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Sample records for hydrothermal synthesis

  1. 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.

  2. 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

  3. 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.

  4. 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.

  5. 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.

  6. Hydrothermal synthesis map of bismuth titanates

    NASA Astrophysics Data System (ADS)

    Sardar, Kripasindhu; Walton, Richard I.

    2012-05-01

    The hydrothermal synthesis of four bismuth titanate materials from common bismuth and titanium precursors under hydrothermal conditions is described. Reaction of NaBiO3·2H2O and anatase TiO2 in concentrated NaOH solution at 240 °C is shown to produce perovskite and sillenite phases Na0.5Bi0.5TiO3 and Bi12TiO20, depending on the ratio of metal precursors used. When KOH solution is used and a 1:1 ratio of the same precursors, a pyrochlore Bi1.43Ti2O6(OH)0.29(H2O)0.66 is formed. The use of a mixture of HNO3 and NaOH is shown to facilitate the formation of the Aurivillius-type bismuth titanate Bi4Ti3O12. 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 LIII-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.

  7. 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.

  8. 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.

  9. Hydrothermal synthesis of vanadium pentoxide nanowires

    NASA Astrophysics Data System (ADS)

    Kumar, J. Santhosh; Thangadurai, P.

    2016-05-01

    Nanowires of V2O5 were prepared via hydrothermal route using NH4VO3 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 V2O5 when annealed at 500°C. Characteristic Raman peaks also expressed the same structural features. Microstructure analysis by SEM showed the nanowire structure of V2O5 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 V2O5.

  10. 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.

  11. 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.

  12. 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.

  13. Versatile hydrothermal synthesis of one-dimensional composite structures

    NASA Astrophysics Data System (ADS)

    Luo, Yonglan

    2008-12-01

    In this paper we report on a versatile hydrothermal approach developed to fabricate one-dimensional (1D) composite structures. Sulfur and selenium formed liquid and adsorbed onto microrods as droplets and subsequently reacted with metallic ion in solution to produce nanoparticles-decorated composite microrods. 1D composites including ZnO/CdS, ZnO/MnS, ZnO/CuS, ZnO/CdSe, and FeOOH/CdS were successfully made using this hydrothermal strategy and the growth mechanism was also discussed. This hydrothermal strategy is simple and green, and can be extended to the synthesis of various 1D composite structures. Moreover, the interaction between the shell nanoparticles and the one-dimensional nanomaterials were confirmed by photoluminescence investigation of ZnO/CdS.

  14. Hydrothermal synthesis of hexagonal magnesium hydroxide nanoflakes

    SciTech Connect

    Wang, Qiang; Li, Chunhong; Guo, Ming; Sun, Lingna; Hu, Changwen

    2014-03-01

    Graphical abstract: Hexagonal Mg(OH){sub 2} nanoflakes were synthesized via hydrothermal method in the presence of PEG-20,000. Results show that PEG-20,000 plays an important role in the formation of this kind of nanostructure. The SAED patterns taken from the different positions on a single hexagonal Mg(OH){sub 2} nanoflake yielded different crystalline structures. The structure of the nanoflakes are polycrystalline and the probable formation mechanism of Mg(OH){sub 2} nanoflakes is discussed. - Highlights: • Hexagonal Mg(OH){sub 2} nanoflakes were synthesized via hydrothermal method. • PEG-20,000 plays an important role in the formation of hexagonal nanostructure. • Mg(OH){sub 2} nanoflakes show different crystalline structures at different positions. • The probable formation mechanism of hexagonal Mg(OH){sub 2} nanoflakes was reported. - Abstract: Hexagonal magnesium hydroxide (Mg(OH){sub 2}) nanoflakes were successfully synthesized via hydrothermal method in the presence of the surfactant polyethylene glycol 20,000 (PEG-20,000). Results show that PEG-20,000 plays an important role in the formation of this kind of nanostructure. The composition, morphologies and structure of the Mg(OH){sub 2} nanoflakes were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HRTEM), and selected area electron diffraction (SAED). The SAED patterns taken from the different positions on a single hexagonal Mg(OH){sub 2} nanoflake show different crystalline structures. The structure of the nanoflakes are polycrystalline and the probable formation mechanism of Mg(OH){sub 2} nanoflakes is discussed. Brunauer–Emmett–Teller (BET) analysis were performed to investigate the porous structure and surface area of the as-obtained nanoflakes.

  15. 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

  16. Formation of Intermediate Carbon Phases in Hydrothermal Abiotic Organic Synthesis

    NASA Astrophysics Data System (ADS)

    Fu, Q.; Foustoukos, D. I.; Seyfried, W. E.

    2005-12-01

    With high dissolved concentrations of methane and other hydrocarbon species revealed at the Rainbow and Logatchev vent systems on the Mid-Atlantic Ridge, it is essential to better understand reaction pathways of abiotic organic synthesis in hydrothermal systems. Thus, we performed a hydrothermal carbon reduction experiment with 13C labeled carbon source at temperature and pressure conditions that approximate those inferred for ultramafic-hosted hydrothermal systems. Pentlandite, a common alteration mineral phase in subseafloor reaction zones, acted as a potential catalyst. Surface analysis techniques (XPS and ToF-SIMS) were used to characterize intermediate carbon species within this process. Time series dissolved H2 and H2S concentrations indicated thermodynamic equilibrium. Dissolved H2 and H2S concentrations of 13 and 2 mmol/kg, respectively, are approximately equivalent to measured values in Rainbow and Logatchev hydrothermal systems. Isotopically pure 13C methane and other alkane species (C2H6 and C3H8) were observed throughout the experiment, and attained steady state conditions. XPS analysis on mineral product surface indicated carbon enrichment on mineral surface following reaction. The majority of surface carbon involves species containing C-C or C-H bonds, such as alkyl or methylene groups. Alcohol and carboxyl groups in fewer amounts were also observed. ToF-SIMS analysis, which can offer isotope identification with high mass resolution, showed that most of these carbon species were 13C-labeled. Unlike gas phase Fischer-Tropsch synthesis, no carbide was observed on mineral product surface during the experiment. Therefore, a reaction pathway is proposed for formation of dissolved linear alkane species in hydrothermal abiotic organic synthesis, where oxygen-bearing organic compounds are expected to form in aqueous products by way of alcohol and carboxyl groups on mineral catalyst surface.

  17. Peptide synthesis under Enceladus hydrothermal condition

    NASA Astrophysics Data System (ADS)

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

    2016-07-01

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

  18. Prebiotic organic synthesis under hydrothermal conditions: an overview

    NASA Astrophysics Data System (ADS)

    Simoneit, Bernd R. T.

    Organic compounds which are obviously synthesized from inorganic precursors (e.g., CO) by hydrothermal activity are currently a research topic in prebiotic chemistry leading to the origin of life. However, such de novo products would be overwhelmed in present Earth environments, by an excess of thermal alteration (pyrolysis) products formed from contemporary life (e.g., hydrocarbons, alkanoic acids, etc.). Thus, organic syntheses must be demonstrated and distinguished from organic matter alteration initially in the laboratory and then in the field. Organic synthesis under hydrothermal conditions is theoretically possible and various established industrial processes are used to synthesize organic compounds from inorganic substrates with the aid of catalysts. A set of Strecker-type synthesis experiments has been carried out under hydrothermal conditions (150 °C), producing various amino acids. The formation of lipid compounds during an aqueous organic synthesis (Fischer-Tropsch-type) reaction was reported, using solutions of oxalic acid (also formic acid) as the carbon and hydrogen sources, and heating at discrete temperatures (50° intervals) from 100 to 400 °C. The maximum lipid yield, especially for oxygenated compounds was in the window of 150-250 °C. The compounds range from C6 to >C33, including n-alkanols, n-alkanoic acids, n-alkyl formates, n-alkanones, and n-alkanes, all with no carbon number preferences. These lipid compounds, especially the acids, can form lipid bilayers or micelles, potential precursors for membranes. Reductive condensation (i.e., dehydration) reactions also occur under simulated hydrothermal conditions and form amide, nitrile and ester bonds. The chemistry and kinetics of the condensation reactions are under further study and have the potential for oligomerization of acid-amides in aqueous medium. Abiotic organic compounds are not biomarkers per se because they do not originate from biosynthesis. Thus, they should be regarded as a

  19. 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

  20. Hydrothermal Synthesis of Meso-porous Materials using Diatomaceous Earth

    NASA Astrophysics Data System (ADS)

    Jing, Z.; Kato, S.; Maeda, H.; Ishida, E. H.

    2007-03-01

    In order to sustain the inherent properties of diatomaceous earth (DE), a low-temperature synthesis of mesoporous material from DE was carried out using a hydrothermal processing technique under saturated steam pressure at 200 °C for 12 h. The experimental results showed that the most important strength-producing constituent in the solidified specimens was tobermorite formed by hydrothermal processing, and the addition of slaked lime was favorable to tobermorite formation. At Ca/Si ratio around 0.83 in the starting material, tobermorite appeared to form readily. A high autoclave curing temperature (200 °C), or a longer curing time (12 h) seemed to accelerate the tobermorite formation, thus leading to a higher strength development.

  1. Surfactant-assisted hydrothermal synthesis of hydroxyapatite nanopowders.

    PubMed

    Bricha, Meriame; Belmamouni, Younes; Essassi, El Mokhtar; Ferreira, José M F; El Mabrouk, Khalil

    2012-10-01

    Rod-like hydroxyapatite nanoparticles (n-HAp) with a highly ordered nanostructure were prepared by hydrothermal synthesis from calcium chloride, and phosphoric acid, as calcium and phosphorus sources, respectively. Various surfactant families such as cationic (CTAB), anionic (SDS) and nonionic (Triton X-100) were used as regulators of the nucleation and crystal growth. The synthesized nanopowders were characterized using X-ray diffraction (XRD), Fourier transform infrared spectrograph (FTIR) and transmission electron microscopy (TEM). The rod-like morphology was obtained regardless of the surfactant used during the hydrothermal treatment, but the aspect ratio of the crystals was found to be surfactant dependent. The mechanism of crystal growth as well-oriented nanostructure is discussed. PMID:23421176

  2. 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.

  3. 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. PMID:25796392

  4. 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.

  5. Hydrothermal synthesis and structure of a potassium tantalum defect pyrochlore

    SciTech Connect

    Duan, N.; Tian, Z.R.; Willis, W.S.; Suib, S.L.; Newsam, J.M.; Levine, S.M.

    1998-09-07

    The synthesis and crystal structure of potassium tantalate (KTa{sub 2}(O,OH){sub 6}{center_dot}1.8H{sub 2}O) with a defect pyrochlore structure are reported. The compound was crystallized directly from tantalum pentoxide in basic solution under hydrothermal conditions at temperatures as low as 200 C. Ion exchange of this substance in acid yielded an H-type defect pyrochlore. Both highly crystalline K-type and H-type materials absorb argon and have BET surface areas of about 14 m{sup 2}/g. The crystal structures were refined by the Rietveld least-squares method from powder X-ray diffraction data. The final R{sub wp} and {chi}{sup 2} were 7.70% and 2.79, respectively. The high thermal stability and control of acidity of these materials, along with the simple and cheap synthesis, may find many applications in sorption, catalysis, and microelectronics.

  6. 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

  7. 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. PMID:26056279

  8. 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.

  9. Hydrothermal synthesis of Mg-Al hydrotalcites by urea hydrolysis

    SciTech Connect

    Rao, M. Mohan . E-mail: mandapati@iict.res.in; Reddy, B. Ramachandra; Jayalakshmi, M.; Jaya, V. Swarna; Sridhar, B.

    2005-02-15

    We report a simple method to prepare hydrotalcites involving both urea hydrolysis and hydrothermal synthetic conditions. Out of a series of Mg/Al ratios tried, pure hydrotalcite like phase was obtained for Mg/Al ratios of 1:1 and 2:1. Unlike in conventional co-precipitation method we succeeded in preparing Mg/Al ratio of 1:1 by this route. The high temperature (180 deg. C) applied and pressure developed in the autoclave during the synthesis might have altered the topochemical transformation. The materials were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, Fourier transform infrared, thermo gravimetric and differential thermal analysis and transmission electron microscopy.

  10. Peptide synthesis in simulated deep sea hydrothermal environments

    NASA Astrophysics Data System (ADS)

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

    The synthesis of oligomeric biomolecules such as peptides is the key step marking the evolution from prebiotic chemistry to biochemistry[1]. While monomer synthesis has been demonstrated to proceed in high-energy impact shock, lightning, cavitation or UV-radiation^dominated environments,[2] monomer oligomerization requires lower energy yields,[3] typically found in geological settings such as deep-sea hydrothermal environments (DSHE). In particular, increasing temperatures are predicted to shift the thermodynamic equilibrium between amino acids and product peptide as well as between precursor and successor peptide toward the product oligopeptide,[4,5] however, this hypothesis has not been tested experimentally. Using hydrothermal gold cells we demonstrate the formation of short peptides from the amino acid glycine in the temperature range 160°C to 260°C and 200 bar, conditions typical of DSHE. We show that glycine and product peptides enter into equilibrium and demonstrate a lowering of the Gibbs energies of diglycine and diketopiperazine formation from glycine with increasing temperature. Our results confirm that the thermodynamic stability of the peptide bond in diglycine and diketopiperazine increases relative to the free amino acid with increasing temperature.[4] They support a high temperature origin of life and the early emergence of peptides during chemical evolution. [1] Imai, E., Honda, H., Hatori, K., Brack, A. & Matsuno, K., (1999) Science, 283, 831. [2] Chyba, C.F. and Sagan, C. (1992) Nature 355, 125. [3] Kawamura K. and Yukioka M. (2001) Thermochim. Acta, 375, 9 [4] Shock, E.L. (1992) Geochim. Cosmochim. Acta, 56, 3481 [5] Amend J.P. and Helgeson H.C. (2000) Biophy. Chem., 84, 105.

  11. 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.

  12. 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

  13. 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

  14. Pyrrhotite catalyzes the synthesis of uracil under hydrothermal conditions

    NASA Astrophysics Data System (ADS)

    López Ibáñez de Aldecoa, A.; Menor-Salván, C.

    2013-09-01

    The hypothesis of a prebiotic origin for metabolic cycles in hydrothermal systems gained interest during last years. The experimental approach to support this hypothesis was oriented mainly to the formation of organic molecules in iron sulfide mineral surfaces from inorganic precursors. In this work, we explore the behavior of previously formed, prebiotically plausible organic molecules in iron sulfide rich, low temperature hydrothermal environments. Using urea as a starting point, we found that uracil and other nitrogen heterocycles could be synthesized using water-urea solution as precursor in a packed pyrrhotite bed reactor, simulating hydrothermal conditions.

  15. Hydrothermal Synthesis and Dielectric Properties of Lead Nickel Niobate Ceramics

    NASA Astrophysics Data System (ADS)

    Lu, Chung-Hsin; Hwang, Wen-Jeng

    1999-09-01

    Lead nickel niobate (Pb(Ni1/3Nb2/3)O3) has been prepared by a newly developed hydrothermal process. During the hydrothermal reaction at 250°C, a pyrochlore phase is formed. After calcining the 250°C-hydrothermally derived precursors at 750°C, a monophasic Pb(Ni1/3Nb2/3)O3 compound is successfully produced. Increasing the hydrothermal temperature significantly facilitates the formation of the perovskite phase. In comparison with the solid-state reaction, the hydrothermal process not only reduces the temperature for synthesizing Pb(Ni1/3Nb2/3)O3, but also decreases its particle size to the submicron range. The dielectric properties of Pb(Ni1/3Nb2/3)O3 strongly depend on the electric field frequency. Increasing the field frequency results in an increase in the apparent Curie temperature, which is associated with a decrease in the maximum dielectric permittivity. The critical exponent and diffuseness calculated by a modified permittivity-temperature equation verify the relaxor characteristics of Pb(Ni1/3Nb2/3)O3.

