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Sample records for supercritical hydrothermal synthesis

  1. Organic-ligand-assisted supercritical hydrothermal synthesis of titanium oxide nanocrystals leading to perfectly dispersed titanium oxide nanoparticle in organic phase

    International Nuclear Information System (INIS)

    Mousavand, Tahereh; Zhang Jing; Ohara, Satoshi; Umetsu, Mitsuo; Naka, Takashi; Adschiri, Tadafumi

    2007-01-01

    Titanium oxide (TiO 2 ) nanocyrstals which are perfectly dispersed in organic solvents are synthesized by organic-ligand-assisted supercritical hydrothermal synthesis. The addition of hexaldehyde to the supercritical hydrothermal synthesis of TiO 2 leads to the in-situ surface modification, which enables the synthsized TiO 2 nanocrystals to be perfectly dispersed in iso-octane because of its hydrophobic nature. Further, the one-pot synthesis of hybrid materials results in the significant reduction of the particles size, probably due to the capping effect of hexaldehyde to suppress the particles growth

  2. Continuous Hydrothermal Flow Synthesis of LaCrO3 in Supercritical Water and Its Application in Dual-Phase Oxygen Transport Membranes

    DEFF Research Database (Denmark)

    Xu, Yu; Pirou, Stéven; Zielke, Philipp

    2018-01-01

    The continuous production of LaCrO3 particles (average edge size 639 nm, cube-shaped) by continuous hydrothermal flow synthesis using supercritical water is reported for the first time. By varying the reaction conditions, it was possible to suggest a reaction mechanism for the formation of this p......The continuous production of LaCrO3 particles (average edge size 639 nm, cube-shaped) by continuous hydrothermal flow synthesis using supercritical water is reported for the first time. By varying the reaction conditions, it was possible to suggest a reaction mechanism for the formation...

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

  4. Time-resolved in situ neutron diffraction under supercritical hydrothermal conditions: a study of the synthesis of KTiOPO4.

    Science.gov (United States)

    Ok, Kang Min; Lee, Dong Woo; Smith, Ronald I; O'Hare, Dermot

    2012-10-31

    In the first in situ neutron powder diffraction study of a supercritical hydrothermal synthesis, the crystallization of KTiOPO(4) (KTP) at 450 °C and 380 bar has been investigated. The time-resolved diffraction data suggest that the crystallization of KTP occurs by the reaction between dissolved K(+)(aq), PO(4)(3-)(aq), and [Ti(OH)(x)]((4-x)+)(aq) species.

  5. Supercritical Synthesis of Biodiesel

    Directory of Open Access Journals (Sweden)

    Michel Vaultier

    2012-07-01

    Full Text Available The synthesis of biodiesel fuel from lipids (vegetable oils and animal fats has gained in importance as a possible source of renewable non-fossil energy in an attempt to reduce our dependence on petroleum-based fuels. The catalytic processes commonly used for the production of biodiesel fuel present a series of limitations and drawbacks, among them the high energy consumption required for complex purification operations and undesirable side reactions. Supercritical fluid (SCF technologies offer an interesting alternative to conventional processes for preparing biodiesel. This review highlights the advances, advantages, drawbacks and new tendencies involved in the use of supercritical fluids (SCFs for biodiesel synthesis.

  6. Supercritical hydrothermal synthesis of Cu2O(SeO3): Structural characterization, thermal, spectroscopic and magnetic studies

    International Nuclear Information System (INIS)

    Larranaga, Aitor; Mesa, Jose L.; Lezama, Luis; Pizarro, Jose L.; Arriortua, Maria I.; Rojo, Teofilo

    2009-01-01

    Cu 2 O(SeO 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 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 2 (g) and CuO(s). The IR spectrum shows the characteristic bands of the (SeO 3 ) 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

  7. Peptide synthesis in early earth hydrothermal systems

    Science.gov (United States)

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

    2009-01-01

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

  8. Silicon nanochains preparation with hydrothermal synthesis

    International Nuclear Information System (INIS)

    Chen, Y.W.; Tang, Y.H.; Pei, L.Z.; Guo, C.; Lin, L.W.

    2007-01-01

    Silicon nanochains over 1 μm in length and 50-100 nm in diameter have been synthesized by hydrothermal synthesis with silicon powders as start materials and de-ionized water as reaction medium, the growth condition was controlled at 470 deg. C and 9.7 MPa in a sealed reaction kettle. The morphology and microstructure of the production were characterized by transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED); the results revealed that the silicon nanochains have diamond structure. Energy dispersive X-ray spectrum (EDS) was used to analyze the composition of the final production and the possible growth mechanism of silicon nanochain under supercritical hydrothermal condition was proposed

  9. Hydrothermal synthesis, characterization and luminescent ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 39; Issue 4. Hydrothermal synthesis, characterization and luminescent properties of lanthanide-doped NaLaF 4 nanoparticles. JIGMET LADOL HEENA KHAJURIA SONIKA KHAJURIA ... Keywords. Citric acid; X-ray diffraction; down-conversion emission; energy transfer.

  10. Hydrothermal synthesis, characterization and luminescent ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 39; Issue 4. Hydrothermal synthesis, characterization and luminescent properties of lanthanide-doped NaLaF 4 nanoparticles. JIGMET LADOL HEENA KHAJURIA SONIKA KHAJURIA HAQ NAWAZ SHEIKH. Volume 39 Issue 4 August 2016 pp 943-952 ...

  11. Production of fuel range oxygenates by supercritical hydrothermal liquefaction of lignocellulosic model systems

    DEFF Research Database (Denmark)

    Pedersen, Thomas Helmer; Rosendahl, Lasse Aistrup

    2015-01-01

    Lignocellulosic model compounds and aspen wood are processed at supercritical hydrothermal conditions to study and understand feedstock impact on biocrude formation and characteristics. Glucose and xylose demonstrate similar yield of biocrude and biochar, similar biocrude characteristics, and it ......Lignocellulosic model compounds and aspen wood are processed at supercritical hydrothermal conditions to study and understand feedstock impact on biocrude formation and characteristics. Glucose and xylose demonstrate similar yield of biocrude and biochar, similar biocrude characteristics...

  12. Zirconia nano-colloids transfer from continuous hydrothermal synthesis to inkjet printing

    DEFF Research Database (Denmark)

    Rosa, Massimo; Gooden, P. N.; Butterworth, S.

    2017-01-01

    Water dispersions of nanometric yttria stabilized zirconia (YSZ) particles synthesized by Continuous Hydrothermal Synthesis are transferred into nano-inks for thin film deposition. YSZ nanoparticles are synthesized in supercritical conditions resulting in highly dispersed crystals of 10 nm in size...

  13. Hydrothermal synthesis of cubic boron nitride crystals

    International Nuclear Information System (INIS)

    Yu Meiyan; Cui Deliang; Kai Li; Yin Yansheng; Wang Qilong; Lei Chu

    2005-01-01

    Cubic boron nitride (cBN) crystals have been successfully synthesized by in situ hydrothermal method. In order to obtain cBN pure phase crystals, two comparative experiments were carried out. The experimental results indicated that compared to one-step in situ hydrothermal method, multi-step in situ hydrothermal method was beneficial to the synthesis of cBN. It is believed that the multi-step in situ hydrothermal method is the optimal route to synthesize pure cBN bulk crystals

  14. Hydrothermal synthesis, crystal structure and luminescence property ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 127; Issue 12. Hydrothermal synthesis, crystal structure and luminescence property of a three dimensional Sm(III) coordination polymer with 2,5-pyridinedicarboxylic acid. Kranthi Kumar Gangu Anima S Dadhich Saratchandra Babu Mukkamala. Volume 127 Issue 12 ...

  15. Hydrothermal synthesis and electrochemical properties of a ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 128; Issue 5. Hydrothermal synthesis and electrochemical properties of a coordination polymer based on dinuclear (Pyrazinyl tetrazolate) Copper(II) cations and βOctamolybdate Anions. SHAOBIN LI LI ZHANG HUIYUAN MA HAIJUN PANG. Regular Article Volume ...

  16. HYDROTHERMAL SYNTHESIS AND CHARACTERIZATION OF A ...

    African Journals Online (AJOL)

    Preferred Customer

    HYDROTHERMAL SYNTHESIS AND CHARACTERIZATION OF A BINUCLEAR. COMPLEX AND A COORDINATION POLYMER OF COPPER(II). Masoumeh Tabatabaee1*, Reza Mohamadinasab1, Kazem Ghaini1 and Hamid Reza Khavasi2. 1Department of Chemistry, Islamic Azad University, Yazd Branch, Yazd, Iran.

  17. Up-Scaled Supercritical Flow Synthesis of Hybrid Materials

    DEFF Research Database (Denmark)

    Hellstern, Henrik Christian; Becker, Jacob; Hald, Peter

    A new, up-scaled supercritical flow synthesis apparatus is currently under construction in Aarhus. A module based system allows for a range of parameter studies with improved parameter control. The dual-reactor setup enables both single phase and core-shell nanoparticle synthesis, and the large...

  18. Supercritical Flow Synthesis of TiO2

    DEFF Research Database (Denmark)

    Hellstern, Henrik Christian; Becker, Jacob; Hald, Peter

    2014-01-01

    A new, up-scaled supercritical flow synthesis apparatus has been constructed in Aarhus. A module based system allows for a range of parameter studies with improved parameter control. The dual-reactor setup enables both single phase and core-shell nanoparticle synthesis. TiO2 is a well-known mater...

  19. Hydrothermal synthesis of nanostructured titania

    International Nuclear Information System (INIS)

    Yoshito, Walter Kenji; Ferreira, Nildemar A.M.; Rumbao, Ana Carolina S. Coutinho; Lazar, Dolores R.R.; Ussui, Valter

    2009-01-01

    Titania ceramics have many applications due to its surface properties and, recently, its nanostructured compounds, prepared by hydrothermal treatments, have been described to improve these properties. In this work, commercial titanium dioxide was treated with 10% sodium hydroxide solution in a pressurized reactor at 150°C for 24 hours under vigorous stirring and then washed following two different procedures. The first one consisted of washing with water and ethanol and the second with water and hydrochloric acid solution (1%). Resulting powders were characterized by X-ray diffraction, N 2 gas adsorption and field emission gun scanning and transmission electronic microscopy. Results showed that from an original starting material with mainly rutile phase, both anatase and H 2 Ti 3 O 7 phase could be identified after the hydrothermal treatment. Surface area of powders presented a notable increase of one order of magnitude and micrographs showed a rearrangement on the microstructure of powders. (author)

  20. Hydrothermal synthesis of nanostructured titania

    International Nuclear Information System (INIS)

    Yoshito, W.K.; Ferreira, N.A.M.; Lazar, D.R.R.; Ussui, V.; Rumbao, A.C.S.

    2011-01-01

    Titania ceramics have many applications due to its surface properties and, recently, its nanostructured compounds, prepared by hydrothermal treatments, have been described to improve these properties. In this work, commercial titanium dioxide was treated with 10% sodium hydroxide solution in a pressurized reactor at 150 deg C for 24 hours under vigorous stirring and then washed following two different procedures. The first one consisted of washing with water and ethanol and the second with water and hydrochloric acid solution (1%). Resulting powders were characterized by X-ray diffraction, N 2 gas adsorption and field emission gun scanning and transmission electronic microscopy. Results showed that from an original starting material with mainly rutile phase, both anatase and H 2 Ti 3 O 7 phase could be identified after the hydrothermal treatment. Surface area of powders presented a notable increase of one order of magnitude and micrographs showed a rearrangement on the microstructure of powders. (author)

  1. Synthesis of biodiesel from edible and non-edible oils in supercritical alcohols and enzymatic synthesis in supercritical carbon dioxide

    Energy Technology Data Exchange (ETDEWEB)

    Vivek Rathore; Giridhar Madras [Indian Institute of Science, Bangalore (India). Department of Chemical Engineering

    2007-12-15

    Biodiesel is an attractive alternative fuel because it is environmentally friendly and can be synthesized from edible and non-edible oils. The synthesis of biodiesel from edible oils like palm oil and groundnut oil and from crude non-edible oils like Pongamia pinnata and Jatropha curcas was investigated in supercritical methanol and ethanol without using any catalyst from 200 to 400{sup o}C at 200 bar. The variables affecting the conversion during transesterification, such as molar ratio of alcohol to oil, temperature and time were investigated in supercritical methanol and ethanol. Biodiesel was also synthesized enzymatically with Novozym-435 lipase in presence of supercritical carbon dioxide. The effect of reaction variables such as temperature, molar ratio, enzyme loading and kinetics of the reaction was investigated for enzymatic synthesis in supercritical carbon dioxide. Very high conversions (>80%) were obtained within 10 min and nearly complete conversions were obtained at within 40 min for the synthesis of biodiesel in supercritical alcohols. However, conversions of only 60-70% were obtained in the enzymatic synthesis even after 8 h. 48 refs., 8 figs., 1 tab.

