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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. 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.

  17. 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...

  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 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.

  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 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.

  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

    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.

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

    PubMed Central

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

    2016-01-01

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

  9. 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.

  10. 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.

  11. 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

  12. 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.

  13. 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.

  14. 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.

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

    NASA Technical Reports Server (NTRS)

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

    2011-01-01

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

  19. 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

  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. 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

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

    PubMed Central

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

    2013-01-01

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

  3. 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

  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. 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

  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. 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.

  10. 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).

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  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 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

  18. 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

  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. 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.

  6. [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

  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. 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.

  10. 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}.

  11. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2012-07-01

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

  13. 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.

  14. 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.

  15. 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

  16. 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

  17. 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.

  18. 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.

  19. 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%.

  20. 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

  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. 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.

  13. 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.

  14. 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

  15. 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

  16. 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

  17. 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

  18. 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.

  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 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

  5. 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

  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. 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.

  12. 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.

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

    PubMed

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

    2001-11-21

    [(C2H5)2NH2]2[(UO2)5(PO4)4] was prepared from U3O8, HONEt2 and phosphoric acid under hydrothermal conditions (180 degrees C, 5 days) and represents the first three-dimensional open-framework uranium phosphate prepared to date. PMID:12240084

  14. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2015-11-01

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

  16. 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.

  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. 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

  20. 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

  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. 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.

  6. 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.

  7. 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

  8. 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

  9. 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.

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

    SciTech Connect

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

    2010-11-15

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

  11. 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. 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.

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

    SciTech Connect

    Song Xuchun Zheng Yifan; Wang Yun

    2008-05-06

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

  14. 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

  15. 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

  16. 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.

  17. 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.

  18. 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

  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. 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.

  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. 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

  7. 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.

  8. 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.

  9. 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.

  10. 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

  11. 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.

  12. 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.

  13. 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.

  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. 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.

  16. 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.

  17. 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.

  18. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2012-12-01

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

  20. 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.

  1. 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.

  2. 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

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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%)

  8. 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

  9. 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.

  10. 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.

  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. 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.

  17. 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

  18. 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

  19. 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

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. 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

  5. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2015-12-01

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

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  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. 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

  13. 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

  14. 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.

  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. 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}.

  17. 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.

  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. 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.

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

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

    SciTech Connect

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

    2007-01-01

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

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

    PubMed Central

    2010-01-01

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

  8. Hydrothermal synthesis of blue-emitting YPO4:Yb3+ nanophosphor

    NASA Astrophysics Data System (ADS)

    Wang, Guangfa; Gao, Linhui; Zhu, Hongliang; Zhou, Weijie

    2016-06-01

    The blue-emitting YPO4 phosphors doped with Yb3+ were prepared by a simple hydrothermal method. All the products were characterized by XRD and TEM, which revealed that they were zircon structure with leaf-like morphology. According to the analysis of photoluminescence spectra, upon ultraviolet (275 nm) excitation, the Yb3+ doped YPO4 phosphor showed an intense blue emission composed of two main bands at 420 and 620 nm assigned to charge transfer state (CTS) → 2F5/2 and CTS → 2F7/2, respectively. Moreover, the optimum doping concentration of Yb3+ in YPO4 phosphor was 1%, which exhibited the maximum emission intensity. The possible physical mechanism of concentration quenching was discussed, and the critical transfer distance determined to be 23.889 Å. In particular, the color purity of the as-synthesized Yb3+ doped YPO4 phosphor was as high as 83%, which made it an excellent candidate for blue-emitting materials.

  9. Facile hydrothermal synthesis of one-dimensional nanostructured α-MnO2 for supercapacitors

    NASA Astrophysics Data System (ADS)

    Wei, Hongmei; Wang, Jinxing; Yang, Shengwei; Zhang, Yangyang; Li, Tengfei; Zhao, Shuoqing

    2016-09-01

    α-MnO2 recently becomes a promising candidate of electrode materials for high effective supercapacitors in which it possesses of unique structure of 2×2 tunnels that can provide more electrons and ions diffusion paths. In this work, different morphologies MnO2 with α-phase crystalline structure have been prepared via a one-step facile hydrothermal method by adding various reagents. Compositions, microstructures and morphologies of these as-synthesized materials were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) and electrochemical properties of α-MnO2 electrodes were studied by the cyclic voltammetry (CV), galvanostatic charge/discharge and electrochemical impedance spectroscopy (EIS) in 1 M Na2SO4 aqueous solution. The specific capacitance of nanowires were 158 F g-1 while the specific capacitance of nanorods were 106 F g-1 at current density of 4 A g-1, and improved performance of the wire-like electrode material was probably ascribed to the larger specific surface area that can provide relatively more active sites for high capacity. Meanwhile, both the nanowires and nanorods of MnO2 presented fine cycle stability after continuous multiple charge/discharge times.

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

    SciTech Connect

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

    2014-09-03

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

  11. 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).

  12. 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

  13. 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

  14. 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

  15. 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

  16. Hydrothermal Synthesis and Luminescence Property of Nanoscaled BiPO4:Eu3+ Powders.

    PubMed

    Shi, Xiaolei; Liu, Yun; Zhang, Jin; Zhang, Kun; Li, Peng; Zuo, Haoqiang

    2016-04-01

    A series of Bi1-xPO4:xEu3+ phosphors were prepared using a simple hydrothermal method. The effects of pH and Eu3+ doping on the structure, morphology and luminescence properties of BiPO4:Eu3+ were investigated systematically. X-ray diffraction (XRD) and field emission scanning electron microscope (FE-SEM) results reveal that the as-prepared BiPO4 crystals are in a low temperature monoclinic phase (LTMP), and have a rod-like structure with a size in the range of 1-5 µm at pH 1. Increasing the pH to 2 transforms the BiPO4 to its hexagonal phase (HP), with peanut-like structures ranging from 50 to 150 nm. At pH 1, when the doping level is increased to 0.07, the phase transformation from LTMP to HP occurs, meaning that the amount of HP components increase with increasing Eu3+ doping. Furthermore, all the diffraction peaks of the Bi1-xPO4:xEu3+ can be fitted very well to HP when x = 0.11. The photoluminescence (PL) spectra suggest that orange-red luminescence can be observed in the series of BiPO4:Eu3+ phosphors, and that concentration quenching occurs when x = 0.07. PMID:27451718

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

    PubMed

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

    2010-07-14

    An investigation of the one-step hydrothermal crystallisation of lithium niobates reveals that reaction between Nb(2)O(5) and aqueous LiOH at 240 degrees C yields materials with a disordered rock-salt structure where the metals are statistically distributed over the cation sites. This contrasts with the well-studied reaction between Nb(2)O(5) and NaOH or KOH that produces ANbO(3) (A = Na, K) perovskites. Powder neutron diffraction shows that materials prepared at short reaction times and lower LiOH concentration (2.5 M) are lithium deficient and have a slight excess of niobium, but that at longer periods of reaction in 5 M LiOH, close to the ideal, stoichiometric Li(0.75)Nb(0.25)O composition is produced. Upon annealing this phase cleanly transforms into the known ordered rock-salt material Li(3)NbO(4), a process we have followed using thermodiffractometry, which indicates that transformation begins at approximately 700 degrees C. Solid-state (93)Nb and (7)Li NMR of the disordered and ordered rock-salt phases shows that both contain single metal sites but there is clear evidence for local disorder in the disordered samples. For the ordered material, NMR parameters derived from experiment are also compared to those calculated using density functional theory and are shown to be in good agreement. PMID:20442945

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

    NASA Astrophysics Data System (ADS)

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

    2011-10-01

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

  19. Hydrothermal synthesis and structural characterization of two novel lanthanide supramolecular coordination polymers with nano-chains

    NASA Astrophysics Data System (ADS)

    Wan, Yong-Hong; Jin, Lin-Pei; Wang, Ke-Zhi

    2003-04-01

    Two novel lanthanide supramolecular coordination polymers, {[Nd 2(phth) 3(phen)(H 2O)]·H 2O} n ( 1, phth=phthalate, phen=1,10-phenanthroline) and {[Ho 2(phth) 3(phen)(H 2O) 2]·3H 2O} n ( 2), have been synthesized by hydrothermal method and characterized by X-ray diffraction. The results show that complex 1 crystallizes in triclinic space group P 1¯ with a=7.605(2) Å, b=12.972(4) Å, c=18.773(6) Å, α=109.778(5)°, β=91.657(5)°, γ=103.951(5)° and Z=2. Complex 1 has a one-dimentional nano-chain structure and the existence of hydrogen bonds and π- π interactions results in 2D network structure. Complex 2 crystallizes in triclinic space group P 1¯ with a=11.695(2) Å, b=13.488(3) Å, c=13.761(3) Å, α=87.09(3)°, β=67.40(3)°, γ=67.41(3)° and Z=2. Complex 2 features a zigzag double-chain and the hydrogen bonds lead to the formation of a three-dimensional network. Both Complex 1 and 2 have two metal environments.

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

    NASA Astrophysics Data System (ADS)

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

    2013-06-01

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

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

    PubMed

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

    2014-07-01

    Pr3+ doped mesoporous TiO2 photocatalysts with a different molar ratio of Pr to Ti were prepared by a hydrothermal method using triblock copolymer as the template. The as-prepared samples were systematically characterized by X-ray diffraction, N2 adsorption-desorption, X-ray photoelectron spectra, transmission electron microscopy and UV-visible diffuse reflectance spectroscopy. The characterizations indicated all the samples had mesoporous structure and narrow pore size distribution. Pr3+ doping enlarged the surface area and decreased the crystallite size. The surface area of the samples varied from 136 to 170 m2/g, and the average crystallite size ranged between 5.04 and 7.60 nm. The effect of Pr3+ doping amount on the photocatalytic activity of mesoporous TiO2 was evaluated by the degradation of methyl orange under UV light irradiation. The results showed that the suitable amount of Pr3+ doped samples exhibited the higher photocatalytic activity than mesoporous TiO2. Among the samples, 1 at.% Pr3+ doped mesoporous TiO2 showed the highest photocatalytic activity. PMID:24757971

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

    PubMed

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

    2014-11-01

    Yttrium-doped ZnO (YZO) nanorods were synthesized by hydrothermal growth on a quartz substrate with various post-annealing temperatures. To investigate the effects of post-annealing on the optical properties and parameters of the nanorods, X-ray diffractometry (XRD), photoluminescence (PL) measurement, and ultraviolet (UV)-visible spectroscopy were used. From the XRD investigation, the full width at half maximum (FWHM) and the dislocation density of the nanorods was found to increase with an increase in the post-annealing temperature. In the PL spectra, the intensity of the near band edge (NBE) emission peak in the UV region also increases with an increase in the temperature of post-annealing. The deep level emission (DLE) peak in the visible region changes with various post-annealing temperatures, and its intensity increases remarkably with post-annealing at 800 degrees C. In this paper, changes in the optical parameters of the nanorods caused by variation in the behavior of Y during post-annealing was investigated, with properties such as absorption coefficients, refractive indices, and dispersion parameters being obtained from transmittance and reflectance analysis. PMID:25958523

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

    NASA Astrophysics Data System (ADS)

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

    2014-09-01

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

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

    PubMed

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

    2015-11-01

    Zinc stannate (Zn2SnO4 or ZTO) nanoparticles were synthesized via hydrothermal method using NaOH as a mineralizer. X-ray diffraction (XRD), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM) of the synthesized ZTO nanoparticles revealed the formation of highly pure ZTO phase with the spinel-like structure. The nanoparticles have spherical shape with an average size of about 25 nm. The Raman spectrum of the sample was dominated by the A(1g) vibration mode of pure ZTO phase. From UV-Vis measurement, a band gap E(g) of 3.465 eV was determined. The photocatalytic activity of the ZTO nanoparticles was evaluated for the photodegradation of rhodamine B (RhB) under visible light irradiation. The influence of catalyst concentration and irradiation time on the photocatalytic process was investigated. The ZTO catalyst showed the best photocatalytic performance at a concentration of 0.2 g/L, and the photodecomposition of RhB followed first-order kinetics with a rate constant k=0.0249 min(-1). The ZTO-assisted photocatalytic degradation of RhB occurred via two competitive processes: a photocatalytic process and a photosensitized process. The detection of hydroxyl radicals by fluorescence measurements suggests that these species play an important role in the photocatalytic process. PMID:26196720

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

    SciTech Connect

    Nefzi, H.; Sediri, F.

    2013-05-01

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

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

    PubMed Central

    2013-01-01

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

  7. Hydrothermal synthesis of blue-emitting YPO4:Yb3+ nanophosphor

    NASA Astrophysics Data System (ADS)

    Wang, Guangfa; Gao, Linhui; Zhu, Hongliang; Zhou, Weijie

    2016-05-01

    The blue-emitting YPO4 phosphors doped with Yb3+ were prepared by a simple hydrothermal method. All the products were characterized by XRD and TEM, which revealed that they were zircon structure with leaf-like morphology. According to the analysis of photoluminescence spectra, upon ultraviolet (275 nm) excitation, the Yb3+ doped YPO4 phosphor showed an intense blue emission composed of two main bands at 420 and 620 nm assigned to charge transfer state (CTS) → 2F5/2 and CTS → 2F7/2, respectively. Moreover, the optimum doping concentration of Yb3+ in YPO4 phosphor was 1%, which exhibited the maximum emission intensity. The possible physical mechanism of concentration quenching was discussed, and the critical transfer distance determined to be 23.889 Å. In particular, the color purity of the as-synthesized Yb3+ doped YPO4 phosphor was as high as 83%, which made it an excellent candidate for blue-emitting materials.

  8. Microwave-assisted hydrothermal synthesis and characterization of ZnO nanorods.

    PubMed

    Ocakoglu, K; Mansour, Sh A; Yildirimcan, S; Al-Ghamdi, Ahmed A; El-Tantawy, F; Yakuphanoglu, F

    2015-09-01

    For the purpose of this study, the nanorods of zinc oxide were synthesized by rapid microwave-assisted hydrothermal route. The microstructure and surface morphology of the sensitized nanorods were characterized by X-ray diffraction (XRD), field emission scanning electron microscope (FE-SEM) and transmission electron microscope (TEM). XRD results indicate that synthesized ZnO nanorods have wurtzite phase. The calculated value of the particle size using Debye Scherrer formula and Williamson Hall plot was found to be 20-28 nm and 35.3 nm, respectively. Low uniformity distribution of rod-like morphology (60-80 nm in diameter and average length about 250 nm) are seen in TEM micrographs. The optical parameters of the prepared ZnO nanorods have been calculated using Kubeleka-Munk approach for the UV-vis diffuse reflectance spectrum. It is found that the direct transition optical band gap of the studied sample is 3.17 eV. The direct current electrical conductivity (σ) was increased from 6.7×10(-8) to 3×10(-7) Ω(-1) cm(-1) with increasing the temperature (T) in the range (300-425 K). The obtained variation of σ with T refers that the conductivity mechanism is controlled by thermally activated process. PMID:25913135

  9. Hydrothermal synthesis of core-shell TiO2 to enhance the photocatalytic hydrogen evolution

    NASA Astrophysics Data System (ADS)

    Jiang, Jinghui; Zhou, Han; Zhang, Fan; Fan, Tongxiang; Zhang, Di

    2016-04-01

    A hydrothermal approach was designed to synthesize core-shell TiO2 with interior cavity by making sodium dodecyl sulfonate (SDS) as the surfactant and the mixture of water and ethanol as the solvent. The control experiment of solvent reveals ethanol and water are responsible for the formation of sphere and interior cavity, respectively. Besides, SDS can assist the growth of core-shell structure, and the sizes of sphere and interior cavity can be tuned by regulating the reaction time or temperature. UV-vis absorption proves core-shell structure with interior cavity can increase the absorption of incident light to enhance the optical activity of final product. The calculated bandgap and photoluminescence (PL) analyses reveal the coexistence of rutile in final product can optimize the bandgap to 3.03 eV and delay the charge recombination. As a result, an effective photocatalytic hydrogen evolution under full spectrum irradiation can be harvested by the as-synthesized core-shell spheres to reach a quantum yield, approximately 9.57% at 340 nm wavelength.

  10. Mechanochemical-hydrothermal synthesis of calcium phosphate powders with coupled magnesium and carbonate substitution

    NASA Astrophysics Data System (ADS)

    Suchanek, Wojciech L.; Byrappa, Kullaiah; Shuk, Pavel; Riman, Richard E.; Janas, Victor F.; TenHuisen, Kevor S.

    2004-03-01

    Magnesium- and carbonate-substituted calcium phosphate powders (Mg-, CO 3-CaP) with various crystallinity levels were prepared at room temperature via a heterogeneous reaction between MgCO 3/Ca(OH) 2 powders and an (NH 4) 2HPO 4 solution using the mechanochemical-hydrothermal route. X-ray diffraction, infrared spectroscopy, and thermogravimetric analysis were performed. It was determined that the powders containing both Mg 2+ and CO 32- ions were incorporated uniformly into an amorphous calcium phosphate phase while in contrast, the as-prepared powder free of these dopants was crystalline phase-pure, stoichiometric hydroxyapatite. Dynamic light scattering revealed that the average particle size of the room temperature Mg-, CO 3-CaP powders was in the range of 482 nm-700 nm with a specific surface area between 53 and 91 m 2/g. Scanning electron microscopy confirmed that the Mg-, CO 3-CaP powders consisted of agglomerates of equiaxed, ≈20-35 nm crystals.

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

    SciTech Connect

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

    2015-01-15

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

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

    NASA Astrophysics Data System (ADS)

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

    2014-09-01

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

  13. Microwave-assisted hydrothermal synthesis and characterization of ZnO nanorods

    NASA Astrophysics Data System (ADS)

    Ocakoglu, K.; Mansour, Sh. A.; Yildirimcan, S.; Al-Ghamdi, Ahmed A.; El-Tantawy, F.; Yakuphanoglu, F.

    2015-09-01

    For the purpose of this study, the nanorods of zinc oxide were synthesized by rapid microwave-assisted hydrothermal route. The microstructure and surface morphology of the sensitized nanorods were characterized by X-ray diffraction (XRD), field emission scanning electron microscope (FE-SEM) and transmission electron microscope (TEM). XRD results indicate that synthesized ZnO nanorods have wurtzite phase. The calculated value of the particle size using Debye Scherrer formula and Williamson Hall plot was found to be 20-28 nm and 35.3 nm, respectively. Low uniformity distribution of rod-like morphology (60-80 nm in diameter and average length about 250 nm) are seen in TEM micrographs. The optical parameters of the prepared ZnO nanorods have been calculated using Kubeleka-Munk approach for the UV-vis diffuse reflectance spectrum. It is found that the direct transition optical band gap of the studied sample is 3.17 eV. The direct current electrical conductivity (σ) was increased from 6.7 ×10-8 to 3 ×10-7Ω-1cm-1 with increasing the temperature (T) in the range (300-425 K). The obtained variation of σ with T refers that the conductivity mechanism is controlled by thermally activated process.

  14. Synthesis of anhydrous K2TiOF4 via a mild hydrothermal method

    NASA Astrophysics Data System (ADS)

    Felder, Justin B.; Yeon, Jeongho; zur Loye, Hans-Conrad

    2015-10-01

    The synthesis of anhydrous K2TiOF4 has been previously attempted by transforming precursor compounds, such as the peroxide (K2Ti(O2)F4), hydrate (K2TiOF4·H2O) and fluoride (K2TiF6). Due to the large structural differences between these precursors and the anhydrous oxyfluorides, however, these preparations have been unsuccessful. Therefore, a direct method of synthesis has been employed to grow single crystals of K2TiOF4 that were characterized by single crystal x-ray diffraction. K2TiOF4 was found to be isostructural with the previously known K2VOF4.

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

    SciTech Connect

    Zhao Junwei; Zheng Shoutian; Liu Wei; Yang Guoyu

    2008-03-15

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

  16. Preparation of NiO-YSZ Composite Powder Through 2-Step Hydrothermal Synthesis and Its Application to Solid Oxide Fuel Cell Anode Functional Layer.

    PubMed

    Kim, Byeongseok; Cho, Kihyun; Choi, Jinyi; Shin, Dongwook

    2015-01-01

    NiO-YSZ composite powders were prepared by 2-step hydrothermal synthesis and applied as an anode functional layer to improve the performance of SOFCs. The precursor solution containing yttrium chloride, zirconium oxychloride, and nickel nitrate was hydrothermally treated at 100-130 degrees C for 36 h and then calcined at 900 degrees C for 4 h. The results of X-ray diffraction, Field-Emission Scanning Electron Microscope and Transmission Electron Microscope showed that the NiO (50-100 nm) and YSZ (200-300 nm) were successfully synthesized and these two phases were well separated with the weak agglomeration. Electrical conductivity of the cermet made from the powders produced by 2-step hydrothermal synthesis was much higher than that of the cermet prepared by ball milling. A single cell with anode functional layer showed a maximum power density of 1.7 W/cm2 at 800 degrees C, which may be owing to the homogeneous distribution and the small particle size of the obtained powders. PMID:26328397

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

    SciTech Connect

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

    2008-03-15

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

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

    PubMed

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

    2016-12-01

    Bi2WO6 nanostructures were synthesized by a hydrothermal route, where the effect of various experimental parameters on the products was investigated. It is demonstrated that the sample morphology and size is highly dependent on the NaOH content (or pH value). At C NaOH = 0-0.0175 mol (pH range of 1-4), the prepared samples present flower-like hierarchical microspheres which are constructed from thin nanosheets via the self-assembly process. The size of the hierarchical microspheres exhibits a decreasing trend with increasing the NaOH content, from 7 μm at C NaOH = 0 mol to 1.5 μm at C NaOH = 0.0175 mol. At C NaOH = 0.03-0.0545 mol (pH: 5-9), the prepared samples exhibit irregular flake-like structures, and their size increases with the increase in NaOH content. At C NaOH = 0.055-0.05525 mol (pH: 10-11), the prepared samples are composed of uniform sphere-like particles with an average size of 85 nm. Compared to the NaOH content, the reaction temperature and time has a relatively small effect on the product morphology and size. The photocatalytic activity of the samples was evaluated by degrading rhodamine B (RhB) under irradiation of simulated sunlight. Among these samples, the samples composed of flower-like hierarchical microspheres have relatively high photocatalytic activity. In particular, the microspheres prepared at C NaOH = 0.01 mol exhibit the highest photocatalytic activity, and the degradation percentage reaches 99 % after 2 h of irradiation. PMID:27067738

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

    SciTech Connect

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

    2012-01-15

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

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

    SciTech Connect

    Gong Haibo; Hao Xiaopeng; Xu Xiangang

    2011-12-15

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

  1. Synthesis of hydrothermally reduced graphene/MnO2 composites and their electrochemical properties as supercapacitors

    NASA Astrophysics Data System (ADS)

    Li, Zhangpeng; Wang, Jinqing; Liu, Sheng; Liu, Xiaohong; Yang, Shengrong

    2011-10-01

    Hydrothermally reduced graphene/MnO2 (HRG/MnO2) composites were synthesized by dipping HRG into the mixed aqueous solution of 0.1 M KMnO4 and 0.1 M K2SO4 for different periods of time at room temperature. The morphology and microstructure of the as-prepared composites were characterized by field-emission scanning electron microscopy, X-ray diffraction, Raman microscope, and X-ray photoelectron spectroscopy. The characterizations indicate that MnO2 successfully deposited on HRG surfaces and the morphology of the HRG/MnO2 shows a three-dimensional porous structure with MnO2 homogenously distributing on the HRG surfaces. Capacitive properties of the synthesized composite electrodes were studied using cyclic voltammetry and electrochemical impedance spectroscopy in a three-electrode experimental setup using 1 M Na2SO4 aqueous solution as electrolyte. The main results of electrochemical tests are drawn as follows: the specific capacitance value of HRG/MnO2-200 (HRG dipped into the mixed solution of 0.1 M KMnO4 and 0.1 M K2SO4 for 200 min) electrode reached 211.5 F g-1 at a potential scan rate of 2 mV s-1; moreover, this electrode shows a good cyclic stability and capacity retention. It is anticipated that the synthesized HRG/MnO2 composites will find promising applications in supercapacitors and other devices in virtue of their outstanding characters of good cycle stability, low cost and environmentally benign nature.

  2. Hydrothermal synthesis and structural characterization of metal-organic frameworks based on new tetradentate ligands.

    PubMed

    Liang, Yue; Yuan, Wei-Guan; Zhang, Shu-Fang; He, Zhan; Xue, Junru; Zhang, Xia; Jing, Lin-Hai; Qin, Da-Bin

    2016-01-28

    The hydrothermal reaction of two new tetradentate ligands with different metal salts of cadmium nitrate, zinc chloride, cobalt nitrate and deprotonated terephthalic acid (H2tp), isophthalic acid (H2ip), 4,4'-oxybisbenzoic acid (H2obba) in H2O/DMF or H2O/methanol gave three metal-organic frameworks (MOFs): {[Zn2(L1)(tp)(formate)2]·H2O}n (), {[Cd2(L2)(ip)2]·2H2O}n (), {[Co2(L2)(obba)2]}n () (L1 = 1,2-bis {2,6-bis [(1H-imidazol-1-yl) methyl]-4-methylphenoxy} ethane, L2 = 1,3-bis {2,6-bis [(1H-imidazol-1-yl) methyl]-4-methylphenoxy} propane). The structures of the frameworks are established by single-crystal X-ray diffraction. Compound is a three-dimensional (3D) framework with a 2-fold interpenetrated form, which exhibits a 2-nodal (3,4)-connected fsh-3,4-P21/c net with a {8(3)}2{8(5)·10} topology. Compound has a 2-nodal (4,8)-connected 3D framework where the dinuclear cadmium cluster secondary building units (SBUs) assemble with isophthalate and ligand L2 to construct a rare topological type sqc22 net with a {3(2)·5(4)}{3(4)·4(4)·5(10)·6(10)} topology. Whereas, Compound can be extended to a 2D interlocked (4,4)-connected 4,4 L28 net with the point symbol {4·6(4)·8}2{4(2)·6(4)}. L1 and L2 are tetradentate ligands with diverse linkers and display different coordination modes. In addition, the thermal stability and photochemical properties of the frameworks are also investigated. PMID:26674324

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

    PubMed

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

    2016-08-24

    Two-dimensional (2D) ferroelectric films have vast applications due to their dielectric, ferroelectric, and piezoelectric properties that meet the requirements of sensors, nonvolatile ferroelectric random access memory (NVFeRAM) devices, and micro-electromechanical systems (MEMS). However, the small surface area of these 2D ferroelectric films has limited their ability to achieve higher memory storage density in NVFeRAM devices and more sensitive sensors and transducer. Thus, conformally deposited ferroelectric films have been actively studied for these applications in order to create three-dimensional (3D) structures, which lead to a larger surface area. Most of the current methods developed for the conformal deposition of ferroelectric films, such as metal-organic chemical vapor deposition (MOCVD) and plasma-enhanced vapor deposition (PECVD), are limited by high temperatures and unstable and toxic organic precursors. In this paper, an innovative fabrication method for barium titanate (BaTiO3) textured films with 3D architectures is introduced to alleviate these issues. This fabrication method is based on converting conformally grown rutile TiO2 nanowire arrays into BaTiO3 textured films using a simple two-step hydrothermal process which allows for thickness-controlled growth of conformal films on patterned silicon wafers coated with fluorine-doped tin oxide (FTO). Moreover, the processing parameters have been optimized to achieve a high piezoelectric coupling coefficient of 100 pm/V. This high piezoelectric response along with high relative dielectric constant (εr = 1600) of the conformally grown textured BaTiO3 films demonstrates their potential application in sensors, NVFeRAM, and MEMS. PMID:27487556

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

    SciTech Connect

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

    2013-02-15

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-04-01

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

  6. Hydrothermal Synthesis and Structural Characterization of Novel Zn-Triazole-Benzenedicarboxylate Frameworks

    SciTech Connect

    Park, Hyunsoo; Moureau, David M.; Parise, John B.

    2008-10-03

    Three new metal-organic coordination polymers were synthesized hydrothermally using Zn2+ ion, 1,2,4-triazole, and 1,4-benzenedicarboxylic acid (BDC): Zn5(H2O)2(C2H2N3)4(C8H4O4)3 {center_dot} 3.9H2O (1), Zn2(C2H2N3)2(C2H3N3)(C8H4O4) {center_dot} 2.5H2O (2), and Zn4(H2O)2(C2H2N3)4(C8H4O4)2 {center_dot} 14H2O (3). Their crystal structures were determined by single-crystal X-ray diffraction. Their thermal properties were examined by thermogravimetric analysis. Structure 1 crystallizes in the monoclinic P21/n space group with a = 10.192(2) {angstrom}, b = 17.764(4) {angstrom}, c = 24.437(5) {angstrom}, {beta} = 91.19(3){sup o}, and V = 4423.3(15) {angstrom}3. Structure 2 crystallizes in the triclinic P space group with a = 7.797(2) {angstrom}, b = 10.047(2) {angstrom}, c = 13.577(3) {angstrom}, {alpha} = 110.18(3){sup o}, {beta} = 105.46(3){sup o}, {gamma} = 93.90(3){sup o}, and V = 947.0(3) {angstrom}3. Structure 3 crystallizes in monoclinic P21/n space group with a = 13.475(3) {angstrom}, b = 26.949(5) {angstrom}, c = 13.509(3) {angstrom}, {beta} = 95.18(3){sup o}, and V = 4885.7(17) {angstrom}3. In structure 1, the units of the triazole-Zn polyhedra are linked by BDC in a zigzag fashion to create the stacking of phenyl groups along the a axis. In structure 2, both triazole and BDC bridge Zn polyhedra in the (011) plane, resulting in the eight-membered channels along the a axis. In the case of structure 3, the BDC links the Zn polyhedra along the b axis to form a pillared open framework. This structure is the most porous of the compounds presented in this work.

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

    SciTech Connect

    Ortiz-Landeros, J.

    2011-05-15

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

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

    NASA Astrophysics Data System (ADS)

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

    2011-12-01

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

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

    PubMed

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

    2013-11-01

    Materials with enhanced physical and biological properties have been used for biomedical applications and can be developed by functionalizing them using various components. Hydroxyapatite (HAP), among other available synthetic material, serves as one of the best tools in orthopaedics and ceramic coatings. The porous structure of HAP helps in bone cell regeneration, chemical integration of bone and also favours the interaction between bone and tissues. Herein, we have demonstrated a simple procedure for the synthesis of HAP using low molecular weight heparin (LMWH), a structural analogue of bone heparan sulphate proteoglycan. The presence of small sized HAP plates with well-defined structures was revealed using electron microscopic analysis. The phase purity of the synthesized HAP was evaluated using X-ray diffraction pattern obtained before and after immersion in simulated body fluid (SBF). PMID:23871522

  10. Hydrothermal Synthesis of Nanocrystalline ZnSe: An in situ Synchrotron Radiation X-ray Powder Diffraction Study

    SciTech Connect

    Joergensen,J.; Jensen, T.; Hanson, J.

    2008-01-01

    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+H2O (route A) and ZnCl2+Se+H2O+Na2SO3 (route B). The route A experiment showed that Zn powder starts reacting with water at 134 C giving ZnO and H2 followed by the formation of ZnSe which takes place in temperature range from 167 to 195 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 C and ZnSe and Se were the only crystalline phases observed at the end of the experiment where the temperature was 195 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.

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

    PubMed

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

    2014-09-01

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

  12. Hydrothermal synthesis, structure and thermal stability of diamine templated layered uranyl-vanadates

    SciTech Connect

    Rivenet, Murielle Vigier, Nicolas; Roussel, Pascal; Abraham, Francis

    2007-02-15

    Six new layered uranyl vanadates (NH{sub 4}){sub 2}[(UO{sub 2}){sub 2}V{sub 2}O{sub 8}] (1), (H{sub 2}EN)[(UO{sub 2}){sub 2}V{sub 2}O{sub 8}] (2), (H{sub 2}DAP)[(UO{sub 2}){sub 2}V{sub 2}O{sub 8}] (3), (H{sub 2}PIP)[(UO{sub 2}){sub 2}(VO{sub 4}){sub 2}].0,8H{sub 2}O (4), (H{sub 2}DMPIP)[(UO{sub 2}){sub 2}V{sub 2}O{sub 8}] (5), (H{sub 2}DABCO)[(UO{sub 2}){sub 2}(VO{sub 4}){sub 2}] (6) were prepared from mild-hydrothermal reactions using 1,2-ethylenediamine (EN); 1,3-diaminopropane (DAP); piperazine (PIP); 1-methylpiperazine (MPIP); 1,4-diazabicyclo[2,2,2]octane (DABCO). The structures of 1, 4, 5 and 6 were solved using single-crystal X-ray diffraction data while the structural models of 2 and 3 were established from powder X-ray diffraction data. In compounds 1, 2, 3 and 5, the uranyl-vanadate layers are built from dimers of edge-shared UO{sub 7} pentagonal bipyramids and dimers of edge-shared VO{sub 5} square pyramids further connected through edge-sharing. In 1 and 3, the layers are identical to that occurring in the carnotite group of uranyl-vanadates. In 2 and 5, the V{sub 2}O{sub 8} dimers differ in orientation leading to a new type of layer. The layers of compound 4 and 6 are built from chains of edge-shared UO{sub 7} pentagonal bipyramids connected by VO{sub 4} tetrahedra and are of uranophane-type anion topology. For the six compounds, the ammonium or organoammonium cation resides in the space between the inorganic layers. Crystallographic data: 1 monoclinic, space group P2{sub 1}/c with a=6.894(2), b=8.384(3), c=10.473(4) A and {beta}=106.066(5){sup o}, 2 monoclinic, space group P2{sub 1}/a with a=13.9816(6), b=8.6165(3), c=10.4237(3) A and {gamma}=93.125(3){sup o}, 3 orthorhombic, space group Pmcn with a=14.7363(8), b=8.6379(4) and c=10.4385(4) A, 4 monoclinic, space group C2/m with a=15.619(2), b=7.1802(8), c=6.9157(8) A and {beta}=101.500(2){sup o}, 5 monoclinic, space group P2{sub 1}/b with a=9.315(2), b=8.617(2), c=10.5246(2) A and {gamma}=114

  13. Hydrothermal synthesis, structure and thermal stability of diamine templated layered uranyl-vanadates

    NASA Astrophysics Data System (ADS)

    Rivenet, Murielle; Vigier, Nicolas; Roussel, Pascal; Abraham, Francis

    2007-02-01

    Six new layered uranyl vanadates (NH 4) 2[(UO 2) 2V 2O 8] ( 1), (H 2EN)[(UO 2) 2V 2O 8] ( 2), (H 2DAP)[(UO 2) 2V 2O 8] ( 3), (H 2PIP)[(UO 2) 2(VO 4) 2].0,8H 2O ( 4), (H 2DMPIP)[(UO 2) 2V 2O 8] ( 5), (H 2DABCO)[(UO 2) 2(VO 4) 2] ( 6) were prepared from mild-hydrothermal reactions using 1,2-ethylenediamine (EN); 1,3-diaminopropane (DAP); piperazine (PIP); 1-methylpiperazine (MPIP); 1,4-diazabicyclo[2,2,2]octane (DABCO). The structures of 1, 4, 5 and 6 were solved using single-crystal X-ray diffraction data while the structural models of 2 and 3 were established from powder X-ray diffraction data. In compounds 1, 2, 3 and 5, the uranyl-vanadate layers are built from dimers of edge-shared UO 7 pentagonal bipyramids and dimers of edge-shared VO 5 square pyramids further connected through edge-sharing. In 1 and 3, the layers are identical to that occurring in the carnotite group of uranyl-vanadates. In 2 and 5, the V 2O 8 dimers differ in orientation leading to a new type of layer. The layers of compound 4 and 6 are built from chains of edge-shared UO 7 pentagonal bipyramids connected by VO 4 tetrahedra and are of uranophane-type anion topology. For the six compounds, the ammonium or organoammonium cation resides in the space between the inorganic layers. Crystallographic data: 1 monoclinic, space group P2 1/ c with a=6.894(2), b=8.384(3), c=10.473(4) Å and β=106.066(5)°, 2 monoclinic, space group P2 1/ a with a=13.9816(6), b=8.6165(3), c=10.4237(3) Å and γ=93.125(3)°, 3 orthorhombic, space group Pmcn with a=14.7363(8), b=8.6379(4) and c=10.4385(4) Å, 4 monoclinic, space group C2/ m with a=15.619(2), b=7.1802(8), c=6.9157(8) Å and β=101.500(2)°, 5 monoclinic, space group P2 1/ b with a=9.315(2), b=8.617(2), c=10.5246(2) Å and γ=114.776(2)°, 6 monoclinic, space group C2/ m with a=17.440(2), b=7.1904(9), c=6.8990(8) Å and β=98.196(2)°.

  14. Hydrothermal Processing

    SciTech Connect

    Elliott, Douglas C.

    2011-03-11

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

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

    SciTech Connect

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

    2014-02-01

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

  16. Mild hydrothermal synthesis, crystal structure, photoluminescence properties and emission quantum yield of a new zirconium germanate with garnet-type structure

    SciTech Connect

    Ferdov, Stanislav; Ferreira, Rute A.S.; Lin Zhi; Wu Zhengying

    2012-06-15

    The mild hydrothermal synthesis, crystal structure, photoluminescence properties and emission quantum yield of a new sodium zirconium germanate are reported. This material and the method for its preparation represent for the first time a germanium garnet-type material synthesized at autogenous pressure and temperature at 230 Degree-Sign C. The crystal structure was determined by starting from the crystallographic parameters of a common garnet structure and it represents not only a new chemical combination of atoms but also combination of oxidation states in garnet structure. The framework consists of interconnected corner sharing GeO{sub 4} tetrahedra and ZrO{sub 6} octahedra which form small cavities that accommodate charge compensation Na{sup +} cations. In the course of synthesis the structure can be functionalized by in situ doping with different percentage of Eu{sup 3+} ions. This structural flexibility is used to explore the photoluminescent behavior of the active centers embedded in garnet-type host. The materials display the Eu{sup 3+5}D{sub 0}{yields}{sup 7}F{sub 0-4} transitions under excitation via intra-{sup 4}f{sub 6} excitation levels and through the O{sup 2-}{yields}Eu{sup 3+} ligand-to-metal charge transfer. A maximum {sup 5}D{sub 0} quantum efficiency and emission quantum yield values (ca. 0.28 and 0.04{+-}0.01, respectively) were found for the low Eu{sup 3+}-containing sample, suggesting the presence of concentration quenching effects at higher Eu{sup 3+}-content (5%). - Graphical abstract: Na{sub 3}Zr{sub 1.8}Ge{sub 3}O{sub 10}(OH){sub 2} prepared at mild hydrothermal conditions. Highlights: Black-Right-Pointing-Pointer New zirconogermanate with garnet-type structure. Black-Right-Pointing-Pointer Hydrothermal synthesis. Black-Right-Pointing-Pointer Crystal structure. Black-Right-Pointing-Pointer Photoluminescent properties.

