensities of PL emission peaks were significantly affected by the morphologies and crystallinity of samples due to the absence of an inversion symmetry at the Eu 3+ lattice site, and the highest luminescence intensity was observed for rod-like YVO 4:Eu 3+ powders.

  6. 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.

  7. 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

    2017-06-01

    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.

  8. 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.

  9. 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

  10. 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).

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

    PubMed

    Tippayawat, Patcharaporn; Phromviyo, Nutthakritta; Boueroy, Parichart; Chompoosor, Apiwat

    2016-01-01

    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. 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. 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 (o)C for 6 h and 200 (o)C 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 pharmaceutical

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

    SciTech Connect

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

    2016-04-15

    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. - Graphical abstract: Phosphate dendrite like and phosphonate platelet crystals.

  13. 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.

  14. 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.

  15. 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

  16. 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.

  17. 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

  18. 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.

  19. 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

  20. 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.

  1. Influence of TiCl4 precursor in hydrothermal synthesis of TiO2 nanostructures

    NASA Astrophysics Data System (ADS)

    Kartikay, Purnendu; Nemala, Siva Sankar; Mallick, Sudhanshu

    2017-05-01

    Rutile TiO2 films were deposited on the FTO substrate by the hydrothermal process using TTIP and TiCl4 as the titania precursor. Our study manifestly exhibits the influence of TiCl4 precursor on the hydrothermal growth of the TiO2 structure. The morphology of prepared film varies from nano-cauliflower to nano-flower to nano-parallelepiped rod-like structure with the addition of TiCl4 as the precursor. When TiCl4 is introduced in the precursor HCl corresponding to four times of the Ti4+ concentration is generated as a by-product during the reaction, these additional HCl promotes the etching of the nanostructure enabling the nanostructure to unfurl. We conclude that the tailoring of the nanostructure can be performed by addition of TiCl4 in the precursor

  2. Chelating Ligand-Mediated Hydrothermal Synthesis of Samarium Orthovanadate with Decavanadate as Vanadium Source

    PubMed Central

    Zuo, Wenli

    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. PMID:24068882

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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

  9. 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.

  10. One-step hydrothermal synthesis of fluorescent nanocrystalline cellulose/carbon dot hydrogels.

    PubMed

    Li, Wei; Wang, Sichun; Li, Ying; Ma, Chunhui; Huang, Zhanhua; Wang, Chunsheng; Li, Jian; Chen, Zhijun; Liu, Shouxin

    2017-11-01

    Fluorescent nanocrystalline cellulose/carbon dots (NCC/CDs) hydrogels were successfully prepared by a facile one-step green hydrothermal carbonization process. The properties of NCC/CDs hydrogels prepared at different temperatures were investigated by fluorescence spectroscopy, transmission electron microscopy, nuclear magnetic resonance spectroscopy, X-ray diffraction, and thermogravimetric analysis. NCC/CDs hydrogels with high crystallinity, high thermal stability, and excellent fluorescence properties can be obtained by controlling the hydrothermal treatment temperature. Small rod-like NCC/CDs hydrogels with a diameter of 2-6nm, a length of 40-60nm, and the cellulose Ι structure were obtained when the hydrothermal carbonization temperature was 240°C. The NCC/CDs hydrogels exhibited an excellent broad spectral response and high fluorescence stability at various pH values. Considering of the wide natural abundance of NCC and the biocompatibility of the NCC/CDs hydrogels, Preparation in this simple, green approach is attractive for future bio-medical applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

  11. 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.

  12. Hydrothermal synthesis of SnO{sub 2} nanorods: Morphology dependence, growth mechanism and surface properties

    SciTech Connect

    Liang, Ying Fang, Bin

    2013-10-15

    Graphical abstract: - Highlights: • Urchin-like nanorod clusters were synthesized by a facile hydrothermal process. • The influence of synthetic parameters on formation of SnO{sub 2} products was studied. • The growth mechanism of SnO{sub 2} nanorods was proposed from valuable insights. • The surface properties of SnO{sub 2} nanorods were investigated. - Abstract: Uniform tetragonal-shaped SnO{sub 2} nanorods and their urchin-like clusters were successfully synthesized via a template-free hydrothermal process. The resulting nanorods were characterized by power X-ray diffraction (PXRD), field emission scanning electron microscope (FESEM), high resolution transmission electron microscope (HRTEM), infrared absorption spectra (IR), X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TG) and ultraviolet–visible (UV–vis) absorption spectra. The influence of precursor, solvent, hydrothermal temperature and treatment time on the formation of SnO{sub 2} nanostructures was investigated. Moreover, the surface properties of SnO{sub 2} nanorods were studied.

  13. 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.

  14. Hydrothermal synthesis, characterization, and photocatalytic properties of Zn{sub 2}SnO{sub 4}

    SciTech Connect

    Fu Xianliang; Wang Xuxu Long Jinlin; Ding Zhengxin; Yan Tingjiang; Zhang Guoying; Zhang Zizhong; Lin Huaxiang; Fu Xianzhi

    2009-03-15

    Nanosized Zn{sub 2}SnO{sub 4} (ZTO) particles were successfully synthesized by a simple hydrothermal process in water/ethylene glycol mixed solution using amines (ethylamine, n-butylamine, n-hexylamine, and n-octylamine) as mineralizer. The products were characterized by X-ray diffractions (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and N{sub 2} adsorption. The results indicated that the hydrothermal conditions, such as alkaline concentration (n-butylamine), reaction temperature, solvent composition, and the kind of amines, had an important influence on the composition, crystallinity, and morphology of the product. The as-synthesized ZTO samples exhibited high activities and durabilities for photodegradation of methyl orange and the activities were mainly affected by the crystallinities of the samples. A hexagonal-shaped ZTO (H-ZTO) sample was prepared in 0.53 M of n-butylamine solution at 180 deg. C for 20 h and its optical properties were characterized by UV-Vis diffuse reflectance and Photoluminescence (PL) spectra. Furthermore, the photocatalytic H{sub 2} evolution reaction from ethanol aqueous solution over H-ZTO was also investigated. - Graphical abstract: Nanosized Zn{sub 2}SnO{sub 4} (ZTO) was successfully synthesized by hydrothermal process. Photocatalytic test showed that the samples exhibited high activity and durability for photodegradation of methyl orange (MO) and photocatalytic production H{sub 2} from ethanol aqueous solution.

  15. 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.

  16. 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

  17. Quick high-temperature hydrothermal synthesis of mesoporous materials with 3D cubic structure for the adsorption of lysozyme.

    PubMed

    Lawrence, Geoffrey; Baskar, Arun V; El-Newehy, Mohammed H; Cha, Wang Soo; Al-Deyab, Salem S; Vinu, Ajayan

    2015-04-01

    Three-dimensional cage-like mesoporous FDU-12 materials with large tuneable pore sizes ranging from 9.9 to 15.6 nm were prepared by varying the synthesis temperature from 100 to 200 °C for the aging time of just 2 h using a tri-block copolymer F-127(EO106PO70EO106) as the surfactant and 1,3,5-trimethyl benzene as the swelling agent in an acidic condition. The mesoporous structure and textural features of FDU-12-HX (where H denotes the hydrothermal method and X denotes the synthesis temperature) samples were elucidated and probed using x-ray diffraction, N2 adsorption, (29)Si magic angle spinning nuclear magnetic resonance, scanning electron microscopy and transmission electron microscopy. It has been demonstrated that the aging time can be significantly reduced from 72 to 2 h without affecting the structural order of the FDU-12 materials with a simple adjustment of the synthesis temperature from 100 to 200 °C. Among the materials prepared, the samples prepared at 200 °C had the highest pore volume and the largest pore diameter. Lysozyme adsorption experiments were conducted over FDU-12 samples prepared at different temperatures in order to understand their biomolecule adsorption capacity, where the FDU-12-HX samples displayed high adsorption performance of 29 μmol g(-1) in spite of shortening the actual synthesis time from 72 to 2 h. Further, the influence of surface area, pore volume and pore diameter on the adsorption capacity of FDU-12-HX samples has been investigated and results are discussed in correlation with the textural parameters of the FDU-12-HX and other mesoporous adsorbents including SBA-15, MCM-41, KIT-5, KIT-6 and CMK-3.

  18. Quick high-temperature hydrothermal synthesis of mesoporous materials with 3D cubic structure for the adsorption of lysozyme

    PubMed Central

    Lawrence, Geoffrey; Baskar, Arun V; El-Newehy, Mohammed H; Cha, Wang Soo; Al-Deyab, Salem S

    2015-01-01

    Three-dimensional cage-like mesoporous FDU-12 materials with large tuneable pore sizes ranging from 9.9 to 15.6 nm were prepared by varying the synthesis temperature from 100 to 200 °C for the aging time of just 2 h using a tri-block copolymer F-127(EO106PO70EO106) as the surfactant and 1,3,5-trimethyl benzene as the swelling agent in an acidic condition. The mesoporous structure and textural features of FDU-12-HX (where H denotes the hydrothermal method and X denotes the synthesis temperature) samples were elucidated and probed using x-ray diffraction, N2 adsorption, 29Si magic angle spinning nuclear magnetic resonance, scanning electron microscopy and transmission electron microscopy. It has been demonstrated that the aging time can be significantly reduced from 72 to 2 h without affecting the structural order of the FDU-12 materials with a simple adjustment of the synthesis temperature from 100 to 200 °C. Among the materials prepared, the samples prepared at 200 °C had the highest pore volume and the largest pore diameter. Lysozyme adsorption experiments were conducted over FDU-12 samples prepared at different temperatures in order to understand their biomolecule adsorption capacity, where the FDU-12-HX samples displayed high adsorption performance of 29 μmol g−1 in spite of shortening the actual synthesis time from 72 to 2 h. Further, the influence of surface area, pore volume and pore diameter on the adsorption capacity of FDU-12-HX samples has been investigated and results are discussed in correlation with the textural parameters of the FDU-12-HX and other mesoporous adsorbents including SBA-15, MCM-41, KIT-5, KIT-6 and CMK-3. PMID:27877767

  19. Quick high-temperature hydrothermal synthesis of mesoporous materials with 3D cubic structure for the adsorption of lysozyme

    NASA Astrophysics Data System (ADS)

    Lawrence, Geoffrey; Baskar, Arun V.; El-Newehy, Mohammed H.; Cha, Wang Soo; Al-Deyab, Salem S.; Vinu, Ajayan

    2015-04-01

    Three-dimensional cage-like mesoporous FDU-12 materials with large tuneable pore sizes ranging from 9.9 to 15.6 nm were prepared by varying the synthesis temperature from 100 to 200 °C for the aging time of just 2 h using a tri-block copolymer F-127(EO106PO70EO106) as the surfactant and 1,3,5-trimethyl benzene as the swelling agent in an acidic condition. The mesoporous structure and textural features of FDU-12-HX (where H denotes the hydrothermal method and X denotes the synthesis temperature) samples were elucidated and probed using x-ray diffraction, N2 adsorption, 29Si magic angle spinning nuclear magnetic resonance, scanning electron microscopy and transmission electron microscopy. It has been demonstrated that the aging time can be significantly reduced from 72 to 2 h without affecting the structural order of the FDU-12 materials with a simple adjustment of the synthesis temperature from 100 to 200 °C. Among the materials prepared, the samples prepared at 200 °C had the highest pore volume and the largest pore diameter. Lysozyme adsorption experiments were conducted over FDU-12 samples prepared at different temperatures in order to understand their biomolecule adsorption capacity, where the FDU-12-HX samples displayed high adsorption performance of 29 μmol g-1 in spite of shortening the actual synthesis time from 72 to 2 h. Further, the influence of surface area, pore volume and pore diameter on the adsorption capacity of FDU-12-HX samples has been investigated and results are discussed in correlation with the textural parameters of the FDU-12-HX and other mesoporous adsorbents including SBA-15, MCM-41, KIT-5, KIT-6 and CMK-3.

  20. 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.

  1. 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.

  2. Hydrothermal synthesis of uniform WO{sub 3} submicrospheres using thiourea as an assistant agent

    SciTech Connect

    Su, X.T.; Xiao, F.; Lin, J.L.; Jian, J.K.; Li, Y.N.; Sun, Q.J.; Wang, J.D.

    2010-08-15

    Nearly monodisperse tungsten trioxide submicrospheres have been synthesized with tungsten acid and HCl as the starting materials and thiourea as a structure-directing agent through a facile hydrothermal method. The obtained products were characterized by X-ray diffraction, transmission electron microscopy, scanning electron microscopy and energy dispersive X-ray, respectively. The results show that the WO{sub 3} submicrospheres are monodisperse with a diameter of about 800-1000 nm. The morphology of the products gradually evolutes from rods to spheres with increase of the reaction time. The formation mechanism of the WO{sub 3} submicrospheres is primarily discussed.

  3. 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.

  4. 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.

  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. 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.

  7. Synthesis of magnetite octahedrons from iron powders through a mild hydrothermal method

    SciTech Connect

    Mao Baodong; Kang Zhenhui; Wang Enbo . E-mail: wangenbo@public.cc.jl.cn; Lian Suoyuan; Gao Lei; Tian Chungui; Wang Chunlei

    2006-12-14

    Magnetite (Fe{sub 3}O{sub 4}) octahedral particles were fabricated from iron powders through a simple one-step alkali-assisted hydrothermal process. The crystallinity, morphology, and structural features of the as-prepared magnetite particles were investigated using powder X-ray diffraction (XRD) and scanning electron microscopy (SEM). The values of saturation magnetization (M {sub s}) and coercivity (H) of the magnetite octahedrons characterized on a vibrating sample magnetometer (VSM) are 89.81 emu/g and 70.6 Oe, respectively. The concentration of NaOH and the reaction temperature played a key role in the formation of the magnetite octahedrons.