  2. Synthesis of fatty acid starch esters in supercritical carbon dioxide

    NARCIS (Netherlands)

    Muljana, Henky; van der Knoop, Sjoerd; Keijzer, Danielle; Picchioni, Francesco; Janssen, Leon P. B. M.; Heeres, Hero J.

    2010-01-01

    This manuscript describes an exploratory study on the synthesis of fatty acid/potato starch esters using supercritical carbon dioxide (scCO(2)) as the solvent. The effects of process variables such as pressure (6-25 MPa), temperature (120-150 degrees C) and various basic catalysts and fatty acid

  3. Hydrothermal synthesis of bismuth germanium oxide

    Science.gov (United States)

    Boyle, Timothy J.

    2016-12-13

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

  4. New large volume hydrothermal reaction cell for studying chemical processes under supercritical hydrothermal conditions using time-resolved in situ neutron diffraction.

    Science.gov (United States)

    Ok, Kang Min; O'Hare, Dermot; Smith, Ronald I; Chowdhury, Mohammed; Fikremariam, Hanna

    2010-12-01

    The design and testing of a new large volume Inconel pressure cell for the in situ study of supercritical hydrothermal syntheses using time-resolved neutron diffraction is introduced for the first time. The commissioning of this new cell is demonstrated by the measurement of the time-of-flight neutron diffraction pattern for TiO(2) (Anatase) in supercritical D(2)O on the POLARIS diffractometer at the United Kingdom's pulsed spallation neutron source, ISIS, Rutherford Appleton Laboratory. The sample can be studied over a wide range of temperatures (25-450 °C) and pressures (1-355 bar). This novel apparatus will now enable us to study the kinetics and mechanisms of chemical syntheses under extreme environments such as supercritical water, and in particular to study the crystallization of a variety of technologically important inorganic materials.

  5. Studies on supercritical hydrothermal syntheses of uranium and lanthanide oxide particles and their reaction mechanisms

    Science.gov (United States)

    Hwang, DongKi; Tsukahara, Takehiko; Tanaka, Kosuke; Osaka, Masahiko; Ikeda, Yasuhisa

    2015-11-01

    In order to develop preparation method of raw metal oxide particles for low decontaminated MOX fuels by supercritical hydrothermal (SH) treatments, we have investigated behavior of aqueous solutions dissolving U(VI), Ln(III) (Ln: lanthanide = Ce, Pr, Nd, Sm, Tb), Cs(I), and Sr(II) nitrate or chloride compounds under SH conditions (temperature = 400-500 °C, pressure = 30-40 MPa). As a result, it was found that Ln(NO3)3 (Ln = Ce, Pr, Tb) compounds produce LnO2, that Ln(NO3)3 (Ln = Nd, Sm) compounds are hardly converted to their oxides, and that LnCl3 (Ln = Ce, Pr, Nd, Sm, Tb), CsNO3, and Sr(NO3)2 do not form their oxide compounds. Furthermore, HNO2 species were detected in the liquid phase obtained after treating HNO3 aqueous solutions containing Ln(NO3)3 (Ln = Ce, Pr, Tb) under SH conditions, and also NO2 and NO compounds were found to be produced by decomposition of HNO3. From these results, it was proposed that the Ln oxide (LnO2) particles are directly formed with oxidation of Ln(III) to Ln(IV) by HNO3 and HNO2 species in the SH systems. Moreover, the uranyl ions were found to form U3O8 and UO3 depending on the concentration of HNO3. From these results, it is expected that the raw metal oxide particles for low decontaminated MOX fuels are efficiently prepared by the SH method.

  6. Analysis of product distribution and characteristics in hydrothermal liquefaction of barley straw in subcritical and supercritical water

    DEFF Research Database (Denmark)

    Zhu, Zhe; Toor, Saqib; Rosendahl, Lasse

    2014-01-01

    In this study, hydrothermal liquefaction of barley straw in subcritical and supercritical water with potassium carbonate catalyst was performed in the temperatures range of 280-400°C. The influence of final reaction temperature on products yield was investigated and some physicochemical properties...... yield (35.24 wt %) as well as the maximum energy recovery of 55.33% were obtained at 300°C. The products obtained were characterized in terms of CHNS elemental composition, higher heating values (HHVs), Fourier transform infrared spectroscopy (FTIR) and gas chromatography-mass spectrometer (GC...

  7. Study on hydrothermal synthesis dynamics of nanoscale xonotlite fibers

    Science.gov (United States)

    Liu, F.; Chen, S.; Lin, Q.; Wang, X. D.; Cao, J. X.

    2018-01-01

    The xonotlite crystals were synthesized via the hydrothermal synthesis manner from CaO and SiO2 as the raw materials with their Si/Ca molar ratio of 1.0. Hydrothermal synthesis dynamics of nanoscale xonotlite fibers was explored by masterly measuring the electrical conductivities and the calcium concentrations of product slurries synthesized at various reaction temperature in this paper. The results indicated that the calculated values of the products’ quality at various reaction temperatures were consistent with the measured values. Based on chemical reaction kinetic, using fourth-order Runge-Kutta method, spline interpolation and least-squares fitting method, the dynamic relationship of xonotlite fibers synthesized via hydrothermal synthesis process is of -{dc}A/{dt}={kc}A4/5.

  8. Amino Acid Synthesis in a Supercritical Carbon Dioxide - Water System

    Directory of Open Access Journals (Sweden)

    Akiyoshi Hoshino

    2009-06-01

    Full Text Available Mars is a CO2-abundant planet, whereas early Earth is thought to be also CO2-abundant. In addition, water was also discovered on Mars in 2008. From the facts and theory, we assumed that soda fountains were present on both planets, and this affected amino acid synthesis. Here, using a supercritical CO2/liquid H2O (10:1 system which mimicked crust soda fountains, we demonstrate production of amino acids from hydroxylamine (nitrogen source and keto acids (oxylic acid sources. In this research, several amino acids were detected with an amino acid analyzer. Moreover, alanine polymers were detected with LC-MS. Our research lights up a new pathway in the study of life’s origin.

  9. Synthesis of p-Phenylenediamine (PPD) using Supercritical Ammonia

    International Nuclear Information System (INIS)

    Cho, Hang-Kyu; Lim, Jong Sung

    2015-01-01

    In this study, investigated the synthesis method of p-Phenylenediamine (PPD) by amination of p-Diiodobenzene (PDIB) under supercritical ammonia and CuI catalyst conditions. We examined the effects of various process variables (e.g., reaction temperature, pressure, amount of ammonia inserted, amount of catalyst inserted, and reaction time) on the production yield of PPD by analyzing the Gas Chromatography (GC). The experimental results demonstrated that PPD was not produced under non-catalyst conditions, and PPD production yield increased with increasing temperature, pressure, amount of catalyst inserted, and reaction time. However, for the reaction temperature case, it was found that 200 .deg. C was the optimal temperature, because thermal degradation of PPD occurred above 250 .deg. C. In addition, we confirmed the structure of PPD and the bonding characteristics of the amine group via FT-IR and H-NMR analysis

  10. Hydrothermal Synthesis of Nanostructured Vanadium Oxides

    Science.gov (United States)

    Livage, Jacques

    2010-01-01

    A wide range of vanadium oxides have been obtained via the hydrothermal treatment of aqueous V(V) solutions. They exhibit a large variety of nanostructures ranging from molecular clusters to 1D and 2D layered compounds. Nanotubes are obtained via a self-rolling process while amazing morphologies such as nano-spheres, nano-flowers and even nano-urchins are formed via the self-assembling of nano-particles. This paper provides some correlation between the molecular structure of precursors in the solution and the nanostructure of the solid phases obtained by hydrothermal treatment. PMID:28883325

  11. Hydrothermal synthesis of titania powders and their photocatalyc properties

    Czech Academy of Sciences Publication Activity Database

    Štengl, Václav; Bakardjieva, Snejana; Murafa, Nataliya; Houšková, Vendula

    2008-01-01

    Roč. 52, č. 4 (2008), s. 278-290 ISSN 0862-5468 R&D Projects: GA ČR GA203/08/0334 Institutional research plan: CEZ:AV0Z40320502 Keywords : anatase * rutile * hydrothermal synthesis Subject RIV: CA - Inorganic Chemistry Impact factor: 0.644, year: 2008

  12. hydrothermal synthesis and characterisation of amine-templated

    African Journals Online (AJOL)

    PROF EKWUEME

    showed that the complexes were insoluble in water, ethanol, DMF and DMSO. KEYWORDS: Hydrothermal synthesis, metal phosphates, p-aminobenzoic acid, ethylacetoacetate, ethylammonium-. 4-aminobenzoate. INTRODUCTION. One of the major areas of materials science is the development of solid state materials with ...

  13. Hydrothermal synthesis and characterisation of amine-templated ...

    African Journals Online (AJOL)

    Hydrothermal synthesis and characterisation of amine-templated metal phosphate framework. ... The complexes were thermally stable up to 3000C, after which the organic components starts decomposing. The solubility test in a wide spectrum of solvents (at room temperature) showed that the complexes were insoluble in ...

  14. Hydrothermal synthesis, structure and characterization of new ...

    Indian Academy of Sciences (India)

    Unknown

    Keywords. Hydrothermal; crystal structure; solid electrolyte; iron (III) pyrophosphate. 1. Introduction ... tion, structure and electrical conductivity and the higher values of ..... type cavity structure. Acknowledgements. The authors would like to express their thanks to DST,. New Delhi, for financial assistance under the projects.

  15. Hydrothermal synthesis, structure and characterization of new ...

    Indian Academy of Sciences (India)

    Unknown

    The structure has tunnel-type cavities and are congenial for ion transportation through them. The compound exhibits moderate thermal stability. Keywords. Hydrothermal; crystal structure; solid electrolyte; iron (III) pyrophosphate. 1. Introduction. NASICON and related compounds belong to the well known family of solid ...

  16. Direct hydrothermal synthesis of metal intercalated hexagonal ...

    Indian Academy of Sciences (India)

    Unknown

    Increasing reaction time, temperature or decreasing pH of the initial solution with concentrated HCl or HNO3 or change in molar ratio of the reactants did not result in a single phase. The reaction of α-MoO3 with thallium chloride under hydrothermal condition yielded a new unidentified phase. In the case of silver we ended ...

  17. Hydrothermal synthesis of fine oxide powders

    Indian Academy of Sciences (India)

    Unknown

    Tokyo Institute of Technology, and Teikyo University of Science and Technology, 3-7-19 Seijo, Setagaya,. Tokyo 157-0066 ... peratures from 100–10,000°C. Hydrothermal is one of the best methods to produce pure fine oxide powders. The authors ... bombs and gas intensifiers for specialized gases, A, H2,. O2, NH3, etc.

  18. Hydrothermal synthesis of hexagonal magnesium hydroxide nanoflakes

    International Nuclear Information System (INIS)

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

    2014-01-01

    Graphical abstract: Hexagonal Mg(OH) 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) 2 nanoflake yielded different crystalline structures. The structure of the nanoflakes are polycrystalline and the probable formation mechanism of Mg(OH) 2 nanoflakes is discussed. - Highlights: • Hexagonal Mg(OH) 2 nanoflakes were synthesized via hydrothermal method. • PEG-20,000 plays an important role in the formation of hexagonal nanostructure. • Mg(OH) 2 nanoflakes show different crystalline structures at different positions. • The probable formation mechanism of hexagonal Mg(OH) 2 nanoflakes was reported. - Abstract: Hexagonal magnesium hydroxide (Mg(OH) 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) 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) 2 nanoflake show different crystalline structures. The structure of the nanoflakes are polycrystalline and the probable formation mechanism of Mg(OH) 2 nanoflakes is discussed. Brunauer–Emmett–Teller (BET) analysis were performed to investigate the porous structure and surface area of the as-obtained nanoflakes

  19. Preparation of α-alumina nanoparticles with various shapes via hydrothermal phase transformation under supercritical water conditions

    Science.gov (United States)

    Hakuta, Y.; Nagai, N.; Suzuki, Y.-H.; Kodaira, T.; Bando, K. K.; Takashima, H.; Mizukami, F.

    2013-12-01

    Alumina (Al2O3) fine particles are widely used as industrial materials including fillers for metal or plastics, paints, polisher, cosmetics and electric substrates, due to its high hardness, chemical stability, and high thermal conductivity. The performance of those industrial products is closely related to the particle size or shape of the alumina particles used, and thus a new synthetic method to control size, shape, and crystal structure of the aluminum oxide is desired for the improvement of the performance. Hydrothermal phase transformation using various aluminum compounds such as oxide, hydroxide, and salt as a staring material, is known as one of the synthetic methods for producing alumina fine particles; however, the influence about the size and shape of the starting aluminum compounds has been little mentioned, although they strongly affect the size and shape of the final products. In this study, we investigated the influence of the shape, size and crystal structure of the starting aluminum compounds on those of the products, and newly succeeded in the production of rod-like α-Al2O3 nanoparticles from fibrous boehmite nanoparticles using hydrothermal phase transformation under supercritical water conditions.