  17. Controllable synthesis of α- and β-MnO(2): cationic effect on hydrothermal crystallization.

    PubMed

    Huang, Xingkang; Lv, Dongping; Yue, Hongjun; Attia, Adel; Yang, Yong

    2008-06-01

    α- and β-MnO(2) were controllably synthesized by hydrothermally treating amorphous MnO(2) obtained via a reaction between Mn(2+) and MnO(4)(-), and cationic effects on the hydrothermal crystallization of MnO(2) were investigated systematically. The crystallization is believed to proceed by a dissolution-recrystallization mechanism; i.e. amorphous MnO(2) dissolves first under hydrothermal conditions, then condenses to recrystallize, and the polymorphs formed are significantly affected by added cations such as K(+), NH(4)(+) and H(+) in the hydrothermal systems. The experimental results showed that K(+)/NH(4)(+) were in competition with H(+) to form polymorphs of α- and β-MnO(2), i.e., higher relative K(+)/NH(4)(+) concentration favoured α-MnO(2), while higher relative H(+) concentration favoured β-MnO(2). PMID:21825766

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

    SciTech Connect

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

    2011-11-15

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

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

    SciTech Connect

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

    2014-06-01

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

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

    NASA Technical Reports Server (NTRS)

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

    2010-01-01

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

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

    SciTech Connect

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

    2013-06-01

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

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

    SciTech Connect

    Fan Weiliu Song Xinyu; Sun Sixiu Zhao Xian

    2007-01-15

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

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

    NASA Astrophysics Data System (ADS)

    Li, Yinyan; Xu, Shiqing

    2016-09-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2015-12-01

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

  5. Hydrothermal synthesis and thermoelectric properties of nanostructured Bi{sub 0.5}Sb{sub 1.5}Te{sub 3} compounds

    SciTech Connect

    Zhang, Yanhua; Xu, Guiying; Mi, Jianli; Han, Fei; Wang, Ze; Ge, Changchun

    2011-05-15

    Research highlights: {yields} Single-phase Bi{sub 0.5}Sb{sub 1.5}Te{sub 3} powders have been synthesized by a hydrothermal route. {yields} Hexagonal Bi{sub 0.5}Sb{sub 1.5}Te{sub 3} naosheets due to the anisotropic growth of the crystals. {yields} The temperature gradients lead to directional arrangement nanosheet-agglomerates. {yields} Nanosheet-agglomerates are beneficial for improving the TE property of products. {yields} A maximum figure of merit of 0.86 is achieved at about 100 {sup o}C. -- Abstract: Single-phase Bi{sub 0.5}Sb{sub 1.5}Te{sub 3} compounds have been prepared by hydrothermal synthesis at 150 {sup o}C for 24 h using SbCl{sub 3}, BiCl{sub 3} and tellurium powder as precursors. X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) have been applied to analyze the phase distributions, microstructures and grain sizes of the as-grown Bi{sub 0.5}Sb{sub 1.5}Te{sub 3} products. It is found that the hydrothermally synthesized Bi{sub 0.5}Sb{sub 1.5}Te{sub 3} nanopowders have a morphology dominated by irregular hexagonal sheets due to the anisotropic growth of the crystals. The Bi{sub 0.5}Sb{sub 1.5}Te{sub 3} nanosheets are parallelly stacked in certain direction to form sheet-agglomerates attribute to the temperature gradients in the solution.

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

    PubMed Central

    2012-01-01

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

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

    SciTech Connect

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

    2014-11-15

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

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

    PubMed

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

    2016-05-01

    Hierarchically structured spherical CuBi2O4 particles were prepared using a facile hydrothermal method without using a surfactant over various hydrothermal reaction periods. The prepared CuBi2O4 samples were examined via X-ray diffraction (XRD), which confirmed the formation of a tetragonal crystal structure. The morphological features were analyzed using field emission scanning electron microscopy (FESEM), which elucidated the construction of the hierarchical microspherical CuBi2O4 particles. The plausible growth mechanism of the hierarchical structure was explained in terms of a time-dependent synthesis process and its crystal structure. The uniform hierarchical CuBi2O4 microspheres were used to fabricate a Li-ion hybrid capacitor (Li-HC) along with activated carbon (AC), the generated device delivers a stable specific capacitance of 26.5 F g(-1) over 1500 cycles at a high current density of 1000 mA g(-1) and a capacity retention of ∼86%. The AC/CB2 Li-ion hybrid cell exhibits high energy density and power density values of 24 W h kg(-1) and 300 W kg(-1), respectively. PMID:26866889

  9. Hydrothermal synthesis of Ni 2FeBO 5 in near-supercritical PWR coolant and possible effects of neutron-induced 10B fission in fuel crud

    NASA Astrophysics Data System (ADS)

    Sawicki, Jerzy A.

    2011-08-01

    The hydrothermal synthesis of a nickel-iron oxyborate, Ni 2FeBO 5, known as bonaccordite, was investigated at pressures and temperatures that might occur at the surface of high-power fuel rods in PWR cores and in supercritical water reactors, especially during localized departures from nucleate boiling and dry-outs. The tests were performed using aqueous mixtures of nickel and iron oxides with boric acid or boron oxide, and as a function of lithium hydroxide addition, temperature and time of heating. At subcritical temperatures nickel ferrite NiFe 2O 4 was always the primary reaction product. High yield of Ni 2FeBO 5 synthesis started near critical water temperature and was strongly promoted by additions of LiOH up to Li/Fe and Li/B molar ratios in a range 0.1-1. The synthesis of bonaccordite was also promoted by other alkalis such as NaOH and KOH. The bonaccordite particles were likely formed by dissolution and re-crystallization by means of an intermediate nickel ferrite phase. It is postulated that the formation of Ni 2FeBO 5 in deposits of borated nickel and iron oxides on PWR fuel cladding can be accelerated by lithium produced in thermal neutron capture 10B(n,α) 7Li reactions. The process may also be aided in the reactor core by kinetic energy of α-particles and 7Li ions dissipated in the crud layer.

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

    PubMed

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

    2016-01-15

    Magnesium phosphate materials have aroused interest of researchers in recent years and are promising for biomedical applications due to their good biocompatibility and biodegradability. In this work, we report the microwave-hydrothermal rapid synthesis of magnesium phosphate pentahydrate nanosheets (MPHSs) using biocompatible creatine phosphate as an organic phosphorus source. This method is facile, rapid, surfactant-free and environmentally friendly. The as-prepared MPHSs have an obvious pH-dependent dissolution performance which can be used as an ideal pH-responsive nanocarrier for drug and gene delivery. Moreover, the MPHSs have a good cytocompatibility and a high ability to promote osteoblast MC-3T3 adhesion and spreading, as well as a relatively high protein adsorption ability using hemoglobin (Hb) as a model protein. Thus, the MPHSs are promising for the applications in biomedical fields such as protein adsorption and bone regeneration. PMID:26473279

  11. Hydrothermal synthesis and characterization of the lutetium borate-nitrate Lu2B2O5(NO3)2·2H2O

    NASA Astrophysics Data System (ADS)

    Ortner, Teresa S.; Wurst, Klaus; Hejny, Clivia; Huppertz, Hubert

    2016-01-01

    The lutetium diborate-dinitrate Lu2B2O5(NO3)2·2H2O was discovered through a hydrothermal synthesis from Lu(NO3)3·H2O and H3BO3. The compound crystallizes in the space group P 1 ̅ (no. 2) with the lattice parameters a=789.52(5), b=988.62(6), c=1460.33(8) pm, α=90.83(1), β=101.75(1), and γ=110.02(1)° (Z=4). Isolated [B2O5]4- units show coplanar alignment and the coordinating [NO3]- groups are stacked perpendicular to the borate plane. Thereby, a novel, open arrangement solely built up from diborate and nitrate groups at a 1:1 ratio is formed. Additionally, Lu2B2O5(NO3)2·2H2O is characterized by vibrational spectroscopy (IR/Raman).

  12. Facile synthesis of alumina hollow microspheres via trisodium citrate-mediated hydrothermal process and their adsorption performances for p-nitrophenol from aqueous solutions.

    PubMed

    Zhou, Jiabin; Wang, Lei; Zhang, Zhong; Yu, Jiaguo

    2013-03-15

    Alumina hollow microspheres with high adsorption affinity toward p-nitrophenol in water were prepared by using urea and trisodium citrate as precipitating and mediating agents, respectively, via a simple one-pot hydrothermal synthesis followed by calcination. The as-prepared samples were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and nitrogen adsorption-desorption isotherms measurement. This study shows that the morphology, specific surface area, and the pore structure of the resulting materials can be controlled by varying the concentration of trisodium citrate. The result of adsorption of p-nitrophenol onto the as-prepared samples revealed that the pseudo-second-order kinetic equation can better describe the adsorption kinetics. Furthermore, adsorption isotherm studies indicated that the resulting alumina microspheres are powerful adsorbents for the removal of p-nitrophenol from water with maximum adsorption capacity of 217.4 mg/g. PMID:23276687

  13. Room temperature synthesis of Bi25FeO39 and hydrothermal kinetic relations between sillenite- and distorted perovskite-type bismuth ferrites.

    PubMed

    Lopes, Armandina M L; Araújo, João P; Ferdov, Stanislav

    2014-12-28

    The time-dependent study at mild hydrothermal conditions revealed the kinetic relation between structurally unrelated bismuth ferrites. We report the synthetic conditions that disclose the in situ transformation of Bi25FeO39 into BiFeO3 by only extending the time for crystallization. We also demonstrate how a careful investigation of the early stages of multiferroics crystallization provides cheap and easy room-temperature access to the important sillenite-type of structure of Bi25FeO39. The crystal structure analysis by the Rietveld method and magnetization measurements provided detailed structure and magnetic relations between the synthesis conditions and the properties of the run product. The BiFeO3 antiferromagnetic behavior with a small ferromagnetic component arising from the particle's surface uncompensated spins is ascertained. PMID:25351519

  14. Highly uniform YF{sub 3}:Ln{sup 3+} (Ln = Ce{sup 3+}, Tb{sup 3+}) walnut-like microcrystals: Hydrothermal synthesis and luminescent properties

    SciTech Connect

    Wang, Xiaojie; Sheng, Tianqi; Fu, Zuoling; Li, Wenhao; Jeong, Jung Hyun

    2013-06-01

    Graphical abstract: The emission spectra of Y{sub 0.98−x}F{sub 3}:0.02Ce{sup 3+}, xTb{sup 3+} microcrystals with different Tb{sup 3+} concentrations demonstrated that energy transfer from the Ce{sup 3+} and Tb{sup 3+} ions is highly efficient. The concentration quenching phenomenon occurs when the x = 0.13. We have discussed it in detail based on experiments and quantitative calculations. Highlights: ► YF{sub 3}:Ce{sup 3+}, Tb{sup 3+} walnut-like microcrystals were prepared by a hydrothermal synthesis. ► The optical properties of YF{sub 3}:Ce{sup 3+}, Tb{sup 3+} phosphors have been investigated in detail. ► The energy transfer distance and efficiency from Ce{sup 3+} to Tb{sup 3+} ions were calculated. ► The dipole–dipole interaction should be the dominant mechanism for energy transfer. - Abstract: Uniform and well-crystallized YF{sub 3} walnut-like microcrystals were prepared by a facile one-step hydrothermal synthesis. The crystalline phase, size, morphology, and luminescence properties were characterized using powder X-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), photoluminescence (PL) and photoluminescent excitation spectra (PLE). The results revealed that the existence of Ce{sup 3+} (sensitizer) can dramatically enhance green emission centered at 545 nm of Tb{sup 3+} (activator) in codoped samples due to an efficient energy transfer from Ce{sup 3+} to Tb{sup 3+}. The critical energy transfer distance between Ce{sup 3+} and Tb{sup 3+} was also calculated by methods of concentration quenching and spectral overlapping. Experimental analysis and theoretical calculations indicated that the dipole–dipole interaction should be the dominant mechanism for the Ce{sup 3+}–Tb{sup 3+} energy transfer.

  15. A new hydrothermal synthesis of spherical Li4Ti5O12 anode material for lithium-ion secondary batteries

    NASA Astrophysics Data System (ADS)

    Yan, Hui; Zhu, Zhi; Zhang, Ding; Li, Wei; Qilu

    2012-12-01

    As-prepared anatase TiO2 with different particle sizes are heated in a lithium hydroxide solution to form Li-Ti-O precursors by using hydrothermal method. Spherical Li4Ti5O12 powders with different particle sizes are obtained by calcining the precursors at 800 °C. The X-ray diffraction (XRD) indicates that elevated hydrothermal reaction temperature and higher concentration of lithium hydroxide solution eliminate the content of impurity in the final product. Scanning electron microscopy (SEM) shows the obtained powders have regular spherical morphology. The obtained Li4Ti5O12 with particle size of about 0.5 μm exhibits excellent electrochemical performance, and the initial discharge capacity reaches 165 mAh g-1 at 35 mA g-1 (0.2 C) and more than 97% of the initial capacity is retained after 70 cycles.

  16. Hydrothermal synthesis and photoelectrochemical performance enhancement of TiO2/graphene composite in photo-generated cathodic protection

    NASA Astrophysics Data System (ADS)

    Zhang, Weiwei; Guo, Hanlin; Sun, Haiqing; Zeng, Rong-Chang

    2016-09-01

    TiO2/graphene composites were synthesized through one-step hydrothermal method. The composites show an enhancement in photo-generated cathodic protection as the time-dependent profiles of photocurrent responses has confirmed. XRD data show that a bicrystalline framework of anatase and brookite formed as graphene provided donor groups in the hydrothermal process. The transfer of photoinduced electrons in the biphasic TiO2 results in effective electron-hole separation. Moreover, graphene lead to a negative shift of the Fermi level as evidenced by Mott-Schottky analysis, which decreases the Schottky barrier formed in the TiO2 and 304 stainless steel interface and results in the enhancement of photo-generated cathodic protection.

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

    SciTech Connect

    Wen, Zhigang; Zheng, Feng; Yu, Hongchun; Jiang, Ziran; Liu, Kanglian

    2013-02-15

    SnO{sub 2} nanorod bundles were synthesized by hydrothermal method. Field-emission scanning electron microscopy and transmission electron microscopy images showed that the as-prepared flowerlike SnO{sub 2} nanorod bundles consist of tetragonal nanorods with size readily tunable. Their electrochemical properties and application as anode for lithium-ion battery were evaluated by galvanostatic discharge–charge testing and cycle voltammetry. SnO{sub 2} nanorod flowers possess improved discharge capacity of 694 mA h g{sup −1} up to 40th cycle at 0.1 C. - Highlights: ► The flowerlike SnO{sub 2} nanorod bundles were synthesized by hydrothermal method. ► SnO{sub 2} nanorod bundles with tunable size by controlling concentration of SnCl{sub 4}. ► A probable formation mechanism of SnO{sub 2} nanorod bundles has been proposed.

  18. Glycine assisted hydrothermal synthesis of α-Fe2O3 nanoparticles and its size dependent properties

    NASA Astrophysics Data System (ADS)

    Biju, C. S.; Raja, D. Henry; Padiyan, D. Pathinettam

    2014-08-01

    α-Fe2O3 with different sizes and morphologies have been successfully synthesized via a biomolecule assisted hydrothermal method. The samples are characterized by X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy, UV-visible diffuse reflectance spectroscopy and vibrating sample magnetometer. A clear blue shift is observed in the optical absorption spectra, indicating that band gap increases with size reduction. Magnetic measurements reveal that coercivity and Morin transition temperature decreases as the size decreases.

  19. Synthesis of Nano-Crystalline CO3O4 Particles by Hydrothermal Method Under Pulsed Magnetic Field

    NASA Astrophysics Data System (ADS)

    Deng, Xiaolong; Li, Ying; Zhu, Mingyuan; Jin, Hongming; Wang, Zhun; Zhu, Zhenzhen; Liu, Huakun

    Nanocrystalline CO3O4 particles were successfully synthesized by hydrothermal method under pulsed magnetic field. The effect of magnetic field and aging time on the morphology and microstructure were examined. Different morphologies were observed from SEM images for the samples fabricated with or without pulsed magnetic field. The pulsed magnetic field made CO3O4 sphere compact and more smooth surface. The hollow sphere morphology and refined grain of CO3O4 were formed after aging process.

  20. Synthesis of bilayer MoS{sub 2} nanosheets by a facile hydrothermal method and their methyl orange adsorption capacity

    SciTech Connect

    Ye, Lijuan; Xu, Haiyan; Zhang, Dingke; Chen, Shijian

    2014-07-01

    Highlights: • Hexagonal phase of MoS{sub 2} nanosheets was synthesized by a facile hydrothermal method. • FE-SEM and TEM images show the sheets-like morphology of MoS{sub 2}. • Bilayer MoS{sub 2} can be grown under the optimized mole ratio of 2:1 of S:Mo at 180 °C for 50 h. • The MoS{sub 2} nanosheets possess high methyl orange adsorption capacity due to the large surface area. - Abstract: Molybdenum disulfide (MoS{sub 2}) nanosheets have received significant attention recently due to the potential applications for exciting physics and technology. Here we show that MoS{sub 2} nanosheets can be prepared by a facile hydrothermal method. The study of the properties of the MoS{sub 2} nanosheets prepared at different conditions suggests that the mole ratio of precursors and hydrothermal time significantly influences the purity, crystalline quality and thermal stability of MoS{sub 2}. X-ray diffraction, Raman spectra and transmission electron microscopy results indicate that bilayer MoS{sub 2} can be grown under an optimized mole ratio of 2:1 of S:Mo at 180 °C for 50 h. Moreover, such ultrathin nanosheets exhibit a prominent photoluminescence and possess high methyl orange adsorption capacity due to the large surface area, which can be potentially used in photodevice and photochemical catalyst.

  1. Controlled synthesis of BiVO{sub 4} with multiple morphologies via an ethylenediamine-assisted hydrothermal method

    SciTech Connect

    Qi, Xuemei; Zhu, Xinyuan; Wu, Jiang; Wu, Qiang; Li, Xian; Gu, Miaoli

    2014-11-15

    Graphical abstract: BiVO{sub 4} samples with various morphologies were synthesized via a simple ethylenediamine (EN) assisted hydrothermal route. One of the mixed crystal phase with spherical and porous morphology showed excellent photocatalytic activity and about 90% Rhodamine B was degraded after 140 min visible light irradiation. - Highlights: • BiVO{sub 4} samples with various morphologies were synthesized by hydrothermal method. • Ethylenediamine mainly acts as alkaline source to adjust pH values of precursor. • BiVO{sub 4} with spherical morphology has excellent photocatalytic activity. - Abstract: In this work, BiVO{sub 4} particles with different crystal structures and morphologies including hexahedral, spherical porous and hyperbranched ones were fabricated in the presence of ethylenediamine by hydrothermal process. The as-fabricated samples were well characterized by X-ray diffraction, scanning electron microscopy, Fourier transform infrared spectroscopy, Raman spectroscopy and ultraviolet–visible absorption spectroscopy. The results showed that the morphology and crystal structure of BiVO{sub 4} particles could be well controlled by only changing the ethylenediamine content in the deionized water solution. Photocatalytic activity of the samples was evaluated by the degradation of Rhodamine B under visible-light irradiation. It was shown that BiVO{sub 4} sample with spherical porous morphology and mixed crystal phase exhibited the best photocatalytic performance after optimizing the ethylenediamine content. The best degradation ratio of Rhodamine B could reach about 87% after 140 min visible-light irradiation.

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

    SciTech Connect

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

    2010-09-15

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

  3. 1-Dodecane-sulfonic-acid-sodium-salt(LAS) assisted hydrothermal synthesis of Cd{sub x}Zn{sub 1-x}S solid solution as efficient photocatalysts under visible light irradiation

    SciTech Connect

    Jia, B.; Guo, L. J.

    2010-03-01

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

  4. Microwave-assisted hydrothermal synthesis of porous SnO{sub 2} nanotubes and their lithium ion storage properties

    SciTech Connect

    Wang, H.E.; Xi, L.J.; Ma, R.G.; Lu, Z.G.; Chung, C.Y.; Bello, I.; Zapien, J.A.

    2012-06-15

    Porous SnO{sub 2} nanotubes have been synthesized by a rapid microwave-assisted hydrothermal process followed by annealing in air. The detailed morphological and structural studies indicate that the SnO{sub 2} tubes typically have diameters from 200 to 400 nm, lengths from 0.5 to 1.5 {mu}m and wall thicknesses from 50 to 100 nm. The SnO{sub 2} nanotubes are self-assembled by interconnected nanocrystals with sizes {approx}8 nm resulting in a specific surface area of {approx}54 m{sup 2} g{sup -1}. The pristine SnO{sub 2} nanotubes are used to fabricate lithium half cells to evaluate their lithium ion storage properties. The porous SnO{sub 2} nanotubes are characteristic with high lithium ion storage capacity, that is found to be 1258, 951, 757, 603, 458, and 288 mAh g{sup -1}, at 0.1, 0.2, 0.5, 1, 2, and 4C, respectively. The enhanced electrochemical properties of the SnO{sub 2} nanotubes can be ascribed to their unique geometry and porous structures. - Graphical abstract: Porous SnO{sub 2} nanotubes are synthesized by a fast microwave-assisted hydrothermal process and exhibit high lithium ion storage properties due to their unique geometry and porous characteristics. Highlights: Black-Right-Pointing-Pointer A microwave-assisted hydrothermal method was used to prepare porous SnO{sub 2} nanotubes. Black-Right-Pointing-Pointer The porous SnO{sub 2} nanotubes have abundant mesopores on their tube walls. Black-Right-Pointing-Pointer The porous SnO{sub 2} nanotubes possess high lithium ion storage properties. Black-Right-Pointing-Pointer Our results may promote the development of high-performance anode materials.

  5. Global synthesis and analysis of deep-sea hydrothermal time-series data: Toward a characterization of the outflow dynamics

    NASA Astrophysics Data System (ADS)

    Barreyre, T.; Sohn, R. A.; Crone, T. J.

    2014-12-01

    Time-series records of mid-ocean ridge hydrothermal fluid properties and flow rates have the potential to help constrain the hydrogeology, subsurface circulation patterns, heat, mass, and chemical fluxes, and habitat conditions within young oceanic crust. This potential has motivated a concerted international effort to acquire such records from a variety of geologically distinct vent fields at numerous locations along the mid-ocean ridge system. However up until now, the global database has not been systematically explored. These records have only been analyzed in a piecemeal fashion, which is problematic because hydrothermal time-series records from individual sites typically exhibit enigmatic modes of episodic and periodic variability that are difficult to interpret in isolation. In this study, we conduct a systematic analysis of the extant set of hydrothermal time-series records from several mid-ocean ridge sites where observatory-style experiments have been conducted (including, LSHF, TAG, EPR 9°50'N and MEF). We show that most temperature records, regardless of location or geological setting, display systematic tide-related variability, with the strongest signal at the principal semidiurnal tidal periods (M2, S2, N2 and K2). Cross-spectral multi-taper methods applied to the temperature and bottom pressure records reveal robust phase relationships, particularly for the high-temperature, black-smoker records, as predicted by poroelastic theory. These results suggest that tidal pressures diffusely propagate through the formation, perturbing fluid velocities and temperatures, resulting in phase lags between the seafloor loading and the exit-fluid temperatures. Here, we use multi-layer analytical and numerical models to constrain the subseafloor permeability, skin depth, and Darcy velocities required to explain the phase lag observations.

  6. Tartaric acid assisted hydrothermal synthesis of different flower-like ZnO hierarchical architectures with tunable optical and oxygen vacancy-induced photocatalytic properties

    NASA Astrophysics Data System (ADS)

    Liu, Tingzhi; Li, Yangyang; Zhang, Hao; Wang, Min; Fei, Xiaoyan; Duo, Shuwang; Chen, Ying; Pan, Jian; Wang, Wei

    2015-12-01

    Different flower-like ZnO hierarchical architectures were prepared by tartaric acid assisted hydrothermal synthesis, especially four flower-like ZnO nanostructures were obtained simultaneously under the same reaction condition. The cauliflower-like ZnO is assembled by spherical shaped nanoparticles, and the chrysanthemum-like and other flower-like ZnO nanostructures are assembled by hexagonal rods/prisms with from planar to semi-pyramid, and to pyramid tips. TA acts as a capping agent and structure-directing agent during the synthesis. All ZnO possess the hexagonal wurtzite structure. The PL spectra can be tuned by changing TA concentration. XRD, PL and Raman spectra confirmed that oxygen vacancies mainly come from the ZnO surface. The flower-like samples of 1:4.5 and 1:3 with the largest aspect ratios have highest photocatalytic performance. They decompose 85% MB within 60 min. Combining PL Gaussian fitting with K, the higher content of oxygen vacancy is, the higher photocatalytic activity is. The enhanced photocatalytic performance is mainly induced by oxygen vacancy of ZnO. The possible formation mechanism, growth and change process of flower-like ZnO were proposed.

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

    NASA Astrophysics Data System (ADS)

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

    2013-06-01

    A simple and novel synthesis process, one-step ionic liquid-assisted hydrothermal synthesis route, has been developed in the work to synthesize Bohemithe (γ-AlOOH) with flower-like structure. The samples were characterized by X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) and Scanning Electron Microscope (SEM). Ionic liquid [Omim]+Cl-, as a template, plays an important role in the morphology and pore structure of the products due to its strong interactions with reaction particles. With the increase in the dosage of ionic liquid [Omim]+Cl-, the morphology of the γ-AlOOH was changed from initial bundles of nanosheets (without ionic liquid) into final well-developed monodispersed 3D flower-like architectures ([Omim]+Cl-=72 mmol). The pore structure was also altered gradually from initial disordered slit-like pore into final relatively ordered ink-bottle pore. Furthermore, the proposed formation mechanism and other influencing factors such as reaction temperature and urea on formation and morphology of the γ-AlOOH have also been investigated.

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

    NASA Astrophysics Data System (ADS)

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

    2016-07-01

    Highly oriented zinc oxide nanorod were successfully grown on seeded p-type silicone substrate by hydrothermal methode. The morphology and the crystallinty of ZnO c-axis (002) arrays were systematically studied using field emission scanning electron microscopy (FESEM) and X-ray diffraction (XRD) methods. The effect of seed layer pre-annealing on nanorods properties was explained according to the nucleation site of ZnO nanoparticles on silicon substrate. In addition, the variation of the equal molarity of zinc nitrate hexahydrate and hexamine concentrations in the reaction vessel play a crucial role related to the ZnO nanorods.

  9. Synthesis of flower- and rod-like nickel sulfide nanostructures by an organic-free hydrothermal process

    SciTech Connect

    Pan Qingtao; Huang Kai; Ni Shibing; Yang Feng; He Deyan

    2008-06-03

    Well-crystalline flower- and rod-like NiS nanostructures have been synthesized by an organic-free hydrothermal process at a low temperature of 200 deg. C. X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) were employed to characterize the as-synthesized NiS nanostructures. The effects of temperature and reaction time on the morphology have been also investigated. The two-step flake-cracking mechanism for the formation of flower- and rod-like NiS nanostructures was discussed. The products were also investigated by photoluminescence (PL) spectroscopy.

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

    SciTech Connect

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

    2014-05-19

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

  11. Microwave-assisted hydrothermal synthesis of coralloid nanostructured nickel hydroxide hydrate and thermal conversion to nickel oxide

    SciTech Connect

    Lai, Teh-Long; Lai, Yuan-Lung; Yu, Jen-Wei; Shu, Youn-Yuen; Wang, Chen-Bin

    2009-10-15

    Coralloid nanostructured nickel hydroxide hydrate has been successfully synthesized by a simple microwave-assisted hydrothermal process using nickel sulfate hexahydrate as precursor and urea as hydrolysis-controlling agent. A pure coralloid nanostructured nickel oxide can be obtained from the nickel hydroxide hydrate after calcination at 400 deg. C. The thermal property, structure and morphology of samples were characterized by thermogravimetry (TG), temperature-programmed reduction (TPR), X-ray (XRD), infrared spectroscopy (IR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM).

  12. Hydrothermal synthesis of superparamagnetic Fe{sub 3}O{sub 4} nanoparticles with ionic liquids as stabilizer

    SciTech Connect

    Liu, Xiao-Di Chen, Hao; Liu, Shan-Shan; Ye, Li-Qun; Li, Yin-Ping

    2015-02-15

    Highlights: • Superparamagnetic Fe{sub 3}O{sub 4} nanoparticles with good dispersity have been synthesized via hydrothermal method. • Ionic liquid [C{sub 16}mim]Cl acts as stabilizer for the Fe{sub 3}O{sub 4} nanoparticles. • Fe{sub 3}O{sub 4} nanoparticles have a saturation magnetization of 67.69 emu/g at 300 K. - Abstract: Superparamagnetic Fe{sub 3}O{sub 4} nanoparticles have been successfully synthesized under hydrothermal condition with the assistant of ionic liquid 1-hexadecyl-3-methylimidazolium chloride ([C{sub 16}mim]Cl). The structure and morphology of the sample have been investigated by X-ray diffraction (XRD), X-ray photoelectron spectra (XPS), transmission electron microscopy (TEM), and high-resolution TEM (HRTEM), and the results indicate that the as-synthesized inverse spinel Fe{sub 3}O{sub 4} nanoparticles have an average diameter of about 10 nm and exhibit relatively good dispersity. More importantly, it is found that [C{sub 16}mim]Cl acts as stabilizer for the Fe{sub 3}O{sub 4} nanoparticles by adsorbing on the particles surfaces to prevent the agglomeration. In addition, the obtained superparamagnetic Fe{sub 3}O{sub 4} nanoparticles have a saturation magnetization of 67.69 emu/g at 300 K.

  13. A facile in-situ hydrothermal synthesis of SrTiO3/TiO2 microsphere composite

    NASA Astrophysics Data System (ADS)

    Wang, Hongxing; Zhao, Wei; Zhang, Yubo; Zhang, Shimeng; Wang, Zihao; Zhao, Dan

    2016-06-01

    TiO2 was successfully used as sacrificed template to synthesise SrTiO3/TiO2 microsphere composite via an in-situ hydrothermal process. The diameter of SrTiO3/TiO2 microsphere was about 700 nm with the same size of the template, and all of the microspheres were in good dispersity. The optimized reaction parameters for the phase and morphology of the as-synthesized samples were investigated. The results showed the SrTiO3/TiO2 microsphere can be synthesized at 170 °C when the concentration of sodium hydroxide was 0.1 M. Lower hydrothermal temperature hampered the formation of the SrTiO3/TiO2 composite, the higher alkali concentration, however, will destroy the morphology of products. The formation mechanism of SrTiO3/TiO2 microsphere composite was proposed and the photocatalytic properties of the samples were characterized using methylene blue solution as the pollutant under the UV light irradiation. The results indicated the proper OH- concentration will provide a channel for Sr2+ to react with Ti4+ located in the template and form the SrTiO3/TiO2 composite, and those with micro-scaled spherical morphology exhibited good photocatalytic activities.

  14. Novel Fe doped mesoporous TiO 2 microspheres: Ultrasonic-hydrothermal synthesis, characterization, and photocatalytic properties

    NASA Astrophysics Data System (ADS)

    Li, Haibin; Liu, Guocong; Chen, Shuguang; Liu, Qicheng

    2010-04-01

    Novel Fe doped mesoporous TiO 2 microspheres were fabricated by an ultrasonic-hydrothermal method when tetrabutyl titanate was used as a precursor and octadecylamine was used as a structure-directing agent. The mesoporous materials were characterized by XRD, SEM, TEM, N 2 adsorption-desorption measurements, XPS, FL, and UV-vis. The results suggest that both ultrasonic treatment and hydrothermal procedure are critical for the fabrication of Fe doped mesoporous TiO 2 microspheres with a combination of regular morphology, large specific surface area, high crystallinity, and high thermal stability. Low-angle XRD and TEM images indicate that the disordered wormhole-like mesostructure of Fe doped TiO 2 microspheres with diameters of about 300-400 nm is actually formed by the agglomerization of nanoparticles with an average size of about 10 nm. The photocatalytic activity of Fe doped mesoporous TiO 2 microspheres was evaluated by the photodegradation of methyl orange. A small amount of Fe 3+ can obviously enhance their photocatalytic activity. The optimal atomic ratio of Fe to Ti for photocatalytic activity is about 0.5 at%.

  15. Sol–gel hydrothermal synthesis of strontium hexaferrite nanoparticles and the relation between their crystal structure and high coercivity properties

    NASA Astrophysics Data System (ADS)

    Hue Dang, Thi Minh; Dung Trinh, Viet; Huan Bui, Doan; Huong Phan, Manh; Chinh Huynh, Dang

    2012-06-01

    Hard magnetic strontium hexaferrite SrFe12O19 nanoparticles were synthesized by the sol–gel hydrothermal method. The factors affecting the synthesized process, such as the mole proportion of the reactants, pH, temperature, the hydrothermal conditions and the calcination process, have been investigated. The crystal structures of these materials were refined by Rietveld method. The obtained materials have single crystal phase, equal nano-size, plate shape and high anisotropy. The high magnetic coercivity of 6.3 kOe with the magnetization at 11.1 kOe of 66 emu g‑1 at room temperature was observed for the strontium hexaferrite nanoparticles. For other nanoparticles (SrLnxFe12-xO19 and SrFe12O19/CoFe2O4) synthesized on the basis of SrFe12O19 the complex completion of the crystal structure distortion and the interaction between magnetic phases were observed.

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

    NASA Astrophysics Data System (ADS)

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

    2014-08-01

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

  17. Hydrothermal synthesis and characterization of Si and Sr co-substituted hydroxyapatite nanowires using strontium containing calcium silicate as precursors.

    PubMed

    Zhang, Na; Zhai, Dong; Chen, Lei; Zou, Zhaoyong; Lin, Kaili; Chang, Jiang

    2014-04-01

    In the absence of any organic surfactants and solvents, the silicon (Si) and strontium (Sr) co-substituted hydroxyapatite [Ca10(PO4)6(OH)2, Si/Sr-HAp] nanowires were synthesized via hydrothermal treatment of the Sr-containing calcium silicate (Sr-CS) powders as the precursors in trisodium phosphate (Na3PO4) aqueous solution. The morphology, phase, chemical compositions, lattice constants and the degradability of the products were characterized. The Si/Sr-HAp nanowires with diameter of about 60nm and up to 2μm in length were obtained after hydrothermal treatment of the Sr-CS precursors. The Sr and Si substitution amount of the HAp nanowires could be well regulated by facile tailoring the Sr substitution level of the precursors and the reaction ratio of the precursor/solution, respectively. The SiO4 tetrahedra and Sr(2+) ions occupied the crystal sites of the HAp, and the lattice constants increased apparently with the increase of the substitution amount. EDS mapping also suggested the uniform distribution of Si and Sr in the synthetic nanowires. Moreover, the Si/Sr-substitution apparently improved the degradability of the HAp materials. Our study suggested that the precursor transformation method provided a facile approach to synthesize the Si/Sr co-substituted HAp nanowires with controllable substitution amount, and the synthetic Si/Sr-HAp nanowires might be used as bioactive materials for hard tissue regeneration applications. PMID:24582251

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

    NASA Astrophysics Data System (ADS)

    Lellala, Kashinath; Namratha, K.; Sudhakar, K.; Byrappa, K.

    2016-05-01

    In the present work, undoped and doped Aluminum/Zinc Oxide - graphene oxide (Al/ZnO-GO) nanocomposite have been successfully synthesized by hydrothermal method from zinc acetate and aluminum nitrate solutions without using of any surfactant/stabilizing agents. The results show that the composites of GO nanosheets are decorated densely by Al/ZnO nanoparticles, which displays a good morphology and blend between GO and Al/ZnO. Hybrid composites exhibit an enhanced photocatalytic performance in reduction of dyes under UV-Vis radiation better than bare ZnO-GO and GO for methylene blue dye. The hydrothermal method leads to particles with a higher crystalline due to ambient temperature of the reaction and autogenously pressure conditions, which alters the phases and crystallizations of the nanocomposite. The optical band gap is narrowed to lower energy values due to controlled addition of aluminum and GO in the composite. The improved optical property in Al-doped ZnO flower decorated on GO can be attributed to the decrease in oxygen deficiency after Al doping. XRD, FTIR, UV-Vis spectroscopy, Raman, and Field Emission Scanning Electron Microscopy characterized the effects of Al doping on the structural characteristics and optical properties on the ZnO-GO.

  19. Hydrothermal synthesis and potential applicability of rhombohedral siderite as a high-capacity anode material for lithium ion batteries

    NASA Astrophysics Data System (ADS)

    Zhao, Shiqiang; Yu, Yue; Wei, Shanshan; Wang, Yuxi; Zhao, Chenhao; Liu, Rui; Shen, Qiang

    2014-05-01

    Natural siderite is a valuable iron mineral composed of ferrous carbonate (FeCO3), which is commonly found in hydrothermal veins and contains no sulfur or phosphorus. In this paper, micro-sized FeCO3 crystallites are synthesized via a facile hydrothermal route, and almost all of them possess a rhombohedral shape similar to that of natural products. When applied as an anode material for lithium ion batteries, the synthetic siderite can deliver an initial specific discharge capacity of ∼1587 mAh g-1 with a coulombic efficiency of 68% at 200 mA g-1, remaining a reversible value of 1018 mAh g-1 over 120 cycles. Even at a high current density of 1000 mA g-1, after 120 cycles the residual specific capacity (812 mAh g-1) is still higher than the theoretical capacity of FeCO3 (463 mAh g-1). Moreover, a novel reversible conversion mechanism accounts for the excellent electrochemical performances of rhombohedral FeCO3 to a great extent, implying the potential applicability of synthetic siderite as lithium ion battery anodes.