  16. 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...

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. Direct synthesis of thermochromic VO2 through hydrothermal reaction

    NASA Astrophysics Data System (ADS)

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

    2014-04-01

    Thermochromic VO2 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 VO2 powders. Ex-situ XRD studies after heat treatment confirmed the thermal stability of the VO2 structure. Thermochromic properties, as a consequence of the reversible structural transformation between monoclinic VO2 and tetragonal phases, were observed by Fourier transform infrared spectroscopy (FTIR).

  8. 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.

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

    NASA Technical Reports Server (NTRS)

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

    2006-01-01

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

  10. Hydrothermal synthesis and near in situ analysis of NiFe2O4 nanoparticles.

    PubMed

    Almeida, Trevor P; Fay, Mike; Zhu, Yanqiu; Brown, Paul D

    2012-11-01

    The hydrothermal synthesis (HS) of NiFe2O4 nanoparticles (NPs) has been investigated using a novel valve-assisted pressure autoclave. This approach has facilitated the rapid quenching of hydrothermal suspensions into liquid nitrogen, providing 'snapshots' representative of the near in situ physical state of the synthesis reaction products as a function of known temperature. The acquired samples were examined using complementary characterisation techniques of transmission electron microscopy and X-ray diffractometry (XRD). The HS of NiFe2O4 NPs (< 25 nm) at pH - 8 proceeded through the formation and dissolution of intermediate amorphous Fe(OH)3 and FeNi3Cl2(OH)8 x H2O sheets with increasing reaction temperature. The near in situ nature of the HS suspension resulted in the formation of NaCI by-product during drying in advance of XRD investigation, not during the HS process. PMID:23421289

  11. 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 +}.

  12. Hydrothermal synthesis, structural determination, and property characterization of transition metal sulfosalts and phosphates

    NASA Astrophysics Data System (ADS)

    Korzenski, Michael Burt

    Supercritical fluids are fascinating media for the synthesis of inorganic compounds. This is due in part to the tremendous versatility of these fluids, especially in providing access to unusual and kinetically stabilized solid phases. It is well understood that the ideal critical point of a solvent in a real solution has little meaning, and a gradual onset of critical properties with increasing temperature is normally observed, rather than a dramatic change in behavior at the magic critical point. In aqueous phases, the term hydrothermal is used for any reaction done in water above it sea level boiling point of 100°C while any reactions done above the critical point of 374°C are said to be supercritical. Hydrothermal synthesis has been used extensively over the past 150 years for the growth of large, high quality, single crystals of many known compounds, and has attained considerable significance over the last 50 years in industry for the growth of electronically important materials such as alpha-quartz and potassium titanyl phosphate (KTP). However, over the past two decades, many chemists have exploited the extraordinary solvating power of hydrothermal fluids for preparative inorganic synthesis, particularly for the preparation of zeolite-type materials. Much of this work was undertaken in the temperature range of 115 to 250°C, and thus work near the supercritical parameters of water (Tc = 374°C Pc = 221 bar) has been largely ignored due to the technological demands of aqueous systems at elevated temperatures and pressures. Therefore, we have decided to explore hydrothermal routes to both novel and known solid-state compounds which possess interesting physical properties. We have chosen to investigate a class of chalcopnictides and phosphates because of their structural diversity which promotes the preparation of chains, sheets and three-dimensional networks.

  13. Coprecipitation-assisted hydrothermal synthesis of PLZT hollow nanospheres

    SciTech Connect

    Zhu, Renqiang; Zhu, Kongjun; Qiu, Jinhao; Bai, Lin; Ji, Hongli

    2010-08-15

    Lanthanum-modified lead zirconate titanate Pb{sub 1-x}La{sub x}(Zr{sub 1-y}Ti{sub y})O{sub 3} (PLZT) hollow nanospheres have been successfully prepared via a template-free hydrothermal method using the well-mixed coprecipitated precursors and the KOH mineralizer. The structure, composition, and morphology of the PLZT hollow nanospheres were characterized by XRD (X-ray diffraction), ICP (inductive coupled plasma emission spectrometer), FTIR (Fourier transform infrared spectra), TG/DTA (thermogravimetric analysis and differential thermal analysis), TEM (transmission electron microscopy) and SEAD (selected area diffraction). The results show that the composition and the morphology control of the PLZT products are determined by the KOH concentration. The PLZT hollow nanospheres with uniform size of about 4 nm were synthesized in the presence of 5 M KOH. The crystalline nanoparticles can be prepared at dilute KOH, in contrast to the amorphous powders prepared at concentrated KOH. Formation mechanisms of the PLZT hollow nanospheres are also discussed.

  14. 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)

  15. Microwave-hydrothermal process for the synthesis of rutile

    SciTech Connect

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

    2005-11-03

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

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

    NASA Astrophysics Data System (ADS)

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

    2011-12-01

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

  17. FAST TRACK COMMUNICATION: A shortcut hydrothermal strategy for the synthesis of zinc nanowires

    NASA Astrophysics Data System (ADS)

    Hu, Jianqiang; Chen, Zhiwu; Xie, Jingsi; Yu, Ying

    2008-02-01

    Synthesis of metal nanowires has opened many new possibilities for designing ideal building blocks for future nanodevices. In this work, zinc nanowires with lengths of micrometre magnitude were synthesized in high yield by a shortcut hydrothermal strategy. The synthesis involves a template-free, non-seed and catalyst-free solution-phase process to high-quality zinc nanowires, which is low-cost and proceeds at relatively short time. In this process, zinc nanowires were prepared through the reduction of zinc acetate with absolute ethanol in the presence of silver nitrate under hydrothermal atmosphere. The strategy suggests that silver ion plays a vital role in the synthesis of zinc nanowires, without which the substituted product is zinc oxide nanowires. X-ray diffraction and energy-dispersive x-ray spectroscopy measurements confirm the final formation of zinc nanowires and component transformation from zinc oxide nanowires in the introduction of silver ion. We believe that with the efficient synthesis, longer zinc nanowires can be fabricated and may find potential applications for superconductors and nanodevices.

  18. 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.

  19. 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.

  20. 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.

  1. Hydrothermal Synthesis and Structural Characterization of Organically Templated Uranyl Diphosphonates

    SciTech Connect

    Adelani, Pius O.; Oliver, Allen G.; Albrecht-Schmitt, Thomas E.

    2011-03-09

    The hydrothermal treatment of uranyl nitrate and 1,4-benzenebisphosphonic acid with a variety of aliphatic amines (tetramethylammonium hydroxide, tetraethylammonium hydroxide, and diethyldimethylammonium hydroxide) and small quantities of hydrofluoric acid at 200 °C results in the crystallization of a series of layered uranyl diphosphonate compounds, [(CH3)4N][(UO2)3(O3PC6H4PO3H)2F(H2O)]·0.5H2O (Me4Ubbp), [(CH3CH2)4N](UO2)[C6H4(PO3H)(PO3H1.5)]2(H2O) (Et4Ubbp), and [(CH3CH2)2N(CH3)2][(UO2)3(O3PC6H4PO3H)2F(H2O)] (Et2Me2Ubbp). All these new compounds have layered structures, but the structures of Me4Ubbp and Et2Me2Ubbp are similar in that they both contain UO6F and UO7 pentagonal bipyramids within dimers that are bridged by the phosphonate into a three-dimensional structure. The structure of Et4Ubbp contains a single crystallographically unique UO7 unit. The edge-sharing pentagonal bipyramids are linked into chains formulated as (UO2)[C6H4(PO3H)(PO3H1.5)]2(H2O)1-. The voids in these structures are filled with the organic templates so that the overall charge balance is maintained. Intense fluorescence was observed from these compounds at room temperature.

  2. 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)

  3. Copper Mediated Hydrothermal Synthesis of Ultra Long Pentagonally Twinned Palladium Nanowires

    NASA Astrophysics Data System (ADS)

    Hanson, Jennifer

    Palladium nanowires (Pd NWs) have attracted considerable attention due to applications in hydrogen sensing and heterogeneous catalysis. Several methods have been reported for the synthesis of Pd NWs including using chemical vapor transport, electrodeposition in porous membranes, electron beam lithography, and colloidal self-assembly; however, it has been challenging to produce large quantities. Hydrothermal methods have been reported recently for the production of high yields of Pd NWs using palladium (II) chloride as a metal precursor, deionized water as the solvent, and polyvinylpyrrolidone for the NW capping agent. Reported prior methods have not been reproducible. With the introduction of trace amounts of Copper (II) ions synthesis is possible and aspect ratios of >500 have been obtained. It is likely that the deionized water used in the synthesis contained trace amounts of copper from metal pipes, thus leading to the synthesis of PdNWs. Copper ions have been shown to act as effective oxygen scavengers during the aqueous synthesis and we postulate that oxidative etching of multiply pentagonally twinned palladium seeds must be avoided in order to achieve high yields of palladium nanowires. This research focuses on the trace addition of copper ions and improvement of the Pd NW synthesis.

  4. Mechano-hydrothermal synthesis of Mg{sub 2}Al–NO{sub 3} layered double hydroxides

    SciTech Connect

    Zhang, Fengrong; Du, Na; Song, Shue; Liu, Jianqiang; Hou, Wanguo

    2013-10-15

    A mechano-hydrothermal method was developed to synthesize Mg{sub 2}Al–NO{sub 3} layered double hydroxide (LDH) from MgO, Al{sub 2}O{sub 3} and NaNO{sub 3} as starting materials. A two-step synthesis was conducted, that is, a mixture of MgO and Al{sub 2}O{sub 3} was milled for 1 h, followed by hydrothermal treatment with NaNO{sub 3} solution. The resulting LDHs were characterized by X-ray diffraction, transmission electron microscopy, scanning electron microscopy, Fourier transform infrared and elemental analyses. Pre-milling played a key role in the LDH formation during subsequent hydrothermal treatment. The process is advantageous in terms of low reaction temperature and short reaction time compared with the conventional hydrothermal method, and the target products are of high crystallinity, good dispersion and regular shape compared with the conventional mechanochemical method. - Graphical abstract: The novel mechano-hydrothermal route to synthesize LDH has advantages in low reaction temperature and short reaction time, and the target product was of high crystallinity, good dispersion and regular shape. Display Omitted - Highlights: • A mechano-hydrothermal route was developed for layered double hydroxide synthesis. • Synthesis could be achieved at low temperature and in a short time. • Resulting layered double hydroxide samples were well dispersed and of regular shape. • A dissolution–recrystallization mechanism was proposed for the formation process.

  5. 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

  6. 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.

  7. 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

  8. 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.

  9. 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.

  10. 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.

  11. Hydrothermal synthesis of La1-XSrXMnO3 dendrites

    NASA Astrophysics Data System (ADS)

    Makovec, Darko; Goršak, Tanja; Zupan, Klementina; Lisjak, Darja

    2013-07-01

    Single-crystalline dendrites of La1-XSrXMnO3 (LSMO) perovskite were synthesized using a simple hydrothermal method without the use of surfactants. The Sr2+, La3+, and Mn2+ ions were co-precipitated with aqueous NaOH under a flow of Ar. The aqueous suspension of the precipitates was hydrothermally treated in an autoclave filled with ambient air at temperatures ranging from 220 °C to 300 °C. The products were characterized using a combination of X-ray diffractometry (XRD) and transmission electron microscopy (TEM, HREM, EDXS). The dendrites formed either in a "tree-like" shape, with the trunk and the branches extending along the <111> directions of the quasi-cubic structure, or in the hexagonal shape of a "snowflake". The mechanism of the dendrite nucleation was proposed, based on phase development. During the hydrothermal treatment at lower temperatures the hexagonal platelet crystals of Sr1-XLaXMnO3 with the hexagonal perovskite structure form first. At higher temperatures the LSMO nucleates epitaxially at the edges of the hexagonal crystals and grows outward, forming the dendrite. To the best of our knowledge, this is the first report on the synthesis of crystalline dendrites of La1-XSrXMnO3 perovskite.

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

    NASA Technical Reports Server (NTRS)

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

    1995-01-01

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

  13. 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. PMID:11536697

  14. 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.

  15. A Two-Step Hydrothermal Synthesis Approach to Monodispersed Colloidal Carbon Spheres

    PubMed Central

    2009-01-01

    This work reports a newly developed two-step hydrothermal method for the synthesis of monodispersed colloidal carbon spheres (CCS) under mild conditions. Using this approach, monodispersed CCS with diameters ranging from 160 to 400 nm were synthesized with a standard deviation around 8%. The monomer concentration ranging from 0.1 to 0.4 M is in favor of generation of narrower size distribution of CCS. The particle characteristics (e.g., shape, size, and distribution) and chemical stability were then characterized by using various techniques, including scanning electron microscopy (SEM), FT-IR spectrum analysis, and thermalgravity analysis (TGA). The possible nucleation and growth mechanism of colloidal carbon spheres were also discussed. The findings would be useful for the synthesis of more monodispersed nanoparticles and for the functional assembly. PMID:20596393

  16. A benign hydrothermal synthesis of nanopencils-like zinc oxide nanoflowers

    NASA Astrophysics Data System (ADS)

    Akhoon, S. A.; Rubab, S.; Shah, M. A.

    2015-11-01

    Synthesis of zinc oxide (ZnO) nanoflowers and nanopencils is normally carried out with the help of structure-directing chemicals and templates. Besides releasing environmentally toxic substances, the use of these chemicals restricts the practical applications of nanostructures. In this paper, we report a typical template-free and environmentally benign synthesis of ZnO nanoflowers with nanopencils-like petals through a facile hydrothermal method. The as-synthesized ZnO nanoflowers were characterized using X-ray diffraction, field emission scanning electron microscopy, tunneling electron microscopy (TEM), high resolution TEM, and energy-dispersive X-ray spectroscopy techniques. The results reveal high quality and impurity-free hexagonal wurtzite phase ZnO nanoflowers of nanopencils-like petals having a length of 100-150 nm and a diameter of 45-60 nm.

  17. 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.

  18. Continuous-flow hydrothermal synthesis for the production of inorganic nanomaterials.

    PubMed

    Dunne, Peter W; Munn, Alexis S; Starkey, Chris L; Huddle, Tom A; Lester, Ed H

    2015-12-28

    As nanotechnology becomes increasingly important and ubiquitous, new and scalable synthetic approaches are needed to meet the growing demand for industrially viable routes to nanomaterial production. Continuous-flow hydrothermal synthesis or supercritical water hydrothermal synthesis (scWHS) is emerging as a versatile solution to this problem. The process was initially developed to take advantage of the tunable chemical and physical properties of superheated water to produce metal oxide nanoparticles by rapid nucleation and precipitation. The development of new mixing regimes and reactor designs has been facilitated by the modelling of reactor systems. These new reactor designs further exploit the properties of supercritical water to promote faster and more uniform mixing of reagent streams. The synthetic approach has been expanded beyond the metal oxide systems for which it was conceived, and now encompasses metal sulfides, metal phosphates, metal nanoparticles and metal-organic frameworks. In many of these cases, some degree of size and shape control can be achieved through careful consideration of both chemistry and reactor design. This review briefly considers the development of scWHS reactor technology, before highlighting some of our recent work in expanding the scope of this synthetic method to include a wide range of materials. PMID:26574533

  19. 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.