  20. Conductivity dependence on synthesis parameters in hydrothermally synthesized ceria nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Anis-ur-Rehman, M., E-mail: marehman@comsats.edu.pk; Saleemi, A.S.; Abdullah, A.

    2013-12-05

    Highlights: •Facile synthesis of CeO{sub 2} with composite mediated hydrothermal method is done. •Synthesis parameters significantly effect on conduction. •Enhanced dc electrical conductivity (0.3386 S cm{sup −1}) is observed at 700 °C. •Better ac conductivity is observed 2.661 S cm{sup −1} at 700 °C for 3 MHz. •Potential material for electrolyte in fuel cells for higher efficiencies. -- Abstract: Nanoparticles of cerium oxide were synthesized by Composite Mediated Hydrothermal Approach (CMHA). The synthesis conditions were optimized to enhance the conduction properties and for narrow range of nanocrystallites. The synthesis parameters like hydrothermal treatment temperature (at 180 °C and 220 °C) and time (for 45 min, 70 min and 90 min) were optimized. The structural properties of the prepared ceria were examined by X-ray diffraction (XRD) data. Scherrer’s formula was used to calculate the crystallite sizes of average and most intense peak. Temperature dependent dc conductivity was measured in temperature range 200–700 °C and found to be increasing with the increase in measuring temperature and controlling the other synthesis conditions. The frequency dependent ac conductivity and dielectric properties were measured in frequency range 20 Hz–3 MHz at different temperatures. The ac conductivity increased (from 0.00091 to 2.661 S cm{sup −1}) with the increase in temperature (from 200 to 700 °C). Raman spectrum was observed for the different bands of cerium oxide and oxygen vacancies at 514 nm excitation laser line.

  1. Methane and methanol oxidation in supercritical water: Chemical kinetics and hydrothermal flame studies

    Energy Technology Data Exchange (ETDEWEB)

    Steeper, R.R.

    1996-01-01

    Supercritical water oxidation (SCWO) is an emerging technology for the treatment of wastes in the presence of a large concentration of water at conditions above water`s thermodynamic critical point. A high-pressure, optically accessible reaction cell was constructed to investigate the oxidation of methane and methanol in this environment. Experiments were conducted to examine both flame and non-flame oxidation regimes. Optical access enabled the use of normal and shadowgraphy video systems for visualization, and Raman spectroscopy for in situ measurement of species concentrations. Flame experiments were performed by steadily injecting pure oxygen into supercritical mixtures of water and methane or methanol at 270 bar and at temperatures from 390 to 510{degrees}C. The experiments mapped conditions leading to the spontaneous ignition of diffusion flames in supercritical water. Above 470{degrees}C, flames spontaneously ignite in mixtures containing only 6 mole% methane or methanol. This data is relevant to the design and operation of commercial SCWO processes that may be susceptible to inadvertent flame formation. Non-flame oxidation kinetics experiments measured rates of methane oxidation in supercritical water at 270 bar and at temperatures from 390 to 442{degrees}C. The initial methane concentration was nominally 0.15 gmol/L, a level representative of commercial SCWO processes. The observed methane concentration histories were fit to a one-step reaction rate expression indicating a reaction order close to two for methane and zero for oxygen. Experiments were also conducted with varying water concentrations (0 to 8 gmol/L) while temperature and initial reactant concentrations were held constant. The rate of methane oxidation rises steadily with water concentration up to about 5 gmol/L and then abruptly falls off at higher concentrations.

  2. Hydrothermal synthesis and physicochemical properties of ruthenium(0) nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Dikhtiarenko, A., E-mail: dikhtiarenkoalla@uniovi.es [Departamento de Quimica Organica e Inorganica, Universidad de Oviedo - CINN, 33006 Oviedo (Spain); Khainakov, S.A.; Garcia, J.R.; Gimeno, J. [Departamento de Quimica Organica e Inorganica, Universidad de Oviedo - CINN, 33006 Oviedo (Spain); Pedro, I. de; Fernandez, J. Rodriguez [CITIMAC, Facultad de Ciencias, Universidad de Cantabria, 39005 Santander (Spain); Blanco, J.A. [Departamento de Fisica, Universidad de Oviedo, 33007 Oviedo (Spain)

    2012-09-25

    Highlights: Black-Right-Pointing-Pointer Ruthenium nanoparticles were synthesized by hydrothermal technique. Black-Right-Pointing-Pointer The average size of the nanoparticles are depend on the reducing agent used. Black-Right-Pointing-Pointer The magnetic response seems to be dominated by a paramagnetic contribution characteristic of the band electronic magnetism of the ruthenium(0) nanoparticles. - Abstract: The synthesis of ruthenium nanoparticles in hydrothermal conditions using mild reducing agents (succinic acid, ascorbic acid and sodium citrate) is reported. The shape of the nanoparticles depends on the type of the reducing agent, while the size is more influenced by the pH of the medium. The magnetic response seems to be dominated by a paramagnetic contribution characteristic of the band electronic magnetism of the nanoparticles.

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

    Science.gov (United States)

    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.

  4. Hydrothermal synthesis and characterization of zirconia based catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Caillot, T., E-mail: Thierry.caillot@ircelyon.univ-lyon1.fr; 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 liquefaction of Spirulina and Nannochloropsis Salina under subcritical and supercritical water conditions

    DEFF Research Database (Denmark)

    Toor, Saqib; Reddy, H.; Deng, S.

    2013-01-01

    residue, and recycling process water for algae cultivation. GC-MS, elemental analyzer, FT-IR, calorimeter and nutrient analysis were used to analyze bio-crude, lipid-extracted algae and water samples produced in the hydrothermal liquefaction process. The highest bio-crude yield of 46% was obtained...

  6. Biocrude production via supercritical hydrothermal co-liquefaction of spent mushroom compost and aspen wood sawdust

    DEFF Research Database (Denmark)

    Jasiunas, Lukas; Pedersen, Thomas Helmer; Toor, Saqib Sohail

    2017-01-01

    to its organic nature (e.g. straw, horse manure and sphagnum) and ample availability with an annual production of over 3.4 million metric tonnes, globally. Locally acquired samples were analyzed and converted hydrothermally. A biocrude yield of 48% on dry ash-free (DAF) basis was obtained...

  7. Microwave-assisted hydrothermal synthesis of lead zirconate fine powders

    Directory of Open Access Journals (Sweden)

    Apinpus Rujiwatra

    2011-01-01

    Full Text Available A rapid synthesis of lead zirconate fine powders by microwave-assisted hydrothermal technique is reported. The influences of type of lead precursor, concentration of potassium hydroxide mineraliser, applied microwave power and irradiation time are described. The synthesised powders were characterised by powder X-ray diffraction, field emission scanning electron microscopy, energy-dispersive X-ray spectroscopic microanalysis and light scattering technique. The merits of the microwave application in reducing reaction time and improving particle mono-dispersion and size uniformity as well as the drawbacks, viz. low purity of the desired phase and increasing demand of mineraliser, are discussed in relation to conventional heating method.

  8. Hydrothermal Synthesis of High Crystalline Silicalite from Rice Husk Ash

    OpenAIRE

    Chaiwat Kongmanklang; Kunwadee Rangsriwatananon

    2015-01-01

    The objective of this research work was to evaluate the hydrothermal synthesis of silicalite with high crystallinity within a small particle size. The current study focused on investigating the effects of silica sources such as rice husk ash (RHA) and silica gel (SG), crystallization time, and ratios of NaOH/SiO2, H2O/NaOH, and SiO2/TPABr. The crystallinity, particle size, and morphology were characterized by FT-IR, XRD, particle size analyser, and SEM. The conclusion of the main findings ind...

  9. Hydrothermal synthesis of magnetite particles with uncommon crystal facets

    Directory of Open Access Journals (Sweden)

    Junki Sato

    2014-09-01

    Full Text Available Hydrothermal synthesis of Fe3O4 (magnetite particles was carried out using organic compounds as morphology control agents to obtain magnetite crystals with uncommon facets. It was established that the morphology of Fe3O4 crystals obtained by hydrothermal treatment of an aqueous solution containing Fe2+ and organic compounds depended on the organic compound used. The shape of the Fe3O4 particles obtained when no additives were used was quasi-octahedral. In contrast, the addition of picolinic acid, citric acid or pyridine resulted in the formation of polyhedral crystals, indicating the presence of not only {1 1 1}, {1 0 0} and {1 1 0} facets but also high-index facets including at least {3 1 1} and {3 3 1}. When citric acid was used as an additive, octahedral crystals with {1 1 1} facets also appeared, and their size decreased as the amount of citric acid was increased. Thus, control of Fe3O4 particle morphology was achieved by a simple hydrothermal treatment using additives.

  10. High Yield Synthesis of Aspect Ratio Controlled Graphenic Materials from Anthracite Coal in Supercritical Fluids.

    Science.gov (United States)

    Sasikala, Suchithra Padmajan; Henry, Lucile; Yesilbag Tonga, Gulen; Huang, Kai; Das, Riddha; Giroire, Baptiste; Marre, Samuel; Rotello, Vincent M; Penicaud, Alain; Poulin, Philippe; Aymonier, Cyril

    2016-05-24

    This paper rationalizes the green and scalable synthesis of graphenic materials of different aspect ratios using anthracite coal as a single source material under different supercritical environments. Single layer, monodisperse graphene oxide quantum dots (GQDs) are obtained at high yield (55 wt %) from anthracite coal in supercritical water. The obtained GQDs are ∼3 nm in lateral size and display a high fluorescence quantum yield of 28%. They show high cell viability and are readily used for imaging cancer cells. In an analogous experiment, high aspect ratio graphenic materials with ribbon-like morphology (GRs) are synthesized from the same source material in supercritical ethanol at a yield of 6.4 wt %. A thin film of GRs with 68% transparency shows a surface resistance of 9.3 kΩ/sq. This is apparently the demonstration of anthracite coal as a source for electrically conductive graphenic materials.

  11. Characterization structural and morphology ZSM-5 zeolite by hydrothermal synthesis

    International Nuclear Information System (INIS)

    Silva, V.J.; Crispim, A.C.; Queiroz, M.B.; Laborde, H.M.; Rodrigues, M.G.F.; Menezes, R.R.

    2009-01-01

    Solid acids are catalytic materials commonly used in the chemical industry. Among these zeolites are the most important business processes including water treatment, gas separation, and cracking long hydrocarbon chains to produce high octane gasoline. Its synthesis, characterization and applications have been widely studied. The objective this study was to synthesize the ZSM-5 zeolite for future use in separation processes and catalysis. The zeolite ZSM-5 was prepared by hydrothermal synthesis at 170°C, using silica, deionized water and the director of structures (TPABr - tetrapropylammonium bromide). The materials were characterized by X ray diffraction (XRD), scanning electron microscopy (SEM) and semiquantitative chemical analysis by X ray fluorescence (XRF). According to the XRD was possible to observe the formation of ZSM-5 zeolite, with peaks intense and well defined. The SEM showed the formation of individual particles, clean, rounded shapes. (author)

  12. Synthesis of higher diamondoids by pulsed laser ablation plasmas in supercritical CO2

    Science.gov (United States)

    Nakahara, Sho; Stauss, Sven; Kato, Toru; Sasaki, Takehiko; Terashima, Kazuo

    2011-06-01

    Pulsed laser ablation (wavelength 532 nm; fluence 18 J/cm2; pulse width 7 ns; repetition rate 10 Hz) of highly oriented pyrolytic graphite was conducted in adamantane-dissolved supercritical CO2 with and without cyclohexane as a cosolvent. Micro-Raman spectroscopy of the products revealed the presence of hydrocarbons possessing sp3-hybridized carbons similar to diamond structures. The synthesis of diamantane and other possible diamondoids consisting of up to 12 cages was confirmed by gas chromatography-mass spectrometry. Furthermore, gas chromatography-mass spectrometry measurements of samples before and after pyrolysis treatment indicate the synthesis of the most compact decamantane, namely, superadamantane. It is thought that oxidant species originating from CO2 during pulsed laser ablation might lead to the selective dissociation of C-H bonds, enabling the synthesis of low H/C ratio molecules. Therefore, laser ablation in supercritical CO2 is proposed as a practical method for synthesizing diamondoids.

  13. Studies on the use of supercritical ammonia for ceramic nitride synthesis and fabrication

    Science.gov (United States)

    Cornell, Linda; Lin, Y. C.; Philipp, Warren H.