  20. L-Cysteine-assisted hydrothermal synthesis of nickel disulfide/graphene composite with enhanced electrochemical performance for reversible lithium storage

    NASA Astrophysics Data System (ADS)

    Chen, Qiannan; Chen, Weixiang; Ye, Jianbo; Wang, Zhen; Lee, Jim Yang

    2015-10-01

    NiS2/graphene composite is synthesized by a facile hydrothermal reaction between NiCl2 and L-cysteine in the presence of graphene oxide sheets. L-Cysteine serves as both the sulfur source for NiS2 and reductant for reduction of graphene oxide sheets. The reduced graphene oxides can be used as a platform for growth of NiS2 particles and restrain NiS2 from agglomerating during hydrothermal process. The results of characterizations show that the sphere-like NiS2 particles exhibit smaller sizes and are well dispersed on the surface of reduced graphene sheets. The electrochemical measurements demonstrate that the NiS2/graphene composite delivers a reversible capacity as high as 1200 mAh g-1 at a current density of 100 mA g-1 and enhanced high-rate capability of 740 mAh g-1 at a high current density of 1000 mA g-1. After 1000 cycles, the NiS2/graphene still preserves the reversible capacity about 810 mAh g-1 at a current density of 500 mA g-1, indicating its excellent cyclic stability.

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

    NASA Astrophysics Data System (ADS)

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

    2013-07-01

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

  2. Effects of quartz particle size and water-to-solid ratio on hydrothermal synthesis of tobermorite studied by in-situ time-resolved X-ray diffraction

    SciTech Connect

    Kikuma, J.; Tsunashima, M.; Ishikawa, T.; Matsuno, S.; Ogawa, A.; Matsui, K.; Sato, M.

    2011-08-15

    Hydrothermal synthesis process of tobermorite (5CaO.6SiO{sub 2}.5H{sub 2}O) has been investigated by in-situ X-ray diffraction using high-energy X-rays from a synchrotron radiation source in combination with a purpose-build autoclave cell. Dissolution rates of quartz were largely affected by its particle size distribution in the starting mixtures. However, the composition (Ca/Si) of non-crystalline C-S-H at the start of tobermorite formation was identical regardless of the quartz dissolution rate. An effect of water-to-solid ratio (w/s) was investigated for samples using fine particle quartz. Tobermorite did not occur with w/s of 1.7 but occurred with w/s higher than 3.0. Surprisingly, however, the dissolution curves of quartz were nearly identical for all samples with w/s from 1.7 to 9, indicating that the dissolution rate is predominated by surface area. Possible reaction mechanism for tobermorite formation will be discussed in terms of Ca and/or silicate ion concentration in the liquid phase and distribution of Ca/Si in non-crystalline C-S-H. - Graphical abstract: Time-resolved XRD data set was obtained at up to 190 deg. C under a saturated steam pressure. Tobermorite (5CaO.6SiO{sub 2}.5H{sub 2}O) formation reaction was investigated in detail for several different starting materials. Highlights: > Hydrothermal formation of tobermorite was monitored by in-situ XRD. > Ca/Si of C-S-H at the start time of tobermorite formation was determined. > The Ca/Si value was identical regardless of the quartz particle size in the starting mixture.

  3. Sodium citrate (Na{sub 3}Cit)-assisted hydrothermal synthesis of uniform spindle-like SrMoO{sub 4}:Eu{sup 3+} phosphors

    SciTech Connect

    Ren, Xiaolei; Zhang, Yu; Li, Qiuyu; Yu, Min

    2014-11-15

    Graphical abstract: A facile hydrothermal method for the synthesis of uniform spindle-like SrMoO{sub 4}:Eu{sup 3+} phosphors with the assistance of sodium citrate (Na{sub 3}Cit). - Highlights: • Well-crystallized spindle-like SrMoO{sub 4}:Eu{sup 3+} phosphors have been synthesized. • The influence of the reaction temperature and reaction time were clearly shown. • The dosage of Na{sub 3}Cit has a strong effect on the spindle-like SrMoO{sub 4}:Eu{sup 3+} phosphors. • The growth mechanism for the formation of final samples was proposed. - Abstract: Highly uniform spindle-like SrMoO{sub 4}:Eu{sup 3+} phosphors have been prepared by a facile hydrothermal method using sodium citrate (Na{sub 3}Cit) as the chelating reagent. X-ray powder diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectrum (EDS), transmission electron microscopy (TEM), X-ray photoelectron spectra (XPS), Fourier transform-infrared spectroscopy (FT-IR) and photoluminescence spectra (PL) were used to characterize the resulting samples. The dosage of sodium citrate, reaction temperature and reaction time play key roles in the formation of the final samples. The possible formation mechanism for SrMoO{sub 4}:Eu{sup 3+} phosphors has been proposed. Upon excitation by ultraviolet radiation, the as-synthesized SrMoO{sub 4}:Eu{sup 3+} phosphors show the characteristic {sup 5}D{sub 0}–{sup 7}F{sub J} (J = 1, 2, 3, 4) emission lines with red emission {sup 5}D{sub 0}–{sup 7}F{sub 2} (613 nm) as the most prominent group.

  4. Hydrothermal synthesis of Li{sub 4}Ti{sub 5}O{sub 12}/C nanostructured composites: Morphology and electrochemical performance

    SciTech Connect

    Vujković, Milica; Stojković, Ivana; Mitrić, Miodrag; Mentus, Slavko; Cvjetićanin, Nikola

    2013-02-15

    Graphical abstract: Display Omitted Highlights: ► Nanostructured composite Li{sub 4}Ti{sub 5}O{sub 12}/C was obtained hydrothermally. ► The amount of carbon black influenced significantly the morphology of the composite. ► Rate capability of Li{sub 4}Ti{sub 5}O{sub 12} was improved by the synthesis in presence of carbon black. ► Coulombic capacity of 150 mAh g{sup −1} was obtained at a discharging rate of even 10 C. -- Abstract: Li{sub 4}Ti{sub 5}O{sub 12}/C composites with low (3 wt.%) and high (33 wt.%) carbon black content as well as carbon-free Li{sub 4}Ti{sub 5}O{sub 12} were prepared in two steps under identical conditions: hydrothermal reaction at 130 °C and post-calcination at 400 °C. The X-ray diffraction experiments confirmed the spinel structure of Li{sub 4}Ti{sub 5}O{sub 12} in all samples. The carbon content altered significantly the morphology of obtained micro/nanoparticles. The Li{sub 4}Ti{sub 5}O{sub 12}/C composite with the high carbon content showed the highest electrical conductivity (2.0 S cm{sup −1}), and displayed also extraordinary electrochemical performance: the cyclovoltammograms consisted of well defined reversible redox peaks at a scan rate as high as 10 mV s{sup −1}, while, by galvanostatic cycling, the coulombic capacity of 150 mAh g{sup −1} was evidenced at a discharging rate of 10 C.

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

    SciTech Connect

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

    2013-07-15

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

  6. Hydrothermal synthesis attempts of dawsonite-type hydroxymetalocarbonate precursor compounds for catalytic Ho, Sm, and La oxides

    SciTech Connect

    Ali, Asma A.; Hasan, Muhammad A.; Zaki, Mohamed I.

    2008-01-08

    Chemical interactions in mixed, aqueous solutions of NH{sub 4}HCO{sub 3} and M(NO{sub 3}){sub 3}.9H{sub 2}O, where M stands for Ho, Sm, or La, were facilitated under various hydrothermal treatment conditions (pH 8-12 and temperature = 75-135 deg. C). The solution chemistry established did not make available necessary concentrations of soluble HCO{sub 3}{sup -} and MO(OH){sub 2}{sup -} species for the formation of dawsonite-type ammonium hydroxymetalocarbonates, NH{sub 4}M(CO{sub 3})(OH){sub 2}, but, alternatively, high concentrations of soluble CO{sub 3}{sup 2-}, and M(H{sub 2}O){sub n}{sup 3+} or M(H{sub 2}O){sub n-1}(OH){sup 2+} facilitating, respectively, precipitation of corresponding hydrated carbonate, M{sub 2}(CO{sub 3}){sub 2}.2H{sub 2}O, or carbonate hydroxide, MCO{sub 3}(OH). X-ray powder diffractometry, infrared spectroscopy, and thermal analyses proved alternative formation of Ho{sub 2}(CO{sub 3}){sub 3}.2H{sub 2}O or LaCO{sub 3}(OH) under the whole set of hydrothermal treatment conditions probed, and Sm{sub 2}(CO{sub 3}){sub 3}.2H{sub 2}O at pH < 10 or SmCO{sub 3}(OH) at pH {>=} 10, thus implying dependence of the composition of the product carbonate compound on the hydrolysability of the initial M(H{sub 2}O){sub n}{sup 3+} species and, hence, the metal ionic size (La > Sm > Ho). Calcination of the various hydrothermal treatment products at {>=}600 deg. C resulted in the thermal genesis of the corresponding sesqui-oxides (M{sub 2}O{sub 3}). Bulk and surface characterization studies of the product oxides, employing N{sub 2} sorptiometry and scanning electron microscopy, in addition to the above analytical techniques, revealed overall strong crystallinity, large average crystallite size, and well-defined particle morphology. They revealed, moreover, surfaces, though of limited accessibilities ({<=}13 m{sup 2}/g), exposing OH groups of various coordination symmetries and, hence, acid-base properties, thus furnishing promising surface catalytic attributes.

  7. Hydrothermal synthesis and luminescent properties of NaLa(MoO{sub 4}){sub 2}:Dy{sup 3+} phosphor

    SciTech Connect

    Li Linlin; Zi Wenwen; Li Guanghuan; Lan Shi; Ji Guijuan; Gan Shucai; Zou Haifeng; Xu Xuechun

    2012-07-15

    Pompon-like NaLa(MoO{sub 4}){sub 2}:Dy{sup 3+} phosphors have been successfully prepared via a hydrothermal method using ammonia as pH value regulator. The hydrothermal process was carried out under aqueous condition without the use of any organic solvent, surfactant, and catalyst. The experimental results demonstrate that the obtained NaLa(MoO{sub 4}){sub 2}:Dy{sup 3+} phosphor powders are single-phase scheelite structure with tetragonal symmetry. Moreover, the phosphor under the excitation of 390 and 456 nm exhibited blue emission (486 nm) and yellow emission (574 nm), corresponding to the {sup 4}F{sub 9/2}{yields}{sup 6}H{sub 15/2} transition and {sup 4}F{sub 9/2}{yields}{sup 6}H{sub 13/2} transition of Dy{sup 3+} ions, respectively. In addition, the yellow-to-blue emission intensity ratio (Y/B) can be changed with the doped concentration of Dy{sup 3+} ions. All chromaticity coordinates of the obtained NaLa(MoO{sub 4}){sub 2}:Dy{sup 3+} phosphors are located in the white-light region. The results indicate that this kind of phosphor may has potential applications in the fields of near UV-excited and blue-excited white LEDs. - Graphical abstract: It can be seen from the SEM images that a pompon-like shape was obtained with an average diameter of about 1 {mu}m, and it is composed of many nanoflakes. Highlights: Black-Right-Pointing-Pointer Pompon-like NaLa(MoO{sub 4}){sub 2}:Dy{sup 3+} phosphors have been successfully prepared via a hydrothermal method. Black-Right-Pointing-Pointer Blue emission at 486 nm and yellow emission at 574 nm were obtained from the samples. Black-Right-Pointing-Pointer The yellow-to-blue emission intensity ratio (Y/B) can be changed with the doped concentration of Dy{sup 3+} ions. Black-Right-Pointing-Pointer NaLa(MoO{sub 4}){sub 2}:Dy{sup 3+} can be efficiently excited by the blue light and the near ultraviolet light.

  8. Aloe vera plant-extracted solution hydrothermal synthesis and magnetic properties of magnetite (Fe3O4) nanoparticles

    NASA Astrophysics Data System (ADS)

    Phumying, Santi; Labuayai, Sarawuth; Thomas, Chunpen; Amornkitbamrung, Vittaya; Swatsitang, Ekaphan; Maensiri, Santi

    2013-06-01

    Magnetite (Fe3O4) nanoparticles have been successfully synthesized by a novel hydrothermal method using ferric acetylacetonate (Fe(C5H8O2)3) and aloe vera plant-extracted solution. The influences of different reaction temperatures and times on the structure and magnetic properties of the synthesized Fe3O4 nanoparticles were investigated. The synthesized nanoparticles are crystalline and have particle sizes of ˜6-30 nm, as revealed by transmission electron microscopy (TEM). The results of X-ray diffraction (XRD), High resolution TEM (HRTEM) and selected area electron diffraction (SAED) indicate that the synthesized Fe3O4 nanoparticles have the inverse cubic spinel structure without the presence of any other phase impurities. The hysteresis loops of the Fe3O4 nanoparticles at room temperature show superparamagnetic behavior and the saturation magnetization of the Fe3O4 samples increases with increasing reaction temperature and time.

  9. Synthesis and enhanced photocatalytic property of feather-like Cd-doped CuO nanostructures by hydrothermal method

    NASA Astrophysics Data System (ADS)

    Wang, Yongqian; Jiang, Tingting; Meng, Dawei; Wang, Dagui; Yu, Meihua

    2015-11-01

    Feather-like Cd-doped CuO nanostructures were fabricated by a one-step hydrothermal method. X-ray diffraction pattern (XRD) and field emission scanning electron microscopy (FESEM) demonstrated that Cd2+ entered the crystal lattice of CuO and substituted Cu2+ without destroying crystal structures to form feather-like CuO nanostructures. The optical property of Cd-doped CuO was investigated by using UV-vis spectrophotometer. A slight blue-shift of optical band gap was observed because of quantum confinement effect. The doped samples exhibited obviously higher absorbance in UV light region and better photocatalytic activity for the photodegradation of methyl blue than the pure CuO nanosheets.

  10. Hydrothermal synthesis and humidity sensing properties of size-controlled Zirconium Oxide (ZrO2) nanorods.

    PubMed

    Wang, Zhuyi; Lu, Yi; Yuan, Shuai; Shi, Liyi; Zhao, Yin; Zhang, Meihong; Deng, Wei

    2013-04-15

    Size-controlled ZrO2 nanorods were prepared via a facile hydrothermal treatment approach in the presence of NH4F as mineralizer. The effects of the type and concentration of mineralizers on the particle size and dispersibility of ZrO2 nanorods were investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM), N2 adsorption-desorption measurements (BET), and X-ray photoelectron spectroscopy (XPS), confirming the essential role of F(-) in tuning the particle size. Humidity sensors based on ZrO2 nanorods with different sizes exhibit different sensitivity depending on their proportion of surface adsorbed oxygen. High sensitivity, linear response, small hysteresis, and rapid response-recovery behavior (5s for adsorption and 38s for desorption) make ZrO2 prepared by our method a good candidate for application in humidity sensor. The complex impedance spectra were used to elucidate its humidity sensing mechanism in detail. PMID:23411357

  11. Hydrothermal synthesis of reduced graphene sheets/Fe2O3 nanorods composites and their enhanced electrochemical performance for supercapacitors

    NASA Astrophysics Data System (ADS)

    Yang, Wanlu; Gao, Zan; Wang, Jun; Wang, Bin; Liu, Lianhe

    2013-06-01

    Reduced graphene nanosheets/Fe2O3 nanorods (GNS/Fe2O3) composite has been fabricated by a hydrothermal route for supercapacitor electrode materials. The obtained GNS/Fe2O3 composite formed a uniform structure with the Fe2O3 nanorods grew on the graphene surface and/or filled between the graphene sheets. The electrochemical performances of the GNS/Fe2O3 hybrid supercapacitor were tested by cyclic voltammetry, electrochemical impedance spectroscopy, and galvanostatic charge-discharge tests in 6 M KOH electrolyte. Comparing with the pure Fe2O3 electrode, GNS/Fe2O3 composite electrode exhibits an enhanced specific capacitance of 320 F g-1 at 10 mA cm-2 and an excellent cycle-ability with capacity retention of about 97% after 500 cycles. The simple and cost-effective preparation technique of this composite with good capacitive behavior encourages its potential commercial application.

  12. Synthesis and properties of boron doped ZnO nanorods on silicon substrate by low-temperature hydrothermal reaction

    NASA Astrophysics Data System (ADS)

    Yu, Qi; Li, Liuan; Li, Hongdong; Gao, Shiyong; Sang, Dandan; Yuan, Jujun; Zhu, Pinwen

    2011-05-01

    Boron doped ZnO nanorods were fabricated by hydrothermal technique on silicon substrate covered with a ZnO seed layer. It is found that the concentration of boric acid in the reaction solution plays a key role in varying the morphology and properties of the products. The growth rate along the [0 0 0 1] orientation (average size in diameter) of the doped ZnO nanorods decreased (increased) with the increase of boric acid concentration. Based on the results of XRD, EDX and XPS, it is demonstrated that the boron dopants tend to occupy the octahedral interstice sites. The photoluminescence of the ZnO nanorods related to boron doping are investigated.

  13. Hydrothermal synthesis and photoluminescence of SrWO{sub 4}:Tb{sup 3+} novel green phosphor

    SciTech Connect

    Liao Jinsheng; Qiu Bao; Wen Herui; Chen Jinglin; You Weixiong

    2009-09-15

    Tb{sup 3+}-doped SrWO{sub 4} phosphors with a scheelite structure have been prepared by hydrothermal reaction. X-ray powder diffraction, field-emission scanning electron microscopy, photoluminescence excitation and emission spectra and decay curve were used to characterize the resulting samples. Scanning electron microscopy image showed that the obtained SrWO{sub 4}:Tb{sup 3+} phosphors appeared to be nearly spherical and their sizes ranged from 1 to 3 {mu}m. Photoluminescence spectra indicated the phosphors emitted strong green light centered at 545 nm under ultraviolet light excitation. Because 12 at.% SWO{sub 4}:Tb{sup 3+} phosphor exhibits intensive green emission under 254 nm excitation in comparison with the commercial green fluorescent lamp phosphor (LaPO{sub 4}:Ce,Tb), the excellent luminescence properties make it a new promising green phosphor for fluorescent lamps application.

  14. Surfactant free hydrothermal synthesis of SnO{sub 2} nanorods with their microstructure and Raman studies

    SciTech Connect

    Amutha, A.; Panigrahi, B. K.; Amirthapanian, S.; Thangadurai, P.

    2014-04-24

    SnO{sub 2} nanorods were prepared by hydrothermal method without any surfactant. Their microstructure was studied with X-ray diffraction, Raman scattering and transmission electron microscopy. The range of nanorods diameter size is ∼3 to 19 nm. The crystal structure was confirmed to be SnO{sub 2} rutile tetragonal structure. The nanorods were single crystalline in nature as confirmed by HRTEM. Electron energy loss studies were carried out. EELS analysis showed presence SnO{sub 2} phase and SnO phase was not observed. New Raman modes (352 and 579 cm{sup −1}) corresponding to small size effects were observed for the SnO{sub 2} nanorods.

  15. Hydrothermal synthesis of TiO2-ZnO-graphene nanocomposite towards photocatalytic and photovoltaic applications

    NASA Astrophysics Data System (ADS)

    Gayathri, S.; Jayabal, P.; Ramakrishnan, V.

    2015-06-01

    Titanium dioxide (TiO2) - Zinc oxide (ZnO) - Graphene (G) nanocomposite was successfully synthesized through facile hydrothermal method. The X-ray diffraction (XRD) pattern and the micro-Raman spectroscopic technique revealed the formation of TiO2-ZnO-Graphene (TZG) nanocomposite. The ZnO and TiO2 nanoparticles decorated graphene sheets were clearly noticeable in the Field Emission Scanning Electron Micrograph (FE-SEM). The UV-Visible absorption spectra clearly indicated that the formation of TZG nanocomposite enriched the absorption in the visible region. Hence, the prepared nanocomposite can be used as photocatalyst to remove organic dyes from water and as photoanode in the fabrication of dye sensitized solar cells (DSSCs).

  16. Hydrothermal synthesis of Mn(OH)O nanowires and their thermal conversion to (1D)-manganese oxides nanostructures

    NASA Astrophysics Data System (ADS)

    Mohamed Ahmed, Khalid Abdelazez; Abbood, Hayder A.; Huang, Kaixun

    2012-11-01

    Manganite Mn(OH)O nanowires were successfully synthesized using a hydrothermal method based on a mild and direct reaction between potassium permanganate and ethylene glycol. Subsequent heat treatment of Mn(OH)O nanowires in air at 400 °C for 4 h and 900 °C for 2 h, was conducted to prepare pyrolusite MnO2 nanobelts and necklace-like bixbyite-C Mn2O3 nanowires, respectively. A variety of techniques, including X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), selected area electron diffraction (SA-ED), high resolution transmission electron microscopy (HR-TEM) and thermogravimetry-differential thermal analyzer (TG-DTA), were employed to characterize the resulting materials. The ethylene glycol and heating furnace imposed an effect on the morphology evolution of one dimensional (1D) manganese oxides nanocrystals.

  17. Hydrothermal synthesis of TiO{sub 2}-ZnO-graphene nanocomposite towards photocatalytic and photovoltaic applications

    SciTech Connect

    Gayathri, S. Jayabal, P.; Ramakrishnan, V.

    2015-06-24

    Titanium dioxide (TiO{sub 2}) - Zinc oxide (ZnO) - Graphene (G) nanocomposite was successfully synthesized through facile hydrothermal method. The X-ray diffraction (XRD) pattern and the micro-Raman spectroscopic technique revealed the formation of TiO{sub 2}-ZnO-Graphene (TZG) nanocomposite. The ZnO and TiO{sub 2} nanoparticles decorated graphene sheets were clearly noticeable in the Field Emission Scanning Electron Micrograph (FE-SEM). The UV-Visible absorption spectra clearly indicated that the formation of TZG nanocomposite enriched the absorption in the visible region. Hence, the prepared nanocomposite can be used as photocatalyst to remove organic dyes from water and as photoanode in the fabrication of dye sensitized solar cells (DSSCs)

  18. Effect of deposition parameters on the structural properties of ZnO nanopowders prepared by microwave-assisted hydrothermal synthesis

    NASA Astrophysics Data System (ADS)

    Caglar, Yasemin; Gorgun, Kamuran; Aksoy, Seval

    2015-03-01

    ZnO nanopowders were synthesized via microwave-assisted hydrothermal method at different deposition (microwave irradiation) times and pH values. The effects of pH and deposition (microwave irradiation) time on the crystalline structure and orientation of the ZnO nanopowders have been investigated by X-ray diffraction (XRD) study. XRD observations showed that the crystalline quality of ZnO nanopowders increased with increasing pH value. The crystallite size and texture coefficient values of ZnO nanopowders were calculated. The structural quality of ZnO nanopowder was improved by deposition parameters. Field emission scanning electron microscope (FESEM) was used to analyze the surface morphology of the ZnO nanopowders. Microwave irradiation time and pH value showed a significant effect on the surface morphology.

  19. One-step hydrothermal synthesis, characterization and magnetic properties of orthorhombic PrCrO{sub 3} cubic particles

    SciTech Connect

    Zhang, Youjin Yao, Chengpeng; Fan, Yun; Zhou, Maozhong

    2014-11-15

    Highlights: • Orthorhombic PrCrO{sub 3} cubic particles were prepared by a simple and facile one-step hydrothermal method. • The possible formation mechanism of PrCrO{sub 3} cubic particles was proposed. • The as-synthesized PrCrO{sub 3} exhibited behaviors of magnetic transition and negative magnetization. - Abstract: Orthorhombic PrCrO{sub 3} cubic particles were synthesized by a simple and facile one-step hydrothermal method of processing temperature 280 °C for 7 days. The products prepared in this paper have been characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and field-emission scanning electron microscopy (FESEM). The magnetic properties of the final sample are also studied. The XRD pattern shows the pure orthorhombic phase for PrCrO{sub 3} particles, the XPS and FTIR results further demonstrate the purity and composition of the product. FESEM images show cubic morphology for the PrCrO{sub 3} particles. The possible growth mechanism for PrCrO{sub 3} cubic particles is proposed. Through the investigation of magnetic properties, it can be seen that the orthorhombic PrCrO{sub 3} cubic particles exhibit behaviors of magnetic transition and negative magnetization. The Néel temperature is about 232 K and the magnetic hysteresis loop under 4 K shows that the coercivity (H{sub C}) and remanence (M{sub r}) is about 1728 Oe and 4.88 emu/g, respectively.

  20. Hydrothermal synthesis and characterization of a two-dimensional piperazinium cobalt–zinc phosphate via a metastable one-dimensional phase

    SciTech Connect

    Torre-Fernández, Laura; Khainakova, Olena A.; Espina, Aránzazu; Amghouz, Zakariae; Khainakov, Sergei A.; Alfonso, Belén F.; Blanco, Jesús A.; García, José R.; García-Granda, Santiago

    2015-05-15

    A two-dimensional piperazinium cobalt–zinc phosphate, formulated as (C{sub 4}N{sub 2}H{sub 12}){sub 1.5}(Co{sub 0.6}Zn{sub 0.4}){sub 2}(HPO{sub 4}){sub 2}(PO{sub 4})·H{sub 2}O (2D), was synthesized under hydrothermal conditions. The crystal structure was determined using single-crystal X-ray diffraction data (monoclinic P2{sub 1}/c, a=8.1165(3) Å, b=26.2301(10) Å, c=8.3595(4) Å, and β=110.930(5)°) and the hydrogen atom positions were optimized by DFT calculations. A single-crystal corresponding to one-dimensional metastable phase, (C{sub 4}N{sub 2}H{sub 12})Co{sub 0.3}Zn{sub 0.7}(HPO{sub 4}){sub 2}·H{sub 2}O (1D), was also isolated and the crystal structure was determined (monoclinic P2{sub 1}/c, a=8.9120(6) Å, b=14.0290(1) Å, c=12.2494(5) Å, and β=130.884(6)°). The bulk was characterized by chemical (C–H–N) analysis, powder X-ray diffraction (PXRD), powder X-ray thermodiffractometry (HT-XRD), transmission electron microscopy (STEM(DF)-EDX and EFTEM), and thermal analysis (TG/SDTA-MS), including activation energy data of its thermal decomposition. The magnetic susceptibility and magnetization measurements show no magnetic ordering down to 4 K. - Graphical abstract: Hydrothermal synthesis and structural characterization of a two-dimensional piperazinium cobalt–zinc phosphate, (C{sub 4}N{sub 2}H{sub 12}){sub 1.5}(Co{sub 0.6}Zn{sub 0.4}){sub 2}(HPO{sub 4}){sub 2}(PO{sub 4})·H{sub 2}O (2D), have been reported. The crystal structure of a one-dimensional piperazinium cobalt–zinc phosphate, (C{sub 4}N{sub 2}H{sub 12})Co{sub 0.3}Zn{sub 0.7}(HPO{sub 4}){sub 2}·H{sub 2}O (1D) a metastable phase during the hydrothermal synthesis, was also determined. The thermal behavior of 2D compound is strongly dependent on the selected heating rate and the magnetic susceptibility and magnetization measurements show no magnetic ordering down to 4 K. - Highlights: • A 2D piperazinium cobalt–zinc phosphate has been synthesized and characterized. • Crystal

  1. Four divalent transition metal carboxyarylphosphonate compounds: Hydrothermal synthesis, structural chemistry and generalized 2D FTIR correlation spectroscopy studies

    SciTech Connect

    Lei Ran; Chai Xiaochuan; Mei Hongxin; Zhang Hanhui; Chen Yiping; Sun Yanqiong

    2010-07-15

    Four divalent transition metal carboxyarylphosphonates, [Ni(4,4'-bipy)H{sub 2}L{sup 1}(HL{sup 1}){sub 2}(H{sub 2}O){sub 2}].2H{sub 2}O 1, [Ni{sub 2}(4,4'-bipy)(L{sup 2})(OH)(H{sub 2}O){sub 2}].3H{sub 2}O 2, Mn(phen){sub 2}(H{sub 2}L{sup 1}){sub 2}3 and Mn(phen)(HL{sup 2}) 4 (H{sub 3}L{sup 1}=p-H{sub 2}O{sub 3}PCH{sub 2}-C{sub 6}H{sub 4}-COOH, H{sub 3}L{sup 2}=m-H{sub 2}O{sub 3}PCH{sub 2}-C{sub 6}H{sub 4}-COOH, 4,4'-bipy=4,4'-bipyridine, phen=1,10-phenanthroline) were synthesized under hydrothermal conditions. 1 features 1D linear chains built from Ni(II) ions bridging 4,4'-bipy. In 2, neighboring Ni{sub 4} cluster units are connected by pairs of H{sub 3}L{sup 2} ligands to form 1D double-crankshaft chains, which are interconnected by pairs of 4,4'-bipy into 2D sheets. 3 exhibits 2D supramolecular layers via the R{sub 2}{sup 2}(8) ringed hydrogen bonding units. 4 has 1D ladderlike chains, in which the 4-membered rings are cross-linked by the organic moieties of the H{sub 3}L{sup 2} ligands. Additionally, 2D FTIR correlation analysis is applied with thermal and magnetic perturbation to clarify the structural changes of functional groups from H{sub 3}L{sup 1} and H{sub 3}L{sup 2} ligands in the compounds more efficiently. - Graphical abstract: A series of divalent transition metal carboxyarylphosphonate compounds were synthesized under hydrothermal conditions. The figure displays 2D sheet structure with large windows in compound 2.

  2. Polyaniline-intercalated layered vanadium oxide nanocomposites-One-pot hydrothermal synthesis and application in lithium battery

    NASA Astrophysics Data System (ADS)

    Chen, Yuping; Yang, Gang; Zhang, Zihui; Yang, Xiaoyan; Hou, Wenhua; Zhu, Jun-Jie

    2010-10-01

    Polyaniline-intercalated layered vanadium oxide nanocomposites were successfully synthesized by an one-pot hydrothermal method and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), Fourier transform infrared spectroscopy (FT-IR), and Raman spectroscopy. The effects of reaction conditions, such as pH value of the precursor solution, reaction temperature and time, and the amount of aniline on the structure and morphology of the obtained samples, were systematically investigated. Based on the experimental results, an in situ intercalation-polymerization-exfoliation mechanism was put forward for the formation of layered nanocomposites. The application of the resulting layered nanocomposite as the cathode material in lithium battery was tested and the results showed that the polyaniline-intercalated layered vanadium oxide nanocomposite prepared at 140 °C had a good cycling performance and might act as a promising cathode material for high-energy-density rechargeable lithium batteries.Polyaniline-intercalated layered vanadium oxide nanocomposites were successfully synthesized by an one-pot hydrothermal method and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), Fourier transform infrared spectroscopy (FT-IR), and Raman spectroscopy. The effects of reaction conditions, such as pH value of the precursor solution, reaction temperature and time, and the amount of aniline on the structure and morphology of the obtained samples, were systematically investigated. Based on the experimental results, an in situ intercalation-polymerization-exfoliation mechanism was put forward for the formation of layered nanocomposites. The application of the

  3. Revealing the Mechanisms behind SnO[subscript 2] Nanoparticle Formation and Growth during Hydrothermal Synthesis: An In Situ Total Scattering Study

    SciTech Connect

    Jensen, Kirsten M.Ø.; Christensen, Mogens; Juhas, Pavol; Tyrsted, Christoffer; Bøjesen, Espen D.; Lock, Nina; Billinge, Simon J.L.; Iversen, Bo B.

    2012-05-09

    The formation and growth mechanisms in the hydrothermal synthesis of SnO{sub 2} nanoparticles from aqueous solutions of SnCl{sub 4} {center_dot} 5H{sub 2}O have been elucidated by means of in situ X-ray total scattering (PDF) measurements. The analysis of the data reveals that when the tin(IV) chloride precursor is dissolved, chloride ions and water coordinate octahedrally to tin(IV), forming aquachlorotin(IV) complexes of the form [SnCl{sub x}(H{sub 2}O){sub 6-x}]{sup (4-x)+} as well as hexaaquatin(IV) complexes [Sn(H{sub 2}O){sub 6-y}(OH){sub y}]{sup (4-y)+}. Upon heating, ellipsoidal SnO{sub 2} nanoparticles are formed uniquely from hexaaquatin(IV). The nanoparticle size and morphology (aspect ratio) are dependent on both the reaction temperature and the precursor concentration, and particles as small as 2 nm can be synthesized. Analysis of the growth curves shows that Ostwald ripening only takes place above 200 C, and in general the growth is limited by diffusion of precursor species to the growing particle. The c-parameter in the tetragonal lattice is observed to expand up to 0.5% for particle sizes down to 2-3 nm as compared to the bulk value. SnO{sub 2} nanoparticles below 3-4 nm do not form in the bulk rutile structure, but as an orthorhombic structural modification, which previously has only been reported at pressures above 5 GPa. Thus, adjustment of the synthesis temperature and precursor concentration not only allows control over nanoparticle size and morphology but also the structure.

  4. Microwave assisted hydrothermal synthesis of Ag/AgCl/WO{sub 3} photocatalyst and its photocatalytic activity under simulated solar light

    SciTech Connect

    Adhikari, Rajesh; Gyawali, Gobinda; Sekino, Tohru; Wohn Lee, Soo

    2013-01-15

    Simulated solar light responsive Ag/AgCl/WO{sub 3} composite photocatalyst was synthesized by microwave assisted hydrothermal process. The synthesized powders were characterized by X-Ray Diffraction (XRD) spectroscopy, X-Ray Photoelectron Spectroscopy (XPS), Transmission Electron Microscopy (TEM), Diffuse Reflectance Spectroscopy (UV-Vis DRS), and BET surface area analyzer to investigate the crystal structure, morphology, chemical composition, optical properties and surface area of the composite photocatalyst. This photocatalyst exhibited higher photocatalytic activity for the degradation of rhodamine B under simulated solar light irradiation. Dye degradation efficiency of composite photocatalyst was found to be increased significantly as compared to that of the commercial WO{sub 3} nanopowder. Increase in photocatalytic activity of the photocatalyst was explained on the basis of surface plasmon resonance (SPR) effect caused by the silver nanoparticles present in the composite photocatalyst. Highlights: Black-Right-Pointing-Pointer Successful synthesis of Ag/AgCl/WO{sub 3} nanocomposite. Black-Right-Pointing-Pointer Photocatalytic experiment was performed under simulated solar light. Black-Right-Pointing-Pointer Nanocomposite photocatalyst was very active as compared to WO{sub 3} commercial powder. Black-Right-Pointing-Pointer SPR effect due to Ag nanoparticles enhanced the photocatalytic activity.

  5. Microwave-assisted hydrothermal synthesis of Ag2(W1 -xMox)O4 heterostructures: Nucleation of Ag, morphology, and photoluminescence properties

    NASA Astrophysics Data System (ADS)

    Silva, M. D. P.; Gonçalves, R. F.; Nogueira, I. C.; Longo, V. M.; Mondoni, L.; Moron, M. G.; Santana, Y. V.; Longo, E.

    2016-01-01

    Ag2W1 -xMoxO4 (x = 0.0 and 0.50) powders were synthesized by the co-precipitation (drop-by-drop) method and processed using a microwave-assisted hydrothermal method. We report the real-time in situ formation and growth of Ag filaments on the Ag2W1 -xMoxO4 crystals using an accelerated electron beam under high vacuum. Various techniques were used to evaluate the influence of the network-former substitution on the structural and optical properties, including photoluminescence (PL) emission, of these materials. X-ray diffraction results confirmed the phases obtained by the synthesis methods. Raman spectroscopy revealed significant changes in local order-disorder as a function of the network-former substitution. Field-emission scanning electron microscopy was used to determine the shape as well as dimensions of the Ag2W1 -xMoxO4 heterostructures. The PL spectra showed that the PL-emission intensities of Ag2W1 -xMoxO4 were greater than those of pure Ag2WO4, probably because of the increase of intermediary energy levels within the band gap of the Ag2W1 -xMoxO4 heterostructures, as evidenced by the decrease in the band-gap values measured by ultraviolet-visible spectroscopy.

  6. Hydrothermal synthesis, X-ray structure refinement, 31P NMR spectra and vibrational study of NaLa(HPO4)2

    NASA Astrophysics Data System (ADS)

    Ben Hassen, C.; Boujelbene, M.; Mhiri, T.

    2013-10-01

    NaLa(HPO4)2 was obtained by hydrothermal synthesis. The structure of NaLa(HPO4)2 was determined by X-ray powder diffraction methods. The results of Rietveld refinement revealed a space group P21/c (No. 14), with lattice parameters of a = 9.7151(17) Å, b = 8.320(12) Å, c = 9.83(2) Å, beta = 114.65(17)°, V = 722 (8) Å3 and Z = 4. Final refinement led to RF = 4.86% and RB = 12.35%.The existence of bound O-H and bound P-O in the structure has been confirmed by IR and Raman spectroscopy. The existence of two crystallographically independent phosphorus atoms in the structure has been confirmed by NMR spectrum. The structure is characterized by LaO6 octahedra which are solely connected to six adjacent HPO4 tetrahedra via common O-corners. This structure contains twelve- and four-membered rings forming channels along [1 1¯ 1]. The cross sections of the channels are given by twelve-membered rings consisting of four lanthanum coordination octahedral and eight hydrogenphosphate groups as well as four-membered rings consisting of two lanthanum coordination octahedra and two hydrogenphosphate tetrahedra. Sodium ions are located within those channels of the twelve-membered rings.

  7. Synthesis of hierarchical Ni{sub 11}(HPO{sub 3}){sub 8}(OH){sub 6} superstructures based on nanorods through a soft hydrothermal route

    SciTech Connect

    Liao, Kaiming; Ni, Yonghong

    2010-02-15

    In this paper, we reported the successful synthesis of hierarchical Ni{sub 11}(HPO{sub 3}){sub 8}(OH){sub 6} superstructures based on nanorods via a facile hydrothermal route, employing NiCl{sub 2}.6H{sub 2}O and NaH{sub 2}PO{sub 2}.H{sub 2}O as the reactants in the presences of polyvinylpyrrolidone (PVP) and CH{sub 3}COONa.3H{sub 2}O. The reaction was carried out at 170 {sup o}C for 10 h. HPO{sub 3}{sup 2-} ions were provided via the dismutation reaction of H{sub 2}PO{sub 2}{sup -} ions in a weak basic solution. The as-obtained products were characterized by X-ray powder diffraction (XRD), energy dispersive spectrometry (EDS), field emission scanning electron microscopy (SEM), selected area electron diffraction (SAED) and high resolution transmission electron microscopy (HRTEM). Some factors influencing the morphology of the hierarchical Ni{sub 11}(HPO{sub 3}){sub 8}(OH){sub 6} nanorods, such as the reaction temperature, time, the amounts of PVP and CH{sub 3}COONa, and the initial concentration of Ni{sup 2+} ions, were systematically investigated. A possible growth mechanism was proposed based on experimental results.