  20. Hydrothermal synthesis of vanadium nitride and modulation of its catalytic performance for oxygen reduction reaction

    NASA Astrophysics Data System (ADS)

    Huang, Taizhong; Mao, Shun; Zhou, Guihua; Wen, Zhenhai; Huang, Xingkang; Ci, Suqin; Chen, Junhong

    2014-07-01

    A creative hydrothermal synthesis method followed by calcination for vanadium nitride (VN) is reported. The oxygen reduction reaction (ORR) study of the catalyst shows that VN possesses a comparable catalytic performance to commercial Pt/C catalyst. The ORR catalytic activity study of vanadium nitride, vanadium carbonitride, and vanadium carbide reveals that tuning anions offers a promising route for the activity enhancement of the non-precious metal catalysts.A creative hydrothermal synthesis method followed by calcination for vanadium nitride (VN) is reported. The oxygen reduction reaction (ORR) study of the catalyst shows that VN possesses a comparable catalytic performance to commercial Pt/C catalyst. The ORR catalytic activity study of vanadium nitride, vanadium carbonitride, and vanadium carbide reveals that tuning anions offers a promising route for the activity enhancement of the non-precious metal catalysts. Electronic supplementary information (ESI) available: Experimental methods; SEM characterization of the catalysts; Tafel test of Pt/C catalyst; BET and cyclic performance tests of VN. See DOI: 10.1039/c4nr02646b

  1. 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. PMID:22983020

  2. 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

  3. 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

  4. 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. PMID

  5. Synthesis mechanism of nanoporous Sn3O4 nanosheets by hydrothermal process without any additives

    NASA Astrophysics Data System (ADS)

    Zhao, Jun-Hua; Tan, Rui-Qin; Yang, Ye; Xu, Wei; Li, Jia; Shen, Wen-Feng; Wu, Guo-Qiang; Zhu, You-Liang; Yang, Xu-Feng; Song, Wei-Jie

    2015-06-01

    Nanoporous anorthic-phase Sn3O4 nanosheets are successfully fabricated via a hydrothermal process without any additives. With the pH value of the precursor increasing from 2.0 to 11.8, the valence of the precursor changes from mixed valence (the ratio of Sn2+ to Sn4+ is 2.7:1) to pure bivalent, and the product transformed from Sn3O4 to SnO mesocrystals. When doping SbCl3 to the alkaline precursor, the valence of the precursor shows mixed valence with the ratio of Sn2+ to Sn4+ being 2.6:1 and Sn3O4 is synthesized after the hydrothermal process. The valence state of Sn species in the precursor is the key factor of the formation of Sn3O4. The synthesis mechanism is discussed and proposed. These experimental results expand the knowledge base that can be used to guide technological applications of intermediate tin oxide materials. Project supported by the National Natural Science Foundation of China (Grant Nos. 21377063, 51102250, 21203226, and 21205127) and the Personnel Training Foundation of Quzhou University (Grant No. BSYJ201412).

  6. 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.

  7. Hydrothermal degradation of lignin: products analysis for phenol formaldehyde adhesive synthesis.

    PubMed

    Yang, Sheng; Yuan, Tong-Qi; Li, Ming-Fei; Sun, Run-Cang

    2015-01-01

    Corncob lignin was treated with pressurized hot water in a cylindrical autoclave in current investigation. With the aim of investigating the effect of reaction temperature and retention time on the distribution of degradation products, the products were divided into five fractions including gas, volatile organic compounds, water-soluble oil, heavy oil, and solid residue. It was found that hydrothermal degradation of corncob lignin in pressurized hot water produced a large amount of phenolic compounds with lower molecular weight than the raw lignin. Some phenolic and benzene derivatives monomers such as vanillin, 2-methoxy-phenol, 2-ethyl-phenol, p-xylene, and 1, 3-dimethyl-benzene were also identified in the degradation products. The products were further analyzed by GC-MS, GPC, 2D-HSQC, and (31)P-NMR to investigate their suitability for partial incorporation into phenol formaldehyde adhesive as a substitution of phenol. The results indicated that the reaction temperature had more effect on the products distribution than the retention time. The optimal condition for heavy oil production appeared at 290 °C with retention time 0 min. The compounds of heavy oil had more active sites than the raw lignin, suggesting that the heavy oil obtained from hydrothermal degradation of lignin is a promising material for phenol formaldehyde adhesive synthesis. PMID:25109457

  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). PMID:19817366

  9. Direct hydrothermal synthesis of ternary Li-Mn-O oxide ion-sieves.

    PubMed

    Zhang, Qin-Hui; Sun, Shu-Ying; Li, Shao-Peng; Yin, Xian-Sheng; Yu, Jian-Guo

    2009-04-01

    Spinel-type ternary LiMn(2)O(4) oxide precursor was synthesized by direct hydrothermal synthesis of Mn(NO(3))(2), LiOH, and H(2)O(2) at 383 K for 8 h, a better technique for controlling the nanocrystalline structure with well-defined pore size distribution and high surface area than the traditional solid state reaction method. The final low-dimensional MnO(2) nanorod ion-sieve with a lithium ion selective adsorption property was further prepared by an acid treatment process to completely extract lithium ions from the Li-Mn-O lattice. The effects of hydrothermal reaction conditions on the nanostructure, chemical stability, and ion-exchange property of the LiMn(2)O(4) precursor and MnO(2) ion-sieve were systematically examined via powder X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), selected-area electron diffraction (SAED), and lithium ion selective adsorption measurements. The results show that this new kind of low-dimensional MnO(2) nanorod can be used for lithium extraction from aqueous environments, including brine, seawater, and waste water. PMID:19426343

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

    NASA Astrophysics Data System (ADS)

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

    2015-02-01

    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.

  11. 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).

  12. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2015-07-01

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

  14. Hydrothermal synthesis and investigation of optical properties of Nb5+-doped lithium silicate nanostructures

    NASA Astrophysics Data System (ADS)

    Alemi, Abdolali; Khademinia, Shahin; Joo, Sang Woo; Dolatyari, Mahboubeh; Bakhtiari, Akbar; Moradi, Hossein; Saeidi, Sorayya; Esmaeilzadeh, Alireza

    2014-01-01

    The hydrothermal synthesis and optical properties of Nb5+-doped lithium metasilicate and lithium disilicate nanomaterials were investigated. The microstructures and morphologies of the synthesized Li2 -2 x Nb2 x SiO3 + δ and Li2 -2 x Nb2 x Si2O5 + δ nanomaterials were studied by powder X-ray diffraction and scanning electron microscopy techniques, respectively. The synthesized niobium-doped lithium metasilicate and lithium disilicate nanomaterials, respectively, are isostructural with the standard bulk Li2SiO3 (space group Cmc21) and Li2Si2O5 (space group Ccc2) materials. The photoluminescence spectra of the synthesized materials are studied. The measured optical properties show dependence of the dopant amounts in the structure.

  15. Hydrothermal synthesis and investigation of optical properties of Nb5+-doped lithium silicate nanostructures

    NASA Astrophysics Data System (ADS)

    Alemi, Abdolali; Khademinia, Shahin; Joo, Sang Woo; Dolatyari, Mahboubeh; Bakhtiari, Akbar; Moradi, Hossein; Saeidi, Sorayya; Esmaeilzadeh, Alireza

    2014-03-01

    The hydrothermal synthesis and optical properties of Nb5+-doped lithium metasilicate and lithium disilicate nanomaterials were investigated. The microstructures and morphologies of the synthesized Li2-2 x Nb2 x SiO3 + δ and Li2-2 x Nb2 x Si2O5 + δ nanomaterials were studied with powder X-ray diffraction and scanning electron microscopy techniques, respectively. The synthesized niobium-doped lithium metasilicate and lithium disilicate nanomaterials, respectively, are isostructural with the standard bulk Li2SiO3 (space group Cmc21) and Li2Si2O5 (space group Ccc2) materials. Photoluminescence spectra of the synthesized materials are studied. The measured optical properties show dependence on the dopant amounts in the structure.

  16. Selective hydrothermally synthesis of hexagonal WS2 platelets and their photocatalytic performance under visible light irradiation

    NASA Astrophysics Data System (ADS)

    Vattikuti, S. V. Prabhakar; Byon, Chan; Chitturi, Veerendra

    2016-06-01

    Hexagonal WS2 platelets have been synthesized via simple hydrothermal synthesis method. The hexagonal WS2 is formed by the oriented attachment (OA)-self-assembly (SA). The thickness of the WS2 platelets was between ∼20 and 100 nm. The specific surface area of these platelets is 94.63 m2 g-1. The hexagonal WS2 platelets exhibited excellent photocatalytic activity compared to irregular WS2 platelets for the degradation of rhodamine B (RhB) under visible light irradiation. This work paves the method for designing hexagonal shaped WS2 platelets with great potential for a wide spectrum of applications in photocatalysis. Moreover, this synthetic procedure may open up an opportunity to tailor the morphologies of the other nanomaterials especially transition metal sulfides.

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

    NASA Astrophysics Data System (ADS)

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

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

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

    SciTech Connect

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

    2013-11-15

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

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

    PubMed Central

    Ma, Ming-Guo

    2012-01-01

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

  20. Low-temperature hydrothermal synthesis of S-doped TiO{sub 2} with visible light photocatalytic activity

    SciTech Connect

    Ho Wingkei; Yu, Jimmy C. . E-mail: jimyu@cuhk.edu.hk; Lee, Shuncheng

    2006-04-15

    A one-step low-temperature hydrothermal route was developed for the synthesis of S-doped TiO{sub 2} photocatalysts from TiS{sub 2} and HCl. Crystalline TiO{sub 2} was formed and sulfur could be efficiently doped into the anatase lattice under hydrothermal conditions. When the initial TiS{sub 2} concentration is increased, the content of S-dopant and optical absorption in the visible region also increase. The photocatalytic activity of the S-doped TiO{sub 2} was evaluated through the degradation of 4-chlorophenol under visible light irradiation. Our results show that the S-doped TiO{sub 2} prepared by this hydrothermal approach possesses much higher photocatalytic activity than that obtained by the traditional high-temperature thermal annealing method.

  1. Hydrothermal synthesis of mesostructured ZnO micropyramids with enhanced photocatalytic performance

    NASA Astrophysics Data System (ADS)

    Pudukudy, Manoj; Yaakob, Zahira

    2013-11-01

    The present article reports the synthesis, characterization and photocatalytic performance of highly oriented three dimensional ZnO micropyramids obtained by the surfactant assisted precipitation- hydrothermal treatment. Pluronic P-123 triblock copolymer was the surfactant employed in the present synthesis. The synthesized ZnO material was characterized for its phase and morphological studies. X-ray diffraction patterns suggested the formation of pure hexagonal wurtzite phase with the mean crystalline size of 39 nm. Electron microscopic studies of the material revealed the hexagonal micropyramid like morphology with an approximate size of 1-3 μm and the ZnO was found to be single crystalline by the SAED analysis. The ZnO micropyramids provided a bimodal mesoporous texture with a low specific surface area (4.5 m2/g). Optical properties investigated using the photoluminescence spectrum indicated that the ZnO has a broad UV and blue emission bands which were attributed due to the annihilation of excitons, and a broad visible green emission corresponds to the oxygen interstitial defects. Under the UV light illumination, several concentrations of methylene blue were degraded completely over the as-synthesized ZnO microcrystals for repeated cycles.

  2. 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.

  3. Synthesis and characterisations of SnO2 nanorods via low temperature hydrothermal method

    NASA Astrophysics Data System (ADS)

    Inderan, Vicinisvarri; Lim, Shin Ye; Ong, Teng Sian; Bastien, Samuel; Braidy, Nadi; Lee, Hooi Ling

    2015-12-01

    In the present study, tin oxide (SnO2) nanorods were successfully synthesized through hydrothermal treatment at a relatively low temperature (180 °C) using various concentrations of metal precursor, SnCl4·5H2O (0.04 M-0.16 M) in a mixed solution of ethanol and water before bringing the pH to 13 by adding 6 M NaOH. The effect of concentration on the morphology and structure of SnO2 were comprehensively studied using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), ultraviolet-visible spectroscopy (UV-vis) and Fourier Transform Infrared (FTIR). It was found that increasing the concentration of tin precursor from 0.04 M to 0.16 M leads to a complete conversion from nanospheres to nanoplates and finally to nanorods. The SEM results confirmed that SnO2 nanorods are obtained for concentrations up to 0.12 M. At synthesis condition of 0.12 M, SnCl4·5H2O and pH 13, single rutile nanorods with preferential growth in the [002] direction were obtained. It was found that the diameter of nanorods formed at 0.12 M is similar to that of nanoplates formed at 0.08 M (20 nm), which suggests that spear-shaped nanorods might have originated from the primary nanoparticles (the particles grown in lower concentration during hydrothermal treatment). Possible reaction mechanisms are proposed to explain the observed morphologies.

  4. 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.

  5. [Application of FTIR technique in microwave-hydrothermal synthesis of saponite].

    PubMed

    Yao, Ming; Liu, Zi-yang; Wang, Kai-xiong; Zhu, Miao-qin; Sun, Hong-jie

    2005-06-01

    FTIR was employed in the structure analysis of the saponites with an ideal chermical formula [Si6.5Al1.5]IV [Mg6]VI O20(OH)4 the starting gel synthesized by microwave-hydrothermally under different pressures (1 x 10(5), 5 x 10(5), 1.5 x 10(6), 2.5 x 10(6) and .5 x 10(6) Pa). It was found that low frequency absorption region in infrared spectrum was sensitive to the crystallization of the product and the amorphous materials produced in synthesis of saponite under the radiation of microwave. The absorptions belong to amorphous materials were decreased with increasing pressure. Saponite synthesized at 3.5 x 10(6) Pa showed no amorphous absorptions (1240, 90-602 cm(-1)), indicating the purity and quality of the synthetic mineral. It was worthy to note that Si(AI)-O stretching vibration infrared absorption could be regarded as an index in assessing the quality of synthetic 2:1 trioctahedral smectite sample with the same chemical compositions. With the increasing pressure, this strong vibration shifted to low frequency (1022, 1020, 1016, 1016, 1005 cm(-1)) in the medium frequency of the whole infrared spectrum. Since the sensitivity, easiness and simplicity, this infrared index would be meaningful in practical saponite-related minerals analysis. In addition, powder X-ray diffraction and scanning electronic microscopy were employed in charactering the saponite synthesized by microwave-hydrothermal method in this work. PMID:16201360

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

    SciTech Connect

    Kaowphong, Sulawan

    2012-05-15

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

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

    SciTech Connect

    Sobhani, Azam; Salavati-Niasari, Masoud

    2012-08-15

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

  8. Thermodynamic Potential for the Abiotic Synthesis of Adenine, Cytosine, Guanine, Thymine, Uracil, Ribose, and Deoxyribose in Hydrothermal Systems

    NASA Astrophysics Data System (ADS)

    Larowe, Douglas E.; Regnier, Pierre

    2008-10-01

    The thermodynamic potential for the abiotic synthesis of the five common nucleobases (adenine, cytosine, guanine, thymine, and uracil) and two monosaccharides (ribose and deoxyribose) from formaldehyde and hydrogen cyanide has been quantified under temperature, pressure, and bulk composition conditions that are representative of hydrothermal systems. The activities of the precursor molecules (formaldehyde and hydrogen cyanide) required to evaluate the thermodynamics of biomolecule synthesis were computed using the concentrations of aqueous N2, CO, CO2 and H2 reported in the modern Rainbow hydrothermal system. The concentrations of precursor molecules that can be synthesized are strongly dependent on temperature with larger concentrations prevailing at lower temperatures. Similarly, the thermodynamic drive to synthesize nucleobases, ribose and deoxyribose varies considerably as a function of temperature: all of the biomolecules considered in this study are thermodynamically favored to be synthesized throughout the temperature range from 0°C to between 150°C and 250°C, depending on the biomolecule. Furthermore, activity diagrams have been generated to illustrate that activities in the range of 10-2- 10-6 for nucleobases, ribose and deoxyribose can be in equilibrium with a range of precursor molecule activities at 150°C and 500 bars. The results presented here support the notion that hydrothermal systems could have played a fundamental role in the origin of life, and can be used to plan and constrain experimental investigation of the abiotic synthesis of nucleic-acid related biomolecules.