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  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. 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.

  14. Hydrothermal synthesis and photocatalytic properties of WO3 nanorods by using capping agent SnCl4·5H2O

    NASA Astrophysics Data System (ADS)

    Hu, Pengfei; Chen, Yong; Chen, Yue; Lin, Zehui; Wang, Zhongchang

    2017-08-01

    Hexagonal tungsten trioxide (h-WO3) nano-rods of different sizes are prepared via hydrothermal synthesis using a capping agent of SnCl4·5H2O. The size of the synthesized WO3 nanoparticles can be controlled by changing concentration of the capping agent SnCl4·5H2O alone. We also investigate microstructures and optical properties of the WO3 nanorods and propose a synthesis mechanism for the nanorods. The photocatalytic activities of the h-WO3 nanorods are evaluated by degradation of Rhodamine-B (RhB), revealing that these nanorods exhibit excellent photocatalytic properties. The capping agent SnCl4·5H2O is found to be critical to governing sizes and properties of the h-WO3 nanorods. Our results demonstrate that functional nano-crystallites with tunable size and morphology can be synthesized via a facile hydrothermal synthesis process by adjusting the concentration of capping agent alone. Such a facile hydrothermal synthesis process should be applicable to other types of nanomaterials and relevant to a wide range of applications.

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. Hydrothermal synthesis of Ni2P nanoparticle and its hydrodesulfurization of dibenzothiophene

    NASA Astrophysics Data System (ADS)

    Zhao, Qi; Han, Yang; Huang, Xiang; Dai, Jinhui; Tian, Jintao; Zhu, Zhibin; Yue, Li

    2017-04-01

    Nanosized nickel phosphide (Ni2P) has been synthesized via hydrothermal reaction with environmental-friendly red phosphorus and nickel chloride. The reaction mechanism has been studied by measurement techniques of IC, XRD ,TEM, EDS, and XPS. The results showed that the particle sizes of as-prepared Ni2P are in nanoscale ranging from 10 to 30 nm. In hydrothermal reaction, red phosphorus reacts with water to its oxyacids, especially its hypophosphorous acid (or hypophosphite) which can reduce nickel chloride to nickel, and then metallic nickel will penetrate into the rest of red phosphorus to generate nano-Ni2P. Furthermore, the catalytic performance of as-synthesized Ni2P for the hydrodesulfurization of dibenzothiophene has been tested. It has been shown that the HDS reaction process over Ni2P catalyst agrees well with the pseudo-first order kinetic equation, and the HDS conversion can reach up to 43.83% in 5 h with a stable increasing catalytic activity during the whole examination process.

  6. 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.

  7. 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.

  8. Hydrothermal synthesis of Eu3+ doped yttria nanoparticles using a supercritical flow reaction system

    NASA Astrophysics Data System (ADS)

    Hayashi, Hiromichi

    2012-01-01

    Highly crystalline Eu3+ doped yttria nanoparticle was synthesized by hydrothermal reaction in supercritical water using a continuous flow reaction system (FHT). The reactants of Y(NO3)3/Eu(NO3)3 mixed solution and KOH solution were used as starting materials and that was heated quickly up to 350-450 °C under the pressure of 30 MPa for 0.1-15 s as reaction time. The XRD results revealed that the crystal phase of as-prepared particles was YOOH and converted into cubic-phase Y2O3 after annealing above 550 °C. Primarily particle size of the YOOH was as small as less than 50 nm, keeping after annealing at 800 °C. Effects of reaction time, annealing temperature and Eu doping amount on photoluminescence were examined. The as-prepared particles exhibited red emission without annealing at high temperatures whereas photoluminescent intensity at 612 nm was increased with an increase in the annealing temperature. Photoluminescent intensity was increased with an increase in the Eu doping amount until 4 mol % and saturated at 8 mol %. The photoluminescent property was compared with reference samples via conventional co-precipitation (CP) and batchwise hydrothermal (BHT) methods. The photoluminescent intensity for annealed samples increased in the order: FHT < BHT < CP owing to the increased particle size.

  9. 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%)

  10. 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.

  11. Hydrothermal synthesis and magnetic properties of CuO hollow microspheres

    SciTech Connect

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

    2014-01-01

    Graphical abstract: - Highlights: • CuO hollow microspheres were synthesized through hydrothermal route. • The possible growth mechanism was proposed according to the experimental results. • CuO hollow microspheres show an anomalous ferromagnetic behavior at 5 K and 300 K. - Abstract: In the present work, CuO hollow microspheres with the diameter about 2 μm were successfully synthesized through a facile hydrothermal method. The phase purity, morphologies and structure features of the as obtained products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and Raman spectroscopy, respectively. It was found that reaction temperature, reaction time and different volume ratios of ethanol and distilled water played important roles on the morphologies of the obtained CuO hollow microspheres. The possible formation mechanism was also proposed according to the corresponding experimental results. The magnetic properties were investigated by superconducting quantum interference device, revealing that the CuO hollow microspheres exhibited an anomalous ferromagnetic behavior at 5 K and 300 K. At the same time, the origin of the ferromagnetism in CuO hollow microspheres was also discussed.

  12. Microwave hydrothermal synthesis of AgInS{sub 2} with visible light photocatalytic activity

    SciTech Connect

    Zhang, Wenjuan; Li, Danzhen; Chen, Zhixin; Sun, Meng; Li, Wenjuan; Lin, Qiang; Fu, Xianzhi

    2011-07-15

    Highlights: {yields} AgInS{sub 2} nanoparticles were synthesized by a microwave hydrothermal method. {yields} This method involves no organic solvents, catalysts, or surfactants. {yields} AgInS{sub 2} showed higher activity for photocatalytic degradation MO than TiO{sub 2-x}N{sub x}. {yields} Holes, O{sub 2}{center_dot}{sup -}, and H{sub 2}O{sub 2} played an important role in the photocatalytic process. -- Abstract: AgInS{sub 2} nanoparticles with superior visible light photocatalytic activity were successfully synthesized by a microwave hydrothermal method. This method is a highly efficient and rapid route that involves no organic solvents, catalysts, or surfactants. The photocatalytic activity of AgInS{sub 2} nanoparticles was investigated through the degradation of dyes under visible light irradiation. Compared with TiO{sub 2-x}N{sub x}, AgInS{sub 2} has exhibited a superior activity for photocatalytic degradation MO under the same condition. The experiment results showed that superoxide radicals (O{sub 2}{center_dot}{sup -}), hydrogen peroxides (H{sub 2}O{sub 2}) and holes (h{sup +}) were the mainly active species for the degradation of organic pollutants over AgInS{sub 2}. Through the determination of flat band potential, the energy band structure of the sample was obtained. A possible mechanism for the degradation of organic pollutant over AgInS{sub 2} was proposed.

  13. Hydrothermal synthesis, crystal structure and luminescence of four novel metal organic frameworks

    NASA Astrophysics Data System (ADS)

    Song, Yi-Shan; Yan, Bing; Chen, Zhen-Xia

    2006-12-01

    Using the principle of crystal engineering, four novel metal-organic coordination polymers, {[Cd 1(nic)2(H 2O)]2[Cd 2(nic)2(H 2O)2]} n (1), [Cd 2(fma)2(phen)2] n (2), [Cd(fma)(bipy)(H 2O)] n (3) and [Zn(mal)(bipy)·3H 2O] n (4) (nic=nicotinate, fma=fumarate, mal=malate, phen=phenanthroline, bipy=2,2'-bipyridine) have been synthesized by hydrothermal reaction of M(CH 3COO)2·2H 2O ( M=Zn, Cd) with nicotinic acid, fumaric acid and cooperative L ( L=phen, bipy), respectively. X-ray analysis reveals that complex 1 possesses an unprecedented two-dimensional topology structure constructed from three-ply-like layers, complex 2 is an infinite 2D undulating network, complex 3 is a 1D zigzag chain and complex 4 belongs to a 1D chain. The results indicate a transformation of fumarate into malate during the course of hydrothermal treatment of complex 4. The photophysical properties have been investigated with luminescent excitation and emission spectra.

  14. 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+}.

  15. 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.

  16. 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.

  17. Zones of life in the subsurface of hydrothermal vents: A synthesis

    NASA Astrophysics Data System (ADS)

    Larson, B. I.; Houghton, J.; Meile, C. D.

    2011-12-01

    Subsurface microbial communities in Mid-ocean Ridge (MOR) hydrothermal systems host a wide array of unique metabolic strategies, but the spatial distribution of biogeochemical transformations is poorly constrained. Here we present an approach that reexamines chemical measurements from diffuse fluids with models of convective transport to delineate likely reaction zones. Chemical data have been compiled from bare basalt surfaces at a wide array of mid-ocean ridge systems, including 9°N, East Pacific Rise, Axial Seamount, Juan de Fuca, and Lucky Strike, Mid-Atlantic Ridge. Co-sampled end-member fluid from Ty (EPR) was used to constrain reaction path models that define diffuse fluid compositions as a function of temperature. The degree of mixing between hot vent fluid (350 deg. C) and seawater (2 deg. C) governs fluid temperature, Fe-oxide mineral precipitation is suppressed, and aqueous redox reactions are prevented from equilibrating, consistent with sluggish kinetics. Quartz and pyrite are predicted to precipitate, consistent with field observations. Most reported samples of diffuse fluids from EPR and Axial Seamount fall along the same predicted mixing line only when pyrite precipitation is suppressed, but Lucky Strike fluids do not follow the same trend. The predicted fluid composition as a function of temperature is then used to calculate the free energy available to autotrophic microorganisms for a variety of catabolic strategies in the subsurface. Finally, the relationships between temperature and free energy is combined with modeled temperature fields (Lowell et al., 2007 Geochem. Geophys., Geosys.) over a 500 m x 500 m region extending downward from the seafloor and outward from the high temperature focused hydrothermal flow to define areas that are energetically most favorable for a given metabolic process as well as below the upper temperature limit for life (~120 deg. C). In this way, we can expand the relevance of geochemical model predictions of

  18. 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.

  19. Hydrothermal synthesis of MoS2 nanoflowers as highly efficient hydrogen evolution reaction catalysts

    NASA Astrophysics Data System (ADS)

    Wang, Dezhi; Pan, Zhou; Wu, Zhuangzhi; Wang, Zhiping; Liu, Zhihong

    2014-10-01

    Amorphous MoS2 nanoflowers assembled by lamellar nanosheets have been successfully synthesized by a facile hydrothermal method. They were characterized by X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM), and evaluated as electrochemical catalysts in the hydrogen evolution reaction (HER). Moreover, the effect of preparation temperature was also discussed. It was found that these catalysts exhibited excellent HER activity compared to commercial bulk MoS2 microparticles due to the special structure of nanoflowers assembled by nanosheets with few layers, exposing much more active sites and reducing intrinsic resistance. And the catalyst obtained at 220 °C showed the best activity with the largest exchange current density and the smallest Tafel slope of 52 mV dec-1, which made it a promising HER electrocatalyst for practical applications.

  20. Continuous supercritical hydrothermal synthesis of iron oxide nanoparticle dispersions and their characterization

    NASA Astrophysics Data System (ADS)

    Daschner de Tercero, M.; Röder, C.; Fehrenbacher, U.; Teipel, U.; Türk, M.

    2014-04-01

    Electrostatically stabilized iron oxide nanoparticle dispersions were synthesized using a continuous hydrothermal process at 673 K and 30 MPa. The average size of the primary particles was in the range 5-30 nm. The influence of the flow conditions as well as the composition of the starting material on the dispersion properties was investigated. A new Raman spectroscopic measurement setup was used for the characterization of the structure of the nanoparticles in dispersed form. The use of differential centrifugal sedimentation for the determination of the size distribution of the dispersed particles proved to be convenient and powerful to determine the influence of the investigated parameters on the dispersion properties. For certain compositions of the starting material and flow conditions using a conventional T-union, narrow size distributions concerning both primary particles and agglomerates could be obtained.

  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. 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.

  3. 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.

  4. Hydrothermal synthesis of Graphene-TiO2 nanowire with an enhanced photocatalytic activity

    NASA Astrophysics Data System (ADS)

    Wu, Huitong; Fan, Jun; Yang, Yuhao; Liu, Enzhou; Hu, Xiaoyun; Ma, Yongning; Fan, Xiao; Tang, Chunni

    2015-07-01

    The hydrothermal method was used to synthesize TiO2 nanowire (NW) and then fabricate graphene-TiO2 nanowire nanocomposite (GNW). Graphene oxide (GO) was prepared via improved Hummers'method. GO reduction to graphene and hybridization between NW and graphene by forming chemical bonding. The as-prepared composites were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscope (SEM), transmission electron microscopy (TEM), and ultraviolet visible (UV-Vis) diffuse reflectance spectra. The photocatalytic activity was evaluated by the photodegradation of methylene blue (MB). The prepared GNW nanocomposite has superior photocatalytic activity in the degradation test, showing an impressive photocatalytic enhancement over NW. At the same time, in comparison with Graphene-TiO2 nanoparticle (NP) nanocomposite (GNP), GNW have a better activity which because NW have more uniform dispersion on graphene with less agglomeration.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. Hydrothermal synthesis and luminescent properties of novel ordered sphere CePO(4) hierarchical architectures.