    1990-01-01

    The extractability of ammonia halides (including ammonium thiocyanate) formed as byproducts from the synthesis of Si(NH)2 via ammonolysis of the corresponding silicon tetrahalides using supercritical NH3 as the extraction medium was investigated. It was found that the NH4SCN byproduct of ammonolysis of Si(SCN)4 can be almost completely extracted from the insoluble Si(NH)2 forming a promising system for the synthesis of pure Si(NH)2, one of the best precursors for Si3N4. In addition it was found that Si3N4, AlN, BN, and Si(NH)2 are insoluble in SC ammonia. Also discussed are design considerations for a supercritical ammonia extraction unit.

  14. Hydrothermal synthesis and characterization of zirconia based catalysts

    Science.gov (United States)

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

    2013-07-01

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

  15. Hydrothermal synthesis of free-template zeolite T from kaolin

    Science.gov (United States)

    Arshad, Sazmal E.; Yusslee, Eddy F.; Rahman, Md. Lutfor; Sarkar, Shaheen M.; Patuwan, Siti Z.

    2017-12-01

    Free-template zeolite T crystals were synthesized via hydrothermal synthesis by utilizing the activated kaolin as silica and alumina source, with the molar composition of 1 SiO2: 0.04 Al2O3: 0.26 Na2O: 0.09 K2O: 14 H2O. Observation of the formation of free-template zeolite crystals were done at temperature 90°C, 100 °C and 110 °C respectively. It was therefore determined that during the 120 h of the synthesis at 90 °C, zeolite T nucleated and formed a first competitive phase with zeolite L. As temperature increases to 100 °C, zeolite T presented itself as a major phase in the system at time 168 h. Subsequently, development of Zeolite T with second competitive phase of zeolite W was observed at temperature 110 °C. In this study, XRD and SEM instruments were used to monitor the behavior of zeolite T crystals with respect of temperature and time. By using natural resource of kaolin clay as a starting material, this paper hence aims to provide new findings in synthesis of zeolite T using low energy consumption and low production cost.

  16. Selective Synthesis of Manganese/Silicon Complexes in Supercritical Water

    Directory of Open Access Journals (Sweden)

    Jiancheng Wang

    2014-01-01

    Full Text Available A series of manganese salts (Mn(NO32, MnCl2, MnSO4, and Mn(Ac2 and silicon materials (silica sand, silica sol, and tetraethyl orthosilicate were used to synthesize Mn/Si complexes in supercritical water using a tube reactor. X-ray diffraction (XRD, X-ray photoelectron spectrometer (XPS, transmission electron microscopy (TEM, and scanning electron microscopy (SEM were employed to characterize the structure and morphology of the solid products. It was found that MnO2, Mn2O3, and Mn2SiO4 could be obtained in supercritical water at 673 K in 5 minutes. The roles of both anions of manganese salts and silicon species in the formation of manganese silicon complexes were discussed. The inorganic manganese salt with the oxyacid radical could be easily decomposed to produce MnO2/SiO2 and Mn2O3/SiO2. It is interesting to found that Mn(Ac2 can react with various types of silicon to produce Mn2SiO4. The hydroxyl groups of the SiO2 surface from different silicon sources enhance the reactivity of SiO2.

  17. Microwave-hydrothermal synthesis of perovskite bismuth ferrite nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Biasotto, G. [Laboratorio Interdisciplinar em Ceramica (LIEC), Departamento de Fisico-Quimica, Instituto de Quimica, UNESP, CEP 14800-900, Araraquara, SP (Brazil); Simoes, A.Z., E-mail: alezipo@yahoo.com [Universidade Estadual Paulista-Unesp, Faculdade de Engenharia de Guaratingueta, Av. Dr. Ariberto Pereira da Cunha, 333, Bairro Pedregulho, CEP 12516-410, Guaratingueta, SP (Brazil); Foschini, C.R.; Zaghete, M.A.; Varela, J.A.; Longo, E. [Laboratorio Interdisciplinar em Ceramica (LIEC), Departamento de Fisico-Quimica, Instituto de Quimica, UNESP, CEP 14800-900, Araraquara, SP (Brazil)

    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.

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

    OpenAIRE

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

    2017-01-01

    As known to all, hydrothermal synthesis is a powerful technique for preparing inorganic and organic materials or composites with different architectures. In this reports, by controlling hydrothermal conditions, nanostructured polyaniline (PANi) in different morphologies were composited with graphene sheets (GNS) and used as electrode materials of supercapacitors. Specifically, ultrathin PANi layers with total thickness of 10?20?nm are uniformly composited with GNS by a two-step hydrothermal-a...

  19. Synthesis of dimethyl carbonate in supercritical carbon dioxide

    Directory of Open Access Journals (Sweden)

    D. Ballivet-Tkatchenko

    2006-03-01

    Full Text Available The reactivity of carbon dioxide with methanol to form dimethyl carbonate was studied in the presence of the n-butylmethoxytin compounds n-Bu3SnOCH3, n-Bu2Sn(OCH32 , and [n-Bu2(CH3OSn]2 O. The reaction occurred under solventless conditions at 423 K and was produced by an increase in CO2 pressure. This beneficial effect is primarily attributed to phase behavior. The mass transfer under liquid-vapor biphasic conditions was not limiting when the system reached the supercritical state for a CO2 pressure higher than 16 MPa. Under these conditions, CO2 acted as a reactant and a solvent.

  20. Sol-gel-cum-hydrothermal synthesis of mesoporous Co-Fe ...

    Indian Academy of Sciences (India)

    cum-hydrothermal synthesis of mesoporous Co-Fe@Al₂O₃−MCM-41 for methylene blue remediation. AMARESH C PRADHAN ANIMESH PAUL G RANGA RAO. Regular Article Volume 129 Issue 3 March 2017 pp 381-395 ...

  1. Microwave-hydrothermal synthesis of barium strontium titanate nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Simoes, A.Z., E-mail: alezipo@yahoo.co [Universidade Federal de Itajuba- Unifei - Campus Itabira, Rua Sao Paulo, 377, Bairro, Amazonas, CEP 35900-37, Itabira, MG (Brazil); Universidade Estadual Paulista- Unesp - Faculdade de Engenharia de Guaratingueta, Av. Dr. Ariberto Pereira da Cunha, 333, Bairro Pedregulho, CEP 12516-410 Guaratingueta, SP (Brazil); Moura, F.; Onofre, T.B. [Universidade Federal de Itajuba- Unifei - Campus Itabira, Rua Sao Paulo, 377, Bairro, Amazonas, CEP 35900-37, Itabira, MG (Brazil); Ramirez, M.A.; Varela, J.A.; Longo, E. [Laboratorio Interdisciplinar em Ceramica (LIEC), Departamento de Fisico-Quimica, Instituto de Quimica, UNESP, CEP 14800-900, Araraquara, SP (Brazil)

    2010-10-22

    Research highlights: {yields} Barium strontium titanate nanoparticles were obtained by the Hydrothemal microwave technique (HTMW) {yields} This is a genuine technique to obtain nanoparticles at low temperature and short times {yields} Barium strontium titanate free of carbonates with tetragonal structure was grown at 130 {sup o}C. - Abstract: Hydrothermal-microwave method (HTMW) was used to synthesize crystalline barium strontium titanate (Ba{sub 0.8}Sr{sub 0.2}TiO{sub 3}) nanoparticles (BST) in the temperature range of 100-130 {sup o}C. The crystallization of BST with tetragonal structure was reached at all the synthesis temperatures along with the formation of BaCO{sub 3} as a minor impurity at lower syntheses temperatures. Typical FT-IR spectra for tetragonal (BST) nanoparticles presented well defined bands, indicating a substantial short-range order in the system. TG-DTA analyses confirmed the presence of lattice OH- groups, commonly found in materials obtained by HTMW process. FE/SEM revealed that lower syntheses temperatures led to a morphology that consisted of uniform grains while higher syntheses temperature consisted of big grains isolated and embedded in a matrix of small grains. TEM has shown BST nanoparticles with diameters between 40 and 80 nm. These results show that the HTMW synthesis route is rapid, cost effective, and could serve as an alternative to obtain BST nanoparticles.

  2. Microwave-Assisted Hydrothermal Synthesis of Cellulose/Hydroxyapatite Nanocomposites

    Directory of Open Access Journals (Sweden)

    Lian-Hua Fu

    2016-09-01

    Full Text Available In this paper, we report a facile, rapid, and green strategy for the synthesis of cellulose/hydroxyapatite (HA nanocomposites using an inorganic phosphorus source (sodium dihydrogen phosphate dihydrate (NaH2PO4·2H2O, or organic phosphorus sources (adenosine 5′-triphosphate disodium salt (ATP, creatine phosphate disodium salt tetrahydrate (CP, or D-fructose 1,6-bisphosphate trisodium salt octahydrate (FBP through the microwave-assisted hydrothermal method. The effects of the phosphorus sources, heating time, and heating temperature on the phase, size, and morphology of the products were systematically investigated. The experimental results revealed that the phosphate sources played a critical role on the phase, size, and morphology of the minerals in the nanocomposites. For example, the pure HA was obtained by using NaH2PO4·2H2O as phosphorus source, while all the ATP, CP, and FBP led to the byproduct, calcite. The HA nanostructures with various morphologies (including nanorods, pseudo-cubic, pseudo-spherical, and nano-spherical particles were obtained by varying the phosphorus sources or adjusting the reaction parameters. In addition, this strategy is surfactant-free, avoiding the post-treatment procedure and cost for the surfactant removal from the product. We believe that this work can be a guidance for the green synthesis of cellulose/HA nanocomposites in the future.

  3. Hydrothermal synthesis, off-axis electron holography and magnetic properties of Fe3O4 nanoparticles

    DEFF Research Database (Denmark)

    Almeida, Trevor P.; Muxworthy, Adrian R.; Williams, Wyn

    2014-01-01

    The hydrothermal synthesis of Fe3O4 nanoparticles (NPs) (<50 nm) from mixed FeCl3 / FeCl2 precursor solution at pH ~ 12 has been confirmed using complementary characterisation techniques of transmission electron microscopy and X-ray diffractometry. Off-axis electron holography allowed for visuali......The hydrothermal synthesis of Fe3O4 nanoparticles (NPs) (holography allowed...

  4. Synthesis of hydrogen cyanide under simulated hydrothermal conditions

    Science.gov (United States)

    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

  5. Hydrothermal Synthesis of High Crystalline Silicalite from Rice Husk Ash

    Directory of Open Access Journals (Sweden)

    Chaiwat Kongmanklang

    2015-01-01

    Full Text Available The objective of this research work was to evaluate the hydrothermal synthesis of silicalite with high crystallinity within a small particle size. The current study focused on investigating the effects of silica sources such as rice husk ash (RHA and silica gel (SG, crystallization time, and ratios of NaOH/SiO2, H2O/NaOH, and SiO2/TPABr. The crystallinity, particle size, and morphology were characterized by FT-IR, XRD, particle size analyser, and SEM. The conclusion of the main findings indicated that the XRD patterns of these samples clearly showed a pure phase of MFI structure corresponding to FT-IR spectra with vibration mode at 550 and 1223 cm−1. The highest crystallinity was obtained at reaction time only 6 hours with the mole ratios of NaOH/SiO2, H2O/NaOH and SiO2/TPABr as 0.24, 155, and 30, respectively. When SG was used as a silica source, it was found that the particle size was smaller than that from RHA. The morphologies of all silicalite samples were coffin and cubic-like shape.

  6. Synthesis of barium titanate crystalline nanoparticles using hydrothermal microwave method

    International Nuclear Information System (INIS)

    Souza, A.E.; Silva, R.A.; Teixeira, S.R.; Moreira, M.L.; Volanti, D.P.; Longo, E.

    2009-01-01

    The hydrothermal microwave method (HTMW) was used in the synthesis of barium titanate (BaTiO 3 ) nanoparticles. The solution was prepared in deionized water by using titanium (IV) isopropoxide (C 12 H 28 O 4 Ti), barium chloride (BaCl 2 .2H 2 O) and potassium hydroxide (KOH). Afterwards it was heated in an adapted conventional microwave oven. The system is composed of a temperature controller with thermocouple, a hermetic camera of reaction made of teflon, a manometer and a safety valve. The solution was heated to 140 deg C, at a 140 deg C/min heating rate, and maintained at this temperature for 40 minutes. The obtained ceramic powder was characterized by using X-ray diffraction (XRD) and field emission scanning electron microscopy (FE-SEM). The XRD data confirms the formation of a high crystalline ceramic material with perovskite structure. The FE-SEM images reveal morphologies with dimensions varying from 27 to 54 nm. (author)

  7. Synthesis of carbonated fatty methyl esters using supercritical carbon dioxide.

    Science.gov (United States)

    Doll, Kenneth M; Erhan, Sevim Z

    2005-11-30

    The two-step syntheses of the cyclic carbonates carbonated methyl oleate (CMO) and carbonated methyl linoleate (CML) are reported. First, synthesis of epoxides through well-precedented chemical reactions of unsaturated fatty methyl esters with hydrogen peroxide and formic acid was accomplished. Next, a carbonation reaction with a simple tetrabutylammonium bromide catalyst was performed, allowing the direct incorporation of carbon dioxide into the oleochemical. These syntheses avoid the use of the environmentally unfriendly phosgene. The carbonated products are characterized by IR, 1H NMR, and 13C NMR spectroscopy and studied by thermogravimetric analysis (TGA). Also reported is the synthesis of a similar cyclic carbonate from the commercially available 2-ethylhexyl epoxy soyate. These carbonates show properties that may make them useful as petrochemical replacements or as biobased industrial product precursors.