  9. 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%.

  10. One-pot hydrothermal synthesis of orange fluorescent silver nanoclusters as a general probe for sulfides.

    PubMed

    Lan, Jing; Zhang, Pu; Wang, Ting Ting; Chang, Yong; Lie, Shao Qing; Wu, Zhu Lian; Liu, Zhong De; Li, Yuan Fang; Huang, Cheng Zhi

    2014-07-01

    Water-soluble fluorescent silver nanoclusters (AgNCs) with almost seven and nine silver atoms and a quantum yield (QY) of 5.38 ± 0.25% were successfully prepared via one-pot hydrothermal synthesis using polymethacrylic acid sodium salt (PMAA-Na) as a template. The as-prepared PMAA-AgNCs displayed a mono-distribution, they were uniform in size and the color of the fluorescence, emitting at 579 nm, was orange when excited at 502 nm. What is more, we found that the as-prepared PMAA-AgNCs could be quenched by sulfides based on the formation of a metal-ligand bond Ag-S, and thus sulfides could be sensitively detected by spectrofluorometry. As proof of concept, thiourea (TU) and other sulfides including cysteine (Cys), glutathione (GSH) and dl-methionine could be detected. For example, the color of the orange fluorescent AgNCs solutions darkened upon the addition of TU and the fluorescence of PMAA-AgNCs was quenched. The detection limit for TU was 6.10 μM in the linear range from 8.57 μM to 2.29 mM. PMID:24834451

  11. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2015-09-01

    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.

  13. Hexagonal SrFe12O19 ferrites: Hydrothermal synthesis and their sintering properties

    NASA Astrophysics Data System (ADS)

    Xia, Ailin; Zuo, Conghua; Chen, Lu; Jin, Chuangui; Lv, Yaohui

    2013-04-01

    Hexagonal M type SrFe12O19 (SrM) ferrites were synthesized by the hydrothermal method, and the effects of molar ratio of OH/ (RO/N), the atomic ratio of Fe/Sr (RF/S) and sintering on the phase composition and magnetic properties of as-synthesized specimens are studied. It is found that the RO/N and RF/S in starting materials affect the phase composition and magnetic properties greatly. Fe2O3 is found as impurity in some specimens, while in all as-synthesized specimens, SrCO3 forms inevitably during the synthesis process. After sintering at 1100 °C, the perovskite type SrFeO3-x ferrite forms as the product of SrCO3 and Fe2O3 at high temperature, and the specimens exhibit the Perminvar magnetic hysteresis loops which show two-phase magnetic behaviors. However, when sintered at 1200 °C, SrFeO3-x further reacts with Fe2O3 to produce SrFe12O19, and the specimens with RF/S=8, 9 and 10 exhibit the single-phase hexagonal structure and magnetic behavior. It is also found that the saturation magnetization and coercivity are both enhanced after sintering at high temperatures due to the elimination of impurities.

  14. 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).

  15. 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.

  16. 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.

  17. 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}.

  18. 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. PMID:27054768

  19. Mesostructured SBA-16 with excellent hydrothermal, thermal and mechanical stabilities: modified synthesis and its catalytic application.

    PubMed

    Sun, Hui; Tang, Qinghu; Du, Yu; Liu, Xianbin; Chen, Yuan; Yang, Yanhui

    2009-05-01

    We report a modified method to synthesize SBA-16 mesostructured silica under refluxing condition using block co-polymer poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) (F127) as template, cetyltrimethylammonium bromide (CTAB) as co-template, and tetraethyl orthosilicate (TEOS) as silica source. The physiochemical properties of SBA-16 silica were characterized by X-ray diffraction (XRD), nitrogen physisorption, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and (29)Si solid-state nuclear magnetic resonance (NMR). The resulting SBA-16 silica exhibited highly ordered mesoporous structure, mono-dispersed spherical morphology, excellent hydrothermal, thermal and mechanical stabilities. It was worth mentioning that the synthesis time can be significantly reduced from 48 h to 8 h, which opened a feasible way to produce SBA-16 silica in a large scale. Moreover, the "super-cage" pore structure of SBA-16 encapsulated gold nanoparticles in a "ship in a bottle" way. The well-confined gold nanoparticles (mean size of 5 nm) with a narrow particle size distribution were highly active in solvent-free benzyl alcohol selective oxidation with molecular oxygen. PMID:19246048

  20. Highly porous nickel oxide thin films prepared by a hydrothermal synthesis method for electrochromic application

    NASA Astrophysics Data System (ADS)

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

    2013-11-01

    We report NiO nanowall thin films prepared by a facile hydrothermal synthesis method and their electrochromic application. The as-prepared porous nanowall NiO thin films show a highly porous structure built up by many interconnected nanoflakes with a thickness of about 30 nm. The electrochromic performances of the NiO films are characterized by means of UV-vis spectroscopy and cyclic voltammetry (CV) measurements. The effect of the annealing temperature on electrochromic properties is discussed. The NiO nanowall film annealed at 300 °C exhibits much better electrochromic performance than those counterparts annealed at higher temperature. The film annealed at 300 °C exhibits a noticeable electrochromism with reversible color changes from transparent to brown dark and presents a transmittance variation with 77% at 550 nm. The NiO nanowall film also shows good reaction kinetics with fast switching speed, and the coloration and bleaching times are 3 s and 4 s, respectively. The improved electrochromic performances are due to the porous morphological characteristics with fast ion and electron transfer resulting in fast reaction kinetics and high color contrast.

  1. 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)…

  2. Monodisperse spindle-like FeWO{sub 4} nanoparticles: Controlled hydrothermal synthesis and enhanced optical properties

    SciTech Connect

    Guo, Jinxue; Zhou, Xiaoyu; Lu, Yibin; Zhang, Xiao; Kuang, Shaoping; Hou, Wanguo

    2012-12-15

    Monodisperse FeWO{sub 4} nanoparticles with specific spindle-like morphology have been synthesized in the presence of citric acid through hydrothermal process. In the synthesis route, citric acid played four roles such as the reducing agent, chelating regents, structure-directing agent and stabilizing agents. In addition, the morphology of FeWO{sub 4} was dramatically tuned by the pH value of the precursor medium. The optical properties of FeWO{sub 4} were investigated with UV-Vis spectra and photoluminescence spectroscopy. The photocatalytic experiments demonstrated that the decomposition efficiency of the monodisperse spindle-like FeWO{sub 4} nanoparticles is 74% after 30 min of UV irradiation, which displayed remarkable enhanced photodegradation activity compared with ordinary FeWO{sub 4} sample (57%) and normal TiO{sub 2} photocatalysts P-25 (56%). - Monodisperse spindle-like FeWO{sub 4} nanoparticles with enhanced photocatalytic activities. Highlights: Black-Right-Pointing-Pointer Monodisperse spindle-like FeWO{sub 4} were synthesized with hydrothermal method. Black-Right-Pointing-Pointer Citric acid plays key roles in the hydrothermal synthesis. Black-Right-Pointing-Pointer Their morphology can be tuned with pH value of the precursor medium. Black-Right-Pointing-Pointer They show enhanced photocatalytic activities with irradiation of UV light.

  3. 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.

  4. 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.

  5. Hydrothermal synthesis of Group 13 metal trifluoride complexes with neutral N-donor ligands.

    PubMed

    Bhalla, Rajiv; Levason, William; Luthra, Sajinder K; McRobbie, Graeme; Monzittu, Francesco M; Palmer, Jazmyn; Reid, Gillian; Sanderson, George; Zhang, Wenjian

    2015-05-28

    The reactions of the hydrated Group 13 fluorides, MF3·3H2O (M = Al, Ga or In) with 2,2':6',2''-terpyridyl, 2,2'-bipyridyl or 1,10-phenanthroline under hydrothermal conditions (180 °C/15 h) produced high yields of the complexes [MF3(terpy)]·3H2O, [MF3(bipy)(OH2)]·2H2O and [MF3(phen)(OH2)]. X-Ray crystal structures of [M'F3(terpy)]·3H2O (M' = Al or Ga), [M'F3(bipy)(OH2)]·2H2O and [GaF3(phen)(OH2)] show that all of them contain distorted octahedral geometries at the metal with mer-trifluoride coordination. Extensive H-bonding (FH-OH) links the molecules. The complexes have been further characterised by microanalysis, IR, (1)H, (19)F{(1)H} and (27)Al NMR spectroscopy. In contrast, reactions of the trifluorides with the acyclic triamine, N,N,N',N',N''-pentamethyldiethylenetriamine, under similar hydrothermal conditions results in cleavage of the triamine and ring-closure to form the 1,1,4-trimethylpiperazinium cation, [⊂Me2N(CH2)2NMe(CH2)2](+), with fluorometallate anions, and confirmed by X-ray analysis of [⊂Me2N(CH2)2NMe(CH2)2]2[Al2F8(OH2)2]·2H2O. The strongly H-bonded [GaF3(terpy)]·3H2O was also obtained by Cl/F exchange from [GaCl3(terpy)] and [NBu4]F or [K(2,2,2-crypt)]F. Crystallisation of a mixture of [NH4][PF6] and [GaF3(terpy)]·3H2O from aqueous solution produced the edge-bridged cationic complex, [{Ga(terpy)F}2(μ-F)2][PF6]2. The synthesis of the more sterically bulky [GaCl3((t)Bu3-terpy)] ((t)Bu3-terpy = 4,4'4''-tris-(t)Bu-2,2':6',2''-terpyridyl) and the crystal structure of [GaCl2((t)Bu3-terpy)][GaCl4], which contains a trigonal bipyramidal cation, are also reported. PMID:25921724

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

    SciTech Connect

    Chai, Hui; Chen, Xuan; Key Laboratory of Advanced Functional Materials, Institute of Applied Chemistry, Xinjiang University, Urumqi 830046, Xinjiang ; Jia, Dianzeng; Key Laboratory of Advanced Functional Materials, Institute of Applied Chemistry, Xinjiang University, Urumqi 830046, Xinjiang ; Bao, Shujuan; Key Laboratory of Advanced Functional Materials, Institute of Applied Chemistry, Xinjiang University, Urumqi 830046, Xinjiang ; 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

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

    DOEpatents

    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.

  8. Synthesis of PbMoO4 nanoparticles by microwave-assisted hydrothermal process and their photocatalytic activity.

    PubMed

    Song, Young In; Lim, Kwon Taek; Lee, Gun Dae; Lee, Man Sig; Hong, Seong-Soo

    2014-11-01

    Lead molybdate (PbMoO4) was successfully synthesized using a microwave-assisted method and characterized by XRD, Raman spectroscopy, SEM, PL and DRS. We also investigated the photocatalytic activity of these materials for the decomposition of Rhodamin B under UV-light irradiation. The XRD and Raman results revealed the successful synthesis of 42-52 nm, well-crystallized PbMoO4 crystals with the microwave-assisted hydrothermal method. The PbMoO4 catalysts prepared using the microwave-assisted process enhanced the photocatalytic activity compared to that prepared by hydrothermal method and the catalysts prepared at a solution pH = 11 and temperature of 105 degrees C showed the highest photocatalytic activity. The PL peaks appeared at about 540 nm for all catalysts and the excitonic PL signal was proportional to the photocatalytic activity for the decomposition of Rhodamin B. PMID:25958553

  9. Spectroscopic investigations on the synthesis of nano-hydroxyapatite from calcined eggshell by hydrothermal method using cationic surfactant as template

    NASA Astrophysics Data System (ADS)

    Prabakaran, K.; Rajeswari, S.

    2009-12-01

    The present work reports the successful synthesis of nano-hydroxyapatite, Ca 10(PO 4) 6(OH) 2 (denoted HAP) from calcined eggshell by hydrothermal method using cationic surfactant (CTAB) as regulator of nucleation and crystal growth. The reaction involved in the synthesis was studied elaborately. The influence of reaction temperature, ageing time and CTAB concentration on the synthesis of nano-HAP are also studied in addition to the effect of sintering temperature on the crystal growth. Spectral characterization involving Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD) techniques were performed for functional group analysis and phase identification of the materials, respectively. Thermal stability of nano-HAP was investigated by thermal analysis (TG/DTA). The physical characteristics, such as morphology and particle size of the synthesized nano-HAP were assessed thoroughly by scanning electron microscopy (SEM) and atomic force microscopy (AFM) techniques. The results have revealed that well-crystallized nano-HAP was synthesized by hydrothermal treatment at 160 °C for 10 h with the addition of CTAB at critical micelle concentration (CMC). It was also found that the synthesized nano-HAP was thermally stable up to 1100 °C.

  10. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2016-04-01

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

  12. Hydrothermal Synthesis and Luminescent Properties of Eu3+ Doped Sr3Al2O6 Phosphor for White LED.

    PubMed

    Li, Xu; Pan, Heng; Tang, Aiwei; Zhang, Jinping; Guan, Li; Su, Hongxin; Dong, Guoyi; Yang, Zhiping; Wang, Huike; Teng, Feng

    2016-04-01

    Eu3+ ions doped Sr3Al2O6 phosphors were successfully synthesized via a hydrothermal method. The precursor was prepared by low temperature hydrothermal method using ammonia as both alkaline source and precipitator. Then the final product was obtained by high temperature sintering. In addition, the structures, morphologies, and luminescent properties of as-prepared products were thoroughly characterized by X-ray powder diffraction (XRD), Scanning electron microscopy (SEM), Fluorescence spectroscopy (PL). XRD shown a single phase Sr3Al2O6 prepared by a facile hydrothermal method at 250 °C for 10 h. In the PL spectra of as-prepared samples, the optimal value of Eu3+ concentration is 2 mol%. From the fluorescent spectra, the emission peaks of Sr3Al2O6: Eul+ phosphors are centered at around 591 nm, and the excitation peaks are centered at around 233 nm, 323 nm, 394 nm, and 468 nm, respectively, which were assigned to the characteristic transition of Eu3+ ions. The influence of ammonia, and the synthesis temperature on the luminescent properties of Sr3Al206: Eu3+ phosphors were studied in detail. The alkaline earth aluminates luminescent materials activated by rare earth ions have good prospects in the field of new-generation light sources. PMID:27451652

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

    PubMed

    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. 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.