  8. Microwave-assisted hydrothermal synthesis of Ag₂(W(1-x)Mox)O₄ heterostructures: Nucleation of Ag, morphology, and photoluminescence properties.

    PubMed

    Silva, M D P; Gonçalves, R F; Nogueira, I C; Longo, V M; Mondoni, L; Moron, M G; Santana, Y V; Longo, E

    2016-01-15

    Ag2W(1-x)MoxO4 (x=0.0 and 0.50) powders were synthesized by the co-precipitation (drop-by-drop) method and processed using a microwave-assisted hydrothermal method. We report the real-time in situ formation and growth of Ag filaments on the Ag2W(1-x)MoxO4 crystals using an accelerated electron beam under high vacuum. Various techniques were used to evaluate the influence of the network-former substitution on the structural and optical properties, including photoluminescence (PL) emission, of these materials. X-ray diffraction results confirmed the phases obtained by the synthesis methods. Raman spectroscopy revealed significant changes in local order-disorder as a function of the network-former substitution. Field-emission scanning electron microscopy was used to determine the shape as well as dimensions of the Ag2W(1-x)MoxO4 heterostructures. The PL spectra showed that the PL-emission intensities of Ag2W(1-x)MoxO4 were greater than those of pure Ag2WO4, probably because of the increase of intermediary energy levels within the band gap of the Ag2W(1-x)MoxO4 heterostructures, as evidenced by the decrease in the band-gap values measured by ultraviolet-visible spectroscopy. PMID:26361214

  9. Hydrothermal synthesis of 3D hierarchical flower-like MoSe2 microspheres and their adsorption performances for methyl orange

    NASA Astrophysics Data System (ADS)

    Tang, Hua; Huang, Hong; Wang, Xiaoshuai; Wu, Kongqiang; Tang, Guogang; Li, Changsheng

    2016-08-01

    In this paper, we report a facile and versatile modified hydrothermal method for synthesis of three-dimensional (3D) hierarchical flower-like MoSe2 microspheres using selenium powders and sodium molybdate as raw materials. The as-prepared MoSe2 was investigated for application as an adsorbent for the removal of dye contaminants from water. Power X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscope (XPS) and N2 adsorption-desorption analysis were carried out to study the microstructure of the as-synthesized product. A possible growth mechanism of MoSe2 flower-like microspheres was preliminarily proposed on the basis of observation of a time-dependent morphology evolution process. Moreover, the MoSe2 sample exhibited good adsorption properties, with maximum adsorption capacity of 36.91 mg/g for methyl orange. The adsorption process of methyl orange on 3D hierarchical flower-like MoSe2 microspheres was systematically investigated, which was found to obey the pseudo-second-order rate equation and Langmuir adsorption model.

  10. Preparation of highly photocatalytic active CdS/TiO2 nanocomposites by combining chemical bath deposition and microwave-assisted hydrothermal synthesis

    NASA Astrophysics Data System (ADS)

    Li, Li; Wang, Lili; Hu, Tianyu; Zhang, Wenzhi; Zhang, Xiuli; Chen, Xi

    2014-10-01

    CdS/TiO2 nanocomposites were prepared from Cd and Ti (1:1 M ratio) using cetyltrimethylammonium bromide by a two-step chemical bath deposition (CBD) and microwave-assisted hydrothermal synthesis (MAHS) method. A series of nanocomposites with different morphologies and activities were prepared by varying the reaction time in the MAHS (2, 4, and 6 h). The crystal structure, morphology, and surface physicochemical properties of the nanocomposites were characterized by X-ray diffraction, UV-visible diffuse reflectance spectroscopy, X-ray photoelectron spectroscopy, scanning electron microscopy, and N2 adsorption-desorption measurements. The results show that the CdS/TiO2 nanocomposites were composed of anatase TiO2 and hexagonal CdS phases with strong absorption in the visible region. The surface morphologies changed slightly with increasing microwave irradiation time, while the Brunauer-Emmett-Teller surface area increased remarkably. The photocatalytic degradation of methyl orange (MO) was investigated under UV light and simulated sunlight irradiation. The photocatalytic activity of the CdS/TiO2 (6 h) composites prepared by the MAHS method was higher than those of CdS, P25, and other CdS/TiO2 nanocomposites. The CdS/TiO2 (6 h) nanocomposites significantly affected the UV and microwave-assisted photocatalytic degradation of different dyes. To elucidate the photocatalytic reaction mechanism for the CdS/TiO2 nanocomposites, controlled experiments were performed by adding different radical scavengers.

  11. Synthesis and Characterization of Piezoelectric (Bi1/2Na1/2)TiO3 Films by a Hydrothermal Method

    NASA Astrophysics Data System (ADS)

    Xu, Fangchao; Kusukawa, Kazuhiro

    Thin films of lead-free piezoelectric ceramics (Bi1/2Na1/2)TiO3 (abbreviated as BNT) were prepared on pure titanium substrates by a hydrothermal method. The properties of BNT films synthesized from the reaction solution with various contents of bismuth and titanium were investigated using SEM, EDX, XRD and other instruments. Moreover, the effects of the concentrations of starting materials on permittivity and piezoelectric effect of deposited BNT films were discussed. The results showed that an impurity of Bi2O3 crystal was produced on the surfaces of all deposited films. With assumption of deposited films as an system of (1-x) (Bi1/2Na1/2)TiO3-xBi2O3, the BNT content was calculated from the Bi/Ti ratio of the EDX results. The optimized synthesis condition was determined on the evaluation target of the calculated BNT content. In addition, the unimorph cantilever type actuators were fabricated by BNT deposited samples, and their piezoelectric responses were measured at their resonance frequencies under AC field. It was noted that the piezoelectric effect of the deposited BNT film was greatly dependent on its crystallization level.

  12. Hydrothermal synthesis, experimental and theoretical characterization of a novel cocrystal compound in the 2:1 stoichiometric ratio containing 6-methyluracil and dipicolinic acid

    NASA Astrophysics Data System (ADS)

    Eshtiagh-Hosseini, H.; Aghabozorg, H.; Mirzaei, M.; Beyramabadi, S. A.; Eshghi, H.; Morsali, A.; Shokrollahi, A.; Aghaei, R.

    2011-05-01

    This paper reports the hydrothermal synthesis, experimental and theoretical studies of a novel cocrystal compound in the 2:1 stoichiometric ratio of 6-methyluracil (6mu) and dipicolinic acid (pydcH 2) formulated as [6mu] 2[pydcH 2] (1), for the first time. DFT calculations were performed to access the most possible geometry of the title cocrystal compound. All calculations were carried out with the B3LYP hybrid density functional level and 6-311+G(d,p) basis sets. The vibrational frequencies together with the 1H and 13C NMR chemical shifts have been calculated on the fully optimized geometry of 1. The theoretical results are in good agreement with the experimental and solution data. The theoretical, solution, and experimental (elemental analysis, mass spectrometry, FTIR, 1H and 13C NMR spectroscopies) results confirmed our proposed structure for 1 in the 2:1 stoichiometric ratio of 6mu and pydcH 2, respectively. The protonation and equilibrium constants of 6mu and pydcH 2 and constituent systems were determined by potentiometric studies and the corresponding distribution diagrams depicted.

  13. Hydrothermal synthesis, electronic structure and tunable luminescence of single-phase Ca5(PO4)3F:Tb3+,Eu3+ microrods.

    PubMed

    Fu, Zuoling; Wang, Xiaojie; Yang, Yanmin; Wu, Zhijian; Duan, Defang; Fu, Xihong

    2014-02-21

    Uniform and well-crystallized calcium fluorapatite [Ca5(PO4)3F, FAP] microrods have been successfully synthesized by a facile one-step hydrothermal synthesis method using sodium citrate as the crystal modifier. X-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), photoluminescence (PL), photoluminescent excitation spectra (PLE) and decay studies were employed to characterize the samples. The electronic structure and orbital population of FAP were also determined by means of density functional theory calculations. Under ultraviolet irradiation, the FAP:Tb(3+),Eu(3+) samples exhibit a blue-light emission of the host matrix, as well as the typical green emission band of the Tb(3+) ions, and a red-light emission of Eu(3+). The highly intense red emission bands of the Eu(3+) ions were attributed to the effective energy transfer from the Tb(3+) to Eu(3+) ions, which has been justified through the luminescence spectra and the fluorescence decay dynamics. The luminescence colors of FAP:Tb(3+),Eu(3+) microrods can be easily tuned by changing the concentration of Eu(3+) ions. The results reveal that the combination of the self-activated luminescence and rare earth-doping emission in FAP:Tb(3+),Eu(3+) microrods could result in tunable emission in a large color gamut, which can be used as a potential candidate for white-light-emitting diodes and other display devices. PMID:24336840

  14. Hydrothermal Growth of Polyscale Crystals

    NASA Astrophysics Data System (ADS)

    Byrappa, Kullaiah

    In this chapter, the importance of the hydrothermal technique for growth of polyscale crystals is discussed with reference to its efficiency in synthesizing high-quality crystals of various sizes for modern technological applications. The historical development of the hydrothermal technique is briefly discussed, to show its evolution over time. Also some of the important types of apparatus used in routine hydrothermal research, including the continuous production of nanosize crystals, are discussed. The latest trends in the hydrothermal growth of crystals, such as thermodynamic modeling and understanding of the solution chemistry, are elucidated with appropriate examples. The growth of some selected bulk, fine, and nanosized crystals of current technological significance, such as quartz, aluminum and gallium berlinites, calcite, gemstones, rare-earth vanadates, electroceramic titanates, and carbon polymorphs, is discussed in detail. Future trends in the hydrothermal technique, required to meet the challenges of fast-growing demand for materials in various technological fields, are described. At the end of this chapter, an Appendix 18.A containing a more or less complete list of the characteristic families of crystals synthesized by the hydrothermal technique is given with the solvent and pressure-temperature (PT) conditions used in their synthesis.

  15. Y{sub 2}O{sub 3}:Eu{sup 3+} microstructures: Hydrothermal synthesis and photoluminescence properties

    SciTech Connect

    Zhong, Shengliang; Wang, Shijin; Liu, Qingyan; Wang, Yuling; Wang, Shangping; Chen, Jianjun; Xu, Rong; Luo, Longfei

    2009-12-15

    Hexagonal microprisms of yttrium hydroxide (Y(OH){sub 3}) with tuned diameter and height have been successfully prepared for the first time via a facile hydrothermal process using sodium citrate as the shape modifying agent. Y(OH){sub 3} microspheres with diameter of ca. 2.5 {mu}m and microtubes with an average length about 13 {mu}m, outer diameter about 3 {mu}m and tube thickness about 800 nm were also obtained in current reaction systems. The possible formation mechanism for the Y(OH){sub 3} microstructures was briefly proposed. Y{sub 2}O{sub 3}:Eu{sup 3+} (5%) microstructures with similar morphologies was obtained after thermal treatment of the as-prepared Y(OH){sub 3}:Eu{sup 3+} microstructures at 700 {sup o}C for 4 h. Results show that the relative emission intensity of the Y{sub 2}O{sub 3}:Eu{sup 3+} microprisms is about 8 times as those of the Y{sub 2}O{sub 3}:Eu{sup 3+} microtubes and microspheres under excitation of 259 nm ultraviolet light. The products were characterized by XRD, SEM, and EDS.

  16. Template-directed hydrothermal synthesis of hydroxyapatite as a drug delivery system for the poorly water-soluble drug carvedilol

    NASA Astrophysics Data System (ADS)

    Zhao, Qinfu; Wang, Tianyi; Wang, Jing; Zheng, Li; Jiang, Tongying; Cheng, Gang; Wang, Siling

    2011-09-01

    In order to improve the dissolution rate and increase the bioavailability of a poorly water-soluble drug, intended to be administered orally, the biocompatible and bioactive mesoporous hydroxyapatite (HA) was successfully synthesized. In the present study, mesoporous HA nanoparticles were produced using Pluronic block co-polymer F127 and cetyltrimethylammonium bromide (CTAB) as templates by the hydrothermal method. The obtained mesoporous HA was employed as a drug delivery carrier to investigate the drug storage/release properties using carvedilol (CAR) as a model drug. Characterizations of the raw CAR powder, mesoporous HA and CAR-loaded HA were carried out by the scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray powder diffraction (XRPD), differential scanning calorimetry (DSC), Fourier transform infrared (FT-IR) spectroscopy, N2 adsorption/desorption, thermogravimetric analysis (TGA), and UV-VIS spectrophotometry. The results demonstrated that CAR was successfully incorporated into the mesoporous HA host. In vitro drug release studies showed that mesoporous HA had a high drug load efficiency and provided immediate release of CAR compared with micronized raw drug in simulated gastric fluid (pH 1.2) and intestinal fluid (pH 6.8). Consequently, mesoporous HA is a good candidate as a drug carrier for the oral delivery of poorly water-soluble drugs.

  17. In-Situ hydrothermal synthesis of a MoS2 nanosheet electrode for electrochemical energy storage applications

    NASA Astrophysics Data System (ADS)

    Patel, Rajkumar; Inamdar, Akbar I.; Kim, Hyung Bae; Im, Hyunsik; Kim, Hyungsang

    2016-06-01

    A molybdenum disulfide (MoS2) nanosheet film was grown directly on a stainless-steel substrate by using an in-situ hydrothermal growth technique at 200 °C. The formation of an MoS2 hexagonal structure with a nanosheet-like morphology was confirmed by using X-ray diffraction (XRD) and field-emission scanning electron microscopy (FE-SEM) while a layered MoS2 nanosheet structure was observed under an energy-filtering transmission electron microscope (EF-TEM). The electrochemical supercapacitor properties of the MoS2 nanosheet electrode were measured in 1-M aqueous Na2SO4 electrolyte by using cyclic voltammetry (CV) and charge/discharge technique, and the electrode's specific capacitances were 91.29 F/g and 146.15 F/g, respectively. The concurrent double-layer capacitance and pseudo-capacitance behaviors of the electrode manifested themselves in the rectangular shape and redox peaks of the CV curve. The mesoporous MoS2 nanosheets were electrochemically stable for up to 1000 charge/discharge cycles.

  18. One-Pot Hydrothermal Synthesis of Magnetite Prussian Blue Nano-Composites and Their Application to Fabricate Glucose Biosensor.

    PubMed

    Jomma, Ezzaldeen Younes; Ding, Shou-Nian

    2016-01-01

    In this work, we presented a simple method to synthesize magnetite Prussian blue nano-composites (Fe₃O₄-PB) through one-pot hydrothermal process. Subsequently, the obtained nano-composites were used to fabricate a facile and effective glucose biosensor. The obtained nanoparticles were characterized using transmission electron microscopy, scanning electron microscopy, Fourier-transform infrared spectroscopy, UV-vis absorbance spectroscopy, cyclic voltammetry and chronoamperometry. The resultant Fe₃O₄-PB nanocomposites have magnetic properties which could easily controlled by an external magnetic field and the electro-catalysis of hydrogen peroxide. Thus, a glucose biosensor based on Fe₃O₄-PB was successfully fabricated. The biosensor showed super-electrochemical properties toward glucose detection exhibiting fast response time within 3 to 4 s, low detection limit of 0.5 µM and wide linear range from 5 µM to 1.2 mM with sensitivity of 32 µA∙mM(-1)∙cm(-2) and good long-term stability. PMID:26901204

  19. Hydrothermal synthesis of fluorinated anatase TiO2/reduced graphene oxide nanocomposites and their photocatalytic degradation of bisphenol A

    NASA Astrophysics Data System (ADS)

    Luo, Lijun; Yang, Ye; Zhang, Ali; Wang, Min; Liu, Yongjun; Bian, Longchun; Jiang, Fengzhi; Pan, Xuejun

    2015-10-01

    The surface fluorinated TiO2/reduced graphene oxide nanocomposites (denoted as F-TiO2-RGO) were synthesized via hydrothermal method. The as-prepared materials were characterized by transmission electron microscopy (TEM), X-ray diffractometer (XRD), Raman spectroscopy, Fourier Transform Infrared spectra (FTIR), X-ray photoelectron spectroscopy (XPS) and X-ray fluorescence (XRF). The results showed that pure anatase TiO2 particles were anchored on the surface of reduced graphene oxide. And the HF added during the preparation process can not only prevent phase transformation from anatase to rutile, but also the F- ion adsorbed on the surface of TiO2-RGO surface can enhance photocatalytic activity of F-TiO2-RGO. The photocatalytic activities of F-TiO2-RGO nanocomposites were evaluated by decomposing bisphenol A under UV light illumination. Under optimal degradation condition, the degradation rate constant of BPA over F-TiO2-10RGO (0.01501 min-1) was 3.41 times than that over P25 (0.00440 min-1). The result indicated that the enhanced photocatalytic activity of F-TiO2-10RGO was ascribed to the adsorbed F ion and RGO in F-TiO2-RGO composite, which can reduce the recombination rate of the photo-generated electrons and holes synergistically.

  20. One-step hydrothermal synthesis of mesoporous anatase TiO₂ microsphere and interfacial control for enhanced lithium storage performance.

    PubMed

    Lee, Kyung-Ho; Song, Seung-Wan

    2011-09-01

    Mesoporous TiO(2) anatase microspheres consisting of self-assembled nanocrystals have been synthesized by a one-step hydrothermal method at 120 (o)C using titanium-peroxo complex, without a post-calcination process. Transmission and scanning electron microscopic imaging reveal that diamond-shaped nanocrystals as primary particles, which are 20 nm in average width and 50 nm in length and oriented with (101) plane of anatase phase, are aggregated to form a secondary microsphere particle with 0.5-1 μm in diameter. BET analysis data show that the TiO(2) anatase particles possess significantly large surface area of 254 m(2) g(-1) with the pore size of ∼14 nm. Mesoporous TiO(2) anatase anode shows an enhanced lithium storage performance in pyrrolidinium-based ionic liquid electrolyte diluted with ethyl methyl carbonate, delivering 195 - 150 mAhg(-1) at the C/2 rate with 77 % capacity retention and 98-99 % Coulombic efficiencies over 50 cycles despite the absence of surface carbon-coating. AC impedance analysis results reveal that the formation of a stable solid electrolyte interphase (SEI) layer in diluted ionic liquid electrolyte induces the enhanced cycling performance. Control of electrode-electrolyte interfacial compatibility enables the enhancement of cycling performance and the preservation of microstructure. The data contribute to provide cost-efficient synthetic method for the TiO(2) and the interfacial control aspect of performance control for safer batteries. PMID:21848346

  1. Synthesis and characterization of ZnO microstructures via a cationic surfactant-assisted hydrothermal microemulsion process

    SciTech Connect

    Liu Yumin Lv Hua; Li Shuangqing; Xi Guoxi; Xing Xinyan

    2011-05-15

    Hexagonal cylinder-like ZnO with a regular twinning microstructure was successfully synthesized via a cationic surfactant-assisted hydrothermal microemulsion route. X-ray diffraction, scanning electron microscopy and Ultraviolet and Visible absorption spectroscopy were employed to characterize the structure, morphologies and properties of the as-prepared samples. The results showed that the reaction temperature, reaction time and molar ratio (w) between water and CTAB exhibited obvious influences on the morphologies and sizes of the products. The Ultraviolet and Visible absorption spectra revealed a strong and broad absorption band from ultraviolet to visible region and the maximum absorption peak appeared at 376 nm. Moreover, the possible growth mechanism for the ZnO microstructures was also discussed in this study. - Research Highlights: {yields} Hexagonal cylinder-like ZnO with twinning microstructure was prepared. {yields} Water/surfactant ratio exhibits obvious influence on the morphology and size of ZnO. {yields} An aggregation mechanism of the ZnO microstructures has been proposed.

  2. Aloe vera mediated hydrothermal synthesis of reduced graphene oxide decorated ZnO nanocomposite: Luminescence and antioxidant properties

    NASA Astrophysics Data System (ADS)

    Kavyashree, D.; Nagabhushana, H.; Ananda Kumari, R.; Basavaraj, R. B.; Suresh, D.; Daruka Prasad, B.; Sharma, S. C.

    2016-05-01

    A zinc oxide/reduced graphene oxide (ZnO/rGO) nanocomposite was fabricated by facile hydrothermal route using Aloe vera gel as surfactant. The PL emission spectrum of the ZnO/rGO composite consists of four peaks at around 380, 394, 449 and 465nm. The PL intensity is found to diminish in ZnO-rGO composites rather than in pure ZnO, which was attributed to electron transfer from ZnO to rGO. A single intense glow curve was recorded in rGo-ZnO for a dose range of 1-8kGy. The TL response curve of rGO-ZnO is found to be a simple glow curve structure, linear dependence over a dose range of 1-8kGy. The obtained ZnO/rGO composite could provide a facile and eco-friendly method for the development of graphene-based nanocomposites with promising applications in radiation dosimetry and antioxidant activities.

  3. Hydrothermal synthesis, crystal structure and properties of a novel chain coordination polymer constructed by tetrafunctional phosphonate anions and cobalt ions

    SciTech Connect

    Guan, Lei; Wang, Ying

    2015-08-15

    A novel cobalt phosphonate, [Co(HL)(H{sub 2}O){sub 3}]{sub n} (1) (L=N(CH{sub 2}PO{sub 3}H){sub 3}{sup 3−}) has been synthesized by hydrothermal reaction at 150 °C and structurally characterized by X-ray diffraction, infrared spectroscopy, elemental and thermogravimetric analysis. Complex 1 features a 1D chain structure with double-channel built from CoO{sub 6} octahedra bridged together by the phosphonate groups. Each cobalt ion is octahedrally coordinated by three phosphonate oxygen atoms and three water molecules. The coordinated water molecules can form the hydrogen bonds with the phosphonate oxygen atoms to link the 1D chains, building a 2D layered structure, further resulting in a 3D network. The luminescence spectrum indicates an emission maximum at 435 nm. The magnetic susceptibility curve exhibits a dominant antiferromagnetic behavior with a weakly ferromagnetic component at low temperatures. - Graphical abstract: The connectivity between cobalt ions and the ligands results in a chain structure with a 1D double-channel structure, which is constructed by A-type subrings and B-type subrings. - Highlights: • The tetrafunctional phosphonate ligand was used as the ligand. • A novel chain structure can be formed by A-type rings and B-type rings. • Two types of rings can form a 1D double-channel structure, along the c-axis.

  4. Hydrothermal synthesis, structural analysis and room-temperature ferromagnetism of Y2O3:Co2+ nanorods

    NASA Astrophysics Data System (ADS)

    Dhak, Prasanta; Patel, Sandeep K. S.; Kim, Min-Kwan; Lee, Jae-Hyeok; Kim, Miyoung; Kim, Sang-Koog

    2016-06-01

    Co2+-doped Y2O3 nanorods of 70-100 nm diameters and 0.3-2 μm lengths with different compositions (x=0.00, 0.04, 0.08) in Y2-xCoxO3 were synthesized by an easy hydrothermal method. The X-ray diffraction, Raman spectra, X-ray photoelectron spectroscopy and transmission electron microscopy (TEM) results indicated the formation of a pure cubic phase structure of Y2O3 doped with Co2+ ions without any secondary phase formation. The TEM analysis indicated that the nanorods were grown along the [100] axis. The pure Y2O3 nanorods showed diamagnetism whereas the Co2+-doped ones exhibited room-temperature ferromagnetism. The existence of such room-temperature ferromagnetic behavior in Co2+-doped Y2O3 nanorods is due mainly to the existence of oxygen vacancies originating after the doping of transition metal ions in the Y2O3 host lattice. Oxygen vacancies act as defect centers in the bound magnetic polaron model to account for this dilute magnetic oxide of medium band gap with low transition-metal-ion concentration. The presence of defect-related oxygen vacancies was further confirmed by photoluminescence spectra analysis of our studied materials.

  5. Hydrothermal synthesis and spectral properties of Ce3+ and Eu2+ ions doped KMgF3 phosphor

    NASA Astrophysics Data System (ADS)

    Zhu, Guoxian; Xie, Mubiao; Yang, Qu; Liu, Yingliang

    2016-07-01

    Phase-pure Ce-/Eu-doped and co-doped KMgF3 phosphors are synthesized by hydrothermal techniques at 200 °C for 5 days. The crystal structure, particle size, morphologies and the energy band structure of the as-synthesized products are investigated by X-ray powder diffraction (XRD), environment scanning electron microscopy (ESEM) and X-ray photoelectron spectroscopy (XPS). The excitation and emission spectra of the rare earth ions doped KMgF3 are measured by the fluorescence spectrophotometer and the effects of Ce3+ ions molar fraction on the luminescence of Eu2+ ions are investigated. In the co-doped Eu2+ and Ce3+ system, the emission intensity of Ce3+ ion gradually increases with the increasing Ce3+ concentration, and the enhancement of Ce3+ fluorescence is due to an efficient energy transfer from Eu2+ to Ce3+ in the host. In addition, the mechanism of energy transfer has been discussed in detail. These results suggest that the phosphors of KMgF3: Ce3+, Eu2+ would become promising tunable laser materials.

  6. Controllable synthesis and luminescence properties of TiO2:Eu3+ nanorods, nanoparticles and submicrospheres by hydrothermal method

    NASA Astrophysics Data System (ADS)

    Qi, Xiaofei; Song, Yanhua; Sheng, Ye; Zhang, Hongguang; Zhao, Huan; Shi, Zhan; Zou, Haifeng

    2014-12-01

    Eu3+-doped TiO2 nanocrystals with three kinds of morphologies (nanorods, nanoparticles, and submicrospheres) have been successfully fabricated in cetyltrimethylammonium bromide (CTAB)/water/cyclohexane/n-pentanol reverse micelle by hydrothermal method for the first time and their photoluminescence (PL) properties have also been studied. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), FT-IR, and PL spectra were used to characterize the samples. The acidic and alkaline conditions of the microemulsion play an important role in determining the geometric morphologies of the final products. TiO2:Eu3+ with three different morphologies all exist only in anatase phase and show high luminescence intensity without further calcinations, which show its advantages of energy saving. The shape of emission spectra was independent of the morphologies of the products but the luminescence intensity of the TiO2:Eu3+ materials is strongly dependent on their morphology. The results show that TiO2:Eu3+ nanorods possess the strongest luminescence intensity among the three nanostructured samples.

  7. Effect of thermal treatment on magnetic and dielectric response of SrM hexaferrites obtained by hydrothermal synthesis

    NASA Astrophysics Data System (ADS)

    Hilczer, Andrzej; Andrzejewski, Bartłomiej; Markiewicz, Ewa; Kowalska, Katarzyna; Pietraszko, Adam

    2014-11-01

    Electric, dielectric and magnetic properties of SrFe12O19 hexaferrite ceramics obtained from hydrothermally synthesized single-phase nanopowders were studied in wide temperature range. The effect of space charge polarization, related to highly conducting grains with poor conducting grain boundaries, was found to be apparent at high temperatures and at low frequencies. The activation energy of relaxation of the (Fe3+-Fe2+) dipoles in low conducting grain boundary regions was found to amount to 0.20 eV for non-annealed ceramics and to increase to 0.32 eV after thermal treatment. The temperature and frequency dependences of the dielectric permittivity for non-annealed and annealed SrFe12O19 ceramics were found to be correlated with respective dependences of the electric conductivity. We relate the observed increase in the saturation magnetization after annealing to an increase in coherent spin rotation in greater grains, which are however still below the critical single-domain size.

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

    NASA Astrophysics Data System (ADS)

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

    2015-11-01

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

  9. Ionic Liquid-Assisted Hydrothermal Method Synthesis of Flower-Like MoS2 and Their Electrochemical Performances.

    PubMed

    Li, Maohua; Yang, Bo; Hao, Junying; Lu, Yi; Long, Zerong; Liu, Yumei

    2016-06-01

    Molybdenum disulfide (MoS2) was prepared successfully via hydrothermal reaction at 200 degrees C in water/ethanol (1:1) solvent system using the ammonium molybdate and sodium thiosulfate as the molybdenum sources and sulfur sources, 1-butyl-3-methylimidazolium chloride salt [BMIM][Cl] as the additive agent. The scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to examine the morphology and structure of flower-like products. X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy spectrum analysis results show that the as-prepared product is a pure phase of MoS2. The prepared products are used as electrode materials for Li-ion batteries and showed excellent cycle stability and high Coulombic efficiency at a current density of 200 mA x g(-1) in the voltage range of 0.01 - 3.00 V (vs. Li/Li+). In addition, this paper also examined the influence of the reaction time and the amount of template agent on morphology, and discussed the reaction mechanism of the formation of flower-like morphology. PMID:27427696

  10. Hydrothermal Synthesis of Hematite-Rich Spherules: Implications for Diagenesis and Hematite Spherule Formation in Outcrops at Meridiani Planum, Mars

    NASA Technical Reports Server (NTRS)

    Golden, D. C.; Ming, D. W.; Morris, R. V.; Graff, T. G.

    2007-01-01

    The Athena science payload onboard the Opportunity rover identified hematite-rich spherules (mean diameter of 4.2 +/- 0.8 mm) embedded in outcrops and occurring as lag deposits at Meridiani Planum. They have formed as diagenetic concretions from the rapid breakdown of pre-existing jarosite and other iron sulfates when chemically distinct groundwater passed through the sediments. Diagenetic, Fe-cemented concretions found in the Jurassic Navajo Formation, Utah and hematite-rich spherules found within sulfate-rich volcanic breccia on Mauna Kea volcano, Hawaii are possible terrestrial analogues for Meridiani spherules. The Navajo Formation concretions form in porous quartz arenite from the dissolution of iron oxides by reducing fluids and subsequent Fe precipitation to form spherical Fe- and Si-rich concretions. The Mauna Kea spherules form by hydrothermal, acid-sulfate alteration of basaltic tephra. The formation of hematite-rich spherules with similar chemical, mineralogical, and morphological properties to the Meridiani spherules is rare on Earth, so little is known about their formation conditions. In this study, we have synthesized in the laboratory hematite-rich spherules that are analogous in nearly all respects to the Meridiani spherules.

  11. One-Pot Hydrothermal Synthesis of Magnetite Prussian Blue Nano-Composites and Their Application to Fabricate Glucose Biosensor

    PubMed Central

    Jomma, Ezzaldeen Younes; Ding, Shou-Nian

    2016-01-01

    In this work, we presented a simple method to synthesize magnetite Prussian blue nano-composites (Fe3O4-PB) through one-pot hydrothermal process. Subsequently, the obtained nano-composites were used to fabricate a facile and effective glucose biosensor. The obtained nanoparticles were characterized using transmission electron microscopy, scanning electron microscopy, Fourier-transform infrared spectroscopy, UV-vis absorbance spectroscopy, cyclic voltammetry and chronoamperometry. The resultant Fe3O4-PB nanocomposites have magnetic properties which could easily controlled by an external magnetic field and the electro-catalysis of hydrogen peroxide. Thus, a glucose biosensor based on Fe3O4-PB was successfully fabricated. The biosensor showed super-electrochemical properties toward glucose detection exhibiting fast response time within 3 to 4 s, low detection limit of 0.5 µM and wide linear range from 5 µM to 1.2 mM with sensitivity of 32 µA∙mM−1∙cm−2 and good long-term stability. PMID:26901204

  12. Facile Hydrothermal Synthesis of Fe3O4/C Core-Shell Nanorings for Efficient Low-Frequency Microwave Absorption.

    PubMed

    Wu, Tong; Liu, Yun; Zeng, Xiang; Cui, Tingting; Zhao, Yanting; Li, Yana; Tong, Guoxiu

    2016-03-23

    Using elliptical iron glycolate nanosheets as precursors, elliptical Fe3O4/C core-shell nanorings (NRs) [25 ± 10 nm in wall thickness, 150 ± 40 nm in length, and 1.6 ± 0.3 in long/short axis ratio] are synthesized via a one-pot hydrothermal route. The surface-poly(vinylpyrrolidone) (PVP)-protected-glucose reduction/carbonization/Ostwald ripening mechanism is responsible for Fe3O4/C NR formation. Increasing the glucose/precursor molar ratio can enhance carbon contents, causing a linear decrease in saturation magnetization (Ms) and coercivity (Hc). The Fe3O4/C NRs reveal enhanced low-frequency microwave absorption because of improvements to their permittivity and impedance matching. A maximum RL value of -55.68 dB at 3.44 GHz is achieved by Fe3O4/C NRs with 11.95 wt % C content at a volume fraction of 17 vol %. Reflection loss (RL) values (≤-20 dB) are observed at 2.11-10.99 and 16.5-17.26 GHz. Our research provides insights into the microwave absorption mechanism of elliptical Fe3O4/C core-shell NRs. Findings indicate that ring-like and core-shell nanostructures are promising structures for devising new and effective microwave absorbers. PMID:26915716

  13. Hydrothermal synthesis, evolution, and electrochemical performance of LiMn0.5Fe0.5PO4 nanostructures.

    PubMed

    Xiang, Wei; Zhong, Yan-Jun; Ji, Jun-Yi; Tang, Yan; Shen, HuiHui; Guo, Xiao-Dong; Zhong, Ben-He; Dou, Shi Xue; Zhang, Zhi-Ye

    2015-07-28

    LiMn0.5Fe0.5PO4 (LMFP) materials are synthesized by the hydrothermal approach in an organic-free and surfactant-free aqueous solution. The phase and morphological evolution of the material intermediates at different reaction temperatures and times are characterized by XRD, SEM and TEM, respectively. The results show that during temperature increase, the solubility product (Ksp) of the precursors (Li3PO4, Fe3(PO4)2 and (Mn,Fe)3(PO4)2) is the decisive parameter for the precipitation processes. Once the temperature locates at the range of 100-110 °C, the unstable precursors dissolve quickly and then LMFP nuclei are formed, followed by a dissolution-reprecipitation process. As the reaction progresses, the primary particles self-aggregate to form rod or plate particles to reduce the overall surface energy through oriented attachment (OA) and the Ostwald ripening (OR) mechanism. Moreover, the resultant concentration of the precursor significantly affects the crystal size of LMFP by altering the supersaturation degree of solution at the nucleation stage. The carbon coated LMFP nanostructure synthesized at 0.6 mol L(-1) (resultant concentration of PO4(3-)) delivers discharge capacities of 155, 100 and 81 mA h g(-1) at 0.1, 5 and 20 C rate, respectively. The understanding of nanostructural evolution and its influence on the electrochemical performance will pave a way for a high-performance LMFP cathode. PMID:26119980

  14. Four divalent transition metal carboxyarylphosphonate compounds: Hydrothermal synthesis, structural chemistry and generalized 2D FTIR correlation spectroscopy studies

    NASA Astrophysics Data System (ADS)

    Lei, Ran; Chai, Xiaochuan; Mei, Hongxin; Zhang, Hanhui; Chen, Yiping; Sun, Yanqiong

    2010-07-01

    Four divalent transition metal carboxyarylphosphonates, [Ni(4,4'-bipy)H 2L 1(HL 1) 2(H 2O) 2]·2H 2O 1, [Ni 2(4,4'-bipy)(L 2)(OH)(H 2O) 2]·3H 2O 2, Mn(phen) 2(H 2L 1) 23 and Mn(phen)(HL 2) 4 (H 3L 1= p-H 2O 3PCH 2-C 6H 4-COOH, H 3L 2= m-H 2O 3PCH 2-C 6H 4-COOH, 4,4'-bipy=4,4'-bipyridine, phen=1,10-phenanthroline) were synthesized under hydrothermal conditions. 1 features 1D linear chains built from Ni(II) ions bridging 4,4'-bipy. In 2, neighboring Ni 4 cluster units are connected by pairs of H 3L 2 ligands to form 1D double-crankshaft chains, which are interconnected by pairs of 4,4'-bipy into 2D sheets. 3 exhibits 2D supramolecular layers via the R 22(8) ringed hydrogen bonding units. 4 has 1D ladderlike chains, in which the 4-membered rings are cross-linked by the organic moieties of the H 3L 2 ligands. Additionally, 2D FTIR correlation analysis is applied with thermal and magnetic perturbation to clarify the structural changes of functional groups from H 3L 1 and H 3L 2 ligands in the compounds more efficiently.

  15. Growth and surface properties of boehmite nanofibers and nanotubes at low temperatures using a hydrothermal synthesis route.