    PubMed

    Yang, Mei; You, Hongpeng; Zheng, Yuhua; Liu, Kai; Jia, Guang; Song, Yanhua; Huang, Yeju; Zhang, Lihui; Zhang, Hongjie

    2009-12-21

    The ordered-sphere CePO(4) hierarchical architectures have been successfully synthesized by a simple hydrothermal method through the controlled growth of the CePO(4) nanorods and self-assemble hierarchical structure under various reaction conditions. The evolution of the morphology of the samples has been investigated in detail. It was found that the coexistence of citric acid and cetaltrimethylammonium bromide in the reaction system plays an important role in the formation of the spherical CePO(4) hierarchical architectures. A possible mechanism of the formation and growth of the hierarchical structure was suggested according to the experimental results and analysis. The effects of the reaction time as well as the variation of the morphologies on the luminescent properties of the products were also studied.

  10. 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.

  11. Sol-precipitation-hydrothermal synthesis and luminescence of GdPO4:Tb3+ submicron cubes

    NASA Astrophysics Data System (ADS)

    Cao, Yanyan; Sun, Peng; Liang, Yingmin; Wang, Rongrong; Zhang, Xiao

    2016-05-01

    GdPO4:Tb3+ submicron cubes were synthesized by a sol-precipitation-hydrothermal process. The XRD result indicated that GdPO4:Tb3+ submicron cubes have pure hexagonal phase. The SEM and TEM images confirmed the formation of cubic morphology. Under the excitation at 273 nm, GdPO4:Tb3+ submicron cubes show emission bands corresponding to Gd3+ and Tb3+. With the increasing Tb3+ concentration, the emission intensities originating from Gd3+ and 5D3 → 7Fj transition of Tb3+ decrease, but the emission intensities originating from 5D4 → 7Fj transition of Tb3+ increase. These results suggested energy transfer from Gd3+ to Tb3+ and the occurrence of cross-relaxation processes in GdPO4:Tb3+ submicron cubes.

  12. 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.

  13. Hydrothermal synthesis of Bi2WO6 hierarchical flowers with their photonic and photocatalytic properties

    NASA Astrophysics Data System (ADS)

    Dumrongrojthanath, Phattharanit; Thongtem, Titipun; Phuruangrat, Anukorn; Thongtem, Somchai

    2013-02-01

    Bi2WO6 hierarchical multi-layered flower-like assemblies were synthesized by a hydrothermal method at 180 °C for 24 h. XRD patterns were specified as pure orthorhombic well-crystallized Bi2WO6 phase. Their FTIR spectra show main absorption bands at 400-1000 cm-1, assigned as the stretching modes of the Bi-O and W-O, and W-O-W bridging stretching modes. SEM analysis shows that the product was 3D hierarchical flower-like assemblies, constructed by orderly arranged 2D layers of nanoplates. The UV-visible absorption shows an absorbance in the ultraviolet region with 3.4 eV band gap. Photocatalytic activity of Bi2WO6 hierarchical flowers was determined from the degradation of rhodamine-B by Xe light at 88% for 360 min irradiation.

  14. 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

  15. Hydrothermal synthesis of new wolframite type trimetallic materials and their use in oxidative dehydrogenation of propane.

    PubMed

    Salamanca, Maurin; Licea, Yordy E; Echavarría, Adriana; Faro, Arnaldo C; Palacio, Luz A

    2009-11-07

    With the aim of obtaining materials with properties for use as catalysts, two new trimetallic oxides containing Co or Ni and Mo and W were synthesized by a hydrothermal method, using milder conditions than those normally used for wolframite type solids. They were characterized by X-ray diffraction, Fourier transformed infrared spectroscopy, laser Raman spectroscopy, temperature-programmed reduction and atomic absorption spectroscopy, indicating that pure wolframite phases were formed. The X-ray diffraction studies confirmed the formation of the structure in the monoclinic system with cell parameters similar to nickel tungsten wolframite. The laser Raman and infrared spectra showed differences among the samples, mainly due to the incorporation of molybdenum atoms in the wolframite structure. Incorporation of molybdenum in the catalysts improved catalytic activity for propane oxidative dehydrogenation, and lower reaction temperatures were required in order to obtain similar propene yields as in bimetallic tungsten wolframites.

  16. 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.

  17. 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.

  18. Hydrothermal synthesis of Cu-Fe3O4 nanocomposites towards catalytic degradation of organic dyes

    NASA Astrophysics Data System (ADS)

    Han, Jishu; Sun, Xiaoxia; Zhao, Ruiyang; Gao, Hongtao; Wang, Lei

    2017-07-01

    Degradation of hazardous organic dyes utilizing multifunctional catalytic materials is supposed to be an efficient and promising method. Here, homogeneous Cu-Fe3O4 nanocomposites are synthesized through a facile and versatile one-pot hydrothermal method. The prepared Cu-Fe3O4 possesses spherical structure with rough surface and average diameter of 230 nm. High catalytic activity and structure stability make Cu-Fe3O4 nanocomposites effectively degrade rhodamine B, methylene blue, methyl orange, and congo red. The existence of magnetic Fe3O4 leads the nanocomposites to separate from the solution through external magnet and reuse for cycle degradation. And during the cyclic utilization, Cu-Fe3O4 nanocomposites keep high catalytic activity and, thus, could be used as an efficient degradation catalyst for the application of organic dyes.

  19. 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.

  20. Controlled synthesis of cadmium carbonate nanowires, nanoribbons, nanorings and sphere like architectures via hydrothermal method

    SciTech Connect

    Ashoka, S.; Nagaraju, G.; Thipperudraiah, K.V.; Chandrappa, G.T.

    2010-11-15

    Crystalline nanowires, nanoribbons, nanorings and sphere like architectures of cadmium carbonate have been synthesized with the spontaneous self-assembly of nanocrystals in aqueous solution under hydrothermal condition. The powder X-ray diffraction (PXRD) patterns of these materials exhibit phase pure hexagonal structure. The perfect circular nanorings with radius 375-437 nm, as a new member of nanostructured cadmium carbonate family are being reported for the first time. The width of the cadmium carbonate nanowires/nanoribbons and nanorings, respectively are found to be in the range 11-30 and 26-50 nm as observed by transmission electron microscope (TEM). The effect of temperature and concentration of urea on the cadmium carbonate morphology is discussed. The plausible growth mechanism for the formation of nanorings is also proposed.

  1. Mechanochemical?hydrothermal synthesis of hydroxyapatite from nonionic surfactant emulsion precursors

    NASA Astrophysics Data System (ADS)

    Chen, Chun-Wei; Riman, Richard E.; TenHuisen, Kevor S.; Brown, Kelly

    2004-10-01

    Nanocrystalline hydroxyapatite [HA, Ca10 (PO4)6 (OH)2] powders were synthesized by the mechanochemical-hydrothermal method using emulsion systems consisting of aqueous phase, petroleum ether (PE) as the oil phase and biodegradable Tomadol 23-6.5 as the nonionic surfactant. (NH4)2HPO4 and Ca (NO3)2 or Ca (OH)2 were used as the phosphorus and calcium sources, respectively. The calcium source and emulsion composition had significant effects on the stoichiometry, crystallinity, thermal stability, particle size and morphology of final products. Disperse HA crystals with a 160 nm length and aspect ratio of ca. 6 were formed in an emulsion system containing 10 wt% PE, 60 wt% water and 30 wt% surfactant. The HA particles had needle morphology with a specific surface area of 190m2 / g. With this technique, HA nanopowders with specific surface areas in the range of 72- 231m2 / g were produced.

  2. Vanadium oxide nanotubes VOx-NTs: Hydrothermal synthesis, characterization, electrical study and dielectric properties

    NASA Astrophysics Data System (ADS)

    Nefzi, H.; Sediri, F.

    2013-05-01

    Vanadium oxide nanotubes (VOx-NTs) have been synthesized via one-step hydrothermal treatment. The compounds were analyzed through X-ray powder diffraction; scanning electron microscope, UV-Visible spectroscopy, X-ray photoelectron spectroscopy (XPS) and complex impedance spectroscopy. The electrical and dielectric properties dependence on temperature (302-523 K) and on frequency (5 Hz to 13 MHz) of VOx-NTs have been reported. The complex impedance plots exhibits the presence of grain and grain boundaries. Dielectric data were analyzed using complex permittivity and complex electrical modulus for the sample at various temperatures. The presence of non-Debye type of relaxation has been confirmed by the complex modulus analysis. AC conductivity exhibits two conduction mechanisms: at high temperature, a translational motion with a sudden hopping and at low temperature, a localized hopping with a small hopping or reorientational motion. DC conductivity indicated, negative temperature coefficient of resistance (NTCR) type behavior.

  3. 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.

  4. 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.

  5. 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.

  6. Hydrothermal synthesis of carbonyl iron-carbon nanocomposite: Characterization and electromagnetic performance

    NASA Astrophysics Data System (ADS)

    Pourabdollahi, Hakimeh; Zarei, Ali Reza

    In this research, the electromagnetic absorption properties of the carbonyl iron-carbon (CI/C) nanocomposite prepared via hydrothermal reaction using glucose as carbon precursor was studied in the range of 8.2-12.4 GHz. In hydrothermal reaction, glucose solution containing CI particles, placed in autoclave for 4 h under 453 K. Using surface coating technology is a method that prevents Cl oxidation and improves CI electromagnetic absorption. The structure, morphology and magnetic performances of the prepared nanocomposites were characterized by X-ray diffraction (XRD), energy dispersive spectrometry (EDS), transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM). The electromagnetic properties including complex permittivity (εr), the permeability (μr), dielectric loss, magnetic loss, reflection loss, and attenuation constant were investigated using a vector network analyzer. For The CI/C nanocomposite, the bandwidth of -10 dB and -20 dB were obtained in the frequency range of 9.8-12.4 and 11.0-11.8 GHz, respectively. As well as, the reflection loss was -46.69 dB at the matching frequency of 11.5 GHz, when the matching thickness was 1.3 mm. While for CI particles the reflection loss for 4.4 mm thickness was -16.86 dB at the matching frequency of 12.3 GHz. The results indicate that the existence layer of carbon on carbonyl iron enhance the electromagnetic absorbing properties. Therefore, this nanocomposite can be suitable for in the radar absorbing coatings.

  7. Hydrothermal synthesis of lindgrenite with a hollow and prickly sphere-like architecture

    SciTech Connect

    Xu Jiasheng; Xue Dongfeng

    2007-01-15

    Lindgrenite [Cu{sub 3}(OH){sub 2}(MoO{sub 4}){sub 2}] with a hollow and prickly sphere-like architecture has been synthesized via a simple and mild hydrothermal route in the absence of any external inorganic additives or organic structure-directing templates. The hierarchical lindgrenite particles are hollow and prickly spheres, which are comprised of numerous small crystal strips that are aligned perpendicularly to the spherical surface. Two factors are important for the formation of hollow and prickly architecture in the present process. One is the general phenomenon of Ostwald ripening in solution, which can be responsible for the hollow structure; the other is that lindgrenite crystals have a rhombic growth habit, which plays an important role in the formation of prickly surface. Furthermore, Cu{sub 3}Mo{sub 2}O{sub 9} with the similar size and morphology can be easily obtained by a simple thermal treatment of the as-prepared lindgrenite in air atmosphere. - Graphical abstract: Lindgrenite [Cu{sub 3}(OH){sub 2}(MoO{sub 4}){sub 2}] with a hollow and prickly sphere-like architecture has been synthesized via a hydrothermal route. The hierarchical lindgrenite particles are hollow and prickly spheres, which are comprised of numerous crystal strips that are aligned perpendicularly to the spherical surface. Cu{sub 3}Mo{sub 2}O{sub 9} with the similar size and morphology can be easily obtained by a thermal treatment of the as-prepared lindgrenite.

  8. Hydrothermal synthesis of silico-manganese nanohybrid for Cu(II) adsorption from aqueous solution

    NASA Astrophysics Data System (ADS)

    Zhu, Qiufeng; Wang, Liting; An, Zehuan; Ye, Hong; Feng, Xudong

    2016-05-01

    A novel silico-manganese nanohybrid adsorbent (SMNA) was synthesized by a facile hydrothermal method, and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), nitrogen adsorption-desorption, Fourier transform infrared spectroscopy (FT-IR) and zeta potential measurement. The adsorption of Cu(II) ions from aqueous solution on the SMNA was investigated with variations in contact time, pH and initial Cu(II) concentration. The results showed that hydrothermal method would generate nanowire/nanorod incomplete crystallite (δ-MnO2) adsorbent. The adsorption of Cu(II) onto SMNA increased sharply within 25 min and reached equilibrium gradually. The maximum adsorption capacities of SMNA for Cu(II) were ∼40-88 mg g-1, which was lower than δ-MnO2 (92.42 mg g-1) but had a lower pH dependency. As compared with δ-MnO2, higher adsorption capacities of SMNA (7.5-15 wt% of silica doping amount) for Cu(II) could be observed when pH of the aqueous solution was low (<4). The pseudo-second-order model was the best choice to describe the adsorption behavior of Cu(II) onto SMNA, suggesting that the removal of Cu(II) by the as-prepared adsorbents was dominated by migration of Cu(II). The possibility of Cu(II) recovery was also investigated and it revealed that SMNA was a promising recyclable adsorbent for removal of heavy metal ions in water and wastewater treatment.