  16. Preparation and characterization of nano-La (S, C)-TiO 2 oriented films by template hydrothermal synthesis

    NASA Astrophysics Data System (ADS)

    Xu, Kejing; Zhu, Guoquan

    2009-04-01

    The La (S, C)-TiO 2 oriented films with honeycomb ceramic wafers as carriers were prepared by template hydrothermal synthesis at low temperature. The effects of the hydrothermal reaction temperature, the amount of template agents and the codoping of La and S on the performances of nano-TiO 2 films were studied. The performances of the films were characterized on the XRD, UV-vis, BET, EDS and SEM. The results showed that the TiO 2 films with anatase phase were obtained when hydrothermal reaction temperature was 150 °C and the reaction time was 10 h, and the oriented films were obtained when the molar ratio of poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) triblock copolymer (PEO-PPO-PEO (P-123)) to Ti was 0.03. The data also revealed that the specific surface area of particles in the film increased from 148 m 2/g to 240 m 2/g, the photocatalytic activity of the oriented film was improved greatly due to the codoping of La and S, and the oriented film could fully decompose methyl orange in water for 3 h.

  17. 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

  18. 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

  19. 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. PMID:24778970

  20. 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

  1. 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.

  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. 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.

  4. Hydrothermal Synthesis and Electrochemical Properties of Spherical α-MnO2 for Supercapacitors.

    PubMed

    Chen, Ya; Qin, Wenqing; Fan, Ruijuan; Wang, Jiawei; Chen, Baizhen

    2015-12-01

    In the present work, spherical α-MnO2 with a high specific capacitance was synthesized by a two-step hydrothermal route. MnCO3 precursors were first prepared by a common hydrothermal method, and then converted to α-MnO2 via a hydrothermal reaction between the precursors and KMnO4 solutions. The effects of hydrothermal temperature on the morphology, crystal structure and specific area of the MnO2 were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD) and BET measurements. The electrochemical capacitive properties of the manganese dioxides with different morphologies and structures were evaluated by cyclic voltammetry and galvonostatic charge-discharge tests. The results showed that the temperature in the second hydrothermal step had prominent impact on the capacitive properties of a-MnO2. The MnO2 synthesized at 150 *C exhibited a highest specific capacitance of 328.4 Fx g(-1) at a charge-discharge current density of 100 mA x g(-1). PMID:26682409

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

    PubMed

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

    2015-12-01

    Bismuth ferrite is a promising material for visible light response photocatalytic applications due to its narrow band gap. In this work, single crystalline BiFeO3 nanoparticles were prepared by a modified hydrothermal process. The effects of hydrothermal temperature, reaction time and precursor xerogel amoumt on the as-prepared BiFeO3 particle size and morphology were investigated by XRD, TEM and HRTEM. The XRD analysis reveals that single crystalline BiFeO3 particles can be obtained when the hydrothermal temperature is kept below 220 degrees C. TEM observation showed that the as-formed BFO particles are in a square or rectangle-like shape and that the particle size is increased with increasing hydrothermal temperature. The hydrothermal reaction time and the amount of xerogel could also influence the as-formed BFO particle morphology and size. The band gap of the as-prepared BFO nanoparticles was identified by UV-vis diffuse reflectance spectrum. The measurement of photodegradation of methyl orange dye in an aqueous solution revealed that the as-prepared BFO nanoparticles exhibit photocatalytic activity under visible light irradiation. PMID:26682398

  6. Stimulatory effect of sulphide on thiotaurine synthesis in three hydrothermal-vent species from the East Pacific Rise.

    PubMed

    Pruski, Audrey M; Fiala-Médioni, Aline

    2003-09-01

    Symbiotic associations between marine invertebrates and sulphur-oxidising bacteria are a common feature in communities from sulphide-rich environments, such as those flourishing in the vicinity of hydrothermal vents. While the bacterial endosymbionts provide the host with an undoubted nutritional advantage, their presence also requires specific adaptations for the transport and storage of sulphide, which is a potent toxin of aerobic respiration. Although different mechanisms such as the reversible binding of sulphide to serum binding proteins or its oxidation to less toxic forms have been described, many questions still remained unanswered. In the last decade, large amounts of thiotaurine, an unusual sulphur-amino acid, have been reported in sulphur-based symbioses from hydrothermal vents and cold seeps. Compounds such as thiotaurine are known to take part in trans-sulphuration reactions, so the involvement of thiotaurine in sulphide metabolism has been suggested. We present here an experimental study on thiotaurine biosynthesis in three sulphur-oxidising symbiont-bearing species from the East Pacific Rise: the vesicomyid Calyptogena magnifica, the mytilid Bathymodiolus thermophilus and the vestimentiferan Riftia pachyptila. In all three species, thiotaurine synthesis is stimulated in vitro by an input of sulphide, as well as by thiosulphate in B. thermophilus. Several distinct metabolic pathways seem to occur, however, since hypotaurine is the only precursor in the bivalves C. magnifica and B. thermophilus, whereas thiotaurine is also produced from taurine in R. pachyptila. Hypotaurine (NH(2)-CH(2)-CH(2)-SO(2)H) and thiotaurine (NH(2)-CH(2)-CH(2)-SO(2)SH) are two free sulphur amino acids whose chemical formulae differ by only one atom of sulphur. It appears that the extent of thiotaurine synthesis is strongly dependent on the initial equilibrium between these two amino acids, since the strongest thiotaurine synthesis rates are found in tissues with the lowest

  7. Control of crystal phase and morphology in hydrothermal synthesis of BiFeO3 crystal

    NASA Astrophysics Data System (ADS)

    Xu, Xuqing; Xu, Qianrui; Huang, Yajun; Hu, Xiuxiu; Huang, Yuqing; Wang, Gaoyu; Hu, Xiaolin; Zhuang, Naifeng

    2016-03-01

    Bismuth ferrite crystal is synthesized by hydrothermal method. The effect of hydrothermal temperature, KOH concentration, supersaturation, cooling rate, and compactedness on the crystal phase and the morphology of product were investigated. The results indicated that BiFeO3 microcrystalline with good quality could been synthesized at 140-240 °C with KOH concentration of 4-14 mol L-1. In addition, it is favorable for improving the crystal quality to reduce the supersaturation and decrease the cooling rate. With the increasing of the compactedness, surface holes and cracks of the as-grown crystals would be reduced. The optimization of hydrothermal condition provides guidance to grow BiFeO3 crystal with a large size and high quality for practical application.

  8. Hydrothermal synthesis of an ortho-metallated Co(III) complex anchored by a carboxylate group with a selective oxidation catalytic property.

    PubMed

    Zhang, Shi-Yuan; Shi, Wei; Ma, Jian-Gong; Zhang, Yu-Qi; Zhang, Zhen-Jie; Cheng, Peng

    2013-03-28

    An air-stable and water-tolerant ortho-metallated complex [Co(tfb)(bpy)(2)](NO(3))·3H(2)O was obtained via hydrothermal synthesis. The mechanism for the formation of Co-C bond was studied using both DFT calculations and experimental analysis. This highly stable complex exhibits good catalytic performance for the selective oxidation of cyclohexane. PMID:23348750

  9. 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...

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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. PMID:12240084

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

    SciTech Connect

    Zhang Jilin; Shi Jianxin; Gong Menglian

    2009-08-15

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

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

    SciTech Connect

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

    2011-04-15

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

  18. Hydrothermal synthesis, structure investigation, and oxide ion conductivity of mixed Si/Ge-based apatite-type phases.

    PubMed

    Li, Henan; Baikie, Tom; Pramana, Stevin S; Shin, J Felix; Keenan, Philip J; Slater, Peter R; Brink, Frank; Hester, James; An, Tao; White, Tim J

    2014-05-19

    Apatite-type oxides ([A(I)4][A(II)6][(BO4)6]O2), particularly those of the rare-earth silicate and germanate systems, are among the more promising materials being considered as alternative solid oxide fuel cell electrolytes. Nonstoichiometric lanthanum silicate and germanate apatites display pure ionic conductivities exceeding those of yttria-stabilized zirconia at moderate temperatures (500-700 °C). In this study, mixed Si/Ge-based apatites were prepared by hydrothermal synthesis under mild conditions rather than the conventional solid-state method at high temperatures. Single-phase and highly crystalline nanosized apatite powders were obtained with the morphology changing across the series from spheres for the Si-based end member to hexagonal rods for the Ge-based end member. Powder X-ray and neutron analysis found all of these apatites to be hexagonal (P63/m). Quantitative X-ray microanalysis established the partial (<15 at%) substitution of La(3+) by Na(+) (introduced from the NaOH hydrothermal reagent), which showed a slight preference to enter the A(I) 4f framework position over the A(II) 6h tunnel site. Moreover, retention of hydroxide (OH(-)) was confirmed by IR spectroscopy and thermogravimetric analysis, and these apatites are best described as oxyhydroxyapatites. To prepare dense pellets for conductivity measurements, both conventional heat treatment and spark plasma sintering methods were compared, with the peculiar features of hydrothermally synthesized apatites and the influence of sodium on the ionic conductivity considered. PMID:24787953

  19. Modulated Hydrothermal Synthesis of UiO-66(Hf)-Type Metal-Organic Frameworks for Optimal Carbon Dioxide Separation.

    PubMed

    Hu, Zhigang; Nalaparaju, Anjaiah; Peng, Yongwu; Jiang, Jianwen; Zhao, Dan

    2016-02-01

    Recently, there has been growing interest in hafnium (Hf) metal-organic frameworks (MOFs). These MOFs may perform better as gas adsorbents than zirconium (Zr) MOFs due to the presence of Brønsted acid sites with high affinity toward adsorbates, together with the outstanding chemical and hydrothermal stabilities similar to their Zr analogues. However, Hf-MOFs have been rarely reported due to the lack of effective synthetic methods. We herein report a modulated hydrothermal synthesis of UiO-66(Hf)-type MOFs. Among these MOFs, UiO-66(Hf)-(OH)2 possesses a very high CO2 gravimetric uptake of 1.81 mmol g(-1) at 0.15 bar and 298 K, which is 400% higher than that of UiO-66(Hf) (0.36 mmol g(-1)). It also exhibits a record-high volumetric CO2 uptake of 167 v/v at 1 bar and 298 K. Ideal adsorbed solution theory calculations showed a CO2/N2 (molar ratio 15:85) selectivity of 93 and CO2/H2 (molar ratio 30:70) selectivity above 1700. Breakthrough simulations also confirmed its optimal CO2 separation attribute. Our results have demonstrated for the first time the strong potential of Hf-MOFs for advanced adsorbents for high-performance CO2-related separations. PMID:26751503

  20. DNA-templated microwave-hydrothermal synthesis of nanostructured hydroxyapatite for storing and sustained release of an antibacterial protein.

    PubMed

    Chen, Xi; Yang, Bin; Qi, Chao; Sun, Tuan-Wei; Chen, Feng; Wu, Jin; Feng, Xi-Ping; Zhu, Ying-Jie

    2016-01-28

    Hydroxyapatite (HA) is promising in various biomedical applications owing to its similar chemical composition, structure and properties to the inorganic component in natural hard tissues. Herein, we report a DNA-templated microwave-assisted hydrothermal strategy for the preparation of HA nanostructured materials. As a kind of natural biomacromolecule, DNA molecules open up a new way to the synthesis of HA nanostructured materials with well-defined structures and morphologies. The HA nanostructured materials with a nanosheet-assembled hierarchical structure and a HA nanorod ordered structure are successfully prepared. The important roles of DNA molecules and pH values in the formation of HA nanostructured materials are investigated, and a possible formation mechanism is proposed. The as-prepared HA nanostructured materials exhibit a relatively high adsorption ability for chicken immunoglobulin Y (IgY) protein and a sustained protein release behavior. The as-prepared HA nanostructured materials after loading the IgY protein show a high antimicrobial activity. Thus, the HA nanostructured materials prepared by the DNA-templated microwave hydrothermal method are promising for the applications in various areas such as the prevention and treatment of dental caries. PMID:26696032

  1. Low temperature hydrothermal synthesis, structure and magnetic properties of RECrO3 (RE = La, Pr, Nd, Sm).

    PubMed

    Wang, Shan; Huang, Keke; Hou, Changmin; Yuan, Long; Wu, Xiaofeng; Lu, Dayong

    2015-10-21

    Perovskite structured rare-earth chromites (RECrO3) are an interesting family of functional materials due to their wide application in numerous areas. Various methods have been used to synthesize this family of materials; however, such methods usually need a high temperature crystallization process above 800 °C, and only produce polycrystalline ceramics. Herein, a series of RECrO3 single crystal samples with uniform particle sizes were prepared via a mild hydrothermal method with temperatures as low as 240-260 °C, and the synthesis conditions were studied in detail. Samples of LaCrO3, PrCrO3, and NdCrO3 were indexed to the Pnma space group, whereas SmCrO3 was indexed to Pbnm. The shapes of the crystals changed from cubic to plate as a result of the crystal lattice distortions induced by the reduction in the size of the A-site rare-earth cation. Raman spectra of the samples showed characteristic vibration modes of CrO6 clusters. Temperature dependent magnetization studies showed a transition from antiferromagnetism to paramagnetism in all the samples. Higher maximum and residual magnetization was achieved in all the hydrothermally prepared samples compared with those prepared by other methods. PMID:26374249

  2. 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

  3. 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. PMID:24734771

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. Chrysanthemum-like Co3O4 architectures: Hydrothermal synthesis and lithium storage performances

    NASA Astrophysics Data System (ADS)

    Ren, Manman; Yuan, Shuming; Su, Liwei; Zhou, Zhen

    2012-04-01

    Three-dimensional chrysanthemum-like Co3O4 was prepared via a facile hydrothermal route without any template, and a subsequent calcination process. With a controlled concentration of the homogeneous precipitation agent, urea, a chrysanthemum-like precursor was hydrothermally obtained at 120 °C for 20 h, and the morphology was kept for Co3O4 after a subsequent calcination at 300 °C for 2 h. Co3O4 chrysanthemum-like architectures are assemblies of nanorods radiating from a common centre, and the nanorods consisted of interconnected nanoparticles with the size of about 30 nm. When tested as an anode material of Li-ion batteries, chrysanthemum-like Co3O4 presented a discharge capacity of ˜450 mA h/g after 50 discharge/charge cycles.

  9. 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

  10. 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

  11. 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.

  12. 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.

  13. One step hydrothermal synthesis of a carbon nanotube/cerium oxide nanocomposite and its electrochemical properties

    NASA Astrophysics Data System (ADS)

    Kalubarme, Ramchandra S.; Kim, Yong-Han; Park, Chan-Jin

    2013-09-01

    A carbon nanotube (CNT)/cerium oxide composite was prepared by a one-pot hydrothermal reaction in the presence of KOH and capping agent polyvinylpyrrolidone. The nanocomposite displayed pronounced capacitive behaviour with very small diffusion resistance. The electrochemical performance of the composite electrode in a symmetric supercapacitor displayed a high energy density of 35.9 Wh kg-1 corresponding to a specific capacitance of 289 F g-1. These composite electrodes also demonstrated a long cycle life with better capacity retention.