    PubMed

    Zhao, Yanyan; Frost, Ray L; Martens, Wayde N; Zhu, Huai Yong

    2007-09-11

    The growth of boehmite nanostructures at low temperature using a soft chemistry route with and without (PEO) surfactant is presented. Remarkably long boehmite 1D nanotubes/nanofibers were formed within a significantly short time by changing the reaction mechanism of aluminum hydroxide. By using the PEO surfactant as a templating agent, boehmite nanotubes up to 170 nm in length with internal and external diameters of 2-5 and 3-7 nm, respectively, were formed at 100 degrees C. A slightly higher temperature (120 degrees C) resulted in the formation of lath-like nanofibers with an average length of 250 nm. Using the cationic surfactant CTAB, nanotubes rather than nanofibers were formed at 120 degrees C. Without surfactant, nanotubes counted for around 20% of the entire sample. A regular interval supply of fresh boehmite precipitate resulted in a larger crystallite size distribution of nanotubes. The morphology of nanotubes was more uniform in samples without the regular addition of aluminum hydroxide. Moreover, for the same hydrothermal time, the final nanotubes for nanomaterials without a regular interval supply of fresh aluminum hydroxide precipitate were longer than those with a regular aluminum hydroxide precipitate supply, which is in contrast to previously published results. Higher Al/PEO concentrations resulted in the formation of shorter nanotubes. A detailed characterization and mechanism are presented. PMID:17705405

  16. Synthesis and performances of bio-sourced nanostructured carbon membranes elaborated by hydrothermal conversion of beer industry wastes

    PubMed Central

    2013-01-01

    Hydrothermal carbonization (HTC) process of beer wastes (Almaza Brewery) yields a biochar and homogeneous carbon-based nanoparticles (NPs). The NPs have been used to prepare carbon membrane on commercial alumina support. Water filtration experiments evidenced the quasi-dense behavior of the membrane with no measurable water flux below an applied nitrogen pressure of 6 bar. Gas permeation tests were conducted and gave remarkable results, namely (1) the existence of a limit temperature of utilization of the membrane, which was below 100°C in our experimental conditions, (2) an evolution of the microstructure of the carbon membrane with the operating temperature that yielded to improved performances in gas separation, (3) the temperature-dependent gas permeance should follow a Knudsen diffusion mechanism, and (4) He permeance was increasing with the applied pressure, whereas N2 and CO2 permeances remained stable in the same conditions. These results yielded an enhancement of both the He/N2 and He/CO2 permselectivities with the applied pressure. These promising results made biomass-sourced HTC-processed carbon membranes encouraging candidates as ultralow-cost and sustainable membranes for gas separation applications. PMID:23497215

  17. Synthesis and performances of bio-sourced nanostructured carbon membranes elaborated by hydrothermal conversion of beer industry wastes

    NASA Astrophysics Data System (ADS)

    El Korhani, Oula; Zaouk, Doumit; Cerneaux, Sophie; Khoury, Randa; Khoury, Antonio; Cornu, David

    2013-03-01

    Hydrothermal carbonization (HTC) process of beer wastes (Almaza Brewery) yields a biochar and homogeneous carbon-based nanoparticles (NPs). The NPs have been used to prepare carbon membrane on commercial alumina support. Water filtration experiments evidenced the quasi-dense behavior of the membrane with no measurable water flux below an applied nitrogen pressure of 6 bar. Gas permeation tests were conducted and gave remarkable results, namely (1) the existence of a limit temperature of utilization of the membrane, which was below 100°C in our experimental conditions, (2) an evolution of the microstructure of the carbon membrane with the operating temperature that yielded to improved performances in gas separation, (3) the temperature-dependent gas permeance should follow a Knudsen diffusion mechanism, and (4) He permeance was increasing with the applied pressure, whereas N2 and CO2 permeances remained stable in the same conditions. These results yielded an enhancement of both the He/N2 and He/CO2 permselectivities with the applied pressure. These promising results made biomass-sourced HTC-processed carbon membranes encouraging candidates as ultralow-cost and sustainable membranes for gas separation applications.

  18. "Secondary Growth" in Hydrothermal Synthesis of Aligned ZnO Nanostructures and Its Application in Dye-Sensitized Solar Cells.

    PubMed

    Liu, Wenjun; Huang, Qiaoling; Huang, Tengji; Cao, Peijiang; Han, Shun; Jia, Fang; Zhu, Deliang; Ma, Xiaocui; Lul, Youming

    2016-04-01

    One-dimensional (1D) aligned ZnO nanostructures were prepared on ZnO film seeded substrates using a low-temperature hydrothermal method, and zinc nitrate and hexamethylenetetramine (HMT) precursors. It was observed that increasing the concentration ratio of Zn2+/HMT from 1 to 100 led to a "secondary growth," and a change in the morphologies of the ZnO nanostructures from arrays of thick nanorods to arrays of thin nanorod-step-thick nanorods. The morphological evolution of ZnO nanostructures with increased growth time at high Zn2+/HMT concentration ratios showed the same transformation. Dye-sensitized solar cells (DSSCs) were fabricated using ZnO nanostructures as the photoanodes, and the electron transport properties were determined by electrochemical impedance spectroscopy (EIS). Although the DSSCs showed low power conversion efficiencies due to the short lengths, the arrays of the thin nanorods demonstrated excellent electron transport with an electron diffusion coefficient (Dn) of 1.57 x 10(-3) cm2/s, and an effective diffusion length (L) of 140 µm. PMID:27451759

  19. One-step hydrothermal synthesis of graphene decorated V2O5 nanobelts for enhanced electrochemical energy storage

    PubMed Central

    Lee, Minoh; Balasingam, Suresh Kannan; Jeong, Hu Young; Hong, Won G.; Lee, Han-Bo-Ram; Kim, Byung Hoon; Jun, Yongseok

    2015-01-01

    Graphene-decorated V2O5 nanobelts (GVNBs) were synthesized via a low-temperature hydrothermal method in a single step. V2O5 nanobelts (VNBs) were formed in the presence of graphene oxide, a mild oxidant, which also enhanced the conductivity of GVNBs. From the electron energy loss spectroscopy analysis, the reduced graphene oxide (rGO) are inserted into the layered crystal structure of V2O5 nanobelts, which further confirmed the enhanced conductivity of the nanobelts. The electrochemical energy-storage capacity of GVNBs was investigated for supercapacitor applications. The specific capacitance of GVNBs was evaluated using cyclic voltammetry (CV) and charge/discharge (CD) studies. The GVNBs having V2O5-rich composite, namely, V3G1 (VO/GO = 3:1), showed superior specific capacitance in comparison to the other composites (V1G1 and V1G3) and the pure materials. Moreover, the V3G1 composite showed excellent cyclic stability and the capacitance retention of about 82% was observed even after 5000 cycles. PMID:25633147

  20. Low Temperature Hydrothermal Synthesis of Visible-Light-Activated I-Doped TiO2 for Improved Dye Degradation.

    PubMed

    Wang, Dongting; Li, Jianwen; Zhou, Guangsheng; Wang, Wenxu; Zhang, Xianxi; Pan, Xu

    2016-06-01

    Iodine doped TiO2 with different iodine/Ti molar ratios has been firstly synthesized with a low temperature hydrothermal route and has been studied systematically in photocatalysis under visible light condition. The resulting iodine doped TiO2 were characterized by X-ray diffraction (XRD), high resolution transmission electron microscopy (TEM), diffuse reflectance spectrum (DRS), and X-ray photoelectron spectroscopy (XPS). The photocatalytic performance investigations were conducted by means of the degradation of Rhodamine B (RhB) under the visible light irradiation in aqueous solution. Under an optimized I/Ti doping ratio of 10 mol%, the photocatalytic performance is greatly better, with degradation efficiency of 95%, which is almost double that of pure TiO2. The superior photocatalytic activity of iodine-doped TiO2 could be mainly attributed to extended visible light absorption originated from the formation of continuous states existed in the band gap of the doped TiO2 introduced by iodine. Active oxygen species, that is, *OH and O2-, were evidenced to be involved in the degradation process and a possible mechanism was also proposed. PMID:27427614

  1. Low-temperature hydrothermal synthesis of α-Fe/Fe3O4 nanocomposite for fast Congo red removal.

    PubMed

    Wang, Lixia; Li, Jianchen; Wang, Zhitao; Zhao, Lijun; Jiang, Qing

    2013-02-21

    A facile low-temperature hydrothermal process to synthesize α-Fe/Fe(3)O(4) nanocomposite is reported. TEM and HRTEM revealed that the α-Fe/Fe(3)O(4) nanocomposite was composed of catenulate α-Fe and lamellar structured Fe(3)O(4). The weight ratio of α-Fe in the α-Fe/Fe(3)O(4) nanocomposite is 35.6%. The α-Fe/Fe(3)O(4) nanocomposite demonstrates an extremely high Congo red (CR) removal efficiency from waste water showing almost complete removal within 3 min. For 100 mg L(-1) of CR aqueous solution, the maximum CR removal can reach 1297.06 mg g(-1). The large saturation magnetization (80.5 emu g(-1)) of the nanocomposite allows fast separation of α-Fe/Fe(3)O(4) nanoparticles loaded with CR from the liquid suspension. The synergistic effect of the nanocomposite may contribute to the enhanced CR removal ability, because the CR can be removed by reduction reaction and adsorption at the same time. Based on the degradation products identified by UV-Vis spectra, XRD and FTIR spectra, a possible degradation mechanism of CR on the α-Fe/Fe(3)O(4) composite was proposed. The significantly reduced treatment time required to remove the CR and the simple, low-cost and pollution-free preparation method make α-Fe/Fe(3)O(4) nanocomposite promising for highly efficient removal of dyes from waste water. PMID:23223415

  2. Hydrothermal synthesis of highly luminescent blue-emitting ZnSe(S) quantum dots exhibiting low toxicity.

    PubMed

    Mirnajafizadeh, Fatemeh; Ramsey, Deborah; McAlpine, Shelli; Wang, Fan; Reece, Peter; Stride, John Arron

    2016-07-01

    Highly luminescent quantum dots (QDs) that emit in the visible spectrum are of interest to a number of imaging technologies, not least that of biological samples. One issue that hinders the application of luminescent markers in biology is the potential toxicity of the fluorophore. Here we show that hydrothermally synthesized ZnSe(S) QDs have low cytotoxicity to both human colorectal carcinoma cells (HCT-116) and human skin fibroblast cells (WS1). The QDs exhibited a high degree of crystallinity, with a strong blue photoluminescence at up to 29% quantum yield relative to 4',6-diamidino-2-phenylindole (DAPI) without post-synthetic UV-irradiation. Confocal microscopy images obtained of HCT-116 cells after incubation with the QDs highlighted the stability of the particles in cell media. Cytotoxicity studies showed that both HCT-116 and WS1 cells retain 100% viability after treatment with the QDs at concentrations up to 0.5g/L, which makes them of potential use in biological imaging applications. PMID:27127041

  3. Hydrothermal synthesis and characterization of aluminum-free Mn-β zeolite: a catalyst for phenol hydroxylation.

    PubMed

    He, Zhen; Wu, Juan; Gao, Bingying; He, Hongyun

    2015-02-01

    Zeolite beta, especially heteroatomic zeolite beta, has been widely used in the industries of fine chemicals and petroleum refining because of its outstanding thermal stability, acid resistance, and unique 3-D open-frame structure. In this paper, aluminum-free Mn-β zeolite was hydrothermally synthesized in the SiO2-MnO2-(TEA)2O-NaF-H2O system. The effect of the chemical composition of the precursor mixture to the crystallization of the Al-free Mn-β zeolite was investigated. The synthesized Al-free Mn-β zeolite was characterized by inductively coupled plasma (ICP), XRD, thermogravimetric/differential thermal analysis (TG/DTA), N2 adsorption-desorption, FT-IR, UV-vis, X-ray photoelectron spectroscopy (XPS), and scanning electron microscope (SEM). The results show that the synthesized zeolite has a structure of β zeolite with good crystallinity and Mn ions present in the framework of the zeolite. The synthesized Al-free Mn-β zeolite shows great catalytic activity toward the phenol hydroxylation reaction using H2O2 as the oxidant. Approximately 35% of phenol conversion and ∼98% of dihydroxybenzene selectivity can be obtained under the optimal conditions. PMID:25556927

  4. KY(MoO4)2:Eu3+ Phosphor: Template-Free Hydrothermal Synthesis and Luminescent Properties.

    PubMed

    Wei, Yanling; Su, Chunhui; Zhang, Hongbo; Fu, Zuoling

    2016-03-01

    KY(MoO4)2 microcrystals with different morphologies, including rhombic, sheet-like, rectangular plate-like, and hexagon plate-like, have been successfully synthesized via a simple hydrothermal method without using any templates, surfactant, or other organic additives by varying the molar ratios of Y(NO3)3/K2MoO4 and pH values of the resultant solutions. X-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), photoluminescence (PL), and photoluminescent excitation spectra (PLE) were employed to characterize the samples. Furthermore, a systematic study on the photoluminescence of Eu3+ doped KY(MoO4)2 samples has been explored by varying experimental conditions. The strongest red emission can be observed clearly at 616 nm. And by controlling the doping concentration of Eu3+ in KY(MoO4)2 solutions, it can be seen that the concentration quenching occurs at 25 at.% for Eu3+. These results suggest that the well-crystallized KY(MoO4)2:Eu3+ microcrystals synthesized in our experiment can be used as a red component for white light emitting diodes (W-LEDs). PMID:27455776

  5. Hydrothermal synthesis of Yb3+, Tm3+ co-doped Gd6MoO12 and its upconversion properties

    NASA Astrophysics Data System (ADS)

    Di, Qiu-Mei; Sun, Yu-Mei; Xu, Qi-Guang; Han, Liu; Xue, Bing; Sun, Jia-Yue

    2015-06-01

    Yb3+, Tm3+ co-doped Gd6MoO12 phosphors with different morphologies are prepared by the hydrothermal method. The dendrites present different morphologies (including hexagonal prisms, spindles, and spheres) after changing the pH value and edetate disodium (EDTA) usage. It is found that each of the two factors plays a crucial role in forming different morphologies. The up-conversion (UC) luminescence is studied. Under 980-nm semiconductor laser excitation, relatively strong blue emission and weak red emission are observed. Finally, the effect of pumping power on the UC luminescence properties and the level diagram mechanism of Gd6MoO12:Yb3+/Tm3+ phosphor are also discussed. Project supported by the National Natural Science Foundation of China (Grant No. 20976002), the Beijing Natural Science Foundation, China (Grant No. 2122012), the Key Projects for Science and Technology of Beijing Education Commission, China (Grant No. KZ201310011013), and the Education and Research Fund of Guangdong Province, China (Grant No. 2011B090400100).

  6. Supercritical hydrothermal synthesis, thermal, spectroscopic and magnetic studies of two new polymorphs of Mn(SeO3).

    PubMed

    Larrañaga, Aitor; Mesa, José L; Pizarro, José L; Lezama, L; Chapman, Jon P; Arriortua, María I; Rojo, Teófilo

    2005-05-01

    Two new manganese(II) selenite polymorphs with formula Mn(SeO3) have been synthesised using supercritical hydrothermal conditions. The crystal structure of both compounds (1) and (2) has been solved from single-crystal X-ray diffraction data. The structures consist of a three-dimensional framework formed by MnO6 octahedra and (SeO3)2- selenite anions with trigonal pyramidal geometry. Compound (1) shows chains of elongated, corner-sharing MnO6 octahedra. These chains are linked alternately by Mn2O10 dimers of edge-sharing octahedra. Conversely, compound (2) exhibits MnO6 octahedra sharing edges with three further octahedra, giving rise to a complex three-dimensional framework. The IR spectra show the characteristic bands of the selenite anion. Studies of luminescence and diffuse reflectance spectroscopy, performed at 6 K and at room temperature, respectively, have been carried out for both compounds. The Dq and Racah parameters are Dq= 830, B= 500 and C= 3790 cm(-1) for (1) and Dq= 795, B= 520 and C= 3785 cm(-1) for (2). The EPR spectra of both compounds are isotropic with a g-value of 1.99(1), which remains unchanged with variation in temperature. Magnetic measurements indicate the presence of antiferromagnetic couplings as the major interactions in both phases, but with compound (2) exhibiting at low temperature a canting of antiferromagnetically aligned spins. The estimated J-exchange parameters are J/k=-2.2 and -1.93 for (1) and (2), respectively, with J'= -0.87 and -0.55 K. PMID:15852125

  7. Hydrothermal synthesis and characterization under dynamic conditions of cobalt oxide nanoparticles supported over magnesium oxide nano-plates.

    PubMed

    Alayoglu, Selim; Rosenberg, Daniel J; Ahmed, Musahid

    2016-06-14

    A nano-catalyst comprised of oxidized Co NPs supported on MgO nano-plates was synthesized via a hydrothermal co-precipitation strategy and calcination in O2 and subsequently in H2 at 250 °C. Spectro-microscopy characterization was performed by scanning transmission electron microscopy, electron energy loss spectroscopy and scanning X-ray transmission microscopy. Surface measurements under H2 and H2 + CO atmospheres were obtained by ambient pressure X-ray photoelectron spectroscopy and in situ X-ray absorption spectroscopy in the 225-480 °C range. These measurements at the atomic and microscopic levels demonstrated that the oxidized Co nanoparticles uniformly decorated the MgO nano-plates. The surfaces are enriched with Co, and with a mixture of Co(OH)2 and CoO under H2 and H2 + CO atmospheres. Under a H2 atmosphere, the outermost surfaces were composed of (lattice) O(2-), CO3(2-) and OH(-). No inorganic carbonates were observed in the bulk. Chemisorbed CO, likely on the oxidized Co surfaces, was observed at the expense of O(2-) under 300 mTorr H2 + CO (2 : 1) at 225 °C. Gas phase CO2 was detected under 32 Torr H2 + CO (2 : 1) at 225 °C upon prolonged reaction time, and was attributed to a surface chemical reaction between O(2-) and chemisorbed CO. Furthermore, sp(3) like carbon species were detected on the otherwise carbon free surface in H2 + CO, which remained on the surface under the subsequent reaction conditions. The formation of sp(3) like hydrocarbons was ascribed to a surface catalytic reaction between the chemisorbed CO and OH(-) as the apparent hydrogen source. PMID:26979489

  8. Synthesis, characterization, and magnetic properties of monodisperse CeO2 nanospheres prepared by PVP-assisted hydrothermal method

    PubMed Central

    2012-01-01

    Ferromagnetism was observed at room temperature in monodisperse CeO2 nanospheres synthesized by hydrothermal treatment of Ce(NO3)3·6H2O using polyvinylpyrrolidone as a surfactant. The structure and morphology of the products were characterized by X-ray diffraction (XRD), Raman spectroscopy, transmission electron microscopy, high-resolution transmission electron microscopy, and field-emission scanning electron microscopy (FE-SEM). The optical properties of the nanospheres were determined using UV and visible spectroscopy and photoluminescence (PL). The valence states of Ce ions were also determined using X-ray absorption near edge spectroscopy. The XRD results indicated that the synthesized samples had a cubic structure with a crystallite size in the range of approximately 9 to 19 nm. FE-SEM micrographs showed that the samples had a spherical morphology with a particle size in the range of approximately 100 to 250 nm. The samples also showed a strong UV absorption and room temperature PL. The emission might be due to charge transfer transitions from the 4f band to the valence band of the oxide. The magnetic properties of the samples were studied using a vibrating sample magnetometer. The samples exhibited room temperature ferromagnetism with a small magnetization of approximately 0.0026 to 0.016 emu/g at 10 kOe. Our results indicate that oxygen vacancies could be involved in the ferromagnetic exchange, and the possible mechanism of formation was discussed based on the experimental results. PMID:22849756

  9. Hydrothermal synthesis of coral-like Au/ZnO catalyst and photocatalytic degradation of Orange II dye

    SciTech Connect

    Chen, P.K.; Lee, G.J.; Davies, S.H.; Masten, S.J.; Amutha, R.; Wu, J.J.

    2013-06-01

    Highlights: ► Coral-like Au/ZnO was successfully prepared using green synthetic method. ► Gold nanoparticles were deposited on the ZnO structure using NaBH{sub 4} and β-D-glucose. ► Coral-like Au/ZnO exhibited superior photocatalytic activity to degrade Orange II. - Abstract: A porous coral-like zinc oxide (c-ZnO) photocatalyst was synthesized by the hydrothermal method. The coral-like structure was obtained by precipitating Zn{sub 4}(CO{sub 3})(OH){sub 6}·H{sub 2}O (ZnCH), which forms nanosheets that aggregate together to form microspheres with the coral-like structure. X-ray diffraction (XRD) studies indicate that after heating at 550 °C the ZnCH microspheres can be converted to ZnO microspheres with a morphology similar to that of ZnCH microspheres. Thermogravimetric analysis (TGA) shows this conversion takes place at approximately 260 °C. A simple electrostatic self-assembly method has been employed to uniformly disperse Au nanoparticles (1 wt.%) on the ZnO surface. In this procedure β-D-glucose was used to stabilize the Au nanoparticles. Scanning electron microscope images indicate that the diameter of coral-like ZnO microspheres (c-ZnO) is about 8 μm. X-ray diffraction reveals that the ZnO is highly crystalline with a wurtzite structure and the Au metallic particles have an average size of about 13 nm. X-ray photoelectron spectroscopic (XPS) studies have confirmed the presence of ZnO and also showed that the Au is present in the metallic state. The photocatalytic degradation of Orange II dye, with either ultraviolet or visible light, is faster on Au/c-ZnO than on c-ZnO.

  10. Hydrothermal synthesis and characteristics of 3-D hydrated bismuth oxalate coordination polymers with open-channel structure

    NASA Astrophysics Data System (ADS)

    Chen, Xinxiang; Cao, Yanning; Zhang, Hanhui; Chen, Yiping; Chen, Xuehuan; Chai, Xiaochuan

    2008-05-01

    Two new 3-D porous bismuth coordination polymers, (C 5NH 6) 2[Bi 2(H 2O) 2(C 2O 4) 4]·2H 2O 1 and (NH 4)[Bi(C 2O 4) 2]·3H 2O 2, have been hydrothermally synthesized and characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic symmetry, P2 1/ c space group with a=10.378(2) Å, b=17.285(3) Å, c=16.563(5) Å, α=90°, β=119.66(2)°, γ=90°, V=2581.8(10) Å 3, Z=4, R1=0.0355 and w R2=0.0658 for unique 4713 reflections I >2 σ( I). Compound 2 crystallizes in the tetragonal symmetry, I4 1/ amd space group with a=11.7026(17) Å, b=11.7026(17) Å, c=9.2233(18) Å, α=90°, β=90°, γ=90°, V=1263.1(4) Å 3, Z=32, R1=0.0208 and w R2=0.0518 for unique 359 reflections I> 2 σ( I). Compounds 1 and 2 are 3-D open-framework structures with a 6 6 uniform net, which consist of honeycomb-like layers connected to each other by oxalate units. While different guest molecules fill in their cavities of honeycomb-like layers, study of ultrasonic treatment on 2 indicates the replacement of NH 4+ by K + on potassium ion exchange. Thermogravimetric analysis indicates that the open-channel frameworks are thermally stable up to 200 °C, and other characterizations are also described by elemental analysis, IR and ultraviolet-visible diffuse reflectionintegral spectrum (UV-Vis DRIS).

  11. Hydrothermal synthesis, characterizations and photoluminescence study of single crystalline hexagonal ZnO nanorods with three dimensional flowerlike microstructures

    NASA Astrophysics Data System (ADS)

    Kale, Rohidas B.; Hsu, Yung-Jung; Lin, Yi-Feng; Lu, Shih-Yuan

    2014-05-01

    A simple, low-cost, and environmentally benign hydrothermal approach has been successfully developed to synthesize uniform, large-scale well-crystallized ZnO nanorods with different aspect ratios that were united together to form three dimensional (3D) flowerlike structures. The method involved direct growth of ZnO 3D microstructures using aqueous solution of Zn(CH3COO)2 as the precursor and NaOH to adjust the pH of resultant solution. Surfactants or templates were not used during the entire synthetic process. Moreover, the morphology evolution of the ZnO nanorods with reaction time suggests a recrystallization-dissolution-growth mechanism that continuously takes place for prolonged interval of time. The XRD pattern of the as-grown ZnO nanorods and relevant analyses confirm the well crystallized hexagonal structure of the ZnO microstructures and no evidence of any other impurity phases. SEM observations reveal that the ZnO product grew in the form of nanorods that were united together to form 3D flowerlike morphology. The high resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED) shows that the ZnO nanorods were single crystalline and grew along the c-axis of the crystal plane. PL measurements of the as-synthesized nanorods exhibit excellent excitation features and strong band-edge UV luminescence even at room temperature. The uniform single crystalline, defect free, and high aspect ratio nanorods may find promising applications in optoelectronics and photo-catalysts. The growth habit of ZnO crystal is also illustrated. This method is suitable for large-scale production of ZnO microstructures and could be extended for syntheses of other metal oxides.

  12. Template-Assisted Hydrothermal Synthesis of Li₂MnSiO₄ as a Cathode Material for Lithium Ion Batteries.

    PubMed

    Xie, Man; Luo, Rui; Chen, Renjie; Wu, Feng; Zhao, Taolin; Wang, Qiuyan; Li, Li

    2015-05-27

    Lithium manganese silicate (Li2MnSiO4) is an attractive cathode material with a potential capacity above 300 mA h g(-1) if both lithium ions can be extracted reversibly. Two drawbacks of low electronic conductivity and structural collapse could be overcome by a conductive surface coating and a porous structure. Porous morphology with inner mesopores offers larger surface area and shorter ions diffusion pathways and also buffers the volume changes during lithium insertion and extraction. In this paper, mesoporous Li2MnSiO4 (M-Li2MnSiO4) prepared using MCM-41 as template through a hydrothermal route is compared to a sample of bulk Li2MnSiO4 (B-Li2MnSiO4) using silica as template under the same conditions. Also, in situ carbon coating technique was used to improve the electronic conductivity of M-Li2MnSiO4. The physical properties of these cathode materials were further characterized by SEM, XRD, FTIR, and N2 adsorption-desorption. It is shown that M-Li2MnSiO4 exhibits porous structure with pore sizes distributed in the range 9-12 nm, and when used as cathode electrode material, M-Li2MnSiO4 exhibits enhanced specific discharge capacity of 193 mA h g(-1) at a constant current of 20 mA g(-1) compared with 120.1 mA h g(-1) of B-Li2MnSiO4. This is attributed to the porous structure which allows the electrolyte to penetrate into the particles easily. And carbon-coated M-Li2MnSiO4 shows smaller charge transfer resistance and higher capacity of 217 mA h g(-1) because carbon coating retains the porous structure and enhances the electrical conductivity. PMID:25932749

  13. Rapid synthesis of Ti-MCM-41 by microwave-assisted hydrothermal method towards photocatalytic degradation of oxytetracycline.

    PubMed

    Chen, Hanlin; Peng, Yen-Ping; Chen, Ku-Fan; Lai, Chia-Hsiang; Lin, Yung-Chang

    2016-06-01

    This study employed microwave-assisted hydrothermal method to synthesize Ti-MCM-41, which are mesoporous materials with a high surface area and excellent photocatalytic ability. Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), and ultraviolet-visible spectroscopy (UV-Vis) were employed. The XRD findings showed that Ti-MCM-41 exhibited a peak at 2θ of 2.2°, which was attributed to the hexagonal MCM-41 structure. The BET (Brunauer-Emmett-Teller) results agreed with the TEM findings that Ti-MCM-41 has a pore size of about 3-5nm and a high surface area of 883m(2)/g. FTIR results illustrated the existence of Si-O-Si and Si-O-Ti bonds in Ti-MCM-41. The appearance of Ti 2p peaks in the XPS results confirmed the FTIR findings that the Ti was successfully doped into the MCM-41 structure. Zeta (ζ)-potential results indicated that the iso-electric point (IEP) of Ti-MCM-41 was at about pH3.02. In this study, the photocatalytic degradation of oxytetracycline (OTC) at different pH was investigated under Hg lamp irradiation (wavelength 365nm). The rate constant (K'obs) for OTC degradation was 0.012min(-1) at pH3. Furthermore, TOC (total organic carbon) and high resolution LC-MS (liquid chromatography-mass spectrometry) analyses were conducted to elucidate the possible intermediate products and degradation pathway for OTC. The TOC removal efficiency of OTC degradation was 87.0%, 74.4% and 50.9% at pH3, 7 and 10, respectively. LC-MS analysis results showed that the degradation products from OTC resulted from the removal of functional groups from the OTC ring. PMID:27266304

  14. Rare earth doped LiYbF{sub 4} phosphors with controlled morphologies: Hydrothermal synthesis and luminescent properties

    SciTech Connect

    Huang, Wenjuan; Lu, Chunhua; Jiang, Chenfei; Jin, Junyang; Ding, Mingye; Ni, Yaru; Xu, Zhongzi

    2012-06-15

    Highlights: ► LiYbF{sub 4} microparticles as an excellent upconverting materials. ► High temperature and long time can favor high crystalline LiYbF{sub 4} microparticles. ► The shape of LiYbF{sub 4} microparticles can be tuned by the molar ratio of EDTA to Yb{sup 3+}. ► Bright green emission can be obtained by changing the doping concentration of Er{sup 3+}. -- Abstract: High quality monodisperse LiYbF{sub 4} microparticles with shape of octahedron had been prepared via a facile hydrothermal route. The crystalline phase, size, morphology and luminescence properties were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), photoluminescence (PL) spectra and Commission Internationale de L’Eclairage (CIE 1931) chromaticity coordinates, respectively. The influences of reaction temperature, reaction time and the molar ratio of EDTA to Yb{sup 3+} on the crystal phases and shapes of as-prepared products had been investigated in detail. The upconversion (UC) luminescence properties of LiYb{sub 1−x}F{sub 4}:xEr{sup 3+} (x =0.1, 0.2, 0.5, 1, 2, 5 and 10 mol%) particles with octahedral microstructures were studied under 976 nm excitation. The results showed that the luminescence colors of the corresponding products could be tuned to bright green by changing the doping concentration of Er{sup 3+} ion. The luminescence mechanisms for the doped Er{sup 3+} ion were thoroughly analyzed, showing great potential in applications such as biolabels, displays and other optical technologies.

  15. Hydrothermal synthesis of titanium dioxide nanoparticles: mosquitocidal potential and anticancer activity on human breast cancer cells (MCF-7).

    PubMed

    Murugan, Kadarkarai; Dinesh, Devakumar; Kavithaa, Krishnamoorthy; Paulpandi, Manickam; Ponraj, Thondhi; Alsalhi, Mohamad Saleh; Devanesan, Sandhanasamy; Subramaniam, Jayapal; Rajaganesh, Rajapandian; Wei, Hui; Kumar, Suresh; Nicoletti, Marcello; Benelli, Giovanni

    2016-03-01

    Mosquito vectors (Diptera: Culicidae) are responsible for transmission of serious diseases worldwide. Mosquito control is being enhanced in many areas, but there are significant challenges, including increasing resistance to insecticides and lack of alternative, cost-effective, and eco-friendly products. To deal with these crucial issues, recent emphasis has been placed on plant materials with mosquitocidal properties. Furthermore, cancers figure among the leading causes of morbidity and mortality worldwide, with approximately 14 million new cases and 8.2 million cancer-related deaths in 2012. It is expected that annual cancer cases will rise from 14 million in 2012 to 22 million within the next two decades. Nanotechnology is a promising field of research and is expected to give major innovation impulses in a variety of industrial sectors. In this study, we synthesized titanium dioxide (TiO2) nanoparticles using the hydrothermal method. Nanoparticles were subjected to different analysis including UV-Vis spectrophotometry, Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), zeta potential, and energy-dispersive spectrometric (EDX). The synthesized TiO2 nanoparticles exhibited dose-dependent cytotoxicity against human breast cancer cells (MCF-7) and normal breast epithelial cells (HBL-100). After 24-h incubation, the inhibitory concentrations (IC50) were found to be 60 and 80 μg/mL on MCF-7 and normal HBL-100 cells, respectively. Induction of apoptosis was evidenced by Acridine Orange (AO)/ethidium bromide (EtBr) and 4',6-diamidino-2-phenylindole dihydrochloride (DAPI) staining. In larvicidal and pupicidal experiments conducted against the primary dengue mosquito Aedes aegypti, LC50 values of nanoparticles were 4.02 ppm (larva I), 4.962 ppm (larva II), 5.671 ppm (larva III), 6.485 ppm (larva IV), and 7.527 ppm (pupa). Overall, our results suggested that TiO2 nanoparticles may be considered as

  16. Hydrothermal synthesis, structure, Raman spectroscopy, and self-irradiation studies of {sup 248}Cm(IO{sub 3}){sub 3}

    SciTech Connect

    Sykora, Richard E.; Assefa, Zerihun; Haire, Richard G. . E-mail: hairerg@ornl.gov; Albrecht-Schmitt, Thomas E. . E-mail: albreth@auburn.edu

    2004-12-01

    The study of curium iodate, Cm(IO{sub 3}){sub 3}, was undertaken as part of a systematic investigation of the 4f- and 5f-elements' iodates. The reaction of {sup 248}CmCl{sub 3} with aqueous H{sub 5}IO{sub 6} under mild hydrothermal conditions results in the reduction of IO{sub 6}{sup 5-} to IO{sub 3}{sup -} anions, and the subsequent formation of Cm(IO{sub 3}){sub 3} single crystals. Crystallographic data are: (193K, MoK{alpha}, {lambda}=0.71073A): monoclinic, space group P2{sub 1}/c, a=7.2014(7)A, b=8.5062(9)A, c=13.4622(14)A, {beta}=100.142(2){sup o}, V=811.76(14), Z=4, R(F)=2.11%, Rw(Fo2)=4.43% for 119 parameters with 1917 reflections with I>2{sigma}(I). The structure consists of Cm{sup 3+} cations bound by iodate anions to form [Cm(IO{sub 3}){sub 8}] units, where the local coordination environment around the curium centers can be described as a distorted dodecahedron. There are three crystallographically unique iodate anions within the structure; two iodates bridge between three Cm centers, and one iodate bridges between two Cm centers and has a terminal oxygen atom. The bridging of the curium centers by the iodate anions creates a three-dimensional structure. Three strong Raman bands with comparable intensities were observed at 846, 804, and 760cm{sup -1} and correspond to the I-O symmetric stretching of the three crystallographically distinct iodate ions. The Raman profile suggests a lack of inter-ionic vibrational coupling of the I-O stretching, while intra-ionic coupling provides symmetric and asymmetric components that correspond to each iodate site. Repeated collection of X-ray diffraction data for a crystal of Cm(IO{sub 3}){sub 3} over a period of time revealed a gradual expansion of the unit cell from self-irradiation. After 71 days, the new parameters were: a=7.2132(7)A, b=8.5310(8)A, c=13.505(1)A, {beta}=100.021(2){sup o}, V=818.3(2)

  17. High-temperature, high-pressure hydrothermal synthesis, characterization, and structural relationships of mixed-alkali metals uranyl silicates

    NASA Astrophysics Data System (ADS)

    Chen, Yi-Hsin; Liu, Hsin-Kuan; Chang, Wen-Jung; Tzou, Der-Lii; Lii, Kwang-Hwa

    2016-04-01

    Three mixed-alkali metals uranyl silicates, Na3K3[(UO2)3(Si2O7)2]·2H2O (1), Na3Rb3[(UO2)3(Si2O7)2] (2), and Na6Rb4[(UO2)4Si12O33] (3), have been synthesized by high-temperature, high-pressure hydrothermal reactions at 550 °C and 1440 bar, and characterized by single-crystal X-ray diffraction, photoluminescence, and thermogravimetric analysis. Compound 1 and 2 are isostructural and contain layers of uranyl disilicate. The smaller cation, Na+, is located in the intralayer channels, whereas the larger cations, K+ and Rb+, and water molecule are located in the interlayer region. The absence of lattice water in 2 can be understood according to the valence-matching principle. The structure is related to that of a previously reported mixed-valence uranium(V,VI) silicate. Compound 3 adopts a 3D framework structure and contains a unique unbranched dreier fourfold silicate chain with the structural formula {uB,41∞}[3Si12O33] formed of Q2, Q3, and Q4 Si. The connectivity of the Si atoms in the Si12O3318- anion can be interpreted on the basis of Zintl-Klemm concept. Crystal data for compound 1: triclinic, P-1, a=5.7981(2) Å, b=7.5875(3) Å, c=12.8068(5) Å, α=103.593(2)°, β=102.879(2)°, γ=90.064(2)°, V=533.00(3) Å3, Z=1, R1=0.0278; compound 2: triclinic, P-1, a=5.7993(3) Å, b=7.5745(3) Å, c=12.9369(6) Å, α=78.265(2)°, β=79.137(2)°, γ=89.936(2)°, V=546.02(4) Å3, Z=1, R1=0.0287; compound 3: monoclinic, C2/m, a=23.748(1) Å, b=7.3301(3) Å, c=15.2556(7) Å, β=129.116(2)°, V=2060.4(2) Å3, Z=2, R1=0.0304.

  18. Photovoltaic performance of dye-sensitized solar cells using TiO2 nanotubes aggregates produced by hydrothermal synthesis

    NASA Astrophysics Data System (ADS)

    Chen, Qiufan; Sun, Xiaonan; Liu, Anping; Zhang, Qifeng; Cao, Guozhong; Zhou, Xiaoyuan

    2015-09-01

    This paper reports the synthesis, detailed structural characterization of aggregated TiO2 nanotubes and the application of such aggregated TiO2 nanotubes as photoelectrodes in solar cells (dye sensitized DSCs). A maximum overall conversion efficiency of 7.9% has been achieved, which use conventional dyes without any additional chemical treatments under circumstances of an open-circuit voltage of 710 mV, a short-circuit current density of 16.8mA/cm2, and a fill factor of 66%. This impressive performance is believed to attribute to the micron-sized aggregate structure which may be favorable for light harvesting, the desired high specific surface area and pure anatase phase for dye absorption. This significant improvement in the conversion efficiency indicates that DSCs based on aggregated TiO2 nanotubes are a promising alternative to semiconductor-based solar cells.

  19. Hydrothermal Processes

    NASA Astrophysics Data System (ADS)

    German, C. R.; von Damm, K. L.

    2003-12-01

    What is Hydrothermal Circulation?Hydrothermal circulation occurs when seawater percolates downward through fractured ocean crust along the volcanic mid-ocean ridge (MOR) system. The seawater is first heated and then undergoes chemical modification through reaction with the host rock as it continues downward, reaching maximum temperatures that can exceed 400 °C. At these temperatures the fluids become extremely buoyant and rise rapidly back to the seafloor where they are expelled into the overlying water column. Seafloor hydrothermal circulation plays a significant role in the cycling of energy and mass between the solid earth and the oceans; the first identification of submarine hydrothermal venting and their accompanying chemosynthetically based communities in the late 1970s remains one of the most exciting discoveries in modern science. The existence of some form of hydrothermal circulation had been predicted almost as soon as the significance of ridges themselves was first recognized, with the emergence of plate tectonic theory. Magma wells up from the Earth's interior along "spreading centers" or "MORs" to produce fresh ocean crust at a rate of ˜20 km3 yr-1, forming new seafloor at a rate of ˜3.3 km2 yr-1 (Parsons, 1981; White et al., 1992). The young oceanic lithosphere formed in this way cools as it moves away from the ridge crest. Although much of this cooling occurs by upward conduction of heat through the lithosphere, early heat-flow studies quickly established that a significant proportion of the total heat flux must also occur via some additional convective process (Figure 1), i.e., through circulation of cold seawater within the upper ocean crust (Anderson and Silbeck, 1981). (2K)Figure 1. Oceanic heat flow versus age of ocean crust. Data from the Pacific, Atlantic, and Indian oceans, averaged over 2 Ma intervals (circles) depart from the theoretical cooling curve (solid line) indicating convective cooling of young ocean crust by circulating seawater

  20. Microwave-hydrothermal synthesis and characterization of nanostructured copper substituted ZnM2O4 (M = Al, Ga) spinels as precursors for thermally stable Cu catalysts.