  9. WO3 nanorolls self-assembled as thin films by hydrothermal synthesis

    NASA Astrophysics Data System (ADS)

    Vankova, S.; Zanarini, S.; Amici, J.; Cámara, F.; Arletti, R.; Bodoardo, S.; Penazzi, N.

    2015-04-01

    We report a novel type of WO3 nanostructure, i.e. nanorolls obtained as a self-assembled thin film on a transparent conductive substrate. The mild conditions of preparation, avoiding the use of HCl, result in an eco-friendly hydrothermal method with reduced crystallization time. FESEM and HR-TEM show that WO3 nanocrystals are made of rolled nanoflakes with a telescope-like appearance at their tip. For their nano-porosity, electrochemical accessibility, good adhesion to substrates and the envisaged presence of nanocavities between the WO3 layers, these materials hold tremendous promise in nano-electronics, electrochromic devices, water photo-splitting cells, Li-ion batteries and nano-templated filters for UV radiation.We report a novel type of WO3 nanostructure, i.e. nanorolls obtained as a self-assembled thin film on a transparent conductive substrate. The mild conditions of preparation, avoiding the use of HCl, result in an eco-friendly hydrothermal method with reduced crystallization time. FESEM and HR-TEM show that WO3 nanocrystals are made of rolled nanoflakes with a telescope-like appearance at their tip. For their nano-porosity, electrochemical accessibility, good adhesion to substrates and the envisaged presence of nanocavities between the WO3 layers, these materials hold tremendous promise in nano-electronics, electrochromic devices, water photo-splitting cells, Li-ion batteries and nano-templated filters for UV radiation. Electronic supplementary information (ESI) available: Characterization techniques; additional FESEM micrographs; typical XRD pattern of WO3 nanoroll thin film; typical Nyquist plots at ambient temperature; indicative diameter and length of WO3 NR by varying the PVA chain length; effect of 2000 cycles of electrochemical switching on the STB, STC and ΔT% coloration efficiency of the WO3 NR. See DOI: 10.1039/c4nr07290a

  10. 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.

  11. 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}.

  12. 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.

  13. 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.

  14. Mg-doped VO2 nanoparticles: hydrothermal synthesis, enhanced visible transmittance and decreased metal-insulator transition temperature.

    PubMed

    Zhou, Jiadong; Gao, Yanfeng; Liu, Xinling; Chen, Zhang; Dai, Lei; Cao, Chuanxiang; Luo, Hongjie; Kanahira, Minoru; Sun, Chao; Yan, Liuming

    2013-05-28

    This paper reports the successful preparation of Mg-doped VO2 nanoparticles via hydrothermal synthesis. The metal-insulator transition temperature (T(c)) decreased by approximately 2 K per at% Mg. The Tc decreased to 54 °C with 7.0 at% dopant. The composite foils made from Mg-doped VO2 particles displayed excellent visible transmittance (up to 54.2%) and solar modulation ability (up to 10.6%). In addition, the absorption edge blue-shifted from 490 nm to 440 nm at a Mg content of 3.8 at%, representing a widened optical band gap from 2.0 eV for pure VO2 to 2.4 eV at 3.8 at% doping. As a result, the colour of the Mg-doped films was modified to increase their brightness and lighten the yellow colour over that of the undoped-VO2 film. A first principle calculation was conducted to understand how dopants affect the optical, Mott phase transition and structural properties of VO2.

  15. 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.

  16. 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.

  17. Hydrothermal synthesis of pencil-like SAPO-5 and observation of its reversed crystal-growth process.

    PubMed

    Yang, Qing; Li, Ming; Zeng, Changfeng; Zhang, Lixiong

    2013-01-02

    SAPO-5 with a novel hexagonal pencil-like morphology was hydrothermally synthesized from hydrogels that contain triethylamine and high concentrations of acetic acid at 180 °C for 48 h. The effect of the acetic acid concentration was examined and indicated that usage of a high concentration of acetic acid is crucial to the synthesis of SAPO-5 with a pencil-like morphology. The time-dependent growth process of novel SAPO-5 was observed by scanning electron microscopy with the aid of acid treatment to remove the amorphous materials for clearer observation. The samples were also characterized by X-ray diffraction and Fourier-transform infrared spectroscopy. The results show that the crystal growth at the early stage follows the reversed crystal-growth route. First, the crystallization occurs on the surface of the aggregated amorphous ellipsoidal particles to form a hexagonal prism crystal shell with the encapsulation of amorphous materials. Then, the amorphous materials wrapped inside start to grow to a hexagonal prism inside the hollow larger hexagonal prism shell. Finally, the interior hexagonal prism continues to grow to the two ends with its length beyond that of the larger one by means of the Ostwald ripening process, thus forming the pencil-like crystal. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. 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.

  19. 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.

  20. Electrical Properties of Nd-Doped BaTiO3 PTC Ceramics Prepared by Hydrothermal Synthesis

    NASA Astrophysics Data System (ADS)

    Hashishin, T.; Sato, E.; Umeki, S.; Kojima, K.; Tamaki, J.

    2011-10-01

    Nd-doped BaTiO3 nanopowders with ca. 200 nm in average diameter were prepared by hydrothermal synthesis at 200 and 240 °C for 24 h. Neodymium (III) nitrate hexahydrate (Nd(NO3)3·6H2O) as a donor dopant was added to the powder mixtures of barium hydroxide (Ba(OH)2) and titanium dioxide (TiO2) ranging from 0.25 to 0.45 mol%. A green compact of the powder mixtures obtained was heated at 1340 °C for 2 h with/without three steps of ramp heating processes. Sintered without these steps, 0.35 mol% Nd-doped BaTiO3 with the resistivity of 124 ohm·cm at R. T. indicated insufficient PTCR effect; resistance change of 3 × 102 in the vicinity of Curie temperature. On the other hand, a pellet of 0.35 mol% Nd-doped BaTiO3 sintered via the step-heating process exhibited the large resistance change of 7.5 × 103.

  1. 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

  2. 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.

  3. 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.

  4. Hydrothermal synthesis of bismuth ferrite Fenton-like catalysts and their properties

    NASA Astrophysics Data System (ADS)

    Zhou, Min; Li, Wenjuan; Du, Yong; Kong, Defen; Wang, Ze; Meng, Yi; Sun, Xiaolan; Yan, Tingjiang; Kong, Desheng; You, Jinmao

    2016-11-01

    Bismuth ferrite, Fenton-like catalysts have been successfully synthesized via simple hydrothermal methods without any templates. Through changing the molar ratio of Bi/Fe, the two main phases BiFeO3 and Bi25FeO40 can be synthesized under different temperatures. Furthermore, different morphologies of the BiFeO3 phase can be adjusted by changing different concentrations of HNO3 and NaOH which were used to dissolve the reactants and adjust the pH values in the prepared process. When the concentration of HNO3/NaOH was 8/12 M, some uniform cylindrical bodies with equal height (1 μm) and width (0.6 μm) were obtained, which have not been reported before. The uniform structures exhibited better activities in the photoassisted Fenton-like oxidation process for the degradation of rhodamine B (RhB) under visible light irradiation (420 nm < λ < 800 nm). Through the detection of the degradation mechanism, it showed that the concerted effect of the catalysts and H2O2 can increase the generation of the charge carriers and accelerate the photogenerated charge transfer between the catalysts and dyes. The BiFeO3 samples also showed magnetic properties at room temperature, which may have potential applications in multiferroic or magnetoelectric sensors and devices.

  5. 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.

  6. 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.

  7. Hydrothermal synthesis and crystal structure of BaV{sub 3}O{sub 8}

    SciTech Connect

    Oka, Yoshio; Yao, Takeshi; Yamamoto, Naoichi

    1995-07-01

    A single crystal of a barium vanadium oxide BaV{sub 3}O{sub 8} in a mixed valence state of V(V) and V(IV) has been grown hydrothermally from VO(OH){sub 2f} and BaCl{sub 2}. The black crystal with a rod-like shape exhibits the monoclinic system P2{sub 1} with a = 7.4347(11) {angstrom}, b = 5.5512(7) {angstrom}, c = 8.2012(7) {angstrom},{beta} = 107.179(8){degrees}, and Z = 2. The structural analysis led to R = 0.058 and R{sub w} = 0.021 for 1579 unique reflections. BaV{sub 3}O{sub 8} was revealed to adopt a layered structure made up of V{sub 3}O{sub 8} layers stacking along the c-axis with interstitial Ba{sup 2+} ions. The V-O framework of the V{sub 3}O{sub 8} layer consists of VO{sub 4} tetrahedra and VO{sub 6} octahedra connected by sharing vertices. The valence states of the V sites are differentiated as V(V) in the tetrahedral sites and as V(IV) in the octahedral sites.

  8. Disordered lithium niobate rock-salt materials prepared by hydrothermal synthesis.

    PubMed

    Modeshia, Deena R; Walton, Richard I; Mitchell, Martin R; Ashbrook, Sharon E

    2010-07-14

    An investigation of the one-step hydrothermal crystallisation of lithium niobates reveals that reaction between Nb(2)O(5) and aqueous LiOH at 240 degrees C yields materials with a disordered rock-salt structure where the metals are statistically distributed over the cation sites. This contrasts with the well-studied reaction between Nb(2)O(5) and NaOH or KOH that produces ANbO(3) (A = Na, K) perovskites. Powder neutron diffraction shows that materials prepared at short reaction times and lower LiOH concentration (2.5 M) are lithium deficient and have a slight excess of niobium, but that at longer periods of reaction in 5 M LiOH, close to the ideal, stoichiometric Li(0.75)Nb(0.25)O composition is produced. Upon annealing this phase cleanly transforms into the known ordered rock-salt material Li(3)NbO(4), a process we have followed using thermodiffractometry, which indicates that transformation begins at approximately 700 degrees C. Solid-state (93)Nb and (7)Li NMR of the disordered and ordered rock-salt phases shows that both contain single metal sites but there is clear evidence for local disorder in the disordered samples. For the ordered material, NMR parameters derived from experiment are also compared to those calculated using density functional theory and are shown to be in good agreement.

  9. 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.

  10. 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.

  11. Hydrothermal Synthesis, Microstructure and Photoluminescence of Eu3+-Doped Mixed Rare Earth Nano-Orthophosphates

    PubMed Central

    2010-01-01

    Eu3+-doped mixed rare earth orthophosphates (rare earth = La, Y, Gd) have been prepared by hydrothermal technology, whose crystal phase and microstructure both vary with the molar ratio of the mixed rare earth ions. For LaxY1–xPO4: Eu3+, the ion radius distinction between the La3+ and Y3+ is so large that only La0.9Y0.1PO4: Eu3+ shows the pure monoclinic phase. For LaxGd1–xPO4: Eu3+ system, with the increase in the La content, the crystal phase structure of the product changes from the hexagonal phase to the monoclinic phase and the microstructure of them changes from the nanorods to nanowires. Similarly, YxGd1–xPO4: Eu3+, Y0.1Gd0.9PO4: Eu3+ and Y0.5Gd0.5PO4: Eu3+ samples present the pure hexagonal phase and nanorods microstructure, while Y0.9Gd0.1PO4: Eu3+ exhibits the tetragonal phase and nanocubic micromorphology. The photoluminescence behaviors of Eu3+ in these hosts are strongly related to the nature of the host (composition, crystal phase and microstructure). PMID:21170409

  12. Room-temperature synthesis, hydrothermal recrystallization, and properties of metastable stoichiometric FeSe.

    PubMed

    Nitsche, F; Goltz, T; Klauss, H-H; Isaeva, A; Müller, U; Schnelle, W; Simon, P; Doert, Th; Ruck, M

    2012-07-02

    Room-temperature precipitation from aqueous solutions yields the hitherto unknown metastable stoichiometric iron selenide (ms-FeSe) with tetragonal anti-PbO type structure. Samples with improved crystallinity are obtained by diffusion-controlled precipitation or hydrothermal recrystallization. The relations of ms-FeSe to superconducting β-FeSe(1-x) and other neighbor phases of the iron-selenium system are established by high-temperature X-ray diffraction, DSC/TG/MS (differential scanning calorimetry/thermogravimetry/mass spectroscopy), (57)Fe Mössbauer spectroscopy, magnetization measurements, and transmission electron microscopy. Above 300 °C, ms-FeSe decomposes irreversibly to β-FeSe(1-x) and Fe(7)Se(8). The structural parameters of ms-FeSe (P4/nmm, a = 377.90(1) pm, c = 551.11(3) pm, Z = 2), obtained by Rietveld refinement, differ significantly from literature data for β-FeSe(1-x). The Mössbauer spectrum rules out interstitial iron atoms or additional phases. Magnetization data suggest canted antiferromagnetism below T(N) = 50 K. Stoichiometric non-superconducting ms-FeSe can be regarded as the true "parent" compound for the "11" iron-chalcogenide superconductors and may serve as starting point for new chemical modifications.

  13. 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

    2017-06-01

    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.

  14. 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.

  15. 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.

  16. 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.