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

    Science.gov (United States)

    Stampler, Evan Scott

    Low temperature (oxide chalcogenides, hexagonal rare-earth manganites, and silver delafossites with mixed cations on the B-site. These materials are of particular interest because they combine multiple functional properties, such as transparency and conductivity, or magnetism and ferroelectricity, in a single-phase material, thus enabling innovative technological applications. Phase-pure products were achieved by the appropriate combination of starting reagents, pH, and reaction temperature to control the solubility of the reactants. Phase-pure BiCuOS and BiCuOSe have been synthesized in high yield by a single-step hydrothermal reaction at low temperature (250°C) and pressure (oxidation of sulfide and selenide. BiCuOS (Eg = 1.09 eV) and BiCuOSe (Eg = 0.75 eV) have smaller band gaps compared to the p-type transparent conductor LaCuOS (Eg = 3.1 eV) but have significantly higher room temperature conductivities (sigma ≈ 0.08 S cm-1 and 3.3 S cm-1, respectively). The high molar solubility of Mn2O3 ([Mn 3+] ≈ 10-3 M) and the slightly amphoteric character of the late rare-earth sesquioxides were exploited in the hydrothermal synthesis of rare-earth manganites, LnMnO3 (Ln=Ho-Lu and Y). While alkaline conditions were necessary for the solubilization of manganese, a reaction temperature approximately 50°C above the transition temperature of the respective rare-earth trihydroxide (100-300°C) accelerated the transition to the more reactive and soluble rare-earth oxide hydroxide and the subsequent reaction to yield the LnMnO3 phase. The high solubility of Ag2O, [Ag+] ≈ 10 -2.5 M, enabled the synthesis of two new silver delafossite solid solutions with the formulae AgAl1-xGaxO2 and AgSc1-xInxO2 and five mixed B-site silver delafossites with the formulae AgBe0.5Ti0.5O2, AgMg0.5Ti0.5O2, AgNi0.5Ti 0.5O2, AgCu0.5Ti0.5O2, and AgZn0.5Ti0.5O2 at a reaction temperature of 210°C. The former were observed when the solubilities of both B-site trivalent cations were ≥ 10-5 M and

  9. Reaction behaviour of Fischer-Tropsch synthesis in supercritical n-hexane media

    Energy Technology Data Exchange (ETDEWEB)

    Linghu, W.; Li, X.; Asami, K.; Fujimoto, K. [Kitakyushu University, Kitakyushu City (Japan)

    2005-10-15

    The reaction performance of supercritical Fischer-Tropsch synthesis in a fixed bed reactor was studied in this work, n-hexane was used as supercritical media. Three kinds of Co catalysts (impregnated catalyst sprayed catalyst and bimodal catalyst) were tested. Under the same Co content condition, the catalytic activity of the sprayed catalyst was similar with that of the bimodal catalyst, but higher than that of the impregnated catalyst. CO conversion over the sprayed catalysts was remarkably higher than that over the impregnated catalysts. Higher lighter fractions selectivity and lower 1-olefins content of FT products were observed over the sprayed catalyst. At the similar CO conversion conditions, however, the 1-olefins content over the sprayed catalyst was similar with that over the impregnated catalyst. For impregnated catalysts, Co conversion increased obviously from 8.3% to. 43.6% when Co content increased from 5 to 15%. CH{sub 4} selectivity for 5% Co catalyst was lower about 2 to 3% than those of 10, 15 and 20% Co catalysts. 12 refs., 6 figs., 3 tabs.

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

    Science.gov (United States)

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

    2017-10-01

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

  11. Hydrothermal synthesis and characterization of rare earth doped yttrium aluminium perovskite – R:YAlO{sub 3} (R = Nd, Eu and Er)

    Energy Technology Data Exchange (ETDEWEB)

    Basavalingu, B., E-mail: bbmysore@gmail.com [Department of Studies in Earth Science, University of Mysore, Mysore 570 006, Karnataka (India); Vijaya Kumar, M.S. [Institute of Space and Astronautical Science (ISAS), Japan Aerospace Exploration Agency (JAXA), 3-1-1 Yoshinodai, Sagamihara, Kanagawa 252-5210 (Japan); Girish, H.N. [Department of Studies in Earth Science, University of Mysore, Mysore 570 006, Karnataka (India); Yoda, S. [Institute of Space and Astronautical Science (ISAS), Japan Aerospace Exploration Agency (JAXA), 3-1-1 Yoshinodai, Sagamihara, Kanagawa 252-5210 (Japan)

    2013-03-05

    Highlights: ► High purity micro-crystalline R:YAP was synthesized by hydrothermal technique. ► The growth temperature does not exceed 700 °C in any step of the synthesis. ► The phase formation was sensitive to the nature of the synthesis temperature and the starting charge. ► R:YAP is considered as direct replacement for YAG owing to its lasing property. -- Abstract: Yttrium aluminium perovskite doped with rare earth ions is a promising material for several technological applications. It is considered as direct replacement for Yttrium Aluminum Garnet (YAG) owing to its structural simplicity and lasing property. It is also known for its mechanical and optical properties. High purity micro crystalline R:YAlO{sub 3} (R = Nd{sup 3+}, Eu{sup 3+} and Er{sup 3+}) is synthesized by employing hydrothermal supercritical fluid technique. The resultant materials were characterized using powder X-ray diffraction for structure and phase identification, scanning electron microscopy and energy dispersive X-ray analysis were performed for particle morphology, phase purity and stoichiometry. These monodispersed polycrystalline materials show high degree of phase purity, good control over the concentration of dopants and exhibit well developed morphological features.

  12. Rapid synthesis of single-phase bismuth ferrite by microwave-assisted hydrothermal method

    International Nuclear Information System (INIS)

    Cao, Wenqian; Chen, Zhi; Gao, Tong; Zhou, Dantong; Leng, Xiaonan; Niu, Feng; Zhu, Yuxiang; Qin, Laishun; Wang, Jiangying; Huang, Yuexiang

    2016-01-01

    This paper describes on the fast synthesis of bismuth ferrite by the simple microwave-assisted hydrothermal method. The phase transformation and the preferred growth facets during the synthetic process have been investigated by X-ray diffraction. Bismuth ferrite can be quickly prepared by microwave hydrothermal method by simply controlling the reaction time, which is further confirmed by Fourier Transform infrared spectroscopy and magnetic measurement. - Graphical abstract: Single-phase BiFeO 3 could be realized at a shortest reaction time of 65 min. The reaction time has strong influences on the phase transformation and the preferred growth facets. - Highlights: • Rapid synthesis (65 min) of BiFeO 3 by microwave-assisted hydrothermal method. • Reaction time has influence on the purity and preferred growth facets. • FTIR and magnetic measurement further confirm the pure phase.

  13. Structural archetypes in nickel(II) hybrid vanadates. Towards a directed hydrothermal synthesis

    International Nuclear Information System (INIS)

    Luis, R. Fernandez de; Urtiaga, M.K.; Mesa, J.L.; Rojo, T.; Arriortua, M.I.

    2009-01-01

    In the present work, we relate the modifications of the initial synthesis parameters (pH value, stoichiometry and concentration) with the different structural archetypes obtained in the {Ni/Bpy/VO} and {Ni/Bpe/VO} systems (4,4'-bipyridine (Bpy), 1,2-di(4-pyridyl) ethylene (Bpe)). The vanadium coordination is partially controlled by the hydrothermal synthesis conditions, and the final crystal structures depend on the synergetic interaction between the metal-organic subnets and the vanadium oxide subunits.

  14. Hydrothermal synthesis of porous Co(OH)2 nanoflake array film and ...

    Indian Academy of Sciences (India)

    2, April 2013, pp. 239–244. c Indian Academy of Sciences. Hydrothermal synthesis of porous Co(OH)2 nanoflake array film and its supercapacitor application. Z CHENa,∗. , Y CHENa, C ZUOa, S ZHOUa, A G XIAOa and A X PANb. aCollege of Chemistry and Chemical Engineering, Hunan University of Arts and Science, ...

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

    Science.gov (United States)

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

    2008-03-28

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

  16. Facile hydrothermal synthesis of CeO2 nanopebbles

    Indian Academy of Sciences (India)

    Administrator

    Abstract. Cerium oxide (CeO2) nanopebbles have been synthesized using a facile hydrothermal method. X-ray diffraction pattern (XRD) and transmission electron microscopy analyses confirm the presence of CeO2 nanopebbles. XRD shows the formation of cubic fluorite CeO2 and the average particle size estimated from.

  17. Facile template-free hydrothermal synthesis and microstrain ...

    Indian Academy of Sciences (India)

    Administrator

    electrodeposition (Kim et al 2006), template basis syn- thesis (Li et al 2000), thermal evaporation (Umar et al. 2006) and electrochemical deposition (Ko et al 2012). Among these techniques, preparing ZnO nanorods via hydrothermal route provides an easy and convenient method with high ability in controlling the physics ...

  18. Sol-Gel/Hydrothermal Synthesis of Mixed Metal Oxide

    African Journals Online (AJOL)

    Mixed metal oxides of titanium and zinc nanocomposites were prepared through sol-gel method under hydrothermal condition ... Keywords: Nanocomposites, Titanium dioxide, Zinc oxide, Particle sizes, Optical property, X-Ray Diffraction. ABSTRACT. 321 ... doping with other semiconductors like zinc oxide, aluminium oxide ...

  19. Hydrothermal synthesis, characterization, and magneticproperties of cobalt chromite nanoparticles

    Czech Academy of Sciences Publication Activity Database

    Zákutná, Dominika; Repko, A.; Matulková, I.; Nižňanský, Daniel; Ardu, A.; Cannas, C.; Mantlíková, Alice; Vejpravová, Jana

    2014-01-01

    Roč. 16, č. 2 (2014), 1-14 ISSN 1388-0764 R&D Projects: GA ČR GAP108/10/1250 Institutional support: RVO:68378271 ; RVO:61388980 Keywords : cobalt chromite * hydrothermal method * nanoparticles * size effect * multiferroic materials Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.184, year: 2014

  20. Synthesis of ZrO2 nanoparticles by hydrothermal treatment

    International Nuclear Information System (INIS)

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

    2014-01-01

    Zirconium oxide (zirconia, ZrO 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 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

  1. Facile template-free hydrothermal synthesis and microstrain ...

    Indian Academy of Sciences (India)

    Administrator

    method with high ability in controlling the physics of rods. Hydrothermal processing has some major differences from other techniques such as preparing the powders di- rectly from solution, ability to control the shape and size of structures, being highly reactive in sintering and not needed in calcination and milling process ( ...

  2. Fatty acid methyl esters synthesis from non-edible vegetable oils using supercritical methanol and methyl tert-butyl ether

    International Nuclear Information System (INIS)

    Lamba, Neha; Modak, Jayant M.; Madras, Giridhar

    2017-01-01

    Highlights: • FAMEs were synthesized from non-edible oils using supercritical MeOH and MTBE. • Effect of time, temperature, pressure and molar ratio on conversions was studied. • Rate constants of reaction with methanol and MTBE differ by an order of magnitude. • Non-catalytic supercritical reactions are one order faster than acid catalyzed synthesis. - Abstract: Fatty acid methyl esters (FAMEs) are useful as biodiesel and have environmental benefits compared to conventional diesel. In this study, these esters were synthesized non-catalytically from non-edible vegetable oils: neem oil and mahua oil with two different methylating agents: methanol and methyl tert-butyl ether (MTBE). The effects of temperature, pressure, time and molar ratio on the conversion of triglycerides were studied. The temperature was varied in the range of 523–723 K with molar ratios upto 50:1 and a reaction time of upto 150 min. Conversion of neem and mahua oil to FAMEs with supercritical methanol was found to be 83% in 15 min and 99% in 10 min, respectively at 698 K. Further, a conversion of 46% of mahua oil and 59% of neem oil was obtained in 15 min at 723 K using supercritical MTBE. The rate constants evaluated using pseudo first order reaction kinetics were in the range of 4.7 × 10 −6 to 1.0 × 10 −3 s −1 for the investigated range of temperatures. The activation energies obtained were in the range of 62–113 kJ/mol for the reaction systems investigated. The supercritical synthesis was found to be superior to the catalytic synthesis of the corresponding FAMEs.