    PubMed

    Conrad, Franziska; Massue, Cyriac; Kühl, Stefanie; Kunkes, Edward; Girgsdies, Frank; Kasatkin, Igor; Zhang, Bingsen; Friedrich, Matthias; Luo, Yuan; Armbrüster, Marc; Patzke, Greta R; Behrens, Malte

    2012-03-21

    Nanostructured Cu(x)Zn(1-x)Al(2)O(4) with a Cu:Zn ratio of ¼:¾ has been prepared by a microwave-assisted hydrothermal synthesis at 150 °C and used as a precursor for Cu/ZnO/Al(2)O(3)-based catalysts. The spinel nanoparticles exhibit an average size of approximately 5 nm and a high specific surface area (above 250 m(2) g(-1)). Cu nanoparticles of an average size of 3.3 nm can be formed by reduction of the spinel precursor in hydrogen and the accessible metallic Cu(0) surface area of the reduced catalyst was 8 m(2) g(-1). The catalytic performance of the material in CO(2) hydrogenation and methanol steam reforming was compared with conventionally prepared Cu/ZnO/Al(2)O(3) reference catalysts. The observed lower performance of the spinel-based samples is attributed to a lack of synergetic interaction of the Cu nanoparticles with ZnO due to the incorporation of Zn(2+) in the stable spinel lattice. Despite its lower performance, however, the nanostructured nature of the spinel catalyst was stable after thermal treatment up to 500 °C in contrast to other Cu-based catalysts. Furthermore, a large fraction of the re-oxidized copper migrates back into the spinel upon calcination of the reduced catalyst, thereby enabling a regeneration of sintered catalysts after prolonged usage at high temperatures. Similarly prepared samples with Ga instead of Al exhibit a more crystalline catalyst with a spinel particle size around 20 nm. The slightly decreased Cu(0) surface area of 3.2 m(2) g(-1) due to less copper incorporation is not a significant drawback for the methanol steam reforming. PMID:22327266

  1. Carbonated hydroxyapatite starting from calcite and different orthophosphates under moderate hydrothermal conditions: Synthesis and surface reactivity in simulated body fluid

    SciTech Connect

    Pham Minh, Doan Nzihou, Ange; Sharrock, Patrick

    2014-12-15

    Highlights: • Carbonated apatite (CAP) could be easily obtained from CaCO{sub 3} and orthophosphates. • Highest CaCO{sub 3} dissolution and apatitic carbonate content were obtained with H{sub 3}PO{sub 4}. • A-B-type CAP was formed. • The synthesized CAP was thermally stable up to 1000 °C. • This CAP showed high biomineralization activity before and after thermal treatment. - Abstract: The one-step synthesis of carbonated hydroxyapatite (CAP) using calcite and different orthophosphates was investigated in a closed batch reactor. Only orthophosphoric acid could lead to the complete decomposition of calcite particles, when the reaction temperature was set at 80 °C. On the other hand, the reaction time and the dilution of the initial calcite suspension had no significant influence on the formation of the solid products. CAP was formed as the main crystalline calcium phosphate with the carbonate content in the range of 4.2–4.6 wt.%. The thermal decarbonation of the synthesized CAP started at 750 °C but it was only significant at 1000 °C under air atmosphere. This thermal decarbonation was total at 1200 °C or above. All CAP samples and products following thermal treatments were found bioactive in the test using simulated body fluid (SBF) solution.

  2. Controlled synthesis of La{sub 1−x}Sr{sub x}CrO{sub 3} nanoparticles by hydrothermal method with nonionic surfactant and their ORR activity in alkaline medium

    SciTech Connect

    Choi, Bo Hyun; Park, Shin-Ae; Park, Bong Kyu; Chun, Ho Hwan; Kim, Yong-Tae

    2013-10-15

    Graphical abstract: We demonstrate that Sr-doped LaCrO{sub 3} nanoparticles were successfully prepared by the hydrothermal synthesis method using the nonionic surfactant Triton X-100 and the applicability of La{sub 1−x}Sr{sub x}CrO{sub 3} to oxygen reduction reaction (ORR) electrocatalysis in an alkaline medium. Compared with the nanoparticles synthesized by the coprecipitation method, they showed enhanced ORR activity. - Highlights: • Sr-doped LaCrO{sub 3} nanoparticles were successfully prepared by the hydrothermal method using the nonionic surfactant. • Homogeneously shaped and sized Sr-doped LaCrO{sub 3} nanoparticles were readily obtained. • Compared with the nanoparticles synthesized by the coprecipitation method, they showed an enhanced ORR activity. • The main origin was revealed to be the decreased particle size due to the nonionic surfactant. - Abstract: Sr-doped LaCrO{sub 3} nanoparticles were prepared by the hydrothermal method with the nonionic surfactant Triton X-100 followed by heat treatment at 1000 °C for 10 h. The obtained perovskite nanoparticles had smaller particle size (about 100 nm) and more uniform size distribution than those synthesized by the conventional coprecipitation method. On the other hand, it was identified with the material simulation that the electronic structure change by Sr doping was negligible, because the initially unfilled e{sub g}-band was not affected by the p-type doping. Finally, the perovskite nanoparticles synthesized by hydrothermal method showed much higher ORR activity by over 200% at 0.8 V vs. RHE than those by coprecipitation method.

  3. Hydrothermal Conditions and the Origin of Cellular Life.

    PubMed

    Deamer, David W; Georgiou, Christos D

    2015-12-01

    The conditions and properties of hydrothermal vents and hydrothermal fields are compared in terms of their ability to support processes related to the origin of life. The two sites can be considered as alternative hypotheses, and from this comparison we propose a series of experimental tests to distinguish between them, focusing on those that involve concentration of solutes, self-assembly of membranous compartments, and synthesis of polymers. Key Word: Hydrothermal systems. PMID:26684507

  4. Preparation of highly photocatalytic active CdS/TiO{sub 2} nanocomposites by combining chemical bath deposition and microwave-assisted hydrothermal synthesis

    SciTech Connect

    Li, Li; Wang, Lili; Hu, Tianyu; Zhang, Wenzhi; Zhang, Xiuli; Chen, Xi

    2014-10-15

    CdS/TiO{sub 2} nanocomposites were prepared from Cd and Ti (1:1 M ratio) using cetyltrimethylammonium bromide by a two-step chemical bath deposition (CBD) and microwave-assisted hydrothermal synthesis (MAHS) method. A series of nanocomposites with different morphologies and activities were prepared by varying the reaction time in the MAHS (2, 4, and 6 h). The crystal structure, morphology, and surface physicochemical properties of the nanocomposites were characterized by X-ray diffraction, UV–visible diffuse reflectance spectroscopy, X-ray photoelectron spectroscopy, scanning electron microscopy, and N{sub 2} adsorption–desorption measurements. The results show that the CdS/TiO{sub 2} nanocomposites were composed of anatase TiO{sub 2} and hexagonal CdS phases with strong absorption in the visible region. The surface morphologies changed slightly with increasing microwave irradiation time, while the Brunauer–Emmett–Teller surface area increased remarkably. The photocatalytic degradation of methyl orange (MO) was investigated under UV light and simulated sunlight irradiation. The photocatalytic activity of the CdS/TiO{sub 2} (6 h) composites prepared by the MAHS method was higher than those of CdS, P25, and other CdS/TiO{sub 2} nanocomposites. The CdS/TiO{sub 2} (6 h) nanocomposites significantly affected the UV and microwave-assisted photocatalytic degradation of different dyes. To elucidate the photocatalytic reaction mechanism for the CdS/TiO{sub 2} nanocomposites, controlled experiments were performed by adding different radical scavengers. - Graphical abstract: CdS/TiO{sub 2} nanocomposites were prepared using CTAB by CBD combined with MAHS method. In addition, with increasing microwave irradiation time, the morphology of CdS/TiO{sub 2} changed from popcorn-like to wedge-like structure. - Highlights: • The CdS/TiO{sub 2} was prepared by CBD combined with MAHS two-step method under CTAB. • The morphologies of as-samples were different with the time of

  5. Microwave-assisted hydrothermal synthesis of Cu/Cu2O hollow spheres with enhanced photocatalytic and gas sensing activities at room temperature.

    PubMed

    Zou, Xinwei; Fan, Huiqing; Tian, Yuming; Zhang, Mingang; Yan, Xiaoyan

    2015-05-01

    Cu/Cu2O nano-heterostructure hollow spheres with a submicron diameter (200-500 nm) were prepared by a microwave-assisted hydrothermal method using Cu(OAc)2·H2O, PVP and ascorbic acid solution as the precursors. The morphology of the products could evolve with the hydrothermal time from solid spheres to thick-shell hollow spheres, then to thin-shell hollow spheres, and finally to nanoparticles. Moreover, the content of Cu in the products could be controlled by adjusting the hydrothermal time. The spontaneous forming of the hollow structure spheres was found to result from the Ostwald ripening effect during the low temperature (100 °C) hydrothermal reaction process. The photocatalytic degradation activities on MO under visible-light irradiation and the gas sensing activities toward the oxidizing NO2 gas of different Cu/Cu2O nano-heterostructure hollow spheres were investigated. As a result, the Cu/Cu2O nano-heterostructure hollow spheres obtained at the hydrothermal time of 30 min, with a rough/porous thin-shell structure and a Cu content of about 10.5 wt%, exhibited the best photocatalytic and gas sensing performances compared with others. PMID:25820327

  6. Hydrothermal synthesis and afterglow luminescence properties of hollow SnO{sub 2}:Sm{sup 3+},Zr{sup 4+} spheres for potential application in drug delivery

    SciTech Connect

    Feng, Pengfei; Zhang, Jiachi Qin, Qingsong; Hu, Rui; Wang, Yuhua

    2014-02-01

    Highlights: • We designed a novel afterglow labeling material SnO{sub 2}:Sm{sup 3+},Zr{sup 4+} for the first time. • Hollow SnO{sub 2}:Sm{sup 3+},Zr{sup 4+} spheres with afterglow were prepared by hydrothermal method. • Hollow SnO{sub 2}:Sm{sup 3+},Zr{sup 4+} is a potential afterglow labeling medium for drug delivery. - Abstract: A novel afterglow labeling material SnO{sub 2}:Sm{sup 3+},Zr{sup 4+} with hollow sphere shape and intense afterglow luminescence is prepared by hydrothermal method at 180 °C for the first time. The morphology and the sphere growth process of this material are investigated by scanning electron microscopy in detail. The afterglow measurement shows that this hydrothermal obtained material exhibits obvious red afterglow luminescence (550–700 nm) of Sm{sup 3+} which can last for 542 s (0.32 mcd/m{sup 2}). The depth of traps in this hydrothermal obtained material is calculated to be as shallow as 0.58 eV. The results demonstrate that although it is necessary to further improve the afterglow performance of the hydrothermal derived hollow SnO{sub 2}:Sm{sup 3+},Zr{sup 4+} spheres, it still can be regarded as a potential afterglow labeling medium for drug delivery.

  7. Hydrothermal synthesis of potassium molybdenum oxide bronzes: structure-inheriting solid-state route to blue bronze and dissolution/deposition route to red bronze

    SciTech Connect

    Eda, Kazuo . E-mail: eda@kobe-u.ac.jp; Chin, Kin; Sotani, Noriyuki; Stanley Whittingham, M.

    2005-01-15

    The hydrothermal syntheses of the alkali metal molybdenum bronzes from starting solids (H{sub x}MoO{sub 3}) with structural affinities to the desired products were investigated. Single-phase potassium blue and red bronzes were prepared by the hydrothermal treatments at around 430K, and characterized by powder X-ray diffraction, IR spectroscopy, and SEM. The formation processes of these two bronzes during the hydrothermal treatments were found to differ. The blue bronze was formed by a structure-inheriting solid-state route from H{sub x}MoO{sub 3} with x<0.3, whereas the red bronze was formed for x>0.3 through a solution dissolution/deposition route via the formation of MoO{sub 3}+MoO{sub 2}.

  8. Synthesis of lead-free piezoelectric powders by ultrasonic-assisted hydrothermal method and properties of sintered (K0.48Na0.52)NBO3 ceramics.

    PubMed

    Isobe, Gaku; Maeda, Takafumi; Bornmann, Peter; Hemsel, Tobias; Morita, Takeshi

    2014-02-01

    (K,Na)NbO3 ceramics have attracted much attention as lead-free piezoelectric materials with high piezoelectric properties. High-quality (K,Na)NbO3 ceramics can be sintered using KNbO3 and NaNbO3 powders synthesized by a hydrothermal method. In this study, to enhance the quality factor of the ceramics, high-power ultrasonic irradiation was employed during the hydrothermal method, which led to a reduction in the particle size of the resultant powders. PMID:24474129

  9. Chemical environments of submarine hydrothermal systems. [supporting abiogenetic theory

    NASA Technical Reports Server (NTRS)

    Shock, Everett L.

    1992-01-01

    The paper synthesizes diverse information about the inorganic geochemistry of submarine hydrothermal systems, provides a description of the fundamental physical and chemical properties of these systems, and examines the implications of high-temperature, fluid-driven processes for organic synthesis. Emphasis is on a few general features, i.e., pressure, temperature, oxidation states, fluid composition, and mineral alteration, because these features will control whether organic synthesis can occur in hydrothermal systems.

  10. In situ synthesis and hydrothermal crystallization of nanoanatase TiO2 -SiO2 coating on aramid fabric (HTiSiAF) for UV protection.

    PubMed

    Deng, Hui; Zhang, Hongda

    2015-10-01

    TiO2 -SiO2 thin film was prepared by sol-gel method and coated on the aramid fabric to prepare functional textiles. The aramid fabric was dipped and withdrawn in TiO2 -SiO2 gel and hydrothermal crystallization at 80(°) C, then its UV protection functionality was evaluated. The crystalline phase and the surface morphology of TiO2 -SiO2 thin film were characterized using SEM, XRD, and AFM respectively. SEM showed hydrothermal crystallization led to a homogeneous dispersion of anatase nonocrystal in TiO2 -SiO2 film, and XRD suggested the mean particle size of the formed anatase TiO2 was less than 30 nm. AFM indicated that hydrothermal treatment enhanced the crystallization of TiO2 . UV protection analysis suggested that the hydrothermally treated coated textile had a better screening property in comparison with TiO2 -SiO2 gel and native aramid fabric. PMID:26303384

  11. Hydrothermal systems and the emergence of life

    NASA Technical Reports Server (NTRS)

    Shock, E. L.

    1994-01-01

    The author reviews current thought about life originating in hyperthermophilic microorganisms. Hyperthermophiles obtain food from chemosynthesis of sulfur and have an RNA nucleotide sequence different from bacteria and eucarya. It is postulated that a hyperthermophile may be the common ancestor of all life. Current research efforts focus on the synthesis of organic compounds in hydrothermal systems.

  12. Hydrothermal systems and the emergence of life.

    PubMed

    Shock, E L

    1994-03-01

    The author reviews current thought about life originating in hyperthermophilic microorganisms. Hyperthermophiles obtain food from chemosynthesis of sulfur and have an RNA nucleotide sequence different from bacteria and eucarya. It is postulated that a hyperthermophile may be the common ancestor of all life. Current research efforts focus on the synthesis of organic compounds in hydrothermal systems. PMID:11539585

  13. Controllable hydrothermal synthesis of rutile TiO{sub 2} hollow nanorod arrays on TiCl{sub 4} pretreated Ti foil for DSSC application

    SciTech Connect

    Xi, Min; Zhang, Yulan; Long, Lizhen; Li, Xinjun

    2014-11-15

    Rutile TiO{sub 2} nanorod arrays (TNRs) were achieved by hydrothermal process on TiCl{sub 4} pretreated Ti foil. Subsequently, TNRs were hydrothermally etched in HCl solution to form hollow TiO{sub 2} nanorod arrays (H-TNRs). The TiCl{sub 4} pretreatment plays key roles in enhancement of Ti foil corrosion resistance ability and crystal nucleation introduction for TNRs growth. TNRs with desired morphology can be obtained by controlling TiCl{sub 4} concentration and the amount of tetrabutyl titanate (TTB) accordingly. TNRs with the length of ∼1.5 μm and diameter of ∼200 nm, obtained on 0.15 M TiCl{sub 4} pretreated Ti foil with 0.6 mL TTB, exhibits relatively higher photocurrent. The increased pore volume of the H-TNRs has contributed to the increased surface area which is benefit for Dye-Sensitized Solar Cells (DSSC) application. And the 180 °C-H-TNRs photoanode obtained from the 0.15-TiCl{sub 4}-TNRs sample demonstrated 128.9% enhancement of photoelectric efficiency of DSSC compared to that of the original TNR photoanode. - Graphical abstract: Rutile hollow TiO{sub 2} nanorod array photoanode obtained from original TiO{sub 2} nanorod array photoanode by hydrothermal etching demonstrates enhanced photoelectric efficiency of DSSC. - Highlights: • TiO{sub 2} nanorods are prepared via hydrothermal process on TiCl{sub 4}-pretreated Ti foil. • Hollow TiO{sub 2} nanorods are obtained by hydrothermal etching of TiO{sub 2} nanorods. • TiCl{sub 4} pretreatment plays a key role in protecting Ti foil from chemical corrosion. • Hollow TiO{sub 2} nanorods photoanode shows enhanced photoelectric efficiency for DSSC.

  14. Synthesis of ZnO nanorod–nanosheet composite via facile hydrothermal method and their photocatalytic activities under visible-light irradiation

    SciTech Connect

    Tan, Wai Kian; Abdul Razak, Khairunisak; Lockman, Zainovia; Kawamura, Go; Muto, Hiroyuki; Matsuda, Atsunori

    2014-03-15

    ZnO composite films consisting of ZnO nanorods and nanosheets were prepared by low-temperature hydrothermal processing at 80 °C on seeded glass substrates. The seed layer was coated on glass substrates by sol–gel dip-coating and pre-heated at 300 °C for 10 min prior to hydrothermal growth. The size of the grain formed after pre-heat treatment was ∼40 nm. A preferred orientation seed layer at the c-axis was obtained, which promoted vertical growth of the ZnO nanorod arrays and formation of the ZnO nanosheets. X-ray diffraction patterns and high-resolution transmission electron microscope (HR-TEM) images confirmed that the ZnO nanorods and nanosheets consist of single crystalline and polycrystalline structures, respectively. Room temperature photoluminescence spectra of the ZnO nanorod–nanosheet composite films exhibited band-edge ultraviolet (UV) and visible emission (blue and green) indicating the formation of ZnO crystals with good crystallinity and are supported by Raman scattering results. The formation of one-dimensional (1D) ZnO nanorod arrays and two-dimensional (2D) ZnO nanosheet films using seeded substrates in a single low-temperature hydrothermal step would be beneficial for realization of device applications that utilize substrates with limited temperature stability. The ZnO nanorods and nanosheets composite structure demonstrated higher photocatalytic activity during degradation of aqueous methylene blue under visible-light irradiation. -- Graphical abstract: Schematic illustration of ZnO nanorod–nanosheet composite structure formation by hydrothermal at low-temperature of 80 °C against time. Highlights: • Novel simultaneous formation of ZnO nanorods and nanosheets composite structure. • Facile single hydrothermal step formation at low-temperature. • Photoluminescence showed ultraviolet and visible emission. • Feasible application on substrates with low temperature stability. • Improved photocatalytic activity under visible

  15. Hydrothermal synthesis and characterization of the first mixed alkali borate-nitrate K{sub 3}Na[B{sub 6}O{sub 9}(OH){sub 3}]NO{sub 3}

    SciTech Connect

    Ortner, Teresa S.; Wurst, Klaus; Perfler, Lukas; Tribus, Martina; Huppertz, Hubert

    2015-01-15

    The first mixed alkali borate-nitrate K{sub 3}Na[B{sub 6}O{sub 9}(OH){sub 3}]NO{sub 3} was synthesized under hydrothermal conditions from Na{sub 2}B{sub 4}O{sub 7}·10H{sub 2}O and K{sub 2}B{sub 4}O{sub 7}·4H{sub 2}O using KNO{sub 3} as a nitrate source. The compound crystallizes in the space group Pnnm (no. 58) with the lattice parameters a=1320.8(3), b=910.7(2), and c=1232.5(3) pm (Z=4). Isolated Sechserrings formed by BO{sub 4} and BO{sub 3} groups are linked through hydrogen bridges to form a three-dimensional network. - Graphical abstract: The first mixed alkali borate-nitrate K{sub 3}Na[B{sub 6}O{sub 9}(OH){sub 3}]NO{sub 3} was synthesized under hydrothermal conditions from Na{sub 2}B{sub 4}O{sub 7}·10H{sub 2}O and K{sub 2}B{sub 4}O{sub 7}·4H{sub 2}O using KNO{sub 3} as a nitrate source. - Highlights: • The first mixed alkali borate-nitrate K{sub 3}Na[B{sub 6}O{sub 9}(OH){sub 3}]NO{sub 3} is reported. • Hydrothermal conditions (240 °C, 3d) were used for the synthesis of K{sub 3}Na[B{sub 6}O{sub 9}(OH){sub 3}]NO{sub 3}. • Borate Sechserrings are interconnected through hydrogen-bonding.

  16. Chemical environments of submarine hydrothermal systems

    NASA Technical Reports Server (NTRS)

    Shock, Everett L.

    1992-01-01

    Perhaps because black-smoker chimneys make tremendous subjects for magazine covers, the proposal that submarine hydrothermal systems were involved in the origin of life has caused many investigators to focus on the eye-catching hydrothermal vents. In much the same way that tourists rush to watch the spectacular eruptions of Old Faithful geyser with little regard for the hydrology of the Yellowstone basin, attention is focused on the spectacular, high-temperature hydrothermal vents to the near exclusion of the enormous underlying hydrothermal systems. Nevertheless, the magnitude and complexity of geologic structures, heat flow, and hydrologic parameters which characterize the geyser basins at Yellowstone also characterize submarine hydrothermal systems. However, in the submarine systems the scale can be considerably more vast. Like Old Faithful, submarine hydrothermal vents have a spectacular quality, but they are only one fascinating aspect of enormous geologic systems operating at seafloor spreading centers throughout all of the ocean basins. A critical study of the possible role of hydrothermal processes in the origin of life should include the full spectrum of probable environments. The goals of this chapter are to synthesize diverse information about the inorganic geochemistry of submarine hydrothermal systems, assemble a description of the fundamental physical and chemical attributes of these systems, and consider the implications of high-temperature, fluid-driven processes for organic synthesis. Information about submarine hydrothermal systems comes from many directions. Measurements made directly on venting fluids provide useful, but remarkably limited, clues about processes operating at depth. The oceanic crust has been drilled to approximately 2.0 km depth providing many other pieces of information, but drilling technology has not allowed the bore holes and core samples to reach the maximum depths to which aqueous fluids circulate in oceanic crust. Such

  17. Size-controlled synthesis of NiFe2O4 nanospheres via a PEG assisted hydrothermal route and their catalytic properties in oxidation of alcohols by periodic acid

    NASA Astrophysics Data System (ADS)

    Paul, Bappi; Purkayastha, Debraj Dhar; Dhar, Siddhartha Sankar

    2016-05-01

    A novel and facile approach for synthesis of spinel nickel ferrites (NiFe2O4) nanoparticles (NPs) employing homogeneous chemical precipitation followed by hydrothermal heating is reported. The synthesis involves use of tributylamine (TBA) as a hydroxylating agent in synthesis of nickel ferrites. Polyethylene glycol (PEG) 4000 was used as surfactant. As-synthesized NiFe2O4 NPs were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), N2 adsorption-desorption isotherm (BET) and vibrating sample magnetometry (VSM). The XRD pattern revealed formation of cubic face-centered NiFe2O4 and TEM image showed spherical particles of sizes 2-10 nm. These NiFe2O4 NPs were used as magnetically recoverable catalyst in oxidation of cyclic alcohols to their corresponding aldehydes by periodic acid. This eco-friendly procedure affords products in very high yield and selectivity. The reusability of the catalyst is proved to be noteworthy as the material exhibits no significant changes in its catalytic activity even after five cycles of reuse.

  18. Microwave-assisted hydrothermal synthesis of marigold-like ZnIn{sub 2}S{sub 4} microspheres and their visible light photocatalytic activity

    SciTech Connect

    Chen Zhixin; Li Danzhen; Xiao Guangcan; He Yunhui; Xu Yijun

    2012-02-15

    Marigold-like ZnIn{sub 2}S{sub 4} microspheres were synthesized by a microwave-assisted hydrothermal method with the temperature ranging from 80 to 195 Degree-Sign C. X-ray diffraction, X-ray photoelectron spectroscopy, nitrogen sorption analysis, UV-visible spectroscopy, scanning electron microscopy and transmission electron microscopy were used to characterize the products. It was found that the crystallographic structure and optical property of the products synthesized at different temperatures were almost the same. The degradation of methyl orange (MO) under the visible light irradiation has been used as a probe reaction to investigate the photocatalytic activity of as-prepared ZnIn{sub 2}S{sub 4}, which shows that the ZnIn{sub 2}S{sub 4} sample synthesized at 195 Degree-Sign C shows the best photocatalytic activity for MO degradation. In addition, the photocatalytic activities of all the samples prepared by the microwave-assisted hydrothermal method are better than those prepared by a normal hydrothermal method, which could be attributed to the formation of more defect sites during the microwave-assisted hydrothermal treatment. - Graphical abstract: Marigold-like ZnIn{sub 2}S{sub 4} microspheres were synthesized by a fast microwave-assisted hydrothermal method at 80-195 Degree-Sign C with a very short reaction time of 10 min. The as-prepared ZnIn{sub 2}S{sub 4} sample can be used as visible light photocatalyst for degradation of organic dyes. Highlights: Black-Right-Pointing-Pointer ZnIn{sub 2}S{sub 4} microspheres were synthesized by microwave-assisted hydrothermal method. Black-Right-Pointing-Pointer The crystal structure and optical property of the products were almost the same. Black-Right-Pointing-Pointer Increment of the temperature renders high surface area due to the bubbling effect. Black-Right-Pointing-Pointer The ZnIn{sub 2}S{sub 4} synthesized at 195 Degree-Sign C shows the best visible catalytic activity for MO.

  19. Hydrothermal synthesis of CuO micro-/nanostructures and their applications in the oxidative degradation of methylene blue and non-enzymatic sensing of glucose/H2O2.

    PubMed

    Prathap, M U Anu; Kaur, Balwinder; Srivastava, Rajendra

    2012-03-15

    In this paper, we report on the amino acids-/citric acid-/tartaric acid-assisted morphologically controlled hydrothermal synthesis of micro-/nanostructured crystalline copper oxides (CuO). These oxides were characterized by means of X-ray diffraction, nitrogen sorption, scanning electron microscopy, Fourier transform infrared, and UV-visible spectroscopy. The surface area of metal oxides depends on the amino acid used in the synthesis. The formation mechanisms were proposed based on the experimental results, which show that amino acid/citric acid/tartaric acid and hydrothermal time play an important role in tuning the morphology and structure of CuO. The catalytic activity of as-synthesized CuO was demonstrated by catalytic oxidation of methylene blue in the presence of hydrogen peroxide (H(2)O(2)). CuO synthesized using tyrosine was found to be the best catalyst compared to a variety of CuO synthesized in this study. CuO (synthesized in this study)-modified electrodes were used for the construction of non-enzymatic sensors, which displayed excellent electrocatalytic response for the detection of H(2)O(2) and glucose compared to conventional CuO. The high electrocatalytic response observed for the CuO synthesized using tyrosine can be correlated with the large surface area, which enhances the accessibility of H(2)O(2)/glucose molecule to the active site that results in high observed current. The methodology adopted in the present study provides a new platform for the fabrication of CuO-based high-performance glucose and other biosensors. PMID:22284573

  20. Synthesis of nanostructured and microstructured ZnO and Zn(OH)2 on activated carbon cloth by hydrothermal and microwave-assisted chemical bath deposition methods

    NASA Astrophysics Data System (ADS)

    Mosayebi, Elham; Azizian, Saeid; Hajian, Ali

    2015-05-01

    Nanostructured and microstructured ZnO and Zn(OH)2 loaded on activated carbon cloth were synthesized by microwave-assisted chemical bath deposition and hydrothermal methods. By hydrothermal method the deposited sample on carbon fiber is pure ZnO with dandelion-like nanostructures. By microwave-assisted chemical bath method the structure and composition of deposited sample depends on solution pH. At pH = 9.8 the deposited sample on carbon fiber is pure ZnO with flower-like microstructure; but at pH = 10.8 the sample is a mixture of ZnO and Zn(OH)2 with flower-like and rhombic microstructures, respectively. The mechanism of crystal grow by microwave-assisted chemical bath method was investigated by SEM method at both pH.

  1. Hydrothermal synthesis of a 3D double-sided comb-like ZnO nanostructure and its growth mechanism analysis.

    PubMed

    Li, Wenqiang; Gao, Shiyong; Li, Lin; Jiao, Shujie; Li, Hongtao; Wang, Jinzhong; Yu, Qingjiang; Zhang, Yong; Wang, Dongbo; Zhao, Liancheng

    2016-07-01

    Self-assembly of two-dimensional (2D) nanosheets and one-dimensional (1D) nanorods into three-dimensional (3D) double-sided comb-like ZnO nanostructures has been successfully performed via a simple one-step hydrothermal method on Si and ITO substrates. It is found that the thickness of the ZnO seeds plays a vital role in the formation of 3D double-sided comb-like ZnO. PMID:27279279

  2. Synthesis of high intrinsic loss power aqueous ferrofluids of iron oxide nanoparticles by citric acid-assisted hydrothermal-reduction route

    SciTech Connect

    Behdadfar, Behshid; Kermanpur, Ahmad; Sadeghi-Aliabadi, Hojjat; Morales, Maria del Puerto; Mozaffari, Morteza

    2012-03-15

    Monodispersed aqueous ferrofluids of iron oxide nanoparticle were synthesized by hydrothermal-reduction route. They were characterized by X-ray diffraction analysis, Fourier transform infrared spectroscopy, scanning and transmission electron microscopy and dynamic light scattering. The results showed that certain concentrations of citric acid (CA) are required to obtain only magnetic iron oxides with mean particle sizes around 8 nm. CA acts as a modulator and reducing agent in iron oxide formation which controls nanoparticle size. The XRD, magnetic and heating measurements showed that the temperature and time of hydrothermal reaction can affect the magnetic properties of obtained ferrofluids. The synthesized ferrofluids were stable at pH 7. Their mean hydrodynamic size was around 80 nm with polydispersity index (PDI) of 0.158. The calculated intrinsic loss power (ILP) was 9.4 nHm{sup 2}/kg. So this clean and cheap route is an efficient way to synthesize high ILP aqueous ferrofluids applicable in magnetic hyperthermia. - Graphical abstract: Monodispersed aqueous ferrofluids of iron oxide nanoparticles were synthesized by hydrothermal-reduction method with citric acid as reductant which is an efficient way to synthesize aqueous ferrofluids applicable in magnetic hyperthermia. Highlights: Black-Right-Pointing-Pointer Aqueous iron oxide ferrofluids were synthesized by hydrothermal-reduction route. Black-Right-Pointing-Pointer Citric acid acted as reducing agent and surfactant in the route. Black-Right-Pointing-Pointer This is a facile, low energy and environmental friendly route. Black-Right-Pointing-Pointer The aqueous iron oxide ferrofluids were monodispersed and stable at pH of 7. Black-Right-Pointing-Pointer The calculated intrinsic loss power of the synthesized ferrofluids was very high.

  3. In situ hydrothermal synthesis of a novel hierarchically porous TS-1/modified-diatomite composite for methylene blue (MB) removal by the synergistic effect of adsorption and photocatalysis.

    PubMed

    Yuan, Weiwei; Yuan, Peng; Liu, Dong; Yu, Wenbin; Laipan, Minwang; Deng, Liangliang; Chen, Fanrong

    2016-01-15

    Hierarchically porous TS-1/modified-diatomite composites with high removal efficiency for methylene blue (MB) were prepared via a facile in situ hydrothermal route. The surface charge state of the diatomite was modified to enhance the electrostatic interactions, followed by in situ hydrothermal coating with TS-1 nanoparticles. The zeolite loading amount in the composites could be adjusted by changing the hydrothermal time. The highest specific surface area and micropore volume of the obtained composites were 521.3m(2)/g and 0.254cm(3)/g, respectively, with an optimized zeolite loading amount of 96.8%. Based on the synergistic effect of efficient adsorption and photocatalysis resulting from the newly formed hierarchically porous structure and improved dispersion of TS-1 nanoparticles onto diatomite, the composites' removal efficiency for MB reached 99.1% after 2h of photocatalytic reaction, even higher than that observed using pure TS-1 nanoparticles. Moreover, the superior MB removal kinetics of the composites were well represented by a pseudo-first-order model, with a rate constant (5.28×10(-2)min(-1)) more than twice as high as that of pure TS-1 nanoparticles (2.43×10(-2)min(-1)). The significant dye removal performance of this novel TS-1/modified-diatomite composite indicates that it is a promising candidate for use in waste water treatment. PMID:26454378

  4. Template-free synthesis of ZnWO{sub 4} powders via hydrothermal process in a wide pH range

    SciTech Connect

    Hojamberdiev, Mirabbos; Zhu, Gangqiang; Xu, Yunhua

    2010-12-15

    ZnWO{sub 4} powders with different morphologies were fabricated through a template-free hydrothermal method at 180 {sup o}C for 8 h in a wide pH range. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-visible and luminescence spectrophotometers were applied to study the effects of pH values on crystallinity, morphology, optical and luminescence properties. The XRD results showed that the WO{sub 3} + ZnWO{sub 4}, ZnWO{sub 4}, and ZnO phases could form after hydrothermal processing at 180 {sup o}C for 8 h with the pH values of 1, 3-11, and 13, respectively. The SEM and TEM observation revealed that the morphological transformation of ZnWO{sub 4} powders occurred with an increase in pH values as follows: star anise-, peony-, and desert rose-like microstructures and soya bean- and rod-like nanostructures. The highest luminescence intensity was found to be in sample consisting of star anise-like crystallites among all the samples due to the presence of larger particles with high crystallinity resulted from the favorable pH under the current hydrothermal conditions.

  5. Hydrothermal systems as environments for the emergence of life

    NASA Technical Reports Server (NTRS)

    Shock, E. L.

    1996-01-01

    Analysis of the chemical disequilibrium provided by the mixing of hydrothermal fluids and seawater in present-day systems indicates that organic synthesis from CO2 or carbonic acid is thermodynamically favoured in the conditions in which hyperthermophilic microorganisms are known to live. These organisms lower the Gibbs free energy of the chemical mixture by synthesizing many of the components of their cells. Primary productivity is enormous in hydrothermal systems because it depends only on catalysis of thermodynamically favourable, exergonic reactions. It follows that hydrothermal systems may be the most favourable environments for life on Earth. This fact makes hydrothermal systems logical candidates for the location of the emergence of life, a speculation that is supported by genetic evidence that modern hyperthermophilic organisms are closer to a common ancestor than any other forms of life. The presence of hydrothermal systems on the early Earth would correspond to the presence of liquid water. Evidence that hydrothermal systems existed early in the history of Mars raises the possibility that life may have emerged on Mars as well. Redox reactions between water and rock establish the potential for organic synthesis in and around hydrothermal systems. Therefore, the single most important parameter for modelling the geochemical emergence of life on the early Earth or Mars is the composition of the rock which hosts the hydrothermal system.

  6. Controllable synthesis, shape evolution, and luminescence properties of uniform and well-dispersed NaEuF{sub 4} microcrystals through hydrothermal route

    SciTech Connect

    Xu, Zhenhe Zhao, Qian; Ding, Fu; Sun, Yaguang

    2013-08-01

    Graphical abstract: Sodium europium fluorides NaEuF{sub 4} microcrystals have been prepared via a facile hydrothermal route. The possible growth mechanism and the luminescent properties of the as-prepared microcrystals have been discussed. - Highlights: • Sodium europium fluorides NaEuF{sub 4} microspheres were prepared by a facile hydrothermal route. • The as-prepared samples NaEuF{sub 4} and EuF{sub 3} exhibit respective red or orange-red emissions. • These finding may find potential applications in the fields of color display, UV laser and biomedicine. - Abstract: Sodium europium fluorides NaEuF{sub 4} microcrystals with uniform and well-dispersed shapes and dimensions have been prepared via a facile hydrothermal route using Na{sub 3}Cit as the chelating ligand and shape modifier. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected-area electron diffraction (SAED), energy-dispersive X-ray (EDX) and photoluminescence spectra (PL) were taken to characterize the samples. A series of controlled experiments reveal that the trisodium citrate (Na{sub 3}Cit) content, pH value of the initial solution, and reaction time have an indispensable role on the phase, size, and morphology of the as-prepared microcrystals. Based on the experimental results, the possible growth mechanism of the microcrystals prepared under different conditions was proposed. Moreover, we systematically investigated the luminescent properties of the as-prepared microcrystals with different morphologies obtained under different amounts of Na{sub 3}Cit, which have potential application in the fields of color display, UV laser and biomedicine.

  7. A facile one-pot hydrothermal synthesis of β-MnO{sub 2} nanopincers and their catalytic degradation of methylene blue

    SciTech Connect

    Cheng, Gao; Yu, Lin Lin, Ting; Yang, Runnong; Sun, Ming; Lan, Bang; Yang, Lili; Deng, Fangze

    2014-09-15

    Branched β-MnO{sub 2} bipods with novel nanopincer morphology were prepared by a facile one-pot hydrothermal method via a redox reaction between NaClO{sub 3} and MnSO{sub 4} in sulfuric acid solution without using any surfactants or templates. The products were characterized in detail by various techniques including X-ray powder diffraction, Raman spectroscopy, X-ray photoelectron spectroscopy, surface area analyzer, field emission scanning electron microscopy and transmission electron microscopy. Results show that the obtained β-MnO{sub 2} nanopincers consist of two sharp nanorods with a diameter of 100–200 nm and a length of 1–2 μm. The concentration of H{sub 2}SO{sub 4} solution plays an important role in controlling the crystal phase and morphology of the final product. A possible formation mechanism for the β-MnO{sub 2} nanopincers was proposed. Moreover, these β-MnO{sub 2} nanostructures exhibited better catalytic performance than the commercial MnO{sub 2} particles to decompose methyl blue (MB) in the presence of H{sub 2}O{sub 2}. - Graphical abstract: Branched β-MnO{sub 2} bipods with novel nanopincer morphology were prepared by a facile one-pot hydrothermal method through oxidizing MnSO{sub 4} with NaClO{sub 3} in H2SO{sub 4} condition without using any surfactants or templates. - Highlights: {sup •} Branched β-MnO{sub 2} nanopincers were prepared by a facile one-pot hydrothermal method. {sup •} Morphology and crystal phase of MnO{sub 2} were controlled by the H{sub 2}SO{sub 4} concentration. {sup •} A possible formation mechanism for the obtained β-MnO{sub 2} nanopincers was proposed. {sup •} The products showed great catalytic performance in degradation of methylene blue.