  17. Simple hydrothermal synthesis of metal oxides coupled nanocomposites: Structural, optical, magnetic and photocatalytic studies

    NASA Astrophysics Data System (ADS)

    Ganeshraja, Ayyakannu Sundaram; Clara, Antoni Samy; Rajkumar, Kanniah; Wang, Yanjie; Wang, Yu; Wang, Junhu; Anbalagan, Krishnamoorthy

    2015-10-01

    The present article is focused on recent developments toward the preparation of room temperature ferromagnetic nanocomposites using better photocatalytic performance. These nanocomposites were successfully prepared by a simple hydrothermal method and their molecular formulas were confirmed as Ti0.90Sn0.10O2 (S1), 0.2CuO-Ti0.73Sn0.06Cu0.21O2-δ (S2), and Ti0.82Sn0.09Fe0.09O2-δ (S3). The ICP, XRD, DRS, FTIR, Raman, XAFS, XPS, EPR, SEM-EDX, HRSEM, HRTEM, photoluminescence and vibrating sample magnetometric measurements were employed to characterize the phase structures, morphologies, optical and magnetic properties of the photocatalysts. The local structures of Sn4+ and Fe3+ were confirmed by 119Sn and 57Fe Mössbauer analysis. The photocatalytic activities of the samples were evaluated by the degradation of methyl orange in water under visible light irradiation. Among the samples, tin doped TiO2 (S1) showed the best photocatalytic performance and stability.

  18. Hydrothermal synthesis, photoluminescence and photocatalytic properties of two silver(I) complexes

    NASA Astrophysics Data System (ADS)

    Yang, Yuan-Yuan; Zhou, Lin-Xia; Zheng, Yue-Qing; Zhu, Hong-Lin; Li, Wen-Ying

    2017-09-01

    Two new dinuclear silver(I) coordination complexes [Ag(Hntph)(tpyz)2/2]n1 and [Ag2(dtrz)2(Hntph)2] 2 (H2ntph=2-nitroterephthalic acid, tpyz=2,3,5-trimethylpyrazine, dtrz=3,5-dimethyl-4H-1,2,4-triazol-4-amine) have been obtained by hydrothermal reactions of Ag(I) salts with H2ntph and various N-donor ligands. Complex 1 exhibits a 2D layer structure constructed by the binuclear Ag2(Hntph)2 units and tpyz ligands. Complex 2 also shows a different binuclear unit Ag2(dtrz)2, which was assembled via hydrogen bonds interactions to a 3D supramolecular architecture. The photocatalytic experiments showed that complex 2 is an excellent visible light candidate for degradation of RhB, and the degradation ratio of RhB reached 91.4% after 7 h under the light of 90 W white LED lamp. Moreover, the photoluminescent properties and the optical band gaps of 1-2 have also been investigated.

  19. 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.

  20. Hydrothermal synthesis and processing of hydrogen titanate nanotubes for nicotine electrochemical sensing

    NASA Astrophysics Data System (ADS)

    Mersal, Gaber A. M.; Mostafa, Nasser Y.; Omar, Abd-Elkader H.

    2017-08-01

    Hydrogen titanate nanotubes (HTNT) were prepared via acid washing of hydrothermally synthesized sodium titantate nanotube. HTNTs with diameters in the range 7-9 nm and length of several hundred nanometers were annealed at different temperatures and used to modify carbon paste electrode (CPE). Cyclic and square wave voltammetric techniques were used to investigate the behavior of nicotine at HTNT modified carbon paste electrode (HTNTCPE). The nicotine-oxidation reaction over HTNTCPE was irreversible and adsorption process is the rate determining step. HTNTs annealed at 500 °C showed the best response to nicotine. The nicotine concentration was determined at the ideal conditions by square wave voltammetry (SWV). The calibration was linear from 0.1 to 500.0 µmol l-1 with a correlation coefficient of 0.995. The detection limits were found to be 0.005 µmol l-1. The present HTNTCPE was used to the determination of nicotine in two cigarette brands and it showed outstanding performance with respect to detection limit and sensitivity.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. Benzene-templated hydrothermal synthesis of metal-organic frameworks with selective sorption properties.

    PubMed

    Choi, Eun-Young; Park, Kyungsoo; Yang, Cheol-Min; Kim, Hyejin; Son, Jung-Ho; Lee, Soon W; Lee, Young Hee; Min, Dongwon; Kwon, Young-Uk

    2004-10-25

    In this paper, we report two metal-organic frameworks [Co3(ndc)3(bipyen)(1.5)]H2O (1) and [Co2(ndc)2bipyen)]C6H6.H2O (2) (bipyen=trans-1,2-bis(4-pyridyl)ethylene, H2ndc=2,6-naphthalenedicarboxylic acid). These compounds were both synthesized from identical hydrothermal reaction conditions except that benzene was added to the reaction for 2. Crystal structures show that the two compounds have triply interpenetrated three-dimensional frameworks and these frameworks have the same primary structure of a two-dimensional network of interconnected [Co2(O2CR)(4/2)] (R=naphthalene group) paddle-wheels and bridging bipyen ligands. Both compounds have guest water molecules and, in addition, 2 has guest benzene molecules. Structural transformations of the host accompanied guest removal, which can be monitored by powder X-ray diffraction. N2 adsorption data of 2 show that there are two different types of pores corresponding to the benzene and water pores. Upon exposure to vapors of several organic molecules, the heat-treated sample of 2 adsorbs benzene and cyclohexene, but does not adsorb toluene, (o-, m-, and p-)xylenes, cycloheptatriene, or cyclohexane.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. Hydrothermal Synthesis of SnQ (Q=Te, Se, S) and Their Thermoelectric Properties.

    PubMed

    Feng, Dan; Ge, Zhenhua; Chen, Yuexing; Li, Ju; He, Jiaqing

    2017-09-08

    Lead-free IV-VI semiconductors SnQ (Q=Te, Se, S) are deemed as promising thermoelectric materials. In this work, we designed a hydrothermal route to selectively synthesize single phase SnTe, SnSe and SnS nanopowders. For all three samples, the phase structure were characterized by X-ray diffraction, SnTe particles with octahedron structure and SnSe/SnS particles with plate-like shape were observed by field emission scanning electron microscopy and transmission electron microscopy, the formation mechanism was discussed in detail. Then, SnTe, SnSe and SnS nanopowders were densified by spark plasma sintering for investigating thermoelectric properties. It was noticed that SnSe and SnS exhibited remarkably anisotropy in both electrical and thermal properties attributed to the layered crystal structure. The highest ZT values 0.79 at 873 K, 0.21 at 773 K, and 0.13 at 773 K were achieved for SnTe, SnSe and SnS bulk samples, respectively. © 2017 IOP Publishing Ltd.

  16. 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).

  17. 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.

  18. 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

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

    NASA Astrophysics Data System (ADS)

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

    2015-01-01

    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.

  20. Hydrothermal synthesis of C3N4/BiOIO3 heterostructures with enhanced photocatalytic properties.

    PubMed

    Wang, Wenjun; Cheng, Hefeng; Huang, Baibiao; Liu, Xiaolei; Qin, Xiaoyan; Zhang, Xiaoyang; Dai, Ying

    2015-03-15

    The C3N4/BiOIO3 composites with heterostructures have been fabricated by simply depositing BiOIO3 on the surface of C3N4 at hydrothermal conditions, using bismuth nitrate and potassium iodate as precursors. C3N4 is an excellent organic semiconductor, which can be excited by visible light. BiOIO3 is a layered bismuth-based compound that has an internal polar field. Coupling C3N4 with BiOIO3 can combine the advantages of the two compounds and obtain better photocatalytic properties. X-ray diffraction, scanning electron microscopy, transmission electron microscopy and Fourier transformation infrared spectra have been carried out to confirm the structures and morphologies of as-prepared products. The absorption properties have been characterized by diffuse reflectance spectra and the photocatalytic activities have been evaluated by photodegradation of methyl orange, Rhodamine B and 2,4-dichlorophenol. Compared with C3N4, all C3N4/BiOIO3 composites exhibit better visible-light-driven photocatalytic properties. It is a synergetic effect that enables the composites to harvest light and promote charge separation, which eventually leads to the enhancement of the photocatalytic efficiencies. Under UV-vis light irradiation, C3N4/BiOIO3 composites also exhibit better activities, and the charge transfer process is similar to a redox mediator-free Z-scheme system. Copyright © 2014 Elsevier Inc. All rights reserved.

  1. 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

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

    PubMed

    Ramimoghadam, Donya; Bin Hussein, Mohd Zobir; Taufiq-Yap, Yun Hin

    2013-01-01

    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. 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. 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.

  3. Continuous production of phosphor YAG:Tb nanoparticles by hydrothermal synthesis in supercritical water

    SciTech Connect

    Hakuta, Yukiya; Haganuma, Tsukasa; Sue, Kiwamu; Adschiri, Tadafumi; Arai, Kunio

    2003-06-19

    Phosphor YAG:Tb ((Y{sub 2.7}Tb{sub 0.3})Al{sub 5}O{sub 12}) nano particles were synthesized by a hydrothermal method at supercritical conditions (400 deg. C and 30 MPa) using a flow reactor. Hydroxide sol solutions formed by stoichiometric aluminum nitrate, yttrium nitrate, terbium nitrate and potassium hydroxide solutions. The relationship between particle size and experimental variables including pH, concentration of coexistent ions and hydroxide sol were investigated. Particles were characterized by XRD, TEM and photo-luminescence measurements. Particle size of YAG:Tb became finer as pH was increased or potassium nitrate concentration of the starting metal salt solution was increased. By removing the coexisting ions (NO{sub 3}{sup -}, K{sup +}) from the metal salt solution, single phase YAG:Tb particles with 20 nm particle size were obtained. The emission spectra of YAG:Tb particles of 14 nm shows a blue shift.

  4. 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.

  5. Microwave hydrothermal synthesis and characterization of rare-earth stannate nanoparticles

    NASA Astrophysics Data System (ADS)

    Huang, Shuang; Xu, Hua-lan; Zhong, Sheng-liang; Wang, Lei

    2017-07-01

    Rare-earth stannate (Ln2Sn2O7 (Ln = Y, La-Lu)) nanocrystals with an average diameter of 50 nm were prepared through a facile microwave hydrothermal method at 200°C within 60 min. The products were well characterized. The effect of reaction parameters such as temperature, reaction time, pH value, and alkali source on the preparation was investigated. The results revealed that the pH value plays an important role in the formation process of gadolinium stannate (Gd2Sn2O7) nanoparticles. By contrast, the alkali source had no effect on the phase composition or morphology of the final product. Uniform and sphere-like nanoparticles with an average size of approximately 50 nm were obtained at the pH value of 11.5. A possible formation mechanism was briefly proposed. Gd2Sn2O7:Eu3+ nanoparticles displayed strong orange-red emission. Magnetic measurements revealed that Gd2Sn2O7 nanoparticles were paramagnetic. The other rare-earth stannate Ln2Sn2O7 (Ln = Y, La-Lu) nanocrystals were prepared by similar approaches.

  6. Vanadium oxide nanotubes VOx-NTs: Hydrothermal synthesis, characterization, electrical study and dielectric properties

    SciTech Connect

    Nefzi, H.; Sediri, F.

    2013-05-01

    Vanadium oxide nanotubes (VOx-NTs) have been synthesized via one-step hydrothermal treatment. The compounds were analyzed through X-ray powder diffraction; scanning electron microscope, UV–Visible spectroscopy, X-ray photoelectron spectroscopy (XPS) and complex impedance spectroscopy. The electrical and dielectric properties dependence on temperature (302–523 K) and on frequency (5 Hz to 13 MHz) of VOx-NTs have been reported. The complex impedance plots exhibits the presence of grain and grain boundaries. Dielectric data were analyzed using complex permittivity and complex electrical modulus for the sample at various temperatures. The presence of non-Debye type of relaxation has been confirmed by the complex modulus analysis. AC conductivity exhibits two conduction mechanisms: at high temperature, a translational motion with a sudden hopping and at low temperature, a localized hopping with a small hopping or reorientational motion. DC conductivity indicated, negative temperature coefficient of resistance (NTCR) type behavior. - Graphical abstract: The imaginary part of dielectric constant decreases with the increase in frequency at all temperatures and the values of ε´´ exhibit considerable frequency dispersion in the lower frequency range . Highlights: •Vanadium oxide nanotubes (VOx-NTs) were synthesized. •Non-debye type of relaxation has been confirmed. •AC conductivity exhibits two conduction mechanisms. •DC conductivity indicated negative temperature coefficient of resistance type behavior.

  7. 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.

  8. Hydrothermal synthesis of magnetite crystals: From sheet to pseudo-octahedron

    SciTech Connect

    Hu, Ming; Ji, Rui-Ping; Jiang, Ji-Sen

    2010-12-15

    In this paper, we developed a hydrothermal method to fabricate sheet-like and pseudo-octahedral magnetite crystals. X-ray diffraction (XRD) confirmed the products were pure spinel-structured magnetite. Scanning electron microscopy (SEM) was used to investigate the morphology of the obtained crystals. By carefully regulating the initial NaOH concentrations, the morphology of the products could be changed from sheet-like crystals to pseudo-octahedral crystals. Transmission electron microscopy (TEM) analysis indicated the sheet-like crystals were the oriented aggregation of nanoparticles. Pseudo-octahedral magnetite crystals were single crystalline, and were obtained by dissolution-recrystallization of the sheet-like crystals. Vibrating sample magnetometer (VSM)) suggested the magnetic properties of the products were strongly related to the morphology. The coercivity of the sheet-like magnetite crystals was 100 Oe, larger than 30 Oe of the pseudo-octahedral crystals, but the saturation magnetization of the sheet-like magnetite crystals was 40 emu/g, smaller than 85 emu/g of the pseudo-octahedral crystals.