  14. Abiotic synthesis of acylglycerols under simulated hydrothermal conditions and micelle formation

    NASA Astrophysics Data System (ADS)

    Simoneit, B.; Rushdi, A.; Deamer, D.

    Abiotic formation of aliphatic lipid compounds i e fatty acids alcohols and acylglycerols has been reported to occur at elevated temperatures and pressures under simulated hydrothermal conditions McCollom et al 1999 Rushdi and Simoneit 2001 2006 Although abiotic chemistry may occur at these conditions the prebiotic self-assembly of micelles to bilayer to vesicles protocells may have occurred elsewhere Amphipathic compounds such as fatty acids and acylglycerols are important candidates for micelle bilayer vesicle formation Thus it is of interest to demonstrate that abiotic lipids amphiphiles precursor compounds for abiotic cellular membranes Deamer 1997 can be synthesized under hydrothermal conditions Hydrothermal experiments were conducted to study condensation reactions of model lipid precursors in aqueous media to form acylglycerols glyceryl alkanoates at elevated temperatures under confining pressures Stainless steel vessels 316SS Sno-Trik high pressure couplings with internal capacities of 286 underline 2 mu l were used for the condensation reactions using a mixture of 0 14 mM glycerol and 0 35 mM of n-alkanoic acid Nine different alkanoic acids ranging from C 7 to C 16 except C 8 were used in these experiments The condensation products were two isomers each of monoacylglycerols and diacylglycerols as well as the corresponding triacylglycerol The product yields were 13-28 for monoacylglycerols 6-13 for diacylglycerols and 1-4 for triacylglycerols The results indicated that 1

  15. 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

    2016-08-01

    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. [Figure not available: see fulltext.

  16. 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.

  17. 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

  18. Hydrothermal synthesis of nickel hydroxide nanostructures in mixed solvents of water and alcohol

    SciTech Connect

    Yang Lixia; Zhu Yingjie Tong Hua; Liang Zhenhua; Li Liang; Zhang Ling

    2007-07-15

    Nickel hydroxide nanosheets and flowers have been hydrothermally synthesized using Ni(CH{sub 3}COO){sub 2}.4H{sub 2}O in mixed solvents of ethylene glycol (EG) or ethanol and deionized water at 200 deg. C for different time. The phase and morphology of the obtained products can be controlled by adjusting the experimental parameters, including the hydrothermal time and the volume ratio of water to EG or ethanol. The possible reaction mechanism and growth of the nanosheets and nanoflowers are discussed based on the experimental results. Porous nickel oxide nanosheets are obtained by heating nickel hydroxide nanosheets in air at 400 deg. C. The products were characterized by using various methods including X-ray diffraction (XRD), fourier transform infrared (FTIR), transmission electron microscopy (TEM), selected-area electron diffraction (SAED), field emission scanning electron microscopy (FESEM). The electrochemical property of {beta}-Ni(OH){sub 2} nanosheets was investigated through the cyclic voltammogram (CV) measurement. - Graphical abstract: Nickel hydroxide nanosheets and flowers have been hydrothermally synthesized using Ni(CH{sub 3}COO){sub 2}.4H{sub 2}O in mixed solvents of ethylene glycol (EG) or ethanol and deionized water at 200 deg. C for different reaction time. Porous nickel oxide nanosheets are obtained by heating nickel hydroxide nanosheets in air at 400 deg. C.

  19. Hydrothermal synthesis of {beta}-nickel hydroxide nanocrystalline thin film and growth of oriented carbon nanofibers

    SciTech Connect

    Zhang Enlei; Tang Yuanhong; Zhang Yong; Guo Chi; Yang Lei

    2009-08-05

    Novel well-crystallized {beta}-nickel hydroxide nanocrystalline thin films were successfully synthesized at low temperature on the quartz substrates by hydrothermal method, and the oriented carbon nanofibers (CNFs) were prepared by acetylene cracking at 750 deg. C on thin film as the catalyst precursor. High resolution transmission electron microscopy (HR-TEM) measurement shows that thin films were constructed mainly with hexagonal {beta}-nickel hydroxide nanosheets. The average diameter of the nanosheets was about 80 nm and thickness about 15 nm. Hydrothermal temperature played an important role in the film growth process, influencing the morphologies and catalytic activity of the Ni catalysts. Ni thin films with high catalytic activity were obtained by reduction of these Ni(OH){sub 2} nanocrystalline thin films synthesized at 170 deg. C for 2 h in hydrothermal condition. The highest carbon yield was 1182%, and was significantly higher than the value of the catalyst precursor which was previously reported as the carbon yield (398%) for Ni catalysts. The morphology and growth mechanism of oriented CNFs were also studied finally.

  20. 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. PMID:19111982

  1. 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.

  2. Synthesis of nano-hydroxyapatite under a sonochemical/hydrothermal condition.

    PubMed

    Manafi, S A; Yazdani, B; Rahimiopour, M R; Sadrnezhaad, S K; Amin, M H; Razavi, M

    2008-06-01

    In this study, hydroxyapatite (denoted as HAp) nanostructure with uniform morphologies, controllable size, nano-dispersion and narrow size distribution in diameter has been synthesized successfully by low-temperature hydrothermal process, and the as-synthesized powders were characterized by XRD, scanning electron microscopy, high-resolution transmission microscopy, FT-IR, Zetasizer and inductively coupled plasma. In the present work, a novel sonochemical technique using CaHPO(4)2H(2)O/NaOH/distilled water with cetyltrimethylammonium bromide ((CH(3)(CH(2))(15)N(+)(CH(3))(3)Br(-)) designated as CTAB) under a hydrothermal condition to synthesize HAp nanostructure was described. Furthermore, the usage of a high basic condition and a water environment are the two crucial keys in ensuring the formation of HAp in the hydrothermal/sonochemical processes. However, the crystallite size and crystallinity degree of the HAp increased with increasing annealing temperature. Indeed, the present work will introduce a new method in synthesizing HAs for scientific and medical engineering. PMID:18458367

  3. Morphology-controlled hydrothermal synthesis of MnCO{sub 3} hierarchical superstructures with Schiff base as stabilizer

    SciTech Connect

    Hu, He; Xu, Jie-yan; Yang, Hong; Liang, Jie; Yang, Shiping; Wu, Huixia

    2011-11-15

    Graphical abstract: MnCO3 microcrystals with hierarchical superstructures were synthesized by using the CO2 in atmosphere as carbonate ions source and Schiff base as shape guiding-agent in water/ethanol system under hydrothermal condition. Highlights: {yields} The most interesting in this work is the use of the greenhouse gases CO{sub 2} in atmosphere as carbonate ions source to precipitate with Mn{sup 2+} for producing MnCO{sub 3} crystals. {yields} This work is the first report related to the small organic molecule Schiff base as shape guiding-agent to produce different MnCO{sub 3} hierarchical superstructures. {yields} We are controllable synthesis of the MnCO{sub 3} hierarchical superstructures such as chrysanthemum, straw-bundle, dumbbell and sphere-like microcrystals. {yields} The as-prepared MnCO{sub 3} could be used precursor to fabricate the Mn{sub 2}O{sub 3} hierarchical superstructures after thermal decomposition at high temperature. -- Abstract: MnCO{sub 3} with hierarchical superstructures such as chrysanthemum, straw-bundle, dumbbell and sphere-like were synthesized in water/ethanol system under environment-friendly hydrothermal condition. In the synthesis process, the CO{sub 2} in atmosphere was used as the source of carbonate ions and Schiff base was used as shape guiding-agent. The different superstructures of MnCO{sub 3} could be obtained by controlling the hydrothermal temperature, the molar ratio of manganous ions to the Schiff base, or the volume ratio of water to ethanol. A tentative growth mechanism for the generation of MnCO{sub 3} superstructures was proposed based on the rod-dumbbell-sphere model. Furthermore, the MnCO{sub 3} as precursor could be further successfully transferred to Mn{sub 2}O{sub 3} microstructure after heating in the atmosphere at 500 {sup o}C, and the morphology of the Mn{sub 2}O{sub 3} was directly determined by that of the MnCO{sub 3} precursor.

  4. 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.

  5. 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. PMID:22136425

  6. Hydrothermal synthesis of Fe-doped TiO2 nanostructure photocatalyst

    NASA Astrophysics Data System (ADS)

    Nghia Nguyen, Van; Khoa Truong Nguyen, Ngoc; Nguyen, Phi Hung

    2011-09-01

    Fe-doped TiO2 catalyst was prepared by the hydrothermal method. The resulting nanopowders were characterized by x-ray diffraction, transmission electron microscopy and Raman and UV-visible spectroscopies. The photocatalytic activity of the Fe-doped TiO2 was tested by decomposition of methylene orange with a concentration of 10 mg l‑1 in aqueous solution. The obtained results showed that methylene orange was significantly degraded after irradiation for 90 min under a halogen lamp and sunlight. The doping effect on the photocatalytic activity of the iron-doped catalyst samples are discussed.

  7. In Situ Hydrothermal Synthesis of Graphene-CuO Nanocomposites for Lithium Battery Applications.

    PubMed

    Murugan, M; Kumar, R Mohan; Alsalme, Ali; Alghamdi, Abdulaziz; Jayavell, R

    2016-01-01

    Graphene-CuO nanocomposites were prepared by in situ hydrothermal method. The properties of the prepared nanocomposites have been studied by XRD, SEM, TEM, TGA, FT-IR, TGA and CV technqiues. The prepared nanocomposites show uniform dispersion of CuO nanoparticles in between the graphene sheets. The interlayer spacing of the graphene sheets has been increased due to the inclusion of CuO nanoparticles as revealed by TEM analysis. The modification in the interlayer spacing and the CuO functionalization in between the layers would be useful in designing high performance lithium ion battery electrodes. PMID:27398460

  8. 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.

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

    SciTech Connect

    Song Yishan; Yan Bing . E-mail: byan@tongji.edu.cn; Chen Zhenxia

    2006-12-15

    Using the principle of crystal engineering, four novel metal-organic coordination polymers, {l_brace}[Cd{sub 1}(nic)2(H{sub 2}O)]2[Cd{sub 2}(nic)2(H{sub 2}O)2]{r_brace} {sub n} (1), [Cd{sub 2}(fma)2(phen)2] {sub n} (2), [Cd(fma)(bipy)(H{sub 2}O)] {sub n} (3) and [Zn(mal)(bipy).3H{sub 2}O] {sub n} (4) (nic=nicotinate, fma=fumarate, mal=malate, phen=phenanthroline, bipy=2,2'-bipyridine) have been synthesized by hydrothermal reaction of M(CH{sub 3}COO)2.2H{sub 2}O (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. -- Graphical abstract: Using the principle of crystal engineering, four novel metal-organic coordination polymers, {l_brace}[Cd{sup 1}(nic){sub 2}(H{sub 2}O)]{sub 2}[Cd{sup 2}(nic){sub 2}(H{sub 2}O){sub 2}]{r_brace} {sub n} , [Cd{sub 2}(fma){sub 2}(phen){sub 2}] {sub n} , [Cd(fma)(bipy)(H{sub 2}O)] {sub n} and [Zn(mal)(bipy).3H{sub 2}O] {sub n} have been synthesized by hydrothermal method. 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, complexes 3 and 4 belong to a 1D chain. The results indicate a transformation of fumarate into malate during the course of hydrothermal treatment of complex 4.

  10. Cadmium sulfide nanocrystals via two-step hydrothermal process in microemulsions: synthesis and characterization.

    PubMed

    Zhang, Peng; Gao, Lian

    2003-10-15

    CdS nanocrystals with an average diameter of 16 nm were synthesized in the CTAB/n-C(5)H(11)OH/n-C(6)H(14)/water quaternary microemulsions by a two-step hydrothermal process at 90 and 130 degrees C. The reaction of carbamide and carbon disulfide was employed as the sulfur source for the preparation of CdS nanocrystals. The resulting crystals were characterized with powder X-ray diffraction, transmission electron microscopy, UV-vis absorption spectroscopy, and photoluminescence spectroscopy. A unique core/shell structure of CdS nanocrystals was suggested for the explanation of the interesting phenomenon. PMID:14527472

  11. 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.

  12. 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.

  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 of anatase nanoleaves and size dependence of anatase-rutile transformation upon heating

    NASA Astrophysics Data System (ADS)

    Lisnycha, T. V.; Kirillov, S. A.; Potapenko, A. V.; Terikovska, T. E.; Kosilov, V. V.; Vyshnevskiy, O. A.

    2016-01-01

    Amorphous TiO2 obtained by adding TiCl4 to an alkaline medium crystallizes slowly and upon 3 years ageing transforms to nanosized anatase containing an admixture of brookite. The hydrothermal treatment of this sample in solutions of lithium hydroxide leads to anatase nanoleaves, and the more concentrated LiOH solution, the greater the nanoleaves and the smaller their specific surface area. The thermal treatment of nanoleaves leads to the bulk rutile, and the greater the specific surface area of anatase nanoleaves, the lower the anatase-rutile transition temperature. This is in line with conclusions based on the thermodynamic stability of nanosized anatase over the bulk rutile.

  15. Synthesis of CdTe QDs by hydrothermal method, with tunable emission fluorescence

    NASA Astrophysics Data System (ADS)

    Liu, Fujun; Laurent, Sophie; Vander Elst, Luce; Muller, Robert N.

    2015-09-01

    Cadmium telluride (CdTe) quantum dots (QDs) were prepared via a hydrothermal method, using 3-mercaptopropionic acid (3-MPA) as the stabilizing agent. With the help of absorption and emission spectra, it was found that prolonging the reaction time and raising the reaction temperature can increase the size of the QDs obtained, and hence induce a red shift of fluorescence emission. Rhodamine 6G was used as the reference to calculate the quantum yield (QY), and this showed that the use of extra Cd ions will distinctly increase the QY of CdTe.

  16. Synthesis and characterization of hydrothermally grown zinc oxide (ZnO) nanorods for optical waveguide application

    NASA Astrophysics Data System (ADS)

    Pandey, Chandan A.; Rahim, Rafis; Manjunath, S.; Hornyak, Gabor L.; Mohammed, Waleed S.

    2015-07-01

    We report a simple method to synthesize Zinc oxide nanorods, grown without using catalysis with less complicity. This was done by hydrothermal treatment of zinc nitrate and hexamine at 90°C and various times (5- 20h) and also we find that the nanorod size and shape depends on heating rate, temperature and heating time. ZnO nanorods have been investigated for their light guiding ability and their effective index of refraction for use in near air index optical systems by developing a ridge waveguide structure. ZnO nanorod waveguides (100 μm w x 2.5 μm h x 1mm l) were grown on a seeded glass substrate template using hydrothermal process at 90°C. Modification of the substrate surface in order to obtain dense perpendicularly-oriented ordered nanorods induced selective growth. These structures were characterized by SEM, EDX, and XRD. The guiding property, i.e. locally excited photoluminescence propagation along the length of the waveguide, was analyzed with imageprocessing program in MATLAB. Following application of a fiber optic white light source on the ZnO nanostructure, we found that light propagation occurred within the glass substrate. No such propagation occurred if light was applied on uncoated areas of the glass. Modeling of waveguide behavior to determine the number propagating modes was exercised using waveguide mode solver in COMSOL.