  8. Selective hydrothermal synthesis of BiOBr microflowers and Bi{sub 2}O{sub 3} shuttles with concave surfaces

    SciTech Connect

    Xiao Peipei; Zhu Lingling; Zhu Yongchun; Qian Yitai

    2011-06-15

    Through controlling the amount of NaOH added, BiOBr and Bi{sub 2}O{sub 3} with different shapes were hydrothermally synthesized in the reaction system of Bi(NO{sub 3}){sub 3}-hexadecyl trimethyl ammonium bromide (CTAB)-NaOH. As 8 mmol of NaOH was added, BiOBr microflowers constructed of nanoflakes were synthesized. The thickness of these single-crystal nanoflakes was about 20 nm. In the similar condition, when the amount of NaOH added was 28 mmol, Bi{sub 2}O{sub 3} shuttles with concave surfaces were obtained. The length of these shuttles was 100 {mu}m and the diameter at the middle of these shuttles was 50 {mu}m. The photocatalytic activity of as-prepared BiOBr microflowers was evaluated by the degradation of methyl orange (MO) under visible-light irradiation ({lambda}>420 nm), which was up to 96% within 90 min. - Graphical abstract: Through controlling the amount of NaOH added, BiOBr microflowers and Bi{sub 2}O{sub 3} shuttles with concave surfaces were hydrothermally synthesized in the reaction system of Bi(NO{sub 3}){sub 3}-hexadecyl trimethyl ammonium bromide (CTAB)-NaOH. Highlights: > BiOBr microflowers constructed of nanoflakes were synthesized hydrothermally. > Bi{sub 2}O{sub 3} shuttles with concave surfaces were also synthesized. > Their formation mechanisms were studied based on the experimental results. > The photocatalytic activity of BiOBr microflowers was evaluated under visible-light irradiation.

  9. Hierarchical Na-doped cubic ZrO{sub 2} synthesis by a simple hydrothermal route and its application in biodiesel production

    SciTech Connect

    Lara-García, Hugo A.; Romero-Ibarra, Issis C.; Pfeiffer, Heriberto

    2014-10-15

    Hierarchical growth of cubic ZrO{sub 2} phase was successfully synthesized via a simple hydrothermal process in the presence of different surfactants (cationic, non-ionic and anionic) and sodium hydroxide. The structural and microstructural characterizations of different ZrO{sub 2} powders were performed using various techniques, such as X-ray diffraction, transmission electron microscopy, N{sub 2} adsorption–desorption, scanning electron microscopy and infrared. Results indicated that sodium addition stabilized the cubic ZrO{sub 2} phase by a Na-doping process, independently of the surfactant used. In contrast, microstructural characteristics varied as a function of the surfactant and sodium presence. In addition, water vapor (H{sub 2}O) and carbon dioxide (CO{sub 2}) sorption properties were evaluated on ZrO{sub 2} samples. Results evidenced that sample surface reactivity changed as a function of the sodium content. Finally, this surface reactivity was evaluated on the biodiesel transesterification reaction using the different synthesized samples, obtaining yields of 93%. - Graphical abstract: Hierarchical growth of cubic Na-ZrO{sub 2} phase was synthesized by hydrothermal processes in the presence of surfactants and sodium. Sodium addition stabilized the cubic phase by a Na-doping process, while the microstructural characteristics varied with surfactants. Finally, this surface reactivity was evaluated on the biodiesel transesterification reaction. - Highlights: • Cubic-ZrO{sub 2} phase was synthesized via a simple hydrothermal process. • ZrO{sub 2} structure and microstructures changed as a function of the surfactant. • Cubic-ZrO{sub 2} phase was evaluated on the biodiesel transesterification reaction.

  10. Synthesis and in-depth analysis of highly ordered yttrium doped hydroxyapatite nanorods prepared by hydrothermal method and its mechanical analysis

    SciTech Connect

    Nathanael, A. Joseph; Mangalaraj, D.; Hong, S.I.; Masuda, Y.

    2011-12-15

    In this study, undoped and yttrium (Y) doped nanocrystalline hydroxyapatite crystals were synthesized by the hydrothermal method at 180 Degree-Sign C for 24 h. Highly ordered and oriented hydroxyapatite (HAp) nanorods were prepared by yttrium doping and their nanostructure and physical properties were compared with those of undoped HAp rods. FESEM images showed that the doping with Y ions reduced the diameter (from 25 nm to 15 nm) and increased the length (from 95 nm to 115 nm) of the synthesized rods. The aspect ratio of the undoped and Y-doped nanorods were calculated to be 4.303 (SD = 0.0959) and 7.61 (SD = 0.0355), respectively. Specific surface area (SSA) analysis showed that SSA also increased from 66.74 m{sup 2}/g to 68.57 m{sup 2}/g with the addition of yttrium. Y-doped HAp nanorod reinforced HMWPE composites displayed the better mechanical performance than those reinforced with pure HAp nanorods. The possible strengthening of nanorods and the increase of SSA due to the reduction in the size of nanorods in the presence of yttrium may have contributed to the strengthening of Y-doped HAp/HMWPE composites. - Graphical Abstract: Highly ordered and oriented yttrium doped hydroxyapatite (HAp) nanorods were prepared by hydrothermal method. For undoped HAp the average length of the nanorod is 95 nm with mean diameter of 24 nm and for a Y doped nanorod the average length is {approx} 115 nm and the mean diameter is 15 nm. Mechanical analysis was carried out by polymer/nanoparticle composite method. Highlights: Black-Right-Pointing-Pointer Yttrium doped hydroxyapatite nanorods were prepared by hydrothermal method. Black-Right-Pointing-Pointer The nanorods have highly uniform size distribution. Black-Right-Pointing-Pointer Yttrium substitution and nanostructure formation was confirmed by careful analysis. Black-Right-Pointing-Pointer Mechanical strength was analyzed by polymer nanoparticle reinforcement method.

  11. Hydrothermal synthesis and characterization of the first mixed alkali borate-nitrate K3Na[B6O9(OH)3]NO3

    NASA Astrophysics Data System (ADS)

    Ortner, Teresa S.; Wurst, Klaus; Perfler, Lukas; Tribus, Martina; Huppertz, Hubert

    2015-01-01

    The first mixed alkali borate-nitrate K3Na[B6O9(OH)3]NO3 was synthesized under hydrothermal conditions from Na2B4O7·10H2O and K2B4O7·4H2O using KNO3 as a nitrate source. The compound crystallizes in the space group Pnnm (no. 58) with the lattice parameters a=1320.8(3), b=910.7(2), and c=1232.5(3) pm (Z=4). Isolated Sechserrings formed by BO4 and BO3 groups are linked through hydrogen bridges to form a three-dimensional network.

  12. A new acid-base indicator containing complex: Hydrothermal synthesis, crystal structure and properties of [Cd(en)2(H2O)2](MO)2

    NASA Astrophysics Data System (ADS)

    Ma, Kui-Rong; Shi, Jing; Zhang, Dao-Jun; Xu, Jia-Ning

    2012-04-01

    The first example of cadmium complex containing methyl orange [MO, (CH3)2NC6H4N = NC6H4SO3Na], formulated as [Cd(en)2(H2O)2](MO)21 (en = ethylenediamine) was synthesized hydrothermally and characterized by single-crystal X-ray diffraction, IR, XRD, elemental analysis and Raman spectroscopic analysis. Compound 1 display a two-dimensional supramolecular layer structure with ladder-like supramolecular chain by X-ray crystallographic analysis. MO anion immobilized by H-bonds, as acid-base indicator, shows a similar behavior in comparison with its solution counterpart in terms of response to pH.

  13. Series of uranyl-4,4'-biphenyldicarboxylates and an occurrence of a cation-cation interaction: hydrothermal synthesis and in situ Raman studies.

    PubMed

    Cantos, Paula M; Jouffret, Laurent J; Wilson, Richard E; Burns, Peter C; Cahill, Christopher L

    2013-08-19

    Three uranium(VI)-bearing materials were synthesized hydrothermally using the organic ligand 4,4'-biphenyldicarboxylic acid: (UO2)(C14O4H8) (1); [(UO2)2(C14O4H8)2(OH)]·(NH4)(H2O) (2); (UO2)2(C14O4H8)(OH)2 (3). Compound 1 was formed after 1 day at 180 °C in an acidic environment (pH(i) = 4.03), and compounds 2 and 3 coformed after 3 days under basic conditions (pH(i) = 7.95). Coformation of all three compounds was observed at higher pH(i) (9.00). Ex situ Raman spectra of single crystals of 1-3 were collected and analyzed for signature peaks. In situ hydrothermal Raman data were also obtained and compared to the ex situ Raman spectra of the title compounds in an effort to acquire formation mechanism details. At pH(i) = 4.00, the formation of 1 was suggested by in situ Raman spectra. At an increased pH(i) (7.90), the in situ data implied the formation of compounds 1 and 3. The most basic conditions (pH(i) = 9.00) yielded a complex mixture of phases consistent with that of increased uranyl hydrolysis. PMID:23909845

  14. Hydrothermal synthesis, characterization and luminescent properties of GdPO{sub 4}·H{sub 2}O:Tb{sup 3+} nanorods and nanobundles

    SciTech Connect

    Song, Hejuan Zhou, Liqun Li, Ling; Hong, Fei; Luo, Xinru

    2013-12-15

    Graphical abstract: - Highlights: • The GdPO{sub 4}·H{sub 2}O:Tb{sup 3+} nanocrystals have been synthesized via a hydrothermal method. • The formation mechanisms of the nanorods and nanobundles were put forward. • The luminescent intensities are associated with the morphologies and sizes. - Abstract: In this paper, the Tb{sup 3+}-doped GdPO{sub 4}·H{sub 2}O nanorods and nanobundles have been synthesized by the hydrothermal method with and without glycine, respectively. The X-ray powder diffraction (XRD), thermogravimetric and differential thermal analysis (TG–DTA), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), energy-dispersive spectra (EDS) and photoluminescence (PL) were employed to characterize the as-obtained products. It was found that the addition of glycine and the pH value have crucial influences on the formation of the resulting morphologies and sizes. The possible formation mechanisms for GdPO{sub 4}·H{sub 2}O:Tb{sup 3+} nanorods and nanobundles were put forward. A detailed investigation on the photoluminescence of GdPO{sub 4}·H{sub 2}O:Tb{sup 3+} different samples revealed that the luminescent properties of products are strongly correlated with the morphologies, sizes, coordination environment and crystal field symmetry.

  15. One-Pot Hydrothermal Synthesis of LiMn2O4 Cathode Material with Excellent High-Rate and Cycling Properties

    NASA Astrophysics Data System (ADS)

    Jiang, Qianqian; Wang, Xingyao; Zhang, Han

    2016-08-01

    The spinel LiMn2O4 was prepared by a one-step hydrothermal method using acetone as the reductant under different hydrothermal temperatures. X-ray diffraction and scanning electron microscopy analysis indicated that optimal LiMn2O4 particles (LMO-120) were synthesized at the temperature of 120°C and the particles were well distributed and about 410 nm in size. Electrochemical performance showed that the as-prepared LiMn2O4 particles exhibited a higher initial discharge capacity than commercial LiMn2O4 (131.5 mAh g-1 versus 115.6 mAh g-1 at 0.2 C). An excellent discharge capacity retention rate of 94.07% was observed after 60 charge-discharge cycles. On the other hand, when cycled at the high rate of 1 C, the optimal LiMn2O4 in this work showed a high discharge capacity of 107.5 mAh g-1 in contrast to only 92.3 mAh g-1 of the commercial LiMn2O4. These results indicate that LMO-120 showed excellent electrochemical performance, especially the prolonged cycling life and high-rate performance, which suggested that this spinel LiMn2O4 has promise for practical application as a high-rate cathode material for lithium ion batteries.

  16. Synthesis of BiFeO3 thin films on single-terminated Nb : SrTiO3 (111) substrates by intermittent microwave assisted hydrothermal method

    NASA Astrophysics Data System (ADS)

    Velasco-Davalos, Ivan; Ambriz-Vargas, Fabian; Kolhatkar, Gitanjali; Thomas, Reji; Ruediger, Andreas

    2016-06-01

    We report on a simple and fast procedure to create arrays of atomically flat terraces on single crystal SrTiO3 (111) substrates and the deposition of ferroelectric BiFeO3 thin films on such single-terminated surfaces. A microwave-assisted hydrothermal method in deionized water and ammonia solution selectively removes either (SrO3)4- or Ti4+ layers to ensure the same chemical termination on all terraces. Measured step heights of 0.225 nm (d111) and uniform contrast in the phase image of the terraces confirm the single termination in pure and Nb doped SrTiO3 single crystal substrates. Multiferroic BiFeO3 thin films were then deposited by the same microwave assisted hydrothermal process on Nb : SrTiO3 (111) substrates. Bi(NO3)3 and Fe(NO3)3 along with KOH served as the precursors solution. Ferroelectric behavior of the BiFeO3 films on Nb : SrTiO3 (100) substrates was verified by piezoresponse force microscopy.

  17. Controllable hydrothermal synthesis of rutile TiO2 hollow nanorod arrays on TiCl4 pretreated Ti foil for DSSC application

    NASA Astrophysics Data System (ADS)

    Xi, Min; Zhang, Yulan; Long, Lizhen; Li, Xinjun

    2014-11-01

    Rutile TiO2 nanorod arrays (TNRs) were achieved by hydrothermal process on TiCl4 pretreated Ti foil. Subsequently, TNRs were hydrothermally etched in HCl solution to form hollow TiO2 nanorod arrays (H-TNRs). The TiCl4 pretreatment plays key roles in enhancement of Ti foil corrosion resistance ability and crystal nucleation introduction for TNRs growth. TNRs with desired morphology can be obtained by controlling TiCl4 concentration and the amount of tetrabutyl titanate (TTB) accordingly. TNRs with the length of ~1.5 μm and diameter of ~200 nm, obtained on 0.15 M TiCl4 pretreated Ti foil with 0.6 mL TTB, exhibits relatively higher photocurrent. The increased pore volume of the H-TNRs has contributed to the increased surface area which is benefit for Dye-Sensitized Solar Cells (DSSC) application. And the 180 °C-H-TNRs photoanode obtained from the 0.15-TiCl4-TNRs sample demonstrated 128.9% enhancement of photoelectric efficiency of DSSC compared to that of the original TNR photoanode.

  18. Morphology-controlled synthesis of Co{sub 3}O{sub 4} by one step template-free hydrothermal method

    SciTech Connect

    Zhou, Keqing; Liu, Jiajia; Wen, Panyue; Hu, Yuan Gui, Zhou

    2015-07-15

    Highlights: • Co{sub 3}O{sub 4} crystals had been synthesized by one step template-free hydrothermal method. • The H{sub 2}O{sub 2} plays a crucial role in morphological control of Co{sub 3}O{sub 4} nanostructures. • The morphology has significant effect on the optical property of Co{sub 3}O{sub 4}. - Abstract: We had developed a facile synthetic route of Co{sub 3}O{sub 4} crystals with different morphologies via one step template-free hydrothermal method. The phase and composition of the Co{sub 3}O{sub 4} were investigated by X-ray powder diffraction and Raman spectrum. The morphology and structure of the synthesized samples were characterized by scanning electron microscopy and transmission electron microscopy. The H{sub 2}O{sub 2} played a crucial role in morphological control of Co{sub 3}O{sub 4} nanostructures. It only obtained Co-based precursor in the absence of H{sub 2}O{sub 2}. On the contrary, the Co{sub 3}O{sub 4} with different morphologies including nanoparticles, nano-discs and well-defined octahedral nanostructures were synthesized in the presence of H{sub 2}O{sub 2}. In addition, the optical property of the obtained Co{sub 3}O{sub 4} samples was investigated by UV–vis spectra.

  19. Hydrothermal synthesis of mesoporous VO{sub 2}·½(H{sub 2}O) nanosheets and study of their electrical properties

    SciTech Connect

    Soltane, L.; Sediri, F.; Gharbi, N.

    2012-07-15

    Highlights: ► Sheet-like nanocrystalline VO{sub 2}·½(H{sub 2}O) was synthesized by a hydrothermal route. ► Reaction time is key factor for structure and morphology. ► Electrical properties were also studied. ► Conductivity value goes from 75 10{sup −6} Ω{sup −1} cm{sup −1} at 298 K to 68 10{sup −5} Ω{sup −1} cm{sup −1} at 386 K. -- Abstract: Layered sheet-like nanocrystalline VO{sub 2}·½(H{sub 2}O) has been synthesized by hydrothermal process using V{sub 2}O{sub 5} as vanadium source and 2-phenylethylamine as a reducing agent and a structure-directing template. Techniques X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR) and nitrogen adsorption/desorption isotherms have been used to characterize the structure, morphology and composition of the materials. Electrical conductivity measurements showed that the as synthesized VO{sub 2}·½(H{sub 2}O) nanosheets has a conductivity value which goes from 75 × 10{sup −6} Ω{sup −1} cm{sup −1} at 298 K, to 68 10{sup −5} Ω{sup −1} cm{sup −1} at 386 K with activation energy of 0.24 eV.

  20. One-Pot Hydrothermal Synthesis of LiMn2O4 Cathode Material with Excellent High-Rate and Cycling Properties

    NASA Astrophysics Data System (ADS)

    Jiang, Qianqian; Wang, Xingyao; Zhang, Han

    2016-05-01

    The spinel LiMn2O4 was prepared by a one-step hydrothermal method using acetone as the reductant under different hydrothermal temperatures. X-ray diffraction and scanning electron microscopy analysis indicated that optimal LiMn2O4 particles (LMO-120) were synthesized at the temperature of 120°C and the particles were well distributed and about 410 nm in size. Electrochemical performance showed that the as-prepared LiMn2O4 particles exhibited a higher initial discharge capacity than commercial LiMn2O4 (131.5 mAh g-1 versus 115.6 mAh g-1 at 0.2 C). An excellent discharge capacity retention rate of 94.07% was observed after 60 charge-discharge cycles. On the other hand, when cycled at the high rate of 1 C, the optimal LiMn2O4 in this work showed a high discharge capacity of 107.5 mAh g-1 in contrast to only 92.3 mAh g-1 of the commercial LiMn2O4. These results indicate that LMO-120 showed excellent electrochemical performance, especially the prolonged cycling life and high-rate performance, which suggested that this spinel LiMn2O4 has promise for practical application as a high-rate cathode material for lithium ion batteries.

  1. One-step hydrothermal synthesis and characterization of V–Cr–O nanospheres and their excellent performance in the ammoxidation of 3,4- and 2,6-DCT

    SciTech Connect

    Xu, Longlong; Zhang, Yifu; Deng, Yuan; Zhong, Yalan; Mo, Shaobo; Cheng, Gongzhen Huang, Chi

    2013-09-01

    Graphical abstract: - Highlights: • V–Cr–O composite was synthesized by a facile one pot hydrothermal route. • The V–Cr–O composite has sphere-like morphology. • The as-obtained V–Cr–O composite has large specific surface area: 117 m{sup 2} g{sup −1}. • V–Cr–O complex was explored as the catalyst for the ammoxidation. - Abstract: Sphere-like V–Cr–O catalyst was successfully synthesized using V{sub 2}O{sub 5}, CrO{sub 3} and H{sub 2}C{sub 2}O{sub 4} solution as the starting materials by a facile one pot hydrothermal approach for the first time. The as-obtained samples were characterized by X-ray powder diffraction, X-ray photoelectron spectroscopy, energy dispersive X-ray spectrometer, hydrogen temperature programmed reduction, scanning electron microscopy and Brunauer–Emmett–Teller. The results indicated that V–Cr–O spheres with the diameter about 4 μm, consisted of lots of nanoparticles, were formed. The as-obtained V–Cr–O catalyst had large specific surface area: 117 m{sup 2} g{sup −1}. Furthermore, V–Cr–O complex was explored as the unsupported catalyst for the synthesis of 3,4- and 2,6-dichlorobenzonitrile by the ammoxidation of 3,4- and 2,6-dichlorotoluene. It was found that it had excellent performance in the ammoxidation reactions, specially, the catalytic temperature was decreased to about 320 °C, which was much lower than the previous reports (380–420 °C)

  2. Template-free synthesis of CdS hollow nanospheres based on an ionic liquid assisted hydrothermal process and their application in photocatalysis

    SciTech Connect

    Li Xinping; Gao Yanan; Yu Li; Zheng Liqiang

    2010-06-15

    Polycrystalline CdS hollow nanospheres with diameter of about 130 nm have been successfully synthesized in high yield by an ionic liquid (IL) assisted template-free hydrothermal method for the first time. Both the molar ratios of Cd/S precursor in the solution and the reaction temperature play important roles in the formation of the CdS hollow nanospheres. The concentrations of capping agent hexamethylenetetramine (HMT) and polyvinylpyrrolidone (PVP) are also crucial for the morphology and size of the final product. IL was found to be a key component in the formation of CdS hollow structures, because solid spheres were obtained in the absence of IL. A subsequent growth mechanism of hollow interior by localized Ostwald ripening process has been further discussed. Such hollow structures show high photocatalytic ability in the photodegradation of methylene blue. - Graphical abstract: TEM images of typical as-prepared CdS hollow nanospheres.

  3. Hydrothermal Synthesis and Luminescence Properties of Eu²⁺- and Eu³⁺-Doped SrAIF₅ Nanorods.

    PubMed

    Zhang, Wei; Hua, Ruinian; Zhao, Jun; Tang, Dongxin; Zhao, Xin; Na, Liyan; Zhang, Jinsu; Chen, Baojiu

    2016-01-01

    Eu²⁺- and Eu³⁺-doped SrAIF₅ nanorods were synthesized via a hydrothermal process. The crystal structure and morphology of the final products were characterized by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM). The prepared nanorods' diameters range from 40 to 50 nm, and lengths range from 400 nm to 2 µm along with the doped concentration of rare earth. The f-f transitions of Eu²⁺ can be observed in the SrAlF₅:Eu²⁺ nanorods at room temperature, and the photo-luminescent (PL) properties of SrAlF₅:Eu³⁺ nanorods are also described. PMID:27398485

  4. One-Step Hydrothermal Synthesis of Butanetetracarboxylic Acid-Coated NaYF₄:Yb³⁺, Er³⁺ Upconversion Phosphors with Enhancement Upconversion Luminescence.

    PubMed

    Zhang, Liming; Mao, Lanlan; Lu, Zhuoxuan; Deng, Yan; He, Nongyue

    2016-01-01

    Butanetetracarboxylic acid (BTCA)/NaYF₄:Yb³⁺, Er³⁺ upconversion phosphors have been successfully synthesized by a one-step hydrothermal method. The SEM and XRD results show the as-prepared phosphors exhibit main hexagonal lattice structures and uniform morphologies. FT-IR spectra confirm that the surface of as-prepared phosphors is inherently modified with the carboxyl groups. Under the excitation of 980 nm, it has been observed that BTCA/NaYF₄:Yb³⁺, Er³⁺ upconversion phosphors have a higher upconversion luminescence efficiency than that coated with citrate, ethylenediamine tetraacetic acid (EDTA), or polyacrylic acid (PAA). These results indicate that the BTCA/NaYF₄:Yb³⁺, Er³⁺ phosphors may have superior optical properties, and thus have great potential for biological applications. PMID:27398591

  5. Hydrothermal synthesis and visible-light-driven photocatalytic degradation for tetracycline of Mn-doped SrTiO3 nanocubes

    NASA Astrophysics Data System (ADS)

    Wu, Guoling; Li, Ping; Xu, Dongbo; Luo, Bifu; Hong, Yuanzhi; Shi, Weidong; Liu, Chunbo

    2015-04-01

    Visible-light-driven manganese doped SrTiO3 nanocubes with various manganese atomic percentages in the range of 3-7%, were prepared by a hydrothermal method. These obtained photocatalysts were systematically characterized by XRD, EDX, TEM, STEM, XPS, UV-vis, PL, EIS. The results demonstrated that the Mn4+ has substituted into the lattice of SrTiO3 nanocubes and the absorption onset shifted toward the visible region. It is beneficial to the photocatalytic degradation of tetracycline under the visible light irradiation. Interestingly, the optimal doping atomic percentages at 5% exhibited the highest degradation rates (66.7%) in 60 min. The high photocatalytic activity could be ascribed to the Mn doping adjustment the energy band of SrTiO3 and the highly effective separation of photo-generated electron-hole pairs. Furthermore, the possible photocatalytic mechanism has been discussed based on the active species trapping experiments and ESR analysis.

  6. Hydrothermal synthesis of oxygen functionalized S-P codoped g-C3N4 nanorods with outstanding visible light activity under anoxic conditions.

    PubMed

    Hu, Shaozheng; Ma, Lin; Xie, Ying; Li, Fayun; Fan, Zhiping; Wang, Fei; Wang, Qiong; Wang, Yanjuan; Kang, Xiaoxue; Wu, Guang

    2015-12-28

    Extending the application of photocatalytic oxidation technology to the anoxic removal of organic pollutants that exist under some oxygen-free conditions is attractive but challenging. In this study, oxygen functionalized S-P codoped g-C3N4 nanorods with outstanding visible light activity under anoxic conditions are synthesized using a hydrothermal post-treatment. S and P codoping inhibits the crystal growth of graphitic carbon nitride, enhances the SBET, decreases the band gap energy, and increases the separation efficiency of photogenerated electrons and holes, which increases the anoxic photocatalytic RhB degradation constant by approximately 6.5 times. Oxygen functionalization not only increases the adsorption ability of graphitic carbon nitride but also captures the photogenerated electrons to produce photogenerated holes for RhB degradation under anoxic conditions, leading to a doubling of the RhB degradation constant. This study provides new insight into the design and fabrication of anoxic photocatalysts. PMID:26571403

  7. An experimental design approach for hydrothermal synthesis of NaYF4: Yb3+, Tm3+ upconversion microcrystal: UV emission optimization

    NASA Astrophysics Data System (ADS)

    Kaviani Darani, Masoume; Bastani, Saeed; Ghahari, Mehdi; Kardar, Pooneh

    2015-11-01

    Ultraviolet (UV) emissions of hydrothermally synthesized NaYF4: Yb3+, Tm3+ upconversion crystals were optimized using the response surface methodology experimental design. In these experimental designs, 9 runs, two factors namely (1) Tm3+ ion concentration, and (2) pH value were investigated using 3 different ligands. Introducing UV upconversion emissions as responses, their intensity were separately maximized. Analytical methods such as XRD, SEM, and FTIR could be used to study crystal structure, morphology, and fluorescent spectroscopy in order to obtain luminescence properties. From the photo-luminescence spectra, emissions centered at 347, 364, 452, 478, 648 and 803 nm were observed. Some results show that increasing each DOE factor up to an optimum value resulted in an increase in emission intensity, followed by reduction. To optimize UV emission, as a final result to the UV emission optimization, each design had a suggestion.

  8. Synthesis of original spherical α-Ni(OH) 2 architectures by microwave-assisted hydrothermal method and their in situ thermal convention to NiO

    NASA Astrophysics Data System (ADS)

    Zhu, Zhenfeng; Zhang, Yanli; Liu, Hui; Wei, Na

    2012-02-01

    The original spherical α-Ni(OH) 2 architectures with many cubic particles growing from the surface were successfully synthesized by a microwave-assisted hydrothermal method using urea as hydrolysis-controlling agent and polyethylene glycol (PEG) as surfactant. The NiO architectures with similar morphology were obtained by simple thermal decomposition of the precursor α-Ni(OH) 2. The as-obtained products were well characterized by XRD, FTIR, TGA, SEM, TEM, UV-Vis and CVs. The experimental results showed that the diameter of spherical α-Ni(OH) 2 architectures was in the range of 2-4 μm. The side length of the cubic particles was uniform about 200 nm. The cyclic voltammetric results showed that the reversible behavior of NiO electrode change better with the increasing of the cycle index. The original NiO we have prepared are expected to have good electrochemical behavior.

  9. One-pot synthesis of Ag+ doped BiVO4 microspheres with enhanced photocatalytic activity via a facile hydrothermal method

    NASA Astrophysics Data System (ADS)

    Zhu, Shiwen; Li, Quanguo; Li, Feng; Cao, Wei; Li, Taohai

    2016-05-01

    The Ag+/BiVO4 photocatalyst was fabricated through a facile hydrothermal method by using K6V10O28·9H2O as the vanadium source. The impact of Ag+ on the product's structure and morphology was studied. It was shown that the amount of Ag+ has no effect on the product's crystal phases but plays an important role on the morphology of the nanoparticles that construct the shell of BiVO4 microspheres. In addition, the Ag+-doped photocatalysts have much higher photocatalytic activities in removing RhB and MB under the UV light illumination than the pure BiVO4. A possible photocatalytic mechanism was proposed in photoexcitation of the BiVO4 electrons which subsequently captured by the dopant. The present work may offer a novel route to reach higher photocatalytic activity by doping the Ag+ in the semiconductor catalysts.

  10. Rapid synthesis of an aluminum-rich MSE-type zeolite by the hydrothermal conversion of an FAU-type zeolite.

    PubMed

    Inagaki, Satoshi; Tsuboi, Yasuyuki; Nishita, Yuji; Syahylah, Tuan; Wakihara, Toru; Kubota, Yoshihiro

    2013-06-10

    An aluminum-rich MSE-type zeolite (Si/Al is as small as 7) has been successfully synthesized in a remarkably short crystallization period of only 3 days by the hydrothermal conversion of an FAU-type zeolite, presumably by the assembly of four-membered-ring (4-R) aluminosilicate oligomers supplied by the double 6-R (D6R) components of the FAU framework with the aid of the structure-directing agents and seed crystals. The dealuminated version of the aluminum-rich MSE-type zeolite showed a high level of coke durability in addition to a significant yield of propylene, which indicates that this novel zeolitic material is suitable for industrial applications as a highly selective and long-lived catalyst. PMID:23606200

  11. Hydrothermal synthesis of Bismuth(III) coordination polymer and its transformation to nano α-Bi2O3 for photocatalytic degradation

    NASA Astrophysics Data System (ADS)

    Huang, Ya-Jing; Zheng, Yue-Qing; Zhu, Hong-Lin; Wang, Jin-Jian

    2016-07-01

    A new Bi(III) coordination polymer Bi2(Hpdc)2(pdc)2·2H2O (H2pdc=pyridine-2,6-dicarboxylic acid) was synthesized by hydrothermal method. Solid state thermal decomposition of this complex under 500 °C for 1 h led to the foliated Bi2O3 nanoparticles, which were then characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Comparative study on their photocatalytic activity toward the degradation of rhodamine B (RhB), methylene blue (MB) and methyl orange (MO) in polluted water was explored, and the mechanism of these photocatalytic degradation was discussed. These results provided some interesting insights into their photocatalytic applications.

  12. Hydrothermal synthesis and photocatalytic activities of Bi{sub 4}Ti{sub 3}O{sub 12}/SrTiO{sub 3} composite micro-platelets

    SciTech Connect

    Zhao, Wei Wang, Hongxing; Feng, Xiangning; Jiang, Wangyang; Zhao, Dan; Li, Jiyuan

    2015-10-15

    Highlights: • Bi{sub 4}Ti{sub 3}O{sub 12}/SrTiO{sub 3} composite was fabricated by combining hydrothermal reaction and molten salt method. • Bi{sub 4}Ti{sub 3}O{sub 12}/SrTiO{sub 3} exhibits higher photocatalytic activity than pure Bi{sub 4}Ti{sub 3}O{sub 12}. • The absorption light of Bi{sub 4}Ti{sub 3}O{sub 12}/SrTiO{sub 3} has been broadened to visible light. - Abstract: In this study, Bi{sub 4}Ti{sub 3}O{sub 12}/SrTiO{sub 3} micro-platelets were successfully synthesized by using hydrothermal and molten salt methods, and the morphology and photocatalytic degradation performance of Bi{sub 4}Ti{sub 3}O{sub 12}/SrTiO{sub 3} was characterized. The results indicated a much higher degradation rate of methylene blue and methylene orange, reaching more than 90% and 65%, respectively, within 3 h under visible-light irradiation. Compared with pure Bi{sub 4}Ti{sub 3}O{sub 12}, the photocatalytic activity of Bi{sub 4}Ti{sub 3}O{sub 12}/SrTiO{sub 3} was significantly better, due to the micron–submicron heterojunction with SrTiO{sub 3} reducing the band gap of Bi{sub 4}Ti{sub 3}O{sub 12}. In addition, the perovskite structure layer facilitates the mobility of the photogenerated carriers and hampers their recombination, which were affected the photocatalytic properties.

  13. Hydrothermal synthesis of Ca{sub 3}Bi{sub 8}O{sub 15} rods and their visible light photocatalytic properties

    SciTech Connect

    Li, Wenjuan; Kong, Desheng; Cui, Xiaoli; Du, Dandan; Yan, Tingjiang; You, Jinmao

    2014-03-01

    Graphical abstract: The novel Ca{sub 3}Bi{sub 8}O{sub 15} rods can utilize the sunlight efficiently with the small band-gap. Using methyl orange (MO) as a model organic pollutant, the photocatalysts exhibited good photocatalytic activity, with the photodegradation conversion ratio of MO being up to 90% after 2 h of visible light (420 nm < λ < 800 nm) irradiation. - Highlights: • Ca{sub 3}Bi{sub 8}O{sub 15} rods were synthesized by a hydrothermal method. • They can utilize the sunlight efficiently with the small band-gap. • They showed good photocatalytic activities in the degradation of MO, RhB and 4-CP. • The conversion ratio of MO was up to 90% after 2 h of visible light irradiation. - Abstract: High efficient visible light Ca{sub 3}Bi{sub 8}O{sub 15} photocatalysts were synthesized by a hydrothermal method. Characterized by X-ray diffractometer, transmission electron microscopy, and the UV–vis diffuse reflectance spectroscopy, the results showed that the novel Ca{sub 3}Bi{sub 8}O{sub 15} rods can utilize the sunlight efficiently with the small band-gap. Using methyl orange (MO) as a model organic pollutant, the photocatalysts exhibited good photocatalytic activity, with the photodegradation conversion ratio of MO being up to 90% after 2 h of visible light (420 nm < λ < 800 nm) irradiation. Furthermore, they also showed good photocatalytic activities in the degradation of rhodamine B and p-chlorophenol. Through the investigation of the degraded mechanism, the main active species played important roles in the degradation process were holes, O{sub 2}·{sup −} and ·OH.

  14. 8-Hydroxypyrene-1,3,6-trisulphonate and octanesulphonate co-assembled layered double hydroxide and its controllable solid-state luminescence by hydrothermal synthesis

    SciTech Connect

    Dang Sile; Yan Dongpeng; Lu Jun

    2012-01-15

    8-Hydroxy-pyrene-1,3,6-trisulphonate (HPTS) and octanesulphonate (OS) have been co-intercalated into the ZnAl layered double hydroxide (LDH) host by a hydrothermal co-precipitation method, with samples denoted as HPTS (x%)-OS/Zn{sub 2}Al-LDH (x stands for the molar percentage content of HPTS with respect to total amount of HPTS and OS). The structure and chemical compositions of the as-prepared compounds were characterized by X-ray diffraction (XRD) and elemental analysis. The steady-state and time-decay fluorescent studies show that HPTS (2%)-OS/Zn{sub 2}Al-LDH has the optimal luminous emission and the longest fluorescent lifetime. Moreover, these samples exhibit controllable dual fluorescence between the blue and green regions upon changing the interlayer HPTS content, external pH values, and host-guest interaction, illustrating that these organic-inorganic samples have potential application in the field of tunable solid luminescent materials. - Graphical Abstract: 8-Hydroxy-pyrene-1,3,6-trisulphonate and octanesulfonate co-intercalated ZnAl layered double hydroxide can exhibit tunable solid-state blue and green fluorescence by treating the sample at acid and neutral media under hydrothermal condition. Highlights: Black-Right-Pointing-Pointer 8-hydroxy-pyrene-1,3,6-trisulphonate (HPTS) was intercalated into ZnAl LDHs. Black-Right-Pointing-Pointer They show the controllable dual fluorescence response to the HPTS content and pH values. Black-Right-Pointing-Pointer Fluorescence of the HPTS/LDH film was insensitive to the quencher (Cu{sup 2+}) concentration.

  15. Flower-like nanostructure MNb{sub 2}O{sub 6} (M = Mn, Zn) with high surface area: Hydrothermal synthesis and enhanced photocatalytic performance

    SciTech Connect

    Huang, Xue; Jing, Yan; Yang, Jia; Ju, Jing; Cong, Rihong; Gao, Wenliang; Yang, Tao

    2014-03-01

    Graphical abstract: - Highlights: • MNb{sub 2}O{sub 6} was prepared by a mild two-step hydrothermal method. • Their flower-like nanostructure morphology was studied by SEM and TEM. • High BET surface areas for MnNb{sub 2}O{sub 6} (∼50 m{sup 2}/g) and ZnNb{sub 2}O{sub 6} (∼100 m{sup 2}/g). • Band gap energies were estimated by UV–vis diffuse reflectance spectra. • Photocatalytic activities were evaluated under UV-light irradiation. - Abstract: Nano-scaled MNb{sub 2}O{sub 6} (M = Mn, Zn) was successfully synthesized via a two-step hydrothermal method. It is important to control the exact pH of the reaction solution in order to obtain pure products. The as-prepared samples both crystallize in the columbite structure. Interestingly, the products possess a flower-like morphology in a pseudo-six-fold symmetry, which is in fact arrayed by two-dimensional nanosheets. Their surface areas (51 m{sup 2}/g for MnNb{sub 2}O{sub 6} and 103 m{sup 2}/g for ZnNb{sub 2}O{sub 6}) are about 25–50 times of those prepared by solid state reaction. UV–vis diffuse reflectance spectra show the nano-scaled sample has a stronger absorption and a narrower band gap than its bulk form. The estimated band gap energies are 2.70 eV (MnNb{sub 2}O{sub 6}) and 3.77 eV (ZnNb{sub 2}O{sub 6}), respectively. The nano-scaled ZnNb{sub 2}O{sub 6} exhibits a double enhancement of photocatalytic activity in the decolorization of methylene blue than bulk ZnNb{sub 2}O{sub 6}.