  9. Hydrothermal Synthesis, Crystal Structure and Electrochemical Behavior of 2d Hybrid Coordination Polymer

    NASA Astrophysics Data System (ADS)

    Fan, Weiqiang; Zhu, Lin; Shi, Weidong; Chen, Fuxiao; Bai, Hongye; Song, Shuyan; Yan, Yongsheng

    2013-04-01

    A novel metal-organic coordination polymer [Cu(phen)(L)0.5(H2O)]n (H4L = (N,N‧-5,5‧-bis(isophthalic acid)-p-xylylenediamine, and phen = 1,10-phenanthroline) has been hydrothermally synthesized and characterized by elemental analysis, IR, TGA, and single-crystal X-ray diffraction. The crystallographic data show that the title compound crystallizes in monoclinic space group P21/n with a = 10.682(2), b = 15.682(3), c = 11.909(2) Å, β = 91.39(3)°, V = 1994.3(7) Å3, C24H17CuN3O5, Mr = 490.95, Dc = 1.635 g/cm3, F(000) = 1004, Z = 4, μ(MoKα) = 1.141 mm-1, the final R = 0.0418 and wR = 0.0983 for 3578 observed reflections (I > 2σ(I)). The structural analyses reveal that the title compound exhibits shows a 2D layer structure, which are further linked by hydrogen bonding interactions to form a three-dimensional supramolecular network. In addition, the thermal stability and electrochemical behavior of title compound has been studied. CCDC: 900413.

  10. 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.

  11. 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.

  12. Hydrothermal synthesis and structural characterization of two 1-D and 2-D Dawson-based phosphotungstates

    SciTech Connect

    Zhao Junwei; Zheng Shoutian; Liu Wei; Yang Guoyu

    2008-03-15

    Two new Dawson-based phosphotungstates (H{sub 2}en){sub 0.5}H[Cu(en){sub 2}(H{sub 2}O)]{sub 2}{l_brace}[Cu(en){sub 2}]({alpha}{sub 1}-P{sub 2}W{sub 17}CuO{sub 61}){r_brace}.8H{sub 2}O (1) (en=ethylenediamine) and [4,4'-H{sub 2}bpy]{sub 2}{l_brace}[Cu(4,4'-bpy){sub 3}][Cu(4,4'-bpy){sub 4}(H{sub 2}O){sub 2}]{sub 2}[Cu(4,4'-bpy)][{alpha}-P{sub 2}W{sub 1=} 8O{sub 62}]{sub 2}{r_brace}.6H{sub 2}O (2) (4,4'-bpy=4,4'-bipyridine) have been hydrothermally synthesized and structurally characterized. 1 crystallizes in the triclinic space group P-1 with a=11.7626(17), b=13.246(2), c=29.350(5) A, {alpha}=87.355(5), {beta}=79.583(5), {gamma}=66.993(3){sup o}, V=4138.3(11) A{sup 3}, Z=2, GOF=1.089, R{sub 1}=0.0563 and wR{sub 2}=0.1505, whereas 2 belongs to the orthorhombic space group Iba2 with a=22.277(8), b=47.04(2), c=22.153(8) A, V=23215(17) A{sup 3}, Z=4, GOF=1.051, R{sub 1}=0.0627 and wR{sub 2}=0.1477. 1 consists of a 1-D linear chain structure constructed from monocopper{sup II}-substituted Dawson polyoxoanions, while 2 represents the first 2-D sheet-like structure with a (4,4)-connected topological net built up from plenary Dawson-type polyoxoanions and Cu{sup II}-4,4'-bpy complex cations in polyoxometalate chemistry. - Graphical abstract: Two Dawson-based phosphotungstates (H{sub 2}en){sub 0.5}H[Cu(en){sub 2}(H{sub 2}O)]{sub 2}{l_brace}[Cu(en){sub 2}]({alpha}{sub 1}-P{sub 2}W{sub 17}CuO{sub 61}){r_brace}.8H{sub 2}O (1) and [4,4'-H{sub 2}bpy]{sub 2}{l_brace}[Cu(4,4'-bpy){sub 3}][Cu(4,4'-bpy){sub 4}(H{sub 2}O){sub 2}]{sub 2}[Cu(4,4'-bpy)][{alpha}-P{sub 2}W{sub 1=} 8O{sub 62}]{sub 2}{r_brace}.6H{sub 2}O (2) have been hydrothermally synthesized and structurally characterized. 1 consists of a 1-D linear chain structure constructed from monocopper-substituted Dawson polyoxoanions, while 2 represents the first 2-D sheet-like structure with a (4,4)-connected topological net built up from saturated Dawson-type polyoxoanions and Cu{sup II}-4,4'-bpy complex cations in

  13. 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.

  14. 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.

  15. Hydrothermal synthesis and electrical properties of NaNbO{sub 3}

    SciTech Connect

    Boukriba, M.; Sediri, F.; Gharbi, N.

    2013-02-15

    Graphical abstract: Display Omitted Highlights: ► Crystalline rhombohedral sodium niobate (r-NaNbO{sub 3}) were synthesized. ► Conductivity goes from 5.5 × 10{sup −6} Ω{sup −1} cm{sup −1} at 280 °C to 7.61 × 10{sup −4} Ω{sup −1} cm{sup −1} at 780 °C. ► Activation energies are in the order of 0.893, 0.507, 0.819 and 0.105 eV. -- Abstract: Triangular prism-like of crystalline rhombohedral sodium niobate (r-NaNbO{sub 3}) were prepared from Nb{sub 2}O{sub 5} in the presence of NaOH via a hydrothermal method at 180 °C for 6 h. Techniques X-ray diffraction, scanning electron microscopy, Fourier transform infrared, Raman and impedance spectroscopy have been used to characterize the structure, morphology, composition and electrical properties of the material. Electrical conductivity measurements showed that the as synthesized r-NaNbO{sub 3} triangular prism has a conductivity value which goes from 5.5 × 10{sup −6} Ω{sup −1} cm{sup −1} at 280 °C to 7.61 × 10{sup −4} Ω{sup −1} cm{sup −1} at 780 °C. The Arrhenius diagram is not linear; it presents four regions of conductivity. The corresponding activation energies are, respectively, in the order of 0.893, 0.507, 0.819 and 0.105 eV, deduced from the Arrhenius relation.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. Spectral and structural characteristics of Lu1 - x - y Ce x Tb y BO3 orthoborates prepared by the hydrothermal synthesis method

    NASA Astrophysics Data System (ADS)

    Shmurak, S. Z.; Kedrov, V. V.; Kiselev, A. P.; Fursova, T. N.; Rybchenko, O. G.

    2017-06-01

    The structure, IR absorption spectra, morphology, and photoluminescence spectral characteristics of Lu1- x- y Ce x Tb y BO3 solid solutions prepared by the hydrothermal synthesis method have been investigated. According to the X-ray powder diffraction data, the Lu1- x- y Ce x Tb y BO3 samples hydrothermally synthesized at a temperature T = 200°C have the vaterite structure, and all the observed diffraction peaks correspond to the hexagonal phase with the space group P63/ mmc, which is isostructural to pure lutetium borate LuBO3. Annealing of these samples at T = 970°C leads to a change in the structural modification and to the transition of the samples to the monoclinic phase with the space group C2/ c. It has been found that, after annealing of these samples at temperatures T = 800-970°C, the luminescence intensity of Tb3+ ions upon excitation in the absorption band of Ce3+ ions increases by more than two orders of magnitude and becomes much higher than that in compounds of the same composition, but prepared by high-temperature synthesis. At the same time, annealing of lutetium borate doped only with terbium does not lead to a significant change in the luminescence intensity of Tb3+ ions. The possible reasons for a multiple increase in the luminescence intensity of terbium ions due to the annealing of the hydrothermally synthesized lutetium orthoborate samples doped with cerium and terbium ions have been discussed.

  2. 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.

  3. 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.

  4. 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

  5. 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.

  6. 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).

  7. Shape-control by microwave-assisted hydrothermal method for the synthesis of magnetite nanoparticles using organic additives

    NASA Astrophysics Data System (ADS)

    Rizzuti, Antonino; Dassisti, Michele; Mastrorilli, Piero; Sportelli, Maria C.; Cioffi, Nicola; Picca, Rosaria A.; Agostinelli, Elisabetta; Varvaro, Gaspare; Caliandro, Rocco

    2015-10-01

    A simple and fast microwave-assisted hydrothermal method is proposed for the synthesis of magnetite nanoparticles. The addition of different surfactants (polyvinylpyrrolidone, oleic acid, or trisodium citrate) was studied to investigate the effect on size distribution, morphology, and functionalization of the magnetite nanoparticles. Microwave irradiation at 150 °C for 2 h of aqueous ferrous chloride and hydrazine without additives resulted in hexagonal magnetite nanoplatelets with a facet-to-facet distance of 116 nm and a thickness of 40 nm having a saturation magnetization of 65 Am2 kg-1. The use of polyvinylpyrrolidone led to hexagonal nanoparticles with a facet-to-facet distance of 120 nm and a thickness of 53 nm with a saturation magnetization of 54 Am2 kg-1. Additives such as oleic acid and trisodium citrate yielded quasi-spherical nanoparticles of 25 nm in size with a saturation magnetization of 70 Am2 kg-1 and spheroidal nanoparticles of 60 nm in size with a saturation magnetization up to 82 Am2 kg-1, respectively. A kinetic control of the crystal growth is believed to be responsible for the hexagonal habit of the nanoparticles obtained without additive. Conversely, a thermodynamic control of the crystal growth, leading to spheroidal nanoparticles, seems to occur when additives which strongly interact with the nanoparticle surface are used. A thorough characterization of the materials was performed. Magnetic properties were investigated by Superconducting Quantum Interference Device and Vibrating Sample magnetometers. Based on the observed magnetic properties, the magnetite obtained using citrate appears to be a promising support for magnetically transportable catalysts.

  8. 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.

  9. 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

  10. 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).

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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

  16. 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

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. Organotemplate-free hydrothermal synthesis of an aluminophosphate molecular sieve with AEN zeotype topology and properties of its derivatives.

    PubMed

    Wang, Yanyan; Sun, Yanjun; Mu, Ying; Zhang, Chuanqi; Li, Jiyang; Yu, Jihong

    2014-12-18

    A facile organotemplate-free route has been developed to synthesize an aluminophosphate molecular sieve in an alkali metal-containing system under hydrothermal conditions. The as-prepared JU93 possesses AEN zeotype topology with small 8-ring pores, and its derivatives show ion conductivity and adsorption selectivity of CO2 over CH4.

  5. Synthesis and characterization of carbon nanospheres obtained by hydrothermal carbonization of wood-derived and other saccharides

    Treesearch

    Qiangu Yan; Rui Li; Hossein Toghiani; Zhiyong Cai; Jilei Zhang

    2015-01-01

    Carbon nanospheres were synthesized by hydrothermal carbonization (HTC) of four different carbon sources: xylose, glucose, sucrose, and pine wood derived saccharides. The obtained carbon nanospheres were characterized for particle morphology and size, and surface functional groups. Morphological and structural differences among these saccharides derived HTC carbons...

  6. 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

  7. 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.

  8. 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. Copyright © 2016 Elsevier Inc. All rights reserved.

  9. 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

  10. 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.

  11. 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.

  12. Hydrothermal synthetic strategies of inorganic semiconducting nanostructures.

    PubMed

    Shi, Weidong; Song, Shuyan; Zhang, Hongjie

    2013-07-07

    Because of their unique chemical and physical properties, inorganic semiconducting nanostructures have gradually played a pivotal role in a variety of research fields, including electronics, chemical reactivity, energy conversion, and optics. A major feature of these nanostructures is the quantum confinement effect, which strongly depends on their size, shape, crystal structure and polydispersity. Among all developed synthetic methods, the hydrothermal method based on a water system has attracted more and more attention because of its outstanding advantages, such as high yield, simple manipulation, easy control, uniform products, lower air pollution, low energy consumption and so on. Precise control over the hydrothermal synthetic conditions is a key to the success of the preparation of high-quality inorganic semiconducting nanostructures. In this review, only the representative hydrothermal synthetic strategies of inorganic semiconducting nanostructures are selected and discussed. We will introduce the four types of strategies based on exterior reaction system adjustment, namely organic additive- and template-free hydrothermal synthesis, organic additive-assisted hydrothermal synthesis, template-assisted hydrothermal synthesis and substrate-assisted hydrothermal synthesis. In addition, the two strategies based on exterior reaction environment adjustment, including microwave-assisted and magnetic field-assisted hydrothermal synthesis, will be also described. Finally, we conclude and give the future prospects of this research area.

  13. Tailoring surface and photocatalytic properties of ZnO and nitrogen-doped ZnO nanostructures using microwave-assisted facile hydrothermal synthesis

    NASA Astrophysics Data System (ADS)

    Rangel, R.; Cedeño, V.; Ramos-Corona, A.; Gutiérrez, R.; Alvarado-Gil, J. J.; Ares, O.; Bartolo-Pérez, P.; Quintana, P.