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

    Science.gov (United States)

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

    2017-12-01

    Submarine hydrothermal vents are generally considered as the likely habitats for the origin and evolution of early life on Earth. In recent years, a novel hydrothermal system in Archean subseafloor has been proposed. In this model, highly alkaline and high temperature hydrothermal fluids were generated in basalt-hosted hydrothermal vents, where H 2 and CO 2 could be abundantly provided. These extreme conditions could have played an irreplaceable role in the early evolution of life. Nevertheless, sufficient information has not yet been obtained for the abiotic synthesis of amino acids, which are indispensable components of life, at high temperature and alkaline condition. This study aims to propose a new method for the synthesis of glycine in simulated Archean submarine alkaline vent systems. We investigated the formation of glycine from ethanolamine under conditions of high temperature (80-160 °C) and highly alkaline solutions (pH = 9.70). Experiments were performed in an anaerobic environment under mild pressure (0.1-8.0 MPa) at the same time. The results suggested that the formation of glycine from ethanolamine occurred rapidly and efficiently in the presence of metal powders, and was favored by high temperatures and high pressures. The experiment provides a new pathway for prebiotic glycine formation and points out the phenomenal influence of high-temperature alkaline hydrothermal vents in origin of life in the early ocean.

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

    Science.gov (United States)

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

    2017-12-01

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

  5. Hydrothermal synthesis of magnetic reduced graphene oxide sheets

    International Nuclear Information System (INIS)

    Shen, Jianfeng; Shi, Min; Ma, Hongwei; Yan, Bo; Li, Na; Ye, Mingxin

    2011-01-01

    Graphical abstract: An environmental friendly and efficient route for preparation of magnetic reduced graphene oxide composite with a one-step hydrothermal method was demonstrated. The reducing process was accompanied by generation of magnetic nanoparticles. Highlights: → A one-step hydrothermal method for preparation of MN-CCG was demonstrated. → Glucose was used as the 'green' reducing agent. → The reducing process was accompanied by generation of magnetic nanoparticles. → The prepared MN-CCG is highly water suspendable and sensitive to magnetic field. -- Abstract: We demonstrated an environmental friendly and efficient route for preparation of magnetic reduced graphene oxide composite (MN-CCG). Glucose was used as the reducing agent in this one-step hydrothermal method. The reducing process was accompanied by generation of magnetic nanoparticles. The structure and composition of the nanocomposite was confirmed by Fourier transform infrared spectroscopy, Raman spectroscopy, X-ray diffraction, thermal gravimetric analysis, atomic force microscopy and transmission electron microscopy. It was found that the prepared MN-CCG is highly water suspendable and sensitive to magnetic field.

  6. Synthesis and characterization of nanosized ceria powders by microwave-hydrothermal method

    International Nuclear Information System (INIS)

    Bonamartini Corradi, A.; Bondioli, F.; Ferrari, A.M.; Manfredini, T.

    2006-01-01

    Nanocrystalline ceria powders (CeO 2 ) have been prepared by adding NaOH to a cerium ammonium nitrate aqueous solution under microwave-hydrothermal conditions. In particular the effect of the synthesis conditions (time, pressure and concentration of both the precursor and the precipitant agent solutions) on the physical properties of the crystals have been evaluated. Microwave-hydrothermal treatment of 5 min at 13.4 atm allows to obtain almost crystallized powders (amorphous phase 4%) as underlined by Rietveld-reference intensity ratio (RIR) results

  7. Hydrothermal synthesis of layered iron-chalcogenide superconductors and related compounds

    Energy Technology Data Exchange (ETDEWEB)

    Pachmayr, Ursula Elisabeth

    2017-04-06

    This thesis provides a new preparative approach to iron-chalcogenide based superconductors. The hydrothermal synthesis of anti-PbO type FeSe, which can be seen as basis structure of the compounds of interest was successfully developed. Along with this, some insights regarding the influence of synthesis parameters were gained featuring a basis for further hydrothermal syntheses of new iron-chalcogenide compounds. The potential of this method, primarily the extension of the so far limited accessibility of iron-chalcogenide based superconductors by solid-state sythesis, was revealed within the present work. The solid-solution FeSe{sub 1-x}S{sub x} was prepared for the whole substitution range, whereas solid-state synthesis exhibits a solubility limit at x = 0.3. Furthermore, the new compounds [(Li{sub 0.8}Fe{sub 0.2})OH]FeX (X = Se, S) were synthesized which are exclusively accessible via hydrothermal method. The compounds, where layers of (Li{sub 0.8}Fe{sub 0.2})OH alternate with FeX layers, feature exceptional physical properties, notably a coexistence of superconductivity and ferromagnetism. They were intensively studied within this work. By combination of solid-state and hydrothermal ion-exchange synthesis even large crystals necessary for subsequent physical measurements are accessible. Apart from these layered iron-chalcogenide superconductors, further compounds which likewise exhibit building blocks of edge-sharing FeSe{sub 4} tetrahedra were found via this synthesis method. The iron selenides A{sub 2}Fe{sub 4}Se{sub 6} (A = K, Rb, Cs) consist of double chains of [Fe{sub 2}Se{sub 3}]{sup 1-}, whereas a new compound Na{sub 6}(H{sub 2}O){sub 18}Fe{sub 4}Se{sub 8} exhibits [Fe{sub 4}Se{sub 8}]{sup 6-} 'stella quadrangula' clusters. This structural diversity as well as the associated physical properties of the compounds demonstrates the numerous capabilities of hydrothermal synthesis in the field of iron-chalcogenide compounds. In particular with regard

  8. Hydrothermal synthesis and characterization of polycrystalline gadolinium aluminum perovskite (GdAlO3, GAP

    Directory of Open Access Journals (Sweden)

    N. Girish H.

    2015-06-01

    Full Text Available Gadolinium aluminum perovskite (GdAlO3, GAP is a promising high temperature ceramic material, known for its wide applications in phosphors. Polycrystalline gadolinium aluminum perovskites were synthesized using a precursor of co-precipitate gel of GdAlO3 by employing hydrothermal supercritical fluid technique under pressure and temperature ranging from 150 to 200 MPa and 600 to 700 °C, respectively. The resulted products of GAP were studied using the characterization techniques, such as powder X-ray diffraction analysis (XRD, infrared spectroscopy (IR, scanning electron microscopy (SEM and energy dispersive analysis of X-ray (EDX. The X-ray diffraction pattern matched well with the reported orthorhombic GAP pattern (JCPDS-46-0395.

  9. Hydrothermal Synthesis of Disulfide-Containing Uranyl Compounds. In Situ Ligand Synthesis versus Direct Assembly

    Energy Technology Data Exchange (ETDEWEB)

    Rowland, Clare E. [George Washington Univ., Washington, DC (United States); Belai, Nebebech [George Washington Univ., Washington, DC (United States); Knope, Karah E. [George Washington Univ., Washington, DC (United States); Cahill, Christopher L. [George Washington Univ., Washington, DC (United States)

    2010-01-29

    Three disulfide-containing uranyl compounds, [UO2(C7H4O2S)3]·H2O (1), [UO2(C7H4O2S)2(C7H5O2S)] (2), and [UO2(C7H4O2S)4] (3) have been hydrothermally synthesized. Both in situ disulfide bond formation from 3- and 4-mercaptobenzoic acid (C7H5O2S, MBA) to yield 3,3'- and 4,4'-dithiobisbenzoic acid (C14H8O4S2, DTBA) and direct assembly with the presynthesized dimeric ligands have been explored. While the starting materials 4-MBA and 4,4'-DTBA both yield 2 via in situ ligand synthesis and direct assembly, respectively, we observe the formation of 1 from the starting material 3-MBA via in situ ligand synthesis and of 3 from the direct assembly of the uranyl cation with 3,3'-DTBA. Concurrently with the synthesis of 1 and 2, we have observed the in situ formation of the crystalline dimeric organic species, 3,3'-DTBA, [(C7H5O2S)2] (4) and 4,4'-DTBA, [(C7H5O2S)2] (5). Herein we report the synthesis and crystallographic characterization of 1-5, as well as observations regarding the utility of product formation via direct assembly and in situ ligand synthesis.

  10. Hydrothermal synthesis of tungsten doped tin dioxide nanocrystals

    Science.gov (United States)

    Zhou, Cailong; Li, Yufeng; Chen, Yiwen; Lin, Jing

    2018-01-01

    Tungsten doped tin dioxide (WTO) nanocrystals were synthesized through a one-step hydrothermal method. The structure, composition and morphology of WTO nanocrystals were characterized by x-ray diffraction, x-ray photoelectron spectroscopy, energy dispersive x-ray spectroscopy, UV-vis diffuse reflectance spectra, zeta potential analysis and high-resolution transmission electron microscopy. Results show that the as-prepared WTO nanocrystals were rutile-type structure with the size near 13 nm. Compared with the undoped tin dioxide nanocrystals, the WTO nanocrystals possessed better dispersity in ethanol phase and formed transparent sol.

  11. Hydrothermal synthesis of nanostructured spinel lithium manganese oxide

    Science.gov (United States)

    Liu, Zhanqiang; Wang, Wen-lou; Liu, Xianming; Wu, Minchang; Li, Dan; Zeng, Zhen

    2004-04-01

    Nanostructured spherical spinel lithium manganese oxide (LiMnO) with about 200 nm in diameter was synthesized for the first time by mild hydrothermal method. The formation of the nanostructured spheres was through self-assembly of the nanoparticles and nanobelts. The influence of the reaction temperature and the time of formation of the nanostructures have been systematically studied. The thermal stability of the nanostructures has been examined by heating-treatment at different temperatures. Powder X-ray diffraction, transmission electron microscopy, high-resolution transmission electron microscopy, thermogravimetric analysis and inductively coupled plasma-atomic emission spectroscopy were used to characterize the products.

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

    Science.gov (United States)

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

    2017-03-01

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

  13. Abiotic synthesis of organic compounds from carbon disulfide under hydrothermal conditions.

    Science.gov (United States)

    Rushdi, Ahmed I; Simoneit, Bernd R T

    2005-12-01

    Abiotic formation of organic compounds under hydrothermal conditions is of interest to bio, geo-, and cosmochemists. Oceanic sulfur-rich hydrothermal systems have been proposed as settings for the abiotic synthesis of organic compounds. Carbon disulfide is a common component of magmatic and hot spring gases, and is present in marine and terrestrial hydrothermal systems. Thus, its reactivity should be considered as another carbon source in addition to carbon dioxide in reductive aqueous thermosynthesis. We have examined the formation of organic compounds in aqueous solutions of carbon disulfide and oxalic acid at 175 degrees C for 5 and 72 h. The synthesis products from carbon disulfide in acidic aqueous solutions yielded a series of organic sulfur compounds. The major compounds after 5 h of reaction included dimethyl polysulfides (54.5%), methyl perthioacetate (27.6%), dimethyl trithiocarbonate (6.8%), trithianes (2.7%), hexathiepane (1.4%), trithiolanes (0.8%), and trithiacycloheptanes (0.3%). The main compounds after 72 h of reaction consisted of trithiacycloheptanes (39.4%), pentathiepane (11.6%), tetrathiocyclooctanes (11.5%), trithiolanes (10.6%), tetrathianes (4.4%), trithianes (1.2%), dimethyl trisulfide (1.1%), and numerous minor compounds. It is concluded that the abiotic formation of aliphatic straight-chain and cyclic polysulfides is possible under hydrothermal conditions and warrants further studies.

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

    Energy Technology Data Exchange (ETDEWEB)

    Sanjeewa, Liurukara D.; McMillen, Colin D.; Willett, Daniel; Chumanov, George; Kolis, Joseph W., E-mail: kjoseph@clemson.edu

    2016-04-15

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

  15. Coprecipitation-assisted hydrothermal synthesis of PLZT hollow nanospheres

    International Nuclear Information System (INIS)

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

    2010-01-01

    Lanthanum-modified lead zirconate titanate Pb 1-x La x (Zr 1-y Ti y )O 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.

  16. Facile Hydrothermal Synthesis of Tellurium Nanostructures for Solar Cells

    Directory of Open Access Journals (Sweden)

    M. Panahi-Kalamuei

    2014-10-01

    Full Text Available Tellurium (Te nanostructures have been successfully synthesized via a simple hydrothermal methodfrom the reaction of a TeCl4 aqueous solution with thioglycolic acid (TGA as a reductant. TGA can be easily oxidized to the corresponding disulfide [SCH2CO2H]2, which in turn can reduce TeCl4 to Te. The obtained Te was characterized by XRD, SEM, EDS, and DRS. The effect of reducing agent on morphology and size of the products were also studied. Additionally, Te thin film was deposited on the FTO-TiO2 by Dr- blading then employed to solar cell application and measured open circuit voltage (Voc, short circuit current (Isc, and fill factor (FF were determined as well. The studies showed that particle morphology and sizes play crucial role on solar cell efficiencies.