  16. Synthesis and characterization of hybrid nanostructures produced in the presence of the titanium dioxide and bioactive organic substances by hydrothermal method

    SciTech Connect

    Zima, Tatyana; Baklanova, Natalya; Bataev, Ivan

    2013-02-15

    Hybrid nanostructures produced by hydrothermal treatment of TiO{sub 2} in the presence of bioactive organic substances such as chitosan, aminoterephthalic acid and their mixture have been investigated. Sodium polytitanates as one-dimensional elongated structures with lengths of several hundred of nanometers were obtained in the presence of chitosan and aminoterephthalic acid. With chitosan the elongated nanostructures are formed by successive superposition of structural fragments-nanostrips with well-ordered multilayered morphology and increased distance between successive layers to 1.2 nm. Quite different amorphous products as agglomerates with roundest and rhomboid morphology are formed when the mixture of chitosan and aminoterephthalic acid is added to the reaction system. One can propose that main reason of such behavior is a low rate of diffusion of dissolved Ti(IV) ions in the high viscous mixed chitosan-aminoterephthalic system. An effect of organic substances on the formation, morphology and transformation of various titanates is discussed. - Graphical abstract: The typical images of hybrid nanostructures produced by hydrothermal treatment of TiO{sub 2} in the presence chitosan and mixed chitosan with aminoterephthalic acid. Highlights: Black-Right-Pointing-Pointer Various shapes of TiO{sub 2} based structures can be produced in the presence of organic. Black-Right-Pointing-Pointer An addition of chitosan results in the formation of the elongated nanostructures. Black-Right-Pointing-Pointer These structures have multilayered morphology and increased distance between layers. Black-Right-Pointing-Pointer Different agglomerates are formed when chitosan and aminoterephthalic acid are mixed.

  17. Hydrothermal synthesis of zinc(II)-phosphonate coordination polymers with different dimensionality (0D, 2D, 3D) and dimensionality change in the solid phase (0D→3D) induced by temperature

    SciTech Connect

    Fernández-Zapico, Eva; Montejo-Bernardo, Jose; Fernández-González, Alfonso; García, José R. García-Granda, Santiago

    2015-05-15

    Three new zinc(II) coordination polymers, [Zn(HO{sub 3}PCH{sub 2}CH{sub 2}COO)(C{sub 12}H{sub 8}N{sub 2})(H{sub 2}O)] (1), [Zn{sub 3}(O{sub 3}PCH{sub 2}CH{sub 2}COO){sub 2}(C{sub 12}H{sub 8}N{sub 2})](H{sub 2}O){sub 3.40} (2) and [Zn{sub 5}(HO{sub 3}PCH{sub 2}CH{sub 2}COO){sub 2}(O{sub 3}PCH{sub 2}CH{sub 2}COO){sub 2}(C{sub 12}H{sub 8}N{sub 2}){sub 4}](H{sub 2}O){sub 0.32} (3), with different structural dimensionality (0D, 2D and 3D, respectively) have been prepared by hydrothermal synthesis, and their structures were determined by single-crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic system (P2{sub 1}/c) forming discrete dimeric units bonded through H-bonds, while compounds 2 and 3 crystallize in the triclinic (P−1) and the monoclinic (C2/c) systems, respectively. Compound 3, showing three different coordination numbers (4, 5 and 6) for the zinc atoms, has also been obtained by thermal treatment of 1 (probed by high-temperature XRPD experiments). The crystalline features of these compounds, related to the coordination environments for the zinc atoms in each structure, provoke the increase of the relative fluorescence for 2 and 3, compared to the free phenanthroline. Thermal analysis (TG and DSC) and XPS studies have been also carried out for all compounds. - Graphical abstract: Three new coordination compounds of zinc with 2-carboxyethylphosphonic acid (H{sub 2}PPA) and phenanthroline have been obtained by hydrothermal synthesis. The crystalline structure depends on the different coordination environments of the zinc atoms (see two comparative Zn{sub 6}-moieties). The influence of the different coordination modes of H{sub 2}PPA with the central atom in all structures have been studied, being found new coordination modes for this ligand. Several compounds show a significant increase in relative fluorescence with respect to the free phenanthroline. - Highlights: • Compounds have been obtained modifying the reaction time and the rate of

  18. Hydrothermal synthesis of Y{sub 2}O{sub 3} coated Y{sub 2}O{sub 3}:Eu{sup 3+} nanotubes for enhanced photoluminescence properties

    SciTech Connect

    Gao, Linhui; Wang, Guangfa; Zhu, Hongliang; Zhou, Weijie; Ou, Guofu

    2015-10-15

    Highlights: • Eu{sup 3+} doped Y{sub 2}O{sub 3} nanotubes. • Hydrothermal synthesis of Y{sub 2}O{sub 3} coated Y{sub 2}O{sub 3}:Eu{sup 3+} nanostructures assissted with a further heat treatment. • Tunable coating ratios of Y{sub 2}O{sub 3} coated Y{sub 2}O{sub 3}:Eu{sup 3+} nanophosphor. • Enhanced photoluminescence intensity of Y{sub 2}O{sub 3}:Eu{sup 3+} more than 60% by Y{sub 2}O{sub 3} surface coating. - Abstract: Novel Y{sub 2}O{sub 3} coated Y{sub 2}O{sub 3}:Eu{sup 3+} nanotubes with different coating ratios were synthesized successfully by a facile two-step process, including hydrothermal synthesis of Y(OH){sub 3} coated Y(OH){sub 3}:Eu{sup 3+} as precursors and then calcination of them at 1000 °C for 2 h. X-ray diffraction patterns and field emission scanning electron microscope images indicated these Y{sub 2}O{sub 3} coated Y{sub 2}O{sub 3}:Eu{sup 3+} phosphors possess tubular nanostructures. The photoluminescence properties of Y{sub 2}O{sub 3} coated Y{sub 2}O{sub 3}:Eu{sup 3+} were systematically investigated by photoluminescence spectra, and photoluminescence enhancement was observed after proper coating. In other words, the coating ratio played a crucial role in photoluminescence efficiency. When it was 1/9, the photoluminescence intensity of {sup 5}D{sub 0} → {sup 7}F{sub 2} emission (about 613 nm) was 60% higher than that of Y{sub 2}O{sub 3}: Eu{sup 3+} phosphors under 255 nm excitation. Therefore, surface coating may be an alternative route for enhanced photoluminescence properties of the Y{sub 2}O{sub 3}:Eu{sup 3+} red-emitting phosphor.

  19. Hydrothermal synthesis of highly crystalline RuS{sub 2} nanoparticles as cathodic catalysts in the methanol fuel cell and hydrochloric acid electrolysis

    SciTech Connect

    Li, Yanjuan; Li, Nan; Yanagisawa, Kazumichi; Li, Xiaotian; Yan, Xiao

    2015-05-15

    Highlights: • Highly crystalline RuS{sub 2} nanoparticles have been first synthesized by a “one-step” hydrothermal method. • The product presents a pure cubic phase of stoichiometric ratio RuS{sub 2} with average particle size of 14.8 nm. • RuS{sub 2} nanoparticles were used as cathodic catalysts in methanol fuel cell and hydrochloric acid electrolysis. • The catalyst outperforms commercial Pt/C in methanol tolerance and stability towards Cl{sup −}. - Abstract: Highly crystalline ruthenium sulfide (RuS{sub 2}) nanoparticles have been first synthesized by a “one-step” hydrothermal method at 400 °C, using ruthenium chloride and thiourea as reactants. The products were characterized by powder X-ray diffraction (XRD), scanning electron microscopy/energy disperse spectroscopy (SEM/EDS), thermo gravimetric-differential thermal analyze (TG-DTA), transmission electron microscopy equipped with selected area electron diffraction (TEM/SAED). Fourier transform infrared spectra (IR), and X-ray photoelectron spectroscopy (XPS). XRD result illustrates that the highly crystalline product presents a pure cubic phase of stoichiometric ratio RuS{sub 2} and the average particle size is 14.8 nm. SEM and TEM images display the products have irregular shape of 6–25 nm. XPS analyst indicates that the sulfur exists in the form of S{sub 2}{sup 2−}. Cyclic voltammetry (CV), rotating disk electrode (RDE), chronoamperometry (CA) and electrochemical impedance spectroscopy (EIS) measurements are conducted to evaluate the electrocatalytic activity and stability of the highly crystalline RuS{sub 2} nanoparticles in oxygen reduction reaction (ORR) for methanol fuel cell and hydrochloric acid electrolysis. The results illustrate that RuS{sub 2} is active towards oxygen reduction reaction. Although the activity of RuS{sub 2} is lower than that of Pt/C, the RuS{sub 2} catalyst outperforms commercial Pt/C in methanol tolerance and stability towards Cl{sup −}.

  20. Synthesis of luminescent nanocrystals and solid solutions in the YNbO{sub 4}–EuNbO{sub 4} system via hydrothermal route

    SciTech Connect

    Hirano, Masanori Dozono, Hayato

    2014-02-01

    Highlights: • Nanocrystals: YNbO{sub 4}:Eu{sup 3+} were directly formed under hydrothermal conditions at 240 °C. • The nanocrystals (10–20 nm) were luminescent and had ellipsoidal morphology. • The complete solid solutions in the YNbO{sub 4}–EuNbO{sub 4} system were also directly formed. • The PL intensity and R/O intensity ratio changed depending on heating temperature. - Abstract: Luminescent nanocrystals having distinctive ellipsoidal morphology and the complete solid solution of monoclinic phase in the YNbO{sub 4}–EuNbO{sub 4} system were hydrothermally formed under weakly basic conditions at 180–240 °C for 5 h. The excitation spectra of the Y{sub 1−x}Eu{sub x}NbO{sub 4} nanocrystals, which consisted of the charge transfer (CT) band around 240–270 nm due to [NbO{sub 4}]{sup 3−}–Eu{sup 3+} interaction and several sharp bands corresponding to the f–f transitions of Eu{sup 3+}, e.g. the most intense absorption band at 395 nm ({sup 7}F{sub 0}→{sup 5}L{sub 6}), showed that the compounds could be excited by both ultraviolet and visible light. A dominant red emission at 610 nm and a weak orange emission at 590 nm assigned to {sup 5}D{sub 0}→{sup 7}F{sub 2} and {sup 5}D{sub 0}→{sup 7}F{sub 1} transitions of Eu{sup 3+}, respectively were observed in the as-prepared nanocrystals containing europium under excitation at 395 nm. The heat treatment at temperatures more than 1000 °C in air was effective for the improvement in the photoluminescence intensity of the as-prepared solid solutions. By the enhancement in the crystallinity and crystallite growth of the monoclinic phase through heat treatment at 1300 °C in air, the luminescence intensity of the as-prepared solid solution, Y{sub 0.75}Eu{sub 0.25}NbO{sub 4} (x = 0.25), which showed the most significant photoluminescence, became more than 5 times as strong as that before the heat treatment.

  1. Zinc(II) and lead(II) metal-organic networks driven by a multifunctional pyridine-carboxylate building block: Hydrothermal synthesis, structural and topological features, and luminescence properties

    NASA Astrophysics Data System (ADS)

    Yang, Ling; Li, Yu; You, Ao; Jiang, Juan; Zou, Xun-Zhong; Chen, Jin-Wei; Gu, Jin-Zhong; Kirillov, Alexander M.

    2016-09-01

    4-(5-Carboxypyridin-2-yl)isophthalic acid (H3L) was applied as a flexible, multifunctional N,O-building block for the hydrothermal self-assembly synthesis of two novel coordination compounds, namely 2D [Zn(μ3-HL)(H2O)]n·nH2O (1) and 3D [Pb2(μ5-HL)(μ6-HL)]n (2) coordination polymers (CPs). These compounds were obtained in aqueous medium from a mixture containing zinc(II) or lead(II) nitrate, H3L, and sodium hydroxide. The products were isolated as stable crystalline solids and were characterized by IR spectroscopy, elemental, thermogravimetric (TGA), powder (PXRD) and single-crystal X-ray diffraction analyses. Compound 1 possesses a 2D metal-organic layer with the fes topology, which is further extended into a 3D supramolecular framework via hydrogen bonds. In contrast, compound 2 features a very complex network structure, which was topologically classified as a binodal 5,6-connected net with the unique topology defined by the point symbol of (47.63)(49.66). Compounds 1 and 2 disclose an intense blue or green luminescent emission at room temperature.

  2. Hydrothermal synthesis of zinc(II)-phosphonate coordination polymers with different dimensionality (0D, 2D, 3D) and dimensionality change in the solid phase (0D→3D) induced by temperature

    NASA Astrophysics Data System (ADS)

    Fernández-Zapico, Eva; Montejo-Bernardo, Jose; Fernández-González, Alfonso; García, José R.; García-Granda, Santiago

    2015-05-01

    Three new zinc(II) coordination polymers, [Zn(HO3PCH2CH2COO)(C12H8N2)(H2O)] (1), [Zn3(O3PCH2CH2COO)2(C12H8N2)](H2O)3.40 (2) and [Zn5(HO3PCH2CH2COO)2(O3PCH2CH2COO)2(C12H8N2)4](H2O)0.32 (3), with different structural dimensionality (0D, 2D and 3D, respectively) have been prepared by hydrothermal synthesis, and their structures were determined by single-crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic system (P21/c) forming discrete dimeric units bonded through H-bonds, while compounds 2 and 3 crystallize in the triclinic (P-1) and the monoclinic (C2/c) systems, respectively. Compound 3, showing three different coordination numbers (4, 5 and 6) for the zinc atoms, has also been obtained by thermal treatment of 1 (probed by high-temperature XRPD experiments). The crystalline features of these compounds, related to the coordination environments for the zinc atoms in each structure, provoke the increase of the relative fluorescence for 2 and 3, compared to the free phenanthroline. Thermal analysis (TG and DSC) and XPS studies have been also carried out for all compounds.

  3. Large-scale synthesis of ultralong Sb{sub 2}S{sub 3} sub-microwires via a hydrothermal process

    SciTech Connect

    Zhu, G.Q. Liu, P.; Miao, H.Y.; Zhu, J.P.; Bian, X.B.; Liu, Y.; Chen, B.; Wang, X.B.

    2008-10-02

    This paper describes an ethylene glycol (EG)-assisted approach to the large-scale ultralong Sb{sub 2}S{sub 3} sub-microwires, formed by a simple hydrothermal reaction between SbCl{sub 3} and Na{sub 2}S in the presence of distilled water. Transmission electron microscopy and scanning electron microscopy studies indicate that these Sb{sub 2}S{sub 3} sub-microwires possess a diameter around 200 nm and length up to 100 {mu}m. High-resolution transmission electron microscopy and selected area electron diffraction studies reveal that each Sb{sub 2}S{sub 3} sub-microwire is a single-crystal along the [0 0 1] direction. The possible formation mechanism of the sub-microwires was discussed. The effects of volume ratio of EG/water, reaction temperature and the concentration of CO(NH{sub 2}){sub 2} on the morphology of Sb{sub 2}S{sub 3} sub-microwires were also investigated.

  4. Highly uniform and monodisperse GdOF:Ln3+ (Ln = Eu, Tb, Tm, Dy, Ho, Sm) microspheres: hydrothermal synthesis and tunable-luminescence properties.

    PubMed

    Zhang, Yang; Kang, Xiaojiao; Geng, Dongling; Shang, Mengmeng; Wu, Yuan; Li, Xuejiao; Lian, Hongzhou; Cheng, Ziyong; Lin, Jun

    2013-10-21

    GdOF:Ln(3+) (Ln = Eu, Tb, Tm, Dy, Ho and Sm) microspheres (1.5 μm) with high uniformity and monodispersity have been synthesized via a facile hydrothermal method followed by heat treatment (600 °C). X-Ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), as well as photoluminescence (PL) and cathodoluminescence (CL) spectra are used to characterize the resulting samples. A series of controlled experiments indicate that sodium citrate (Cit(3-)) as a shape modifier introduced into the reaction system plays a critical role in the shape evolution of the final products. Furthermore, the shape and size of the products can be further manipulated by adjusting the dosage of Cit(3-) and pH values in the initial solution. The possible formation mechanism for these microspheres has been presented. Under UV light and low-voltage electron beam excitation, GdOF:Ln(3+) microspheres show the characteristic f-f transitions of Ln(3+) (Eu, Tb/Ho, Tm, Dy and Sm) ions and give bright red, green, blue, yellow and yellowish-orange emission, respectively. In addition, multicolored luminescence containing white emission have been successfully confected for co-doped GdOF:Ln(3+) phosphors by changing the doped Ln(3+) ions and adjusting their doping concentrations due to the simultaneous luminescence of Ln(3+) in the GdOF host, making these materials have potential applications in field-emission display devices. PMID:23942823

  5. Effects of precursor concentration on the properties of ZnO nanowires grown on (1-102) r-plane sapphire substrates by hydrothermal synthesis.

    PubMed

    Mun, D-H; Bak, S J; Ha, J-S; Lee, H-J; Lee, J K; Lee, S H; Moon, Y B

    2014-08-01

    In this study, we grew ZnO nanowires hydrothermally on (1-102) r-plane sapphire substrates in an aqueous solution which contained zinc nitrate hexahydrate and hexamethylenetetramine (HMT) at 90 °C. First, the AZO seed layer of 80 nm thickness was deposited on the r-plane sapphire substrate by a radio frequency magnetron sputter. After that, we grew the ZnO nanowires on the seed layer by changing the precursor concentration of the aqueous solution from 0.025 M to 0.01 M. When the molar concentration of the precursor was changed, the diameter, length, density and number of ZnO nanowires also changed significantly: diameter, length and density increased with increasing molar concentration but the number of ZnO nanowires decreased. The ZnO nanowires grown at the higher molar concentration tended to grow along with the c-axis direction, as revealed by atomic force microscope and X-ray diffraction peaks. Furthermore, the PL spectra measured at room-temperature revealed a UV emission of 380 nm which can be attributed to the radiative recombination of free and bound excitons (Near Band edge Emission). The NBE emission was also increased with increasing molar concentration. PMID:25936038

  6. AlOOH-reduced graphene oxide nanocomposites: one-pot hydrothermal synthesis and their enhanced electrochemical activity for heavy metal ions.

    PubMed

    Gao, Chao; Yu, Xin-Yao; Xu, Ren-Xia; Liu, Jin-Huai; Huang, Xing-Jiu

    2012-09-26

    This work described the preparation, characterization, and electrochemical behavior toward heavy metal ions of the AlOOH-reduced graphene oxide nanocomposites. This new material was synthesized through a green one-pot hydrothermal method. The morphologic and structure of the nanocomposites were characterized using atomic force microscopy, X-ray diffraction, Raman spectroscopy, X-ray photoemission spectroscopy, Fourier transform-infrared spectroscopy, and transmission electron microscopy. Electrochemical properties were characterized by cyclic voltammetry and electrochemical impedance spectroscopy. The chemical and electrochemical parameters that have influence on deposition and stripping of metal ions, such as pH value, deposition potential, and deposition time, were also studied. Due to the strong affinity of AlOOH to heavy metal ions and the fast electron-transfer kinetics of graphene, the combination of solid-phase extraction and stripping voltammetric analysis allowed fast and sensitive determination of Cd(II) and Pb(II) in drinking water, making these new nanocomposites promising candidates for practical applications in the fields of detecting heavy metal ions. Most importantly, these new nanocomposites may possess many unknown properties waiting to be explored. PMID:22924704

  7. Low-Temperature Hydrothermal Synthesis of Green Luminescent Carbon Quantum Dots (CQD), and Optical Properties of Blends of the CQD with Poly(3-hexylthiophene)

    NASA Astrophysics Data System (ADS)

    Feng, Xiaoting; Zhao, Yongqiang; Yan, Lingpeng; Zhang, Yi; He, Yuheng; Yang, Yongzhen; Liu, Xuguang

    2015-10-01

    Carbon quantum dots (CQD) emitting green photoluminescence (PL; emission peak at 500 nm) with satisfactory quantum yield (12.1%) were synthesized by a low-temperature hydrothermal method (90°C for 2 h) with l-ascorbic acid as carbon source and ethanediamine as catalyst. The as-prepared CQD dispersed readily in aqueous media, were of average diameter 6.2 nm, and their PL performance was excitation-independent. The photoluminescence wavelength of the CQD was pH-independent but the photoluminescence intensity was pH-dependent. Films of the composite materials poly(3-hexylthiophene) (P3HT) and the CQD were prepared by spin-coating and characterized by ultraviolet-visible absorption spectrophotometry and fluorescence spectrometry. The results revealed enhanced ultraviolet-visible absorption of the P3HT-CQD film compared with pure P3HT and substantially reduced PL intensity of the blend film. Experimental and theoretical results indicate the feasibility of using the CQD as a new acceptor material in polymeric photovoltaic devices.

  8. Microwave-Assisted Hydrothermal Rapid Synthesis of Amorphous Calcium Phosphate Mesoporous Microspheres Using Adenosine 5'-Diphosphate and Application in pH-Responsive Drug Delivery.

    PubMed

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

    2015-11-01

    Herein we report a rapid and green strategy for the preparation of amorphous calcium phosphate mesoporous microspheres (ACP-MSs) using adenosine 5'-diphosphate disodium salt (ADP) as an organic phosphorus source by a microwave-assisted hydrothermal method. The effects of the pH value, the reaction time, and temperature on the crystal phase and morphology of the product are investigated. The ADP biomolecules used in this strategy play an important role in the formation of ACP-MSs. The as-prepared ACP-MSs are efficient for anticancer drug delivery by using doxorubicin (Dox) as a model drug, and the Dox-loaded ACP-MSs show a high ability to damage cancer cells. Moreover, the ACP-MSs drug delivery system exhibits a pH-responsive drug-release behavior due to the degradation of ACP-MSs at a low pH value, thus, it is promising for applications in pH-responsive drug delivery. PMID:26248600

  9. A new inorganic-organic hybrid In2Se3(en) as hollow nanospheres: hydrothermal synthesis and near-infrared photoluminescence properties.

    PubMed

    Liu, Pei; Yu, Shuai; Fan, Weiqiang; Shi, Weidong

    2013-02-28

    A new inorganic-organic hybrid In(2)Se(3)(en) was synthesized as hollow nanospheres via a facile and controllable hydrothermal method in a system containing ethylenediamine (en) and hydrazine hydrate. These as-obtained hybrid hollow nanospheres with an average diameter of 200 nm were assembled by irregularly small-sized (ca. 20 nm) nanoparticles. These hollow nanospheres were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy and thermogravimetric analysis (TGA). The surface chemical composition of the In(2)Se(3)(en) hollow nanospheres were studied by X-ray photoelectron spectroscopy (XPS). The possible gas bubble-template growth mechanism is proposed to understand the formation of In(2)Se(3)(en) hollow nanospheres. Room-temperature UV-vis diffuse reflection spectra and photoluminescence (PL) spectra indicate that the as-obtained hybrid nanospheres possess a maximum absorption at 470 nm and single strong near-infrared emission peak centered at 1092 nm. The near-infrared luminescence endows the hybrid nanospheres with potential application in telecommunications, biolabeling and biomedical imaging, etc. PMID:23307063

  10. One-pot synthesis and photoluminescence properties of core/porous-shell olive-like BaWO4 microstructure by a template-assisted hydrothermal method

    NASA Astrophysics Data System (ADS)

    Zhang, Suyue; Wang, Yunlong; Wang, Cuiping; Zhang, Hui; Shen, Yuhua; Xie, Anjian

    2016-02-01

    Core/porous-shell olive-like crystalline BaWO4 is synthesized by a combined simple hydrothermal method and soft template approach. The prepared product shows an olive-like shape with diameter of ˜2 μm, length of ˜4 μm, and the thickness of the shell of about 65 nm, which are orderly assembled by many nanoparticles. A possible formation mechanism of olive-like BaWO4 microstructure involving interfacial recognization of ions, nucleation, aggregation, in situ growth and Ostwald ripening process is proposed. Polyacrylic acid sodium (PAAS) as a template plays an important role in inducing the nucleation and growth of olive-like BaWO4 microcrystalline. Other shapes of BaWO4 microcrystalline are also fabricated by varying the concentration of PAAS and Ba2+. The olive-like product with a core-shell structure which exists a large number of pores on crystal surface shows excellent photoluminescence property, which have potentially applied prospects in fields such as light display systems etc.

  11. Controlled hydrothermal synthesis of BiOxCly/BiOmIn composites exhibiting visible-light photocatalytic degradation of crystal violet.

    PubMed

    Jiang, Yu-Rou; Lin, Ho-Pan; Chung, Wen-Hsin; Dai, Yong-Ming; Lin, Wan-Yu; Chen, Chiing-Chang

    2015-01-01

    A series of BiOxCly/BiOmIn composites were prepared using autoclave hydrothermal methods. The composition and morphologies of the BiOxCly/BiOmIn composites were controlled by adjusting the experimental conditions: the reaction pH value, temperature, and KCl/KI molar ratio. The products were characterized using X-ray diffraction, scanning electron microscopy-electron dispersive X-ray spectroscopy, UV-vis diffuse reflectance spectroscopy, Brunauer-Emmett-Teller specific surface areas, cathodoluminescence, high-resolution transmission electron microscopy, and high-resolution X-ray photoelectron spectroscopy. The photocatalytic efficiencies of composite powder suspensions were evaluated by monitoring the crystal violet (CV) concentrations. In addition, the quenching effects of various scavengers indicated that the reactive O2(-) played a major role, and OH or h(+) played a minor role in CV degradation. The intermediates formed during the decomposition process were isolated, identified, and characterized using high performance liquid chromatography-photodiode array-electrospray ionization-mass spectrometry to elucidate the CV decomposition mechanism. PMID:25464322

  12. Hydrothermal synthesis of (C6N2H14)2(UVI2UIVO4F12), a mixed-valent one-dimensional uranium oxyfluoride.

    PubMed

    Allen, S; Barlow, S; Halasyamani, P S; Mosselmans, J F; O'Hare, D; Walker, S M; Walton, R I

    2000-08-21

    A new hybrid organic-inorganic mixed-valent uranium oxyfluoride, (C6N2H14)2(U3O4F12), UFO-17, has been synthesized under hydrothermal conditions using uranium dioxide as the uranium source, hydrofluoric acid as mineralizer, and 1,4-diazabicyclo[2.2.2]octane as template. The single-crystal X-ray structure was determined. Crystals of UFO-17 belonged to the orthorhombic space group Cmcm (no. 63), with a = 14.2660(15) A, b = 24.5130(10) A, c = 7.201(2) A, and Z = 4. The structure reveals parallel uranium-containing chains of two types: one type is composed of edge-sharing UO2F5 units; the other has a backbone of edge-sharing UF8 units, each sharing an edge with a pendant UO2F5 unit. Bond-valence calculations suggest the UF8 groups contain UIV, while the UO2F5 groups contain UVI. EXAFS data give results consistent with the single-crystal X-ray structure determination, while comparison of the uranium LIII-edge XANES of UFO-17 with that of related UIV and UVI compounds supports the oxidation-state assignment. Variable-temperature magnetic susceptibility measurements on UFO-17 and a range of related hybrid organic-inorganic uranium(IV) and uranium(VI) fluorides and oxyfluorides further support the formulation of UFO-17 as a mixed-valent UIV/UVI compound. PMID:11196771

  13. One-pot hydrothermal synthesis of CuBi co-doped mesoporous zeolite Beta for the removal of NOx by selective catalytic reduction with ammonia

    PubMed Central

    Xie, Zhiguo; Zhou, Xiaoxia; Wu, Huixia; Chen, Lisong; Zhao, Han; Liu, Yan; Pan, Linyu; Chen, Hangrong

    2016-01-01

    A series of CuBi co-doped mesoporous zeolite Beta (CuxBiy-mBeta) were prepared by a facile one-pot hydrothermal treatment approach and were characterized by XRD, N2 adsorption-desorption, TEM/SEM, XPS, H2-TPR, NH3-TPD and in situ DRIFTS. The catalysts CuxBiy-mBeta were applied to the removal of NOx by selective catalytic reduction with ammonia (NH3-SCR), especially the optimized Cu1Bi1-mBeta achieved the high efficiency for the removal of NOx and N2 selectivity, superior water and sulfur resistance as well as good durability. The excellent catalytic performance could be attributed to the acid sites of the support and the synergistic effect between copper and bismuth species. Moreover, in situ DRIFTS results showed that amides NH2 and NH4+ generated from NH3 adsorption could be responsible for the high selective catalytic reduction of NOx to N2. In addition, a possible catalytic reaction mechanism on Cu1Bi1-mBeta for the removal of NOx by NH3-SCR was proposed for explaining this catalytic process. PMID:27445009

  14. Hydrothermal Synthesis of TiO2@SnO2 Hybrid Nanoparticles in a Continuous-Flow Dual-Stage Reactor.

    PubMed

    Hellstern, Henrik L; Bremholm, Martin; Mamakhel, Aref; Becker, Jacob; Iversen, Bo B

    2016-03-01

    TiO2@SnO2 hybrid nanocomposites were successfully prepared in gram scale using a dual-stage hydrothermal continuous-flow reactor. Temperature and pH in the secondary reactor were found to selectively direct nucleation and growth of the secondary material into either heterogeneous nanocomposites or separate intermixed nanoparticles. At low pH, 2 nm rutile SnO2 nanoparticles were deposited on 9 nm anatase TiO2 particles; the presence of TiO2 was found to suppress formation of larger SnO2 particles. At high pH SnO2 formed separate particles and no deposition on TiO2 was observed. Ball-milling of TiO2 and SnO2 produced no TiO2@SnO2 composites. This verifies that the composite particles must be formed by nucleation and growth of the secondary precursor on the TiO2 . High concentration of secondary precursor led to formation of TiO2 particles embedded in aggregates of SnO2 nanoparticles. The results demonstrate how nanocomposites may be produced in high yield by green chemistry. PMID:26822385

  15. Hydrothermal Synthesis of TiO2 Porous Hollow Nanospheres for Coating on the Photoelectrode of Dye-Sensitized Solar Cells

    NASA Astrophysics Data System (ADS)

    Madhu Mohan, Varishetty; Murakami, Kenji

    2012-02-01

    Various sizes of TiO2 hollow nanosphers were synthesized by a hydrolysis followed by the hydrothermal treatment using different water content and titanium isopropoxide (TTIP) while the remaining components such as methylamine, ethanol and acetonitrile were kept as a constant. We synthesized the various sizes of spheres, 150, 250, 400, 450, and 600 nm in diameter; those are represented as SP150, SP250, SP400, SP450, and SP600. The prepared spheres diameters were confirmed by scanning electron microscopy (SEM). These spheres were coated by using a simple spray technique with the TiO2 colloidal solution as a scattering layer for the TiO2 photoelectrode of dye-sensitized solar cells. Optical absorption measurements did not find a difference in the dye adsorption amount with and without the scattering layer. The scattering effect was observed by incident photon to current conversion efficiency (IPCE) measurements especially in the wavelength region of 550-700 nm. The current-voltage (I-V) measurements show that the scattering layer with 450 nm spheres coated on the photoelectrode gave the improved photovoltaic performances compared to other diameters of the spheres. In the present study, the best energy conversion efficiency of 9.56% was obtained for the photoelectrode with the scattering layer, while the pure photoelectrode without the layer gave 8.4%.

  16. Synthesis of LaVO4/TiO2 heterojunction nanotubes by sol-gel coupled with hydrothermal method for photocatalytic air purification.

    PubMed

    Zou, Xuejun; Li, Xinyong; Zhao, Qidong; Liu, Shaomin

    2012-10-01

    With the aim of improving the effective utilization of visible light, the LaVO(4)/TiO(2) heterojunction nanotubes were fabricated by sol-gel coupled with hydrothermal method. The photocatalytic ability was demonstrated through catalytic removal of gaseous toluene species. The nanotube samples were characterized by scanning electron microscope (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), surface photovoltage (SPV), Raman spectra and N(2) adsorption-desorption measurements. The characterization results showed that the samples with high specific surface areas were of typical nanotubular morphology, which would lead to the high separation and transfer efficiency of photo induced electron-hole pairs. The as-prepared nanotubes exhibited high photocatalytic activity in decomposing toluene species under visible light irradiation with fine photochemical stability. The enhanced photocatalytic performance of LaVO(4)/TiO(2) nanotubes might be attributed to the matching band potentials, the interconnected heterojunction of LaVO(4) versus TiO(2), and the large specific surface areas of nanotubes. PMID:22795044

  17. Poly(vinyl pyrrolidone)-assisted hydrothermal synthesis and enhanced visible-light photocatalytic performance of oxygen-rich bismuth oxychlorides.

    PubMed

    Chang, Fei; Luo, Jieru; Wang, Xiaofang; Xie, Yunchao; Deng, Baoqing; Hu, Xuefeng

    2015-12-01

    A series of novel oxygen-rich bismuth oxychloride (Bi12O17Cl2) were synthesized through a facile poly(vinyl pyrrolidone) (PVP)-assisted hydrothermal route. These obtained Bi12O17Cl2 samples were characterized by various physicochemical techniques. It was found that a proper addition amount of PVP could promote the transformation of Bi12O17Cl2 morphology from irregular clusters to three-dimensional hierarchical flower-like microspheres that were nominated as sample BP2. As-synthesized samples were subjected to a photocatalytic degradation of dye Rhodamine B (RhB) or 2,4-dichlorophenol (2,4-DCP) under visible light. Among all candidates, the sample BP2 with a hierarchical flower-like morphology showed the best degradation efficiency for RhB and 2,4-DCP. The apparent rate constant of sample BP2 in terms of degradation of RhB was nearly 5.7 and 45 times that of unmodified BP0 and N-TiO2. The enhanced photocatalytic performance could be ascribed to synergetic effects including unique hierarchical morphologies, large specific surface area, small particle size, good crystallinity, and suitable band structures. A possible mechanism of catalytic degradation was finally proposed basing upon the active species trapping experiments. PMID:26280163

  18. Supercritical hydrothermal synthesis of Cu{sub 2}O(SeO{sub 3}): Structural characterization, thermal, spectroscopic and magnetic studies

    SciTech Connect

    Larranaga, Aitor

    2009-01-08

    Cu{sub 2}O(SeO{sub 3}) has been synthesized in supercritical hydrothermal conditions, using an externally heated steel reactor with coupled hydraulic pump for the application of high pressure. The compound crystallizes in the P2{sub 1}3 cubic space group. The unit cell parameter is a = 9.930(1) A with Z = 12. The crystal structure has been refined by the Rietveld method. The limit of thermal stability is, approximately, 490 deg. C. Above this temperature the compound decomposes to SeO{sub 2}(g) and CuO(s). The IR spectrum shows the characteristic bands of the (SeO{sub 3}){sup 2-} oxoanion. In the diffuse reflectance spectrum two intense absorptions characteristic of the Cu(II) cations in five-coordination are observed. The ESR spectra are isotropic from room temperature to 5 K, with g = 2.11(2). The thermal evolution of the intensity and line width of the signals suggest a ferromagnetic transition in the 50-45 K range. Magnetic measurements, at low temperatures, confirm the existence of a ferromagnetic transition with a critical temperature of 55 K.

  19. Synthesis of uniform and size-controllable carbon nanospheres by a simple hydrothermal method and fabrication of carbon nanosphere super-hydrophobic surface

    NASA Astrophysics Data System (ADS)

    Joula, Mohsen Heidari; Farbod, Mansoor

    2015-08-01

    A simple hydrothermal method was used to produce high yield, monodisperse and tightly controllable size of carbon nanospheres (CNSs) by adjusting the concentration of initial sucrose solution in a sealed autoclave at 170 °C for 8 h. By changing the solution concentration from 0.5 to 0.1 mol l-1, the sizes of carbon spheres (CS) were reduced from about 2500 to about 300 nm. Also by increasing the solution volume to the vessel volume ratio (Vs/Vv) from 5/6 to 11/13, the yield of CS was increased from 25% up to about 55% of initial raw materials. It was found that by post-annealing of the 300 nm CNSs at 435 °C for 30 min, their diameters were reduced to 100 nm. Moreover, annealing in air atmosphere had a noticeable influence on the surface functional groups and bonds of CNSs. In addition, CNSs were used to fabricate hydrophobic surfaces by coating their ethanolic colloidal solution on glass substrates. The measured contact angle (CA) of a water droplet was about 153°, indicating that the CNSs thick layers were super-hydrophobic. The size dependence of CNSs on the different parameters has been discussed.

  20. Hydrothermal synthesis and characterization of a two-dimensional piperazinium cobalt-zinc phosphate via a metastable one-dimensional phase

    NASA Astrophysics Data System (ADS)

    Torre-Fernández, Laura; Khainakova, Olena A.; Espina, Aránzazu; Amghouz, Zakariae; Khainakov, Sergei A.; Alfonso, Belén F.; Blanco, Jesús A.; García, José R.; García-Granda, Santiago

    2015-05-01

    A two-dimensional piperazinium cobalt-zinc phosphate, formulated as (C4N2H12)1.5(Co0.6Zn0.4)2(HPO4)2(PO4)·H2O (2D), was synthesized under hydrothermal conditions. The crystal structure was determined using single-crystal X-ray diffraction data (monoclinic P21/c, a=8.1165(3) Å, b=26.2301(10) Å, c=8.3595(4) Å, and β=110.930(5)°) and the hydrogen atom positions were optimized by DFT calculations. A single-crystal corresponding to one-dimensional metastable phase, (C4N2H12)Co0.3Zn0.7(HPO4)2·H2O (1D), was also isolated and the crystal structure was determined (monoclinic P21/c, a=8.9120(6) Å, b=14.0290(1) Å, c=12.2494(5) Å, and β=130.884(6)°). The bulk was characterized by chemical (C-H-N) analysis, powder X-ray diffraction (PXRD), powder X-ray thermodiffractometry (HT-XRD), transmission electron microscopy (STEM(DF)-EDX and EFTEM), and thermal analysis (TG/SDTA-MS), including activation energy data of its thermal decomposition. The magnetic susceptibility and magnetization measurements show no magnetic ordering down to 4 K.