    2017-08-01

    Microwave hydrothermal synthesis, using an experimental 23 factorial design, was used to produce tunable ZnO nano- and microstructures, and their potential as photocatalysts was explored. Photocatalytic reactions were conducted in a microreactor batch system under UV and visible light irradiation, while monitoring methylene blue degradation, as a model system. The variables considered in the microwave reactor to produce ZnO nano- or microstructures, were time, NaOH concentration and synthesis temperature. It was found that, specific surface area and volume/surface area ratio were affected as a consequence of the synthesis conditions. In the second stage, the samples were plasma treated in a nitrogen atmosphere, with the purpose of introducing nitrogen into the ZnO crystalline structure. The central idea is to induce changes in the material structure as well as in its optical absorption, to make the plasma-treated material useful as photocatalyst in the visible region of the electromagnetic spectrum. Pristine ZnO and nitrogen-doped ZnO compounds were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), specific surface area (BET), XPS, and UV-Vis diffuse reflectance spectroscopy. The results show that the methodology presented in this work is effective in tailoring the specific surface area of the ZnO compounds and incorporation of nitrogen into their structure, factors which in turn, affect its photocatalytic behavior.

  14. Hydrothermal synthesis, characterization, and thermal properties of alumino silicate azide sodalite, Na8[AlSiO4]6(N3)2

    NASA Astrophysics Data System (ADS)

    Borhade, A. V.; Wakchaure, S. G.; Dholi, A. G.; Kshirsagar, T. A.

    2017-07-01

    First time we report the synthesis, structural characterization and thermal behavior of an unusual N3 - containing alumino-silicate sodalite mineral. Azide sodalite, Na8[AlSiO4]6(N3)2 has been synthesized under hydrothermal conditions at 433 K in steel lined Teflon autoclave. The structural and microstructural properties of azide sodalite mineral was characterized by various methods including FT-IR, XRD, SEM, TGA, and MAS NMR. Crystal structure have been refined by Rietveld method in P\\bar 43n space group, indicating that the N3 - sodalite has cubic in lattice. High temperature study was carried out to see the effect of thermal expansion on cell dimension ( a o) of azide sodalite. Thermal behavior of sodalite was also assessed by thermogravimetric method.

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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. Copyright © 2013 Elsevier Inc. All rights reserved.

  1. 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.

  2. Ethanol-assisted hydrothermal synthesis and electrochemical properties of coral-like {beta}-Co(OH){sub 2} nanostructures

    SciTech Connect

    Tang Shaochun; Vongehr, Sascha; Wang Yang; Chen Lan; Meng Xiangkang

    2010-09-15

    Highly uniform, porous {beta}-Co(OH){sub 2} nanostructures with an appearance reminding of certain spherical corals were synthesized via a facile, one-step hydrothermal route using ethanol-water mixtures as solvents. The rough surfaces of the nanostructures consist of numerous randomly distributed, interconnecting nanoflakes, resulting in a network-like structure with many cavities. The coral-like product has a high Brunauer-Emmet-Teller specific surface area of 163 m{sup 2}/g. The diameter of the coral-like {beta}-Co(OH){sub 2} nanostructures is adjustable from 800 nm to 2 {mu}m. The effects of the ethanol/water ratio, the Co{sup 2+} concentration, the hydrothermal temperature, and the reaction time on the formation of the coral-like structures were investigated. Cyclic voltammetry and galvanostatic charge-discharge tests show that the {beta}-Co(OH){sub 2} possesses excellent capacitive properties. This is mainly attributed to the high porosity, which allows a deep penetration by electrolytes. - Abstract: Coral-like {beta}-Co(OH){sub 2} nanostructures were synthesized via a facile ethanol-assisted hydrothermal route. Their high porosity facilitates a deep penetration by electrolytes and thus contributes to the excellent capacitive properties.

  3. 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.

  4. One-step hydrothermal synthesis and electrochemical performance of sodium-manganese-iron phosphate as cathode material for Li-ion batteries

    NASA Astrophysics Data System (ADS)

    Karegeya, Claude; Mahmoud, Abdelfattah; Vertruyen, Bénédicte; Hatert, Frédéric; Hermann, Raphaël P.; Cloots, Rudi; Boschini, Frédéric

    2017-09-01

    The sodium-manganese-iron phosphate Na2Mn1.5Fe1.5(PO4)3 (NMFP) with alluaudite structure was obtained by a one-step hydrothermal synthesis route. The physical properties and structure of this material were obtained through XRD and Mössbauer analyses. X-ray diffraction Rietveld refinements confirm a cationic distribution of Na+ and presence of vacancies in A(2)', Na+ and small amounts of Mn2+ in A(1), Mn2+ in M(1), 0.5 Mn2+ and Fe cations (Mn2+,Fe2+ and Fe3+) in M(2), leading to the structural formula Na2Mn(Mn0.5Fe1.5)(PO4)3. The particles morphology was investigated by SEM. Several reactions with different hydrothermal reaction times were attempted to design a suitable synthesis protocol of NMFP compound. The time of reaction was varied from 6 to 48 h at 220 °C. The pure phase of NMFP particles was firstly obtained when the hydrothermal reaction of NMFP precursors mixture was maintained at 220 °C for 6 h. When the reaction time was increased from 6 to 12, 24 and 48 h, the dandelion structure was destroyed in favor of NMFP micro-rods. The combination of NMFP (NMFP-6H, NMFP-12H, NMFP-24H and NMFP-48H) structure refinement and Mössbauer characterizations shows that the increase of the reaction time leads to the progressive increment of Fe(III) and the decrease of the crystal size. The electrochemical tests indicated that NMFP is a 3 V sodium intercalating cathode. The comparison of the discharge capacity evolution of studied NMFP electrode materials at C/5 current density shows different capacities of 48, 40, 34 and 34 mA h g-1 for NMFP-6H, NMFP-12H, NMFP-24H and NMFP-48H respectively. Interestingly, all samples show excellent capacity retention of about 99% during 50 cycles.

  5. One-step hydrothermal synthesis and electrochemical performance of sodium-manganese-iron phosphate as cathode material for Li-ion batteries

    DOE PAGES

    Karegeya, Claude; Mahmoud, Abdelfattah; Vertruyen, Bénédicte; ...

    2017-06-23

    The sodium-manganese-iron phosphate Na2Mn1.5Fe1.5(PO4)3 (NMFP) with alluaudite structure was obtained by a one-step hydrothermal synthesis route. The physical properties and structure of this material were obtained through XRD and Mössbauer analyses. X-ray diffraction Rietveld refinements confirm a cationic distribution of Na+ and presence of vacancies in A(2)’, Na+ and small amounts of Mn2+ in A(1), Mn2+ in M(1) , 0.5 Mn2+ and Fe cations (Mn2+,Fe2+ and Fe3+) in M(2), leading to the structural formula Na2Mn(Mn0.5Fe1.5)(PO4)3. The particles morphology was investigated by SEM. Several reactions with different hydrothermal reaction times were attempted to design a suitable synthesis protocol of NMFP compound.more » The time of reaction was varied from 6 to 48 hours at 220°C. The pure phase of NMFP particles was firstly obtained when the hydrothermal reaction of NMFP precursors mixture was maintained at 220°C for 6 hours. When the reaction time was increased from 6 to 12, 24 and 48 hours, the dandelion structure was destroyed in favor of NMFP micro-rods. The combination of NMFP (NMFP-6H, NMFP-12H, NMFP-24H and NMFP-48H) structure refinement and Mössbauer characterizations shows that the increase of the reaction time leads to the progressive increment of Fe(III) and the decrease of the crystal size. The electrochemical tests indicated that NMFP is a 3 V sodium intercalating cathode. The comparison of the discharge capacity evolution of studied NMFP electrode materials at C/5 current density shows different capacities of 48, 40, 34 and 34 mAhg-1 for NMFP-6H, NMFP-12H, NMFP-24H and NMFP-48H respectively. Interestingly, all samples show excellent capacity retention of about 99 % during 50 cycles.« less

  6. 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.

  7. Effect of the mineralizer solution in the hydrothermal synthesis of gadolinium-doped (10% mol Gd) ceria nanopowders.

    PubMed

    Dell'Agli, Gianfranco; Spiridigliozzi, Luca; Marocco, Antonello; Accardo, Grazia; Ferone, Claudio; Cioffi, Raffaele

    2016-05-18

    Gadolinium-doped ceria is an attractive electrolyte material for potential application in solid oxide fuel cells (SOFCs) operating at intermediate temperatures typically with 10%-20% substitution of Ce+4 by Gd+3. In particular, 10% gadolinium-doped ceria seems to have the highest values of conductivities among the other dopant compositions. Nanosized powders of gadolinium-doped ceria were prepared by hydrothermal treatment using coprecipitate as a precursor and in the presence of 3 different mineralizer solutions. The powders obtained were characterized by X-ray diffraction analysis, scanning electron microscopy, transmission electron microscopy and thermal analysis, while the electrical behavior of the corresponding pellets were ascertained by AC impedance spectroscopy. Nanocrystalline gadolinium-doped ceria powders with fluorite cubic crystal structure were obtained by hydrothermal treatment. Independent of the mineralizer used, these powders were able to produce very dense ceramics, especially when selecting an optimized sintering cycle. In contrast, the electrical behavior of the samples was influenced by the mineralizer solution, and the samples synthesized in the neutral and alkaline solutions showed higher values of electrical conductivity, in the range of temperatures of interest. By the coprecipitation method, it has been possible to synthesize nanosized gadolinium-doped cerium oxide in a fluorite structure, stable in a wide range of temperatures. Hydrothermal treatment directly on the as-synthesized coprecipitates, without any drying step, had a very positive effect on the powders, which can be sintered with a high degree of densification, especially with an optimized sintering cycle. Furthermore, the electrical behavior of these samples was very interesting, especially for the samples synthesized using neutral mineralizer solution and basic mineralizer solution.

  8. 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.

  9. One-step hydrothermal synthesis of LiMn2O4 cathode materials for rechargeable lithium batteries

    NASA Astrophysics Data System (ADS)

    Lv, Xiawu; Chen, Shulin; Chen, Cheng; Liu, Lihu; Liu, Fan; Qiu, Guohong

    2014-05-01

    LiMn2O4 cathode materials with high discharge capacity and good cyclic stability were prepared by a simple one-step hydrothermal treatment of KMnO4, aniline and LiOH solutions at 120-180 °C for 24 h. The aniline/KMnO4 molar ratio (R) and hydrothermal temperature exhibited an obvious influence on the component and phase structures of the resulting product. The precursor KMnO4 was firstly reduced to birnessite when R was less than 0.2:1 at 120-150 °C. Pure-phased LiMn2O4 was formed when R was 0.2:1, and the LiMn2O4 was further reduced to Mn3O4 when R was kept in the range of 0.2-0.3 at 120-150 °C. Moreover, LiMn2O4 was fabricated when R was 0.15:1 at 180 °C. Octahedron-like LiMn2O4 about 300 nm was prepared at 120 °C, and particle size decreased with an increase in hydrothermal temperature. Especially, LiMn2O4 synthesized at 150 °C exhibited the best electrochemical performance with the highest initial discharge capacity of 127.4 mAh g-1 and cycling capacity of 106.1 mAh g-1 after 100 cycles. The high discharge capacity and cycling stability of the as-prepared LiMn2O4 cathode for rechargeable lithium batteries were ascribed to the appropriate particle size and larger cell volume.

  10. 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

  11. Hydrothermal synthesis of highly crystalline ZnO nanorod arrays: Dependence of morphology and alignment on growth conditions

    SciTech Connect

    Azzez, Shrook A.; Hassan, Z.; Alimanesh, M.; Rasheed, Hiba S.; Sabah, Fayroz A.; Abdulateef, Sinan A.; Hassan, J. J.

    2016-07-06

    Highly oriented zinc oxide nanorod were successfully grown on seeded p-type silicon 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

    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.

  13. Synthesis of anatase titania-carbon nanotubes nanocomposites with enhanced photocatalytic activity through a nanocoating-hydrothermal process

    NASA Astrophysics Data System (ADS)

    Wang, Qun; Yang, Dong; Chen, Daimei; Wang, Yabo; Jiang, Zhongyi

    2007-12-01

    Anatase TiO2 nanoparticles were covalently anchored onto acid-treated multi-walled carbon nanotubes (MWNTs) through a nanocoating-hydrothermal process to obtain TiO2-MWNTs nanocomposites. The composition and structural properties of the nanocomposites were characterized by XRD, BET, TG, TEM, HRTEM, EDX, XPS, and FTIR, and the formation of ester-bond linkage between TiO2 nanoparticles and MWNTs was demonstrated. The enhanced photocatalytic activity of TiO2-MWNTs nanocomposites was probed by photodegradation reaction of methylene blue under visible-light irradiation.

  14. Oxidation suppression during hydrothermal phase reversion allows synthesis of monolayer semiconducting MoS2 in stable aqueous suspension.

    PubMed

    Wang, Zhongying; Zhang, Yin-Jia; Liu, Muchun; Peterson, Andrew; Hurt, Robert H

    2017-05-04

    This letter demonstrates a simple method to achieve high-yields of 1H semiconducting MoS2 monolayers in concentrated, colloidally-stable aqueous suspension. The method is based on oxidation suppression during the hydrothermal processing step used for metal-to-semiconductor phase reversion. Accompanying DFT calculations on elementary steps in the MoS2 wet oxidation reaction suggest that a two-site corrosion mechanism is responsible for the observed high reactivity and low stability of 1T metallic MoS2.