  17. Synthesis of Morphology Controlled Aluminum Oxide by Hydrothermal Reaction

    Energy Technology Data Exchange (ETDEWEB)

    Yang, L; Yin, S; Sato, T, E-mail: tsusato@tagen.tohoku.ac.jp [Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai 980-8577 (Japan)

    2011-10-29

    Plate-like and wire-like aluminum oxides were successfully synthesized by hydrothermal method without any template additives. Al(NO{sub 3}){sub 3{center_dot}}9H{sub 2}O aqueous solution and precipitator were mixed and introduced to a Teflon lined autoclave, followed by heat treatment at 200deg. C for 24 h. By controlling the concentration of starting material and precipitator, the products with different morphologies were selectively obtained, i.e., the 2-dimensional platelike particles with a diameter of about 8{mu}m were synthesized at low aluminum concentration (0.1 mol/L), while 1-dimensional wire-like products of about 10{mu}m in length were synthesized at high aluminum concentration (0.2 mol/L). The plate-like particles and wire-like particles consisted of single phase of aluminum oxide hydroxide (boehmite, AlOOH) and the sodium aluminate, respectively.

  18. Hydrothermal Synthesis of Nanoclusters of ZnS Comprised on Nanowires

    OpenAIRE

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

    2013-01-01

    Cetyltrimethyl ammonium bromide cationic (CTAB) surfactant was used as template for the synthesis of nanoclusters of ZnS composed of nanowires, by hydrothermal method. The structural and morphological studies were performed by using X-ray diffraction (XRD), scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM) techniques. The synthesized ZnS nanoclusters are composed of nanowires and high yield on the substrate was observed. The ZnS nanocrystalline co...

  19. Single step hydrothermal based synthesis of M(II)Sb2O6 (M = Cd ...

    Indian Academy of Sciences (India)

    1987) and CoSb2O6 (Reimers and Greedan 1989) could be prepared at temperatures 1273, 1173 and 1323 K, respec- tively. Herein, we detail the results of our investigation based on hydrothermal reaction of the ilmenite NaSbO3 with the divalent metal salt solutions for the successful synthesis of. CdSb2O6 and ZnSb2O6.

  20. Structural archetypes in nickel(II) hybrid vanadates. Towards a directed hydrothermal synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Luis, R. Fernandez de; Urtiaga, M.K. [Dpto. Mineralogia y Petrologia, Facultad de Ciencia y Tecnologia, Universidad del Pais Vasco/UPV/EHU, Apdo. 644, 48080 Bilbao (Spain); Mesa, J.L.; Rojo, T. [Dpto. Quimica Inorganica, Facultad de Ciencia y Tecnologia, Universidad del Pais Vasco UPV/EHU, Apdo. 644, 48080 Bilbao (Spain); Arriortua, M.I. [Dpto. Mineralogia y Petrologia, Facultad de Ciencia y Tecnologia, Universidad del Pais Vasco/UPV/EHU, Apdo. 644, 48080 Bilbao (Spain)], E-mail: maribel.arriortua@ehu.es

    2009-07-01

    In the present work, we relate the modifications of the initial synthesis parameters (pH value, stoichiometry and concentration) with the different structural archetypes obtained in the {l_brace}Ni/Bpy/VO{r_brace} and {l_brace}Ni/Bpe/VO{r_brace} systems (4,4'-bipyridine (Bpy), 1,2-di(4-pyridyl) ethylene (Bpe)). The vanadium coordination is partially controlled by the hydrothermal synthesis conditions, and the final crystal structures depend on the synergetic interaction between the metal-organic subnets and the vanadium oxide subunits.

  1. Materials processing using supercritical fluids

    Directory of Open Access Journals (Sweden)

    Orlović Aleksandar M.

    2005-01-01

    Full Text Available One of the most interesting areas of supercritical fluids applications is the processing of novel materials. These new materials are designed to meet specific requirements and to make possible new applications in Pharmaceuticals design, heterogeneous catalysis, micro- and nano-particles with unique structures, special insulating materials, super capacitors and other special technical materials. Two distinct possibilities to apply supercritical fluids in processing of materials: synthesis of materials in supercritical fluid environment and/or further processing of already obtained materials with the help of supercritical fluids. By adjusting synthesis parameters the properties of supercritical fluids can be significantly altered which further results in the materials with different structures. Unique materials can be also obtained by conducting synthesis in quite specific environments like reversed micelles. This paper is mainly devoted to processing of previously synthesized materials which are further processed using supercritical fluids. Several new methods have been developed to produce micro- and nano-particles with the use of supercritical fluids. The following methods: rapid expansion of supercritical solutions (RESS supercritical anti-solvent (SAS, materials synthesis under supercritical conditions and encapsulation and coating using supercritical fluids were recently developed.

  2. Mild Hydrothermal Synthesis of Ni–Cu Nanoparticles

    Directory of Open Access Journals (Sweden)

    G. H. Mohamed Saeed

    2010-01-01

    Full Text Available Magnetic Ni-rich Ni–Cu nanoparticles with Ni : Cu mass ratio (S of 2.0 and 2.6 were prepared using a mixture of polyoxyethylene (10 isooctylphenyl ether (Triton X-100 and sodium dodecyl sulfate (SDS in a mild hydrothermal condition at 95ºC. X-ray diffractometry (XRD showed that the nanoparticles prepared at S=2.0 possessed Ni–Cu alloy characteristic whereas the characteristic was absent at S=2.6. The XRD data was enhanced by Fourier transform infrared spectroscopy (FTIR which exhibited metal-metal (Ni–Cu band at 455 cm−1. Based on transmission electron microscopy (TEM, the average particle sizes for the nanoparticles prepared at S=2.0 and 2.6 were in the range of 19–23 nm. The as-prepared nanoparticles exhibited paramagnetic behaviour measured using a vibrating sample magnetometer (VSM and the specific saturation magnetization decreased at the higher concentration of Ni.

  3. Hydrothermal Synthesis and Crystal Structure of Ionic Conductive Metal Tungstates

    Energy Technology Data Exchange (ETDEWEB)

    Shimanouchi, R F; Tsuji, T; Yagi, R; Matsumoto, Y; Nishizawa, H, E-mail: rshima@kochi-u.ac.jp [Department of Natural Science, Faculty of Science, Kochi University, 2-5-1, Akebono-cho, Kochi city, KOCHI 780 (Japan)

    2011-10-29

    Trivalent ion conducting materials with the Sc{sub 2}(WO{sub 4}){sub 3}-type crystal structure, A{sub 2}(WO{sub 4}){sub 3} (A = Sc, In, Y) and solid solutions, (Sc,In){sub 2}(WO{sub 4}){sub 3} were synthesized via an autogenous hydrothermal reaction of aqueous solutions of ScCl{sub 3}, InCl{sub 3}, Y(CH{sub 3}COO){sub 3}, and H{sub 2}WO{sub 4} in a Teflon-lined mini-autoclave for 5 h at a temperature of 523 K. Fine powder samples were pressed into discs under 50 MPa and sintered at 1273 K for 10 h. The impedance measurements of sintered materials showed the dependence of electric conductivity on the size of the conducting cation. From the precise crystallographic data obtained by Rietveld refinements of solid solutions, it was considered that the change of volume of Sc(In)O{sub 6}-octahedra and WO{sub 4}-tetrahedra.

  4. Hydrothermal synthesis of siderite nano-particles and characterizations

    Science.gov (United States)

    Oza, Mahatta; Joshi, M. J.

    2017-05-01

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

  5. Hydrothermal synthesis of highly water-dispersible anatase nanocrystals from transparent aqueous sols of titanate colloids

    International Nuclear Information System (INIS)

    Ban, Takayuki; Tanaka, Yusuke; Ohya, Yutaka

    2011-01-01

    Transparent colloidal aqueous solutions of anatase nanocrystals were hydrothermally synthesized from aqueous transparent sols with tetramethylammonium titanate colloids, the surfaces of which were modified with citric acid, by structural conversion of the titanate to anatase. This modification hindered coalescence of the titanate colloids during the hydrothermal synthesis. Although the amount of citric acid adsorbed on the colloids was reduced during hydrothermal treatment, a small amount of citric acid was adsorbed on the resulting anatase nanocrystals. Moreover, the use of the titanate colloids as a precursor was compared with the use of a citrato Ti complex, tetramethylammonium citratotitanate. The hydrothermal treatment of the transparent aqueous solutions of the Ti complex yielded opaque solutions with large anatase colloids, suggesting that the titanate colloids were useful for preparing transparent anatase colloidal solutions. Because the shape and size of resulting colloids may be dependent on the size and shape of starting colloids, the use of titanate colloids as a precursor may make it easy to control size and shape of anatase colloids.

  6. Synthesis of light-selective poly(ethylene-co-vinyl acetate) nanofilms in supercritical carbon dioxide

    Science.gov (United States)

    Xu, William (Zhiming)

    Due to the increased requirements of environmental protection, significant effort has been made to develop new "green" chemistry and engineering methods. Two effective approaches for "green" processes are: (1) to employ routes with fewer synthetic and separation steps, and (2) to replace volatile organic solvents with environmentally friendly solvents. Supercritical carbon dioxide (scCO2) has emerged as such a viable "green" alternative to organic solvents for several applications including extraction, polymerization, and nanotechnology, etc. In addition, it is an enabling solvent, allowing new types of chemistry and materials to be formed. In order to effectively utilize scCO2, it is required to study its effect on the relevant chemical process. This thesis focuses on the copolymerization of ethylene and vinyl acetate in scCO2, and the application of scCO2 in the synthesis of novel poly(vinyl acetate) (PVAc) and poly(ethylene-co-vinyl acetate) (PEVA) nanocomposites. Firstly, the kinetics of the process was investigated. The thermal decomposition of the free-radical initiator diethyl peroxydicarbonate (DEPDC) was monitored by in situ attenuate total reflection Fourier transform infrared spectroscopy (ATR-FTIR) in heptane, and in scCO2. The rate constant and activation energy of the thermal decomposition of DEPDC in scCO2 were determined, and a decomposition mechanism was proposed. Further, with a knowledge of the initiator kinetics, in situ ATR-FTIR was employed to monitor the initial formation of copolymers of ethylene and vinyl acetate during polymerization in scCO2. The reactivity ratios for the copolymerization of ethylene and vinyl acetate in scCO2 were determined using both the Kelen-Tudos and the non-linear least-squares methods. The potential of scCO2 was further examined to synthesize advanced and novel nanomaterials based on an understanding of the polymerization mechanism. A novel one-step synthesis route was developed for making silica

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

    Science.gov (United States)

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

    2017-01-01

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

  8. Bismuth molybdate catalysts prepared by mild hydrothermal synthesis: Influence of pH on the selective oxidation of propylene

    DEFF Research Database (Denmark)

    Schuh, Kirsten; Kleist, Wolfgang; Høj, Martin

    2015-01-01

    A series of bismuth molybdate catalysts with relatively high surface area was prepared via mild hydrothermal synthesis. Variation of the pH value and Bi/Mo ratio during the synthesis allowed tuning of the crystalline Bi-Mo oxide phases, as determined by X-ray diffraction (XRD) and Raman spectrosc...

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

    International Nuclear Information System (INIS)

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

    2013-01-01

    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

  10. Production of Yttria-doped zirconia by hydrothermal synthesis: thermodynamical analysis

    International Nuclear Information System (INIS)

    Nascimento Dias, A.J. do; Ogasawara, T.

    1993-01-01

    After a short review of the literature on Hydrothermal Synthesis of Zirconia, the computation and construction of the Standard Hydrogen Scale Potential versus pH diagrams have been performed starting from data supplied by Thermodynamic Tables. Diagrams have been developed for several temperatures (in the range 298.15 K up to 573.15 K) and for activities of the Y and Zr in the aqueous solution ranging from 0,0001 M up to 1 M. The resultant diagrams have been analyzed and interpreted. The results gotten from the study give good elucidation of the phenomena taking place in the hydrothermal treatment of the Zirconia Powders inside an autoclave at temperatures between 473.15 K and 573.15 K. The conditions for crystallization of the doped zirconia at temperatures lower than 573.15 K are better visualized. (author)

  11. Controlled Synthesis of Manganese Dioxide Nanostructures via a Facile Hydrothermal Route

    Directory of Open Access Journals (Sweden)

    Suh Cem Pang

    2012-01-01

    Full Text Available Manganese dioxide nanostructures with controllable morphological structures and crystalline phases were synthesized via a facile hydrothermal route at low temperatures without using any templates or surfactants. Both the aging duration and aging temperatures were the main synthesis parameters used to influence and control the rate of morphological and structural evolution of MnO2 nanostructures. MnO2 nanostructures comprise of spherical nanoparticulate agglomerates and highly amorphous in nature were formed at lower temperature and/or short aging duration. In contrast, MnO2 nanostructures of sea-urchin-like and nanorods-like morphologies and nanocrystalline in nature were prepared at the combined higher aging temperatures and longer aging durations. These nanostructures underwent notable phase transformation from δ-MnO2 to α-MnO2 upon prolonged hydrothermal aging duration and exhibited accelerated rate of phase transformation at higher aging temperature.