  17. Hydrothermal synthesis of N-doped spherical carbon from carboxymethylcellulose for CO2 capture

    NASA Astrophysics Data System (ADS)

    Wu, Qiong; Li, Wei; Liu, Shouxin; Jin, Chunde

    2016-04-01

    Spherical carbonaceous adsorbents (CSn) with micro-porosity developed for CO2 capture were prepared by a simple hydrothermal carbonization of carboxymethylcellulose (CMC) in the presence of urea, and activated in a high temperature N2 atmosphere. The effects of specific surface area, pore structure, and N content on the CO2 adsorption capacity were systematically investigated. Urea was found to react with surface carbonyl groups and other intermediate products generated by CMC hydrothermal carbonization, which produced highly spherical morphologies that also exhibited some ordered lattice structures. The particle size of N-doped CSn was larger than that of particles prepared without urea. Nitrogen was mainly present in pyridine (N-6), pyrrolic/pyridone (N-5) and quaternary (N-Q) forms. The high CO2 capture capacity was produced by a combination of N-doping and developing micro-pore structures. At an adsorption pressure of 1 bar, the capacity was dominated by the micro-porosity. However, during initial, lower pressures the N content dominated the CO2 adsorption capacity.

  18. 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.

  19. 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.

  20. Hydrothermal synthesis of microalgae-derived microporous carbons for electrochemical capacitors

    NASA Astrophysics Data System (ADS)

    Sevilla, M.; Gu, W.; Falco, C.; Titirici, M. M.; Fuertes, A. B.; Yushin, G.

    2014-12-01

    N-doped highly microporous carbons have been successfully fabricated from N-rich microalgae by the combination of low-cost hydrothermal carbonization and industry-adopted KOH activation processes. The hydrothermal carbonization process was found to be an essential step for the successful conversion of microalgae into a carbon material. The materials thus synthesized showed BET surface areas in the range ∼1800-2200 m2 g-1 exclusively ascribed to micropores. The carbons showed N contents in the 0.7-2.7 wt.%, owing to the use of N-rich microalgae as a carbon precursor. When tested in symmetric double layer capacitors (occasionally called supercapacitors) based on aqueous LiCl electrolytes, pseudocapacitance was only observable for the sample synthesized at the lowest temperature, 650 °C, which is the one exhibiting the largest amount of N- and O-containing groups. The samples synthesized at 700-750 °C exhibited excellent rate capability (only 20% of capacitance loose at 20 A g-1), with specific capacitances of 170-200 F g-1 at 0.1 A g-1. These materials showed excellent long-term cycling stability under high current densities.

  1. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2012-12-01

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

  3. 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.

  4. Rod-like nanocrystalline B-VO{sub 2}: Hydrothermal synthesis, characterization and electrochemical properties

    SciTech Connect

    Soltane, L.; Sediri, F.

    2014-05-01

    Graphical abstract: - Highlights: • Rod-like nanocrystalline VO{sub 2}(B) was prepared by hydrothermal process. • Reaction time on the morphology has been investigated. • CV has revealed reversible redox behavior with charge–discharge cycling. • Average coulombic efficiency is upper 98%. • Energy-related applications such as cathodes in lithium batteries. - Abstract: Rod-like nanocrystalline VO{sub 2}(B) has been successfully synthesized via a simple hydrothermal process by using V{sub 2}O{sub 5} as vanadium source and 4-butylaniline H{sub 3}C–(CH{sub 2}){sub 3}–(C{sub 6}H{sub 4})–HH{sub 2} as reducing and structure directing agent. The compounds were analyzed through X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy and UV–visible spectroscopy. The VO{sub 2}(B) nanorods are up to several micrometers in length and about 80 nm in thickness with a large optical band gap of ∼2.709 eV. Thin films of VO{sub 2}(B) nanorods deposited on ITO substrates were electrochemically characterized by cyclic voltammetry. The voltammograms show reversible redox behavior with charge–discharge cycling process corresponding to the reversible lithium intercalation/deintercalation into the crystal lattice. The average coulombic efficiency to this redox processes is upper 98% during the electrochemistry measurements.

  5. Hydrothermal synthesis of nanostructured zinc oxide and study of their optical properties

    SciTech Connect

    Moulahi, A.; Sediri, F.; Gharbi, N.

    2012-03-15

    Highlights: Black-Right-Pointing-Pointer Nanostructured ZnO were successfully obtained by a hydrothermal route. Black-Right-Pointing-Pointer Inorganic precursor and molar ratio are key factors for morphology and particle size. Black-Right-Pointing-Pointer Optical properties were also studied. -- Abstract: Nanostructured ZnO (nanorods, nanoshuttles) have been synthesized by hydrothermal approach using ZnCl{sub 2} or Zn(NO{sub 3}){sub 2}{center_dot}6H{sub 2}O as zinc sources and cetyltrimethylammonium bromide as structure-directing agent. Techniques X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-visible absorption, Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy have been used to characterize the structure, morphology and composition of the nanostructured zinc oxide. The optical properties of the as-obtained materials were also studied and showing that it is possible to apply the ZnO nanoshuttles and nanorods on the UV filter, photocatalysis, and special optical devices.

  6. 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%)

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

    PubMed

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

    2012-03-21

    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 Pm ̅3n 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. PMID:22327221

  8. 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.

  9. Hydrothermal synthesis and performance of a novel nanocrystalline Pb(2)Sn(2)O(6) photocatalyst.

    PubMed

    Wang, Wanjun; Bi, Jinhong; Wu, Ling; Li, Zhaohui; Wang, Xuxu; Fu, Xianzhi

    2008-12-17

    A novel nanocrystalline Pb(2)Sn(2)O(6) photocatalyst was prepared successfully for the first time by a hydrothermal process at 180 degrees C for 12 h. The samples were characterized by an x-ray diffractometer (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), surface area (BET) and ultraviolet-visible (UV-vis) spectroscopes. The results showed that the pH value played an important role in controlling the phase formation and crystallite sizes of the Pb(2)Sn(2)O(6). A single phase could be obtained at a pH>/=9. A possible reaction mechanism in the hydrothermal process was also proposed. The average particle size for the sample prepared at pH = 13 was only about 9 nm, and the BET surface area was as large as 76.7 m(2) g(-1). The N(2) adsorption-desorption isotherms and pore size distribution curve demonstrate a mesoporous structure with a narrow pore size distribution. As a novel photocatalyst, the prepared Pb(2)Sn(2)O(6) samples exhibit powerful photocatalytic activity for the decomposition of methyl orange under 365 nm UV light irradiation. Furthermore, it was found that the degradation process may be initiated directly by photogenerated holes rather than commonly sensed hydroxyl radicals. PMID:19942782

  10. 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.

  11. Hydrothermal synthesis of nanocrystalline ZnSe: An in situ synchrotron radiation X-ray powder diffraction study

    SciTech Connect

    Jorgensen, J.-E. Jensen, T.R.; Hanson, J.C.

    2008-08-15

    The hydrothermal synthesis of nanocrystalline ZnSe has been studied by in situ X-ray powder diffraction using synchrotron radiation. The formation of ZnSe was studied using the following starting mixtures: Zn+Se+H{sub 2}O (route A) and ZnCl{sub 2}+Se+H{sub 2}O+Na{sub 2}SO{sub 3} (route B). The route A experiment showed that Zn powder starts reacting with water at 134 deg. C giving ZnO and H{sub 2} followed by the formation of ZnSe which takes place in temperature range from 167 to 195 deg. C. The route B experiment shows a considerably more complex reaction path with several intermediate phases and in this case the formation of ZnSe starts at 141 deg. C and ZnSe and Se were the only crystalline phases observed at the end of the experiment where the temperature was 195 deg. C. The sizes of the nanocrystalline particles were determined to 18 and 9 nm in the route A and B experiments, respectively. Nanocrystalline ZnSe was also synthesized ex situ using the route A and B methods and characterized by conventional X-ray powder diffraction and transmission electron microscopy. An average crystalline domain size of ca. 8 nm was determined by X-ray powder diffraction in fair agreement with TEM images, which showed larger aggregates of nanoparticles having approximate diameters of 10 nm. Furthermore, a method for purification of the ZnSe nanoparticles was developed and the prepared particles showed signs of anisotropic size broadening of the diffraction peaks. - Graphical abstract: Stack of powder diagrams showing the formation of nanocrystalline ZnSe under hydrothermal conditions.

  12. 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

  13. 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.

  14. 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.

  15. Fe{sub 3}O{sub 4}–CNTs nanocomposites: Inorganic dispersant assisted hydrothermal synthesis and application in lithium ion batteries

    SciTech Connect

    Guo, Qixun Guo, Pengfei; Li, Juntao Yin, Hao; Liu, Jie; Xiao, Feilong; Shen, Daoxiang; Li, Ning

    2014-05-01

    Fe{sub 3}O{sub 4}–CNTs nanocomposites with a particle size of ∼80 nm have been synthesized through an organic-free hydrothermal synthesis strategy by using Sn(OH){sub 6}{sup 2−} as an inorganic dispersant, and served as anode materials of lithium ion batteries. Nano-sized and micro-sized Fe{sub 3}O{sub 4} without CNTs have also been prepared for comparison. The cycle performances of the as-obtained Fe{sub 3}O{sub 4} are highly size-dependent. The Fe{sub 3}O{sub 4}–CNTs nanocomposites can deliver reversible discharge capacity of ∼700 mA h/g at a current density of 50 mA/g after 50 cycles. The discharge capacity of the micro-sized Fe{sub 3}O{sub 4} decreased to 171 mA h/g after 50 cycles. Our work not only provides new insights into the inorganic dispersant assisted hydrothermal synthesis of metal oxides nanocrystals but also gives guidance for finding new nanocomposites as anode materials of lithium ion batteries. - Graphical abstract: Fe{sub 3}O{sub 4}–CNTs nanocomposites have been prepared through an inorganic dispersant assisted hydrothermal synthesis strategy, and served as anode materials of lithium ion batteries with enhanced performance. - Highlights: • Sn(OH){sub 6}{sup 2−} is a good inorganic dispersant for the hydrothermal synthesis of nano Fe{sub 3}O{sub 4}. • The cycle performances of nano Fe{sub 3}O{sub 4} anode are much better than that of micro Fe{sub 3}O{sub 4} anode. • Compositing CNTs can enhance the cycle performances of nano Fe{sub 3}O{sub 4} anode.

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

    SciTech Connect

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

    2009-09-15

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

  17. Hydrothermal synthesis of micrometer doping CaWO4 phosphors assisted by polymerization

    NASA Astrophysics Data System (ADS)

    Wang, Liyong; Han, Yuanyuan; Wang, Dan; Wang, Shiqi; Lu, Guoxin; Liang, Danyang; Wang, Xiaoyu; Pei, Nana; Gao, Lan

    2016-07-01

    CaWO4 crystals were prepared by hydrothermal method assisting with phenol-formaldehyde polymer. The morphology can be controlled by polymer, and X-ray diffraction patterns results present a scheelite-type tetragonal structure, characteristic infrared active modes for O-W-O in the range from 500 cm‑1 to 4000 cm‑1 by Fourier transform infrared spectroscopic techniques. Raman results indicate that the crystals possess seven Raman active modes in the range from 100 cm‑1 to 1000 cm‑1. A scanning electron microscopy study reveals that the particles exhibit uniform morphology. Luminescent properties were investigated by photoluminescence measurements, multicolor phosphors were obtained when Ca2+ was substituted partly by lanthanide ions.

  18. 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.

  19. 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

  20. Microwave-hydrothermal method for the synthesis of composite materials for removal of arsenic from water.

    PubMed

    Andjelkovic, Ivan; Jovic, Bojan; Jovic, Milica; Markovic, Marijana; Stankovic, Dalibor; Manojlovic, Dragan; Roglic, Goran

    2016-01-01

    Composite material Zr-doped TiO2, suitable for the removal of arsenic from water, was synthetized with fast and simple microwave-hydrothermal method. Obtained material, Zr-TiO2, had uniform size and composition with zirconium ions incorporated into crystal structure of titanium dioxide. Synthetized composite material had large specific surface area and well-developed micropore and mesopore structure that was responsible for fast adsorption of As(III) and As(V) from water. The influence of pH on the adsorption capacity of arsenic was studied. The kinetics and isotherm experiments were also performed. The treatment of natural water sample containing high concentration of arsenic with composite material Zr-TiO2 was efficient. The concentration of arsenic was reduced to the value recommended by WHO. PMID:26310708

  1. 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. PMID:24749449

  2. Hydrothermal synthesis and dielectric properties of chrysanthemum-like ZnO particles

    NASA Astrophysics Data System (ADS)

    Yan, Jun-Feng; Zhang, Zhi-Yong; You, Tian-Gui; Zhao, Wu; Yun, Jiang-Ni

    2009-09-01

    By orthogonal design theory, technological parameters of chrysanthemum-like ZnO particles prepared in a hydrothermal process are optimized. This paper reports a set of technological parameters for growing chrysanthemum-like ZnO particles on a large scale. It investigates the morphologies and crystalline structures of the as-synthesized three-dimensional ZnO particles with a scanning electron microscope, x-ray diffractometer and transmission electron microscope, and the possible growth mechanism on the three-dimensional ZnO particles. The experimental results indicate that the values of in', in″ and tan δe gradually increase in the X band with the improvement of the developmental level of chrysanthemum-like ZnO particles, implying that the electromagnetic wave absorbing property depends on the morphologies of three-dimensional ZnO particles.

  3. Hydrothermal synthesis of zirconium dioxide coating on the surface of wood with improved UV resistance

    NASA Astrophysics Data System (ADS)

    Wan, Caichao; Lu, Yun; Sun, Qingfeng; Li, Jian

    2014-12-01

    Nano-ZrO2 aggregations were successfully layer-by-layer deposited on the wood surface by a simple mild one-pot hydrothermal method. The resulting ZrO2/wood nanocomposites were characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS) and thermogravimetric analysis (TGA). The results indicated that the strong hydrogen bonds between the amorphous ZrO2 and the hydroxide radicals of wood surface were formed, and the strong interaction contributed to the enhancement of the nanocomposites heat stability. Moreover, compared with the original wood, the ZrO2/wood showed more superior UV-resistant ability through a 600-h QUV accelerated aging test.

  4. Hydrothermal synthesis and infrared emissivity property of flower-like SnO{sub 2} particles

    SciTech Connect

    Tian, J. X.; Zhang, Z. Y.; Yan, J. F.; Ruan, X. F.; Yun, J. N.; Zhao, W.; Zhai, C. X.

    2014-04-15

    The flower-like SnO{sub 2} particles are synthesized through a simple hydrothermal process. The microstructure, morphology and the infrared emissivity property of the as-prepared products are characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscope (TEM), and infrared spectroradio meter (ISM) respectively. The results show that the as-prepared SnO{sub 2} products are all indexed to tetragonal cassiterite phase of SnO{sub 2}. The different molarity ratios of the OH{sup −} concentration to Sn{sup 4+} concentration ([OH{sup −}]:[Sn{sup 4+}]) and the polyacrylamide (PAM) lead to the different morphological structures of SnO{sub 2}, which indicates that both the [OH{sup −}]:[Sn{sup 4+}] and the PAM play an important role in the morphological evolution respectively. The infrared emissivities of the as-prepared SnO{sub 2} products are discussed.