  15. One-pot hydrothermal synthesis of silver nanoplates on optical fiber tip for surface-enhanced Raman scattering

    SciTech Connect

    Cao, Jie E-mail: mqinhe@aiofm.ac.cn; Zhao, Di; Lei, Xing; Liu, Ye; Mao, Qinghe E-mail: mqinhe@aiofm.ac.cn

    2014-05-19

    We report on surface-enhanced Raman scattering (SERS) fiber probe based on silver nanoplates which are fabricated on the tapered tip of the multimode fiber, by a simple, effective and low-cost hydrothermal method. The field-emission scanning electron microscopy and the transmission electron microscopy show that the obtained fiber probe is composed of nanoplates with the thickness of about 40 nm and an average length of 300 nm. The SERS activity of the tapered fiber probe with an optimal cone angle has demonstrated excellent results using the probing molecule of 4-aminothiophenol.

  16. 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.

  17. One step hydrothermal synthesis of transition metal based coordination polymers along with magnetic and electrical conductive Ag and Au nanospheres and rods

    NASA Astrophysics Data System (ADS)

    Agarwal, Rashmi A.

    2017-07-01

    Herein, a one step in situ co-synthesis of porous coordination polymers of Ni(II), Co(II) and Mn(II) encapsulating Ag/Ag2O and Au/Au2O3 nanoparticle clusters (spheres and rods) is reported by employing precursors of metal and PCPs, under hydrothermal conditions. No surfactant and reductant have been used. After synthesis of these clusters at high temperature they come out from the cavities of polymers and nucleation process continues inside the cavities. These Ag/Ag2O and Au/Au2O3 nanoclusters encapsulated frameworks show strong paramagnetic and ferromagnetic (soft) properties respectively at room temperature. While electrical characterization data shows that Ag/Ag2O/PCP displays very high conductivity in the range of 1.80×104 S/m which represents the higher end of semiconductance in comparison to Au/Au2O3/PCP which has conductance of 5.9×10-4 S/m representing semiconductivity in the lower mid range at room temperature.

  18. 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.

  19. 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.

  20. Surfactant-assisted hydrothermal synthesis of TiO2/reduced graphene oxide nanocomposites and their photocatalytic performances

    NASA Astrophysics Data System (ADS)

    Hu, Ju; Li, Hansheng; Muhammad, Sohail; Wu, Qin; Zhao, Yun; Jiao, Qingze

    2017-09-01

    Titanium dioxide/reduced graphene oxide nanocomposites (TiO2/RGO-X, X=S, T or C, was denoted sodium dodecyl benzene sulfonate, Triton X-100 and cetyl trimethyl ammonium bromide, respectively) were synthesized using a one-step surfactant-assisted hydrothermal method. The characterization of phase structure and morphology of the as-obtained nanocomposites reveals that TiO2 in the TiO2/RGO-X exhibits the morphologies of nanoparticles, nanowires and array-like nanowires on the surface of RGO, respectively. Compared with the control TiO2/RGO nanocomposite, TiO2/RGO-X presents an excellent photocatalytic activity. With uniform array-like TiO2 nanowires on the surface of RGO, the TiO2/RGO-C shows a significant enhancement in the photocatalytic efficiency. Besides, a deeper insight into the growth mechanism of TiO2/RGO nanocomposites is put forward. This work indicates that the surfactant-assisted hydrothermal method is an effective approach to improve the structure, morphology and photocatalytic performance of TiO2/RGO composites. Moreover, the surfactants with various types can interact with the precursors of TiO2 and RGO in different ways.

  1. 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)

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. Hydrothermal synthesis and characterization of hybrid Al/ZnO-GO composite for significant photodegrdation of dyes

    SciTech Connect

    Lellala, Kashinath; Namratha, K.; Byrappa, K. E-mail: kbyrappa@gmail.com; Sudhakar, K.

    2016-05-06

    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.

  8. Facile in situ hydrothermal synthesis of BiVO4/MWCNT nanocomposites as high performance visible-light driven photocatalysts

    NASA Astrophysics Data System (ADS)

    Liu, Bo; Li, Zhongyu; Xu, Song; Ren, Xiaolu; Han, Dandan; Lu, Dayong

    2014-08-01

    Visible-light responsive monoclinic BiVO4/MWCNT nanocomposites were facilely prepared via an in situ hydrothermal method by using sodium dodecyl sulfonate (SDS) as a guiding surfactant. The as-prepared BiVO4/MWCNT nanocomposites were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman spectroscopy, field emission scanning electron microscopy (FE-SEM), the Fourier transform infrared spectroscopy (FTIR) and UV-vis diffuse reflectance spectroscopy. The results showed that the hydrothermal temperature and adding SDS had significant influence on the morphology and size of BiVO4. The photocatalytic activities of BiVO4/MWCNT nanocomposites were investigated by degrading methylene blue (MB) under visible-light irradiation. Remarkable enhancement in photodecomposition of MB was observed with BiVO4/MWCNT composite compared with bare BiVO4 particles. This improvement of photocatalytic was attributed to the effective charge transfer from BiVO4 nanocrystals to MWCNT, which promoted the migration efficiency of photogenerated electron-hole. Furthermore, a possible mechanism for the photocatalytic oxidative degradation was also discussed.

  9. 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}.

  10. 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.

  11. 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.

  12. 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.

  13. 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. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. 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.

  15. Direct synthesis of Al-SBA-15 containing aluminosilicate species plugs in an acid-free medium and structural adjustment by hydrothermal post-treatment

    NASA Astrophysics Data System (ADS)

    Shi, Lei; Xu, Yan; Zhang, Na; Lin, Sen; Li, Xiangping; Guo, Peng; Li, Xuebing

    2013-07-01

    A series of Al-SBA-15 with controllable aluminosilicate plug structures inside straight mesopores has been hydrothermally synthesized in a one-step synthesis in an environmentally friendly acid-free medium, using triblock copolymer Pluronic P123 as a structure-directing agent, water as solvent, tetraethyl orthosilicate (TEOS) and aluminum nitrate (Al(NO)3·9H2O) as silica and aluminum sources, respectively. The effects of the P123/Si molar ratio in the initial solution and aging temperature on the structural properties of the resulting materials were investigated by powder X-ray diffraction (XRD), nitrogen adsorption-desorption at 77 K, transmission electron microscopy (TEM), scanning electron microscopy (SEM), thermogravimetric (TG), FT-IR spectra and inductively coupled plasma (ICP) analyses. The nature of the Al species and the acidity of the resultant samples were studied by solid state 27Al MAS NMR and pyridine adsorption measurements. The specific surface area (935-755 m2g-1), pore volume (1.03-0.56 cm3g-1) and especially the concentration and distribution of open type mesopores (0-68% to the total pores) of the synthesized Al-SBA-15 can be controlled by a simple adjustment of the P123/Si molar ratio in the initial solution. Moreover, increasing the aging temperature higher than 363 K can remarkably decrease the formation of plug structures to obtain “open” form mesopores. The observation by TEM of alternate defined gray and white areas inside the mesopores gives the strong evidence of isolated microporous aluminosilicate plugs inside the channels. In addition, a moderate hydrothermal post-treatment can finely modify the mesostructures through the partial or complete dissolution of the aluminosilicate plugs.

  16. Direct synthesis of Al-SBA-15 containing aluminosilicate species plugs in an acid-free medium and structural adjustment by hydrothermal post-treatment

    SciTech Connect

    Shi, Lei; Xu, Yan; Zhang, Na; Lin, Sen; Li, Xiangping; Guo, Peng; Li, Xuebing

    2013-07-15

    A series of Al-SBA-15 with controllable aluminosilicate plug structures inside straight mesopores has been hydrothermally synthesized in a one-step synthesis in an environmentally friendly acid-free medium, using triblock copolymer Pluronic P123 as a structure-directing agent, water as solvent, tetraethyl orthosilicate (TEOS) and aluminum nitrate (Al(NO){sub 3}·9H{sub 2}O) as silica and aluminum sources, respectively. The effects of the P123/Si molar ratio in the initial solution and aging temperature on the structural properties of the resulting materials were investigated by powder X-ray diffraction (XRD), nitrogen adsorption–desorption at 77 K, transmission electron microscopy (TEM), scanning electron microscopy (SEM), thermogravimetric (TG), FT-IR spectra and inductively coupled plasma (ICP) analyses. The nature of the Al species and the acidity of the resultant samples were studied by solid state {sup 27}Al MAS NMR and pyridine adsorption measurements. The specific surface area (935–755 m{sup 2}g{sup −1}), pore volume (1.03–0.56 cm{sup 3}g{sup −1}) and especially the concentration and distribution of open type mesopores (0–68% to the total pores) of the synthesized Al-SBA-15 can be controlled by a simple adjustment of the P123/Si molar ratio in the initial solution. Moreover, increasing the aging temperature higher than 363 K can remarkably decrease the formation of plug structures to obtain “open” form mesopores. The observation by TEM of alternate defined gray and white areas inside the mesopores gives the strong evidence of isolated microporous aluminosilicate plugs inside the channels. In addition, a moderate hydrothermal post-treatment can finely modify the mesostructures through the partial or complete dissolution of the aluminosilicate plugs. - Graphical abstract: The plugs-containing structures can be interpreted as the distribution of individual isolated plugs along the mesoporous channel. - Highlights: • Al-SBA-15 with controllable

  17. 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.

  18. 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.

  19. 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

  20. 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.

  1. 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.

  2. 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.

  3. 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

  4. 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)

  5. 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.

  6. 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.

  7. 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).

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. Hydrothermal synthesis of BiVO4/Bi2MoO6 composites with enhanced photocatalytic activity

    NASA Astrophysics Data System (ADS)

    Xu, Chaoqi; Qian, Hongzhi; Yong, Haibo; Huang, Xiaogu; Wang, Wei; Wen, Yan; Zhong, Kun; Zhou, Yingjie; Lai, Min

    2017-07-01

    BiVO4/Bi2MoO6 composites have been fabricated via the one-step hydrothermal method. The properties of composites were tailored by altering the V/Mo molar ratios. Photocatalytic activities were evaluated by measuring degradation of RhB under visible-light irradiation. BiVO4/Bi2MoO6 composites with V/Mo molar ratio of 8:1 possessing the optimal photocatalytic performance. The enhanced photocatalytic activity was attributed to the efficient charge carrier separation of composite heterostructures. In addition, the study of adsorption and photocatalytic activity suggested that a moderate amount of adsorption has a positive effect on photocatalytic reaction.

  13. Template-free hydrothermal synthesis different morphologies of visible-light-driven BiVO4 photocatalysts.

    PubMed

    Xu, Cai; Zhu, Gangqiang; Wu, Junlin; Liang, Jia

    2014-06-01

    Monoclinic BiVO4 nano- and microstructures with a diversity of well-defined morphologies, such as nanoplates, dendrite leaves-like structures, sub-microrods, and microflowers were synthesized via a template-free hydrothermal process with bismuth nitrate and ammonium metavanadate as metal source. The crystal structures, morphologies and optical properties of the as-prepared samples were characterized by X-ray powder diffraction (XRD), transmission electron microscope (TEM), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and UV-visible absorption spectra (UV-vis). Results showed that the pH value of the solution and the volume of ethylenediamine have great effect on the formation of these unique structures. The photocatalytic activity of these as-prepared samples had been tested by degradation of methylene blue under visible light, indicating that showed good photocatalytic performance.

  14. 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+.

  15. 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.

  16. Synthesis and characterization of Co-doped zinc oxide nanorods prepared by ultrasonic spray pyrolysis and hydrothermal methods

    NASA Astrophysics Data System (ADS)

    Febrianti, Y.; Putri, N. A.; Sugihartono, I.; Fauzia, V.; Handoko, D.

    2017-07-01

    ZnO nanorods was synthesized by using ultrasonic spray pyrolysis deposition process and grown by hydrothermal method on a glass substrate. The influences of varying Co doping in structural, morphological and optical properties were investigated by X-Ray Diffractometer (XRD), Scanning Electron Microscopy (SEM), and UV-Visible (UV-Vis) spectrometry, respectively. All the nanorods exhibit polycrystalline wurtzite structure with smaller crystalline size on the Co-doped nanorods. The nanorods also show no orientation alignment and random particle size. Interestingly, the nanorods with 3 wt.% Co doped shows high absorbance at UV and visible region indicating that optical properties of the ZnO nanorods have been modified by Co doping.

  17. Hydrothermal synthesis and electrochemical properties of KMn8O16 nanorods for lithium-ion battery applications.

    PubMed

    Zheng, Hao; Zhang, Qing; Kim, Seung-Joo; Jiang, Xueya; Dan, Meiyu; Gao, Hong; Li, Shengbiao; Wang, Shiquan; Feng, Chuanqi

    2013-04-01

    KMn8O16 nanorods were prepared through a facile hydrothermal method by using KMnO4 and MnSO4 as reactants. The KMn8O16 samples synthesized at different temperatures (100-160 degrees C) were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and its electrochemical properties were tested by galvanostatic charge/discharge system. The effect of reaction temperature on the morphology and electrochemical properties was investigated. As electrode materials for the lithium ion battery cycled between 1.5 and 4.2 V, the KMn8O16 nanorods synthesized at 160 degrees C show the highest reversible discharge capacity (160.1 mA h/g even after 50 cycles at current density of 50 mA/g) and the best cycling stability. These results indicate that the KMn8O16 nanorods could be a promising cathode material for lithium ion batteries.

  18. 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.

  19. 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.

  20. 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.