  5. Hydrothermal synthesis of sodium vanadate nanobelts as high-performance cathode materials for lithium batteries

    NASA Astrophysics Data System (ADS)

    Yang, Kaiwen; Fang, Guozhao; Zhou, Jiang; Qin, Mulan; Tang, Yan; Pan, Anqiang; Liang, Shuquan

    2016-09-01

    The sodium vanadate (Na0.76V6O15) nanobelts have been successfully synthesized via a facile hydrothermal reaction followed by annealing. The ultra-long nanobelts have a length ranging from several micrometers to several dozens of micrometers. As cathode materials for lithium-ion batteries, the Na0.76V6O15 nanobelts exhibit high discharge capacity, excellent cyclic stability and good rate capability. High discharge capacity of 248 and 214 mA h g-1 can be obtained at the current density of 300 and 500 mA g-1, respectively. Meanwhile, it maintains a stable capacity of 113 mA h g-1 after 200 cycles at a high current density of 2000 mA g-1 with no capacity decay. The superior electrochemical performances may be attributed to the novel nanobelts structure and excellent structural stability of Na0.76V6O15.

  6. One-step hydrothermal synthesis of carboxyl-functionalized upconversion phosphors for bioapplications.

    PubMed

    Yang, Jianping; Shen, Dengke; Li, Xiaomin; Li, Wei; Fang, Yin; Wei, Yong; Yao, Chi; Tu, Bo; Zhang, Fan; Zhao, Dongyuan

    2012-10-22

    In this paper, we report a facile one-step hydrothermal method to synthesize phase-, size-, and shape-controlled carboxyl-functionalized rare-earth fluorescence upconversion phosphors by using a small-molecule binary acid, such as malonic acid, oxalic acid, succinic acid, or tartaric acid as capping agent. The crystals, from nano- to microstructures with diverse shapes that include nanospheres, microrods, hexagonal prisms, microtubes, microdisks, polygonal columns, and hexagonal tablets, can be obtained with different reaction times, reaction temperatures, molar ratios of capping agent to sodium hydroxide, and by varying the binary acids. Fourier transform infrared, thermogravimetric analysis, and upconversion luminescence spectra measurements indicate that the synthesized NaYF(4):Yb/Er products with hydrophilic carboxyl-functionalized surface offer efficient upconversion luminescent performance. Furthermore, the antibody/secondary antibody conjugation can be realized by the carboxyl-functionalized surfaces of the upconversion phosphors, thus indicating the potential bioapplications of these kinds of materials. PMID:22996059

  7. 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. PMID:21852740

  8. Hydrothermal synthesis of Fe2O3/ZnO heterojunction photoanode for photoelectrochemical water splitting

    NASA Astrophysics Data System (ADS)

    Chen, Chao; Bai, Hongye; da, Zulin; Li, Meng; Yan, Xu; Jiang, Jinhui; Fan, Weiqiang; Shi, Weidong

    2015-05-01

    We report a photoanode based on Fe2O3/zinc oxide (ZnO) heterojunction synthesized by hydrothermal method for photoelectrochemical (PEC) water splitting. The forming heterojunction is systemically characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results from the I-V characteristic curve and conversation efficiency of Fe2O3/ZnO heterojunction reveal that the forming heterojunction would be a benefit for electron transferring from conduction band of ZnO to that of Fe2O3. However, the quantity of ZnO film has an effect on the photocurrent density, the suitable of which has shown enhanced PEC performance.

  9. 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.

  10. 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.

  11. Hydrothermal synthesis of layered sodium manganese oxide nanowires and their electrochemical performance.

    PubMed

    Liu, Xian-Ming; Huang, Zhen-Dong; Oh, Sei-Woon; Ma, Peng-Cheng; Ma, Jun; Li, Bao-Hua; Kim, Jang-Kyo

    2010-11-01

    A new method for preparing black birnessite nanowires is introduced. Layer-structured manganese oxide nanowires were synthesized by a facile hydrothermal method, and using both NaMnO4 and CH3CH2OH as the precursors in a concentrated NaOH solution. The structure, composition, appearance and electrochemical performance of the product were characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), energy diffraction (ED), high-resolution transmission electron microscopy (HRTEM), thermogravimetric analysis (TGA) and constant current charge/discharge. The XRD patterns showed a single phase corresponding to a crystalline birnessite-based manganese oxide. TEM studies suggested their wire-like structures. The TGA measurement demonstrated that they possessed an excellent thermal stability up to 400 degrees C. In the potential window of 2.0-4.3 V, the product exhibited excellent cyclic stability and rapid charge-discharge performance. PMID:21137939

  12. 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.

  13. 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.

  14. 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

  15. 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.

  16. 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.

  17. 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}.

  18. Metastable (Bi, M)2(Fe, Mn, Bi)2O(6+x) (M = Na or K) pyrochlores from hydrothermal synthesis.

    PubMed

    Daniels, Luke M; Playford, Helen Y; Grenèche, Jean-Marc; Hannon, Alex C; Walton, Richard I

    2014-12-15

    The hydrothermal syntheses, structures, and magnetism of two new pyrochlore oxides of compositions (Na0.60Bi1.40)(Fe1.06Mn0.17Bi0.77)O6.87 and (K0.24Bi1.51)(Fe1.07Mn0.15Bi0.78)O6.86 are described. With preparation at 200 °C for 6 h in solutions of sodium or potassium hydroxide, the alkali metals introduced from these mineralizers are essential to the synthesis of the phases. The average long-range order of the pyrochlore structure, with space group Fd3̅m, was investigated and refined against X-ray and neutron diffraction data, and it was shown that disorder is present in both the metal and coordinating oxygen positions, along with metal-mixing across both the A and B sites of the structure. XANES analysis confirms the presence of Mn(4+), mixed valence Bi(3+) and Bi(5+), and Fe(3+), the last also verified by (57)Fe Mössbauer spectroscopy. Magnetic measurements show a lack of long-range magnetic ordering that is typical of geometrically frustrated pyrochlores. The observed glasslike interactions occur at low temperatures, with the onset temperature depending upon the magnitude of the applied external field. Variable temperature X-ray diffraction shows that these pyrochlores are metastable and collapse on heating at ca. 395 °C, which suggests that their formation by conventional solid-state synthesis would be impossible. PMID:25413441

  19. 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.

  20. Platelet-like hexagonal SrFe12O19 particles: Hydrothermal synthesis and their orientation in a magnetic field

    NASA Astrophysics Data System (ADS)

    Zhang, Tao; Peng, Xiaoling; Li, Jing; Yang, Yanting; Xu, Jingcai; Wang, Panfeng; Jin, Dingfeng; Jin, Hongxiao; Hong, Bo; Wang, Xinqing; Ge, Hongliang

    2016-08-01

    Platelet-like hexagonal SrFe12O19 particles were prepared by hydrothermal synthesis, and the effects of molar ratio of Fe/Sr (RFe/Sr) on the phase compositions, morphologies and magnetic properties of as-prepared samples were investigated. The optimum RFe/Sr is identified as 8:1. The hexagonal platelet-like particles are nano-scale in thickness and micro-scale in diameter. The low coercivity is a consequence of the large shape anisotropy of the as-synthesized particles. The platelet-like hexagonal SrFe12O19 particles were then dispersed in epoxy resin and formed ordered arrangement structure which took root in the curing epoxy matrix under an external magnetic field of 8000 Oe. The microstructures, morphologies and magnetic properties of the bulk samples orientated and nonaligned were studied. The platelet-like particles arrange with the platelet perpendicular to the magnetic field direction in the orientated samples. This demonstrates that the easy axis of the particle is perpendicular to the platelet, and that the magnetocrystalline anisotropy still plays a leading role in the changing effective anisotropy with the rapidly growing shape anisotropy. The remanence (Mr) of the bulk samples is changed obviously after orientation, while the coercivity nearly remains constant. That is, the maximum energy products (BH)max can be effectively adjusted by given a suitable magnetic field.

  1. Microwave-hydrothermal synthesis of nanostructured Na-birnessites and phase transformation by arsenic(III) oxidation

    SciTech Connect

    Dias, Anderson Sa, Rodrigo G.; Spitale, Matheus C.; Athayde, Maycon; Ciminelli, Virginia S.T.

    2008-06-03

    Microwave-hydrothermal synthesis was employed to produce Na-birnessites. Crystalline, single-phase materials were obtained at temperatures as low as 120 deg. C and times as short as 1 min. X-ray diffraction and Raman spectroscopy were used to characterize the structural features of the nanostructured powders. Birnessites possessed a monoclinic structure in space group C2/m with nine Raman-active bands, all of which were observed for the first time due to optimized acquisition of the spectroscopic data. The highly reactive materials produced were submitted to sorption experiments with As(III). An oxidative precipitation occurred with the production of Mn(II) arsenate at higher arsenic concentrations. In addition, the formation of hausmannite (Mn{sub 3}O{sub 4}) was confirmed by X-ray diffraction and Raman analyses of the reacted solid phase. The observed 14 Raman-active modes were adjusted according to the tetragonal I4{sub 1}/amd space group for hausmannite. An additional band related to the breathing mode of the arsenate was observed, leading to the conclusion that adsorption onto hausmannite takes place in addition to the oxidative precipitation of manganese arsenate.

  2. 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.

  3. Hydrothermal synthesis of hierarchical SnO2 nanostructures made of superfine nanorods for smart gas sensor

    NASA Astrophysics Data System (ADS)

    Kuang, Xinliang; Liu, Tianmo; Shi, Dongfeng; Wang, Wenxia; Yang, Mingping; Hussain, Shahid; Peng, Xianghe; Pan, Fusheng

    2016-02-01

    We report synthesis of hierarchical SnO2 nanostructures by a facile hydrothermal method. Extensive structural characterizations demonstrate that the well-defined hierarchical nanostructures are composed of numerous one-dimensional nanorods, the diameter and density of which can be precisely tailored by adjusting the dosage of NaOH. Interestingly, with more NaOH added, smaller and denser nanorods are formed, which is consistent with the assumption. We proposed that the nucleation process was facilitated in such case leading to all-direction rapider growth. Moreover, the nucleation process could be started by the decomposition of preformed ZnSn(OH)6 induced by alkali etching. Based on the comparative experiments, a possible growth mechanism for hierarchical SnO2 nanostructures has been proposed and discussed in detail. The gas sensing properties of the as-prepared hierarchical SnO2 nanostructures were all tested. It was found that the S3 sample which assembled with smallest and densest nanorods showed the excellent sensitivities toward ethanol.

  4. Hydrothermal synthesis of rutile-anatase TiO2 nanobranched arrays for efficient dye-sensitized solar cells

    NASA Astrophysics Data System (ADS)

    Kwon, Soon Jin; Im, Hyo Been; Nam, Jung Eun; Kang, Jin Kyu; Hwang, Taek Sung; Yi, Kwang Bok

    2014-11-01

    Rutile-anatase TiO2 nanobranched arrays were prepared in two sequential hydrothermal-synthesis steps. The morphologies and crystalline nanostructures of the samples were investigated by controlling growth time and the concentration of the titanium precursor. All samples were characterized by field-emission scanning electron microscopy and X-ray diffraction analysis. It was found that treating the surfaces of rutile TiO2 nanorods with aqueous TiCl4 solutions allows the anatase TiO2 nanobranches to grow perpendicular to the main rutile TiO2 nanorods attached to the FTO glass. Irregularly shaped, dense TiO2 structures formed in the absence of TiCl4 treatment. A light-to-electricity conversion efficiency of 3.45% was achieved using 2.3 μm tall TiO2 nanobranched arrays in a dye-sensitized solar cell. This value is significantly higher than that observed for pure rutile TiO2 nanorods.

  5. Hydrothermal synthesis and photoluminescence investigation of NaY(MoO4)2:Eu3+ nanophosphor.

    PubMed

    Park, Sung Wook; Noh, Hyeon Mi; Moon, Byung Kee; Choi, Byung Chun; Jeong, Jung Hyun; Yang, Hyun Kyoung

    2014-11-01

    An intense red-emitting NaY(MoO4)2:Eu3+ nanophosphor was developed using a hydrothermal technique. A highly pure and single-phase NaY(MoO4)2:Eu3+ nanopowder was obtained after sintering the as-prepared sample at 800 degrees C. The crystal structure and photoluminescence properties of this double molybdate were investigated. X-ray diffraction analysis showed that the NaY(MoO4)2 nanoparticles have a scheelite-type tetragonal structure, without mixed phases. Rietveld analysis provided the atomic coordinates and Mo-O-rare-earth angles. The morphology of the molybdate precursor was controlled by adjusting the synthesis conditions. The pH was found to play a crucial role in the particle size and morphology distribution. The crystalline powder phosphor exhibited intense and efficient red emissions attributed to efficient energy-transfer from MoO4(2-) to Eu3+. The chromaticity coordinates (x,y) of the NaY(MoO4)2:Eu3+ phosphor sample correspond to (0.662, 0.337). The NaY(MoO4)2:Eu3+ powder exhibited a deep-red emission under near-ultraviolet (UV) excitation, indicating a promising red phosphor for white-light-emitting diodes based on near-UV light-emitting diodes. PMID:25958592

  6. 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).

  7. 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. PMID:25521555

  8. 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

  9. Hydrothermal synthesis of flower-like MoS2 nanospheres for electrochemical supercapacitors.

    PubMed

    Zhou, Xiaoping; Xu, Bin; Lin, Zhengfeng; Shu, Dong; Ma, Lin

    2014-09-01

    Flower-like MoS2 nanospheres were synthesized by a hydrothermal route. The structure and surface morphology of the as-prepared MoS2 was characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The supercapacitive behavior of MoS2 in 1 M KCl electrolyte was studied by means of cyclic voltammetry (CV), constant current charge-discharge cycling (CD) and electrochemical impedance spectroscopy (EIS). The XRD results indicate that the as-prepared MoS2 has good crystallinity. SEM images show that the MoS2 nanospheres have uniform sizes with mean diameter about 300 nm. Many nanosheets growing on the surface make the MoS2 nanospheres to be a flower-like structure. The specific capacitance of MoS2 is 122 F x g(-1) at 1 A x g(-1) or 114 F x g(-1) at 2 mv s(-1). All the experimental results indicate that MoS2 is a promising electrode material for electrochemical supercapacitors. PMID:25924398

  10. Hydrothermal-reduction synthesis of manganese oxide nanomaterials for electrochemical supercapacitors.

    PubMed

    Zhang, Xiong; Chen, Yao; Yu, Peng; Ma, Yanwei

    2010-11-01

    In the present work, amorphous manganese oxide nanomaterials have been synthesized by a common hydrothermal method based on the redox reaction between MnO4(-) and Fe(2+) under an acidic condition. The synthesized MnO2 samples were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and electrochemical studies. XRD results showed that amorphous manganese oxide phase was obtained. XPS quantitative analysis revealed that the atomic ratio of Mn to Fe was 3.5 in the MnO2 samples. TEM images showed the porous structure of the samples. Electrochemical properties of the MnO2 electrodes were studied using cyclic voltammetry and galvanostatic charge-discharge cycling in 1 M Na2SO4 aqueous electrolyte, which showed excellent pseudocapacitance properties. A specific capacitance of 192 Fg(-1) at a current density of 0.5 Ag(-1) was obtained at the potential window from -0.1 to 0.9 V (vs. SCE). PMID:21138016