  12. Microwave hydrothermal synthesis and characterization of PZT 52/48 powders

    International Nuclear Information System (INIS)

    Teixeira, G.F.; Gasparotto, G.; Santos, N.A.; Zaghete, M.A.; Varela, J.A.; Longo, E.

    2009-01-01

    Full text: Lead Zirconate Titanate (PZT) is a ceramic witch has great interest because of their ferroelectric, piezoelectric, and other electrical properties. In this work Pb(ZrxTi1-x)O3 powders were synthesized by microwave hydrothermal synthesis (M-H) at 180°C without excess lead content. This method allows obtaining particles whit nanometer size, good stoichiometric controls, high purity and crystalline degree at low temperatures and short times of synthesis. Powders were synthesized with molar concentration of 0.15 mol.L -1 during different times: 30 min, 2, 4, 6 and 8 h. After that the powders were characterized by X-ray diffraction (XRD), Field Emission Gun (FEG) and photoluminescence (PL). Through analysis it is observed that the crystalline phase of PZT is obtained from 2 hours of synthesis and this same time also presents more intense PL emission. (author)

  13. FORMATION MECHANISM OF NANOSIZED TIN OXIDE (SnO2 POWDER DURING HYDROTHERMAL SYNTHESIS

    Directory of Open Access Journals (Sweden)

    M. Ozan ÖZER

    2011-06-01

    Full Text Available Preparation of nanosized SnO₂ electroceramic powders via hydrothermal synthesis was investigated as a function of initial concentration and treatment time in order to understand the formation and growth mechanisms. SnO₂ powder was successfully synthesized from the hydrous tin oxide by hydro- thermal synthesis at 200°C. Crystalline SnO₂ particles with a specific surface area as high as 170 m₂/g were produced in a single step without requiring any calcination process. As initial concentration of metal cation increases from 0.0125 to 0.05 M, an Ostwald ripening type growth process was observed in the crystallite size from 3.1 to 4.6 nm. Evolution of tin oxide particles was also investigated by al- tering the treatment time from 1 to 24 h and a diffusion controlled growth behavior was observed as a function of synthesis time.

  14. Hydrothermal synthesis of silica rich zeolites and microporous martials

    International Nuclear Information System (INIS)

    Durrani, S.K.; Chughtai, N.A.; Akhtar, J.; Arif, M.; Ahmed, M.

    1999-01-01

    A fast crystallization method for synthesis of silica rich aluminosilicate and ferro silicate zeotype materials has been reported. The method also permits for the complete crystallization of silico alumino phosphate microporous materials. Aluminosilicate and ferro silicate silica rich zeotype materials and silico alumino phosphate microporous materials have been synthesized from the reaction mixture of colloidal silica sol, reactive aluminum, ferrous and phosphorous salts, and the essential organic templates at 373-473 K and were characterized by TG/DTA/DSC, X-ray diffraction, scanning electron microscopy and other analytical techniques. Crystallinity and unit cell parameters of the synthesized materials were found to be the function of Al and Fe content of zeolites. (author)

  15. Simulation for scale-up of a confined jet mixer for continuous hydrothermal flow synthesis of nanomaterials

    OpenAIRE

    Ma, CY; Liu, JJ; Zhang, Y; Wang, XZ

    2015-01-01

    Reactor performance of confined jet mixers for continuous hydrothermal flow synthesis of nanomaterials is investigated for the purpose of scale-up from laboratory scale to pilot-plant scale. Computational fluid dynamics (CFD) models were applied to simulate hydrothermal fluid flow, mixing and heat transfer behaviours in the reactors at different volumetric scale-up ratios (up to 26 times). The distributions of flow and heat transfer variables were obtained using ANSYS Fluent with the tracer c...

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

    Science.gov (United States)

    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

  17. Synthesis and characterization of CuO flower-nanostructure processing by a domestic hydrothermal microwave

    Energy Technology Data Exchange (ETDEWEB)

    Volanti, D.P. [Laboratorio Interdisciplinar em Ceramica, Departamento de Fisico-Quimica, Instituto de Quimica, Universidade Estadual Paulista, P.O. Box 355, 14801-907 Araraquara, SP (Brazil); Keyson, D. [Laboratorio de Ensino de Ciencias e Laboratorio de Combustiveis e Materiais, Departamento de Quimica, Universidade Federal da Paraiba, 58051-900 Joao Pessoa, PB (Brazil); Cavalcante, L.S. [Laboratorio Interdisciplinar de Eletroquimica e Ceramica, Departamento de Quimica, Universidade Federal de Sao Carlos, P.O. Box 676, 13565-905 Sao Carlos, SP (Brazil)], E-mail: laeciosc@bol.com.br; Simoes, A.Z. [Laboratorio Interdisciplinar em Ceramica, Departamento de Fisico-Quimica, Instituto de Quimica, Universidade Estadual Paulista, P.O. Box 355, 14801-907 Araraquara, SP (Brazil); Joya, M.R. [Departamento de Fisica, Universidade Federal de Sao Carlos, P.O. Box 676, 13565-905 Sao Carlos, SP (Brazil); Longo, E.; Varela, J.A. [Laboratorio Interdisciplinar em Ceramica, Departamento de Fisico-Quimica, Instituto de Quimica, Universidade Estadual Paulista, P.O. Box 355, 14801-907 Araraquara, SP (Brazil); Pizani, P.S. [Departamento de Fisica, Universidade Federal de Sao Carlos, P.O. Box 676, 13565-905 Sao Carlos, SP (Brazil); Souza, A.G. [Laboratorio de Ensino de Ciencias e Laboratorio de Combustiveis e Materiais, Departamento de Quimica, Universidade Federal da Paraiba, 58051-900 Joao Pessoa, PB (Brazil)

    2008-07-14

    The synthesis and characterization of CuO flower-nanostructure processed in domestic hydrothermal microwave oven was presented. Phase analysis was carried out using X-ray diffraction (XRD) and micro-Raman scattering (MRS) and the results confirmed the CuO flower-nanostructure as a single-phase. The field-emission scanning electron microscopy (FEG-SEM) was used to estimate the average spheres diameter while transmission electron microscope (TEM) to observe the thorn of the flower-nanostructures. The mechanism of CuO flower-nanostructures formation is proposed and explained.

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

    Science.gov (United States)

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

    2017-05-01

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

  19. Synthesis and characterization of CuO flower-nanostructure processing by a domestic hydrothermal microwave

    International Nuclear Information System (INIS)

    Volanti, D.P.; Keyson, D.; Cavalcante, L.S.; Simoes, A.Z.; Joya, M.R.; Longo, E.; Varela, J.A.; Pizani, P.S.; Souza, A.G.

    2008-01-01

    The synthesis and characterization of CuO flower-nanostructure processed in domestic hydrothermal microwave oven was presented. Phase analysis was carried out using X-ray diffraction (XRD) and micro-Raman scattering (MRS) and the results confirmed the CuO flower-nanostructure as a single-phase. The field-emission scanning electron microscopy (FEG-SEM) was used to estimate the average spheres diameter while transmission electron microscope (TEM) to observe the thorn of the flower-nanostructures. The mechanism of CuO flower-nanostructures formation is proposed and explained

  20. Use of supercritical fluid solution expansion processes for drug delivery, particle synthesis, and thin film deposition

    Energy Technology Data Exchange (ETDEWEB)

    Hybertson, B.M.

    1992-01-01

    Properties of the gases and aerosols resulting from the expansion of supercritical fluid solutions were studied. Film deposition, particle formation, and drug delivery processes using supercritical fluids were developed. Thin films of palladium, copper, aluminum, silver, and silicon dioxide were deposited by a method called supercritical fluid transport-chemical deposition (SFT-CD). In each case, a precursor compound was dissolved in a supercritical fluid and the solution was allowed to expand through a restrictor nozzle into a reaction chamber at subcritical pressure, resulting in the formation of aerosol particles of the precursor. A chemical reaction was induced to occur at the surface of a substrate, resulting in deposition of a thin film. Micron-sized particles of aluminum fluoride and copper oxide were synthesized by a method called supercritical fluid transport-chemical formation of particles (SFT-CFP). The process was similar to that in SFT-CD, but the chemical reactions were induced to occur in the gas phase instead of at a substrate surface, resulting in the formation of fine particles. A new method of pulmonary drug delivery called supercritical fluid drug delivery (SFDD) was conceived and demonstrated. In SFDD a drug compound is dissolved in a supercritical fluid, and the solution is allowed to expand through a restrictor nozzle. The resultant aerosol is directly inhaled by a human or animal subject and the fine drug particles are deposited in the lungs. Menthol, vanillin, camphor, cholesterol, Sudan III, and Oil Blue N were used as model drug compounds for SFDD. Delivery of [alpha]-tocopherol to rat lung tissue was demonstrated, with observed increases of 80-290% above background levels.

  1. Applications of subcritical and supercritical water conditions for extraction, hydrolysis, gasification, and carbonization of biomass: a critical review

    Directory of Open Access Journals (Sweden)

    D. Lachos-Perez

    2017-06-01

    Full Text Available This review summarizes the recent essential aspects of subcritical and supercritical water technology applied tothe extraction, hydrolysis, carbonization, and gasification processes. These are clean and fast technologies which do not need pretreatment, require less reaction time, generate less corrosion and residues, do not usetoxic solvents, and reduce the synthesis of degradation byproducts. The equipment design, process parameters, and types of biomass used for subcritical and supercritical water process are presented. The benefits of catalysis to improve process efficiency are addressed. Bioactive compounds, reducing sugars, hydrogen, biodiesel, and hydrothermal char are the final products of subcritical and supercritical water processes. The present review also revisits advances of the research trends in the development of subcriticaland supercritical water process technologies.

  2. Time-resolved neutron diffraction analyses of hydrothermal synthesis using a novel autoclave cell

    International Nuclear Information System (INIS)

    Polak, E.; Munn, J.; Barnes, P.; Tarling, S.E.

    1990-01-01

    An autoclave cell has been designed for performing time-resolved neutron diffraction analyses of the dynamic processes occurring during hydrothermal syntheses under hostile (corrosive and explosive) conditions: Such conditions include those of hot NaOH/NaOD solutions and pressurized steam. The cell is also capable of measuring differential pressures and accurate sample temperatures as required for the study of reactions which are temperature sensitive. The cell is described and examples of its successful use are given illustrating the synthesis of basic zeolites and a layered calcium silicate hydrate. This technique has considerable potential for studying a variety of synthesis processes of industrial importance, such as in the production of catalysts and the hydration of cements. (orig.)

  3. Synthesis of Mesoporous Nanocrystalline Zirconia by Surfactant-Assisted Hydrothermal Approach.

    Science.gov (United States)

    Nath, Soumav; Biswas, Ashik; Kour, Prachi P; Sarma, Loka S; Sur, Ujjal Kumar; Ankamwar, Balaprasad G

    2018-08-01

    In this paper, we have reported the chemical synthesis of thermally stable mesoporous nanocrystalline zirconia with high surface area using a surfactant-assisted hydrothermal approach. We have employed different type of surfactants such as CTAB, SDS and Triton X-100 in our synthesis. The synthesized nanocrystalline zirconia multistructures exhibit various morphologies such as rod, mortar-pestle with different particle sizes. We have characterized the zirconia multistructures by X-ray diffraction study, Field emission scanning electron microscopy, Attenuated total refection infrared spectroscopy, UV-Vis spectroscopy and photoluminescence spectroscopy. The thermal stability of as synthesized zirconia multistructures was studied by thermo gravimetric analysis, which shows the high thermal stability of nanocrystalline zirconia around 900 °C temperature.

  4. Development of novel micro swirl mixer for producing fine metal oxide nanoparticles by continuous supercritical hydrothermal method.

    Science.gov (United States)

    Kawasaki, Shin-ichiro; Sue, Kiwamu; Ookawara, Ryuto; Wakashima, Yuichiro; Suzuki, Akira

    2010-01-01

    Novel micro swirl mixers were developed to synthesize nanoparticles, and the effect of their mixing performance on the characteristics of the synthesized nanoparticles was determined. The results were compared with those obtained using simple T-shaped mixers under the same reaction conditions. The synthesis of NiO, whose characteristics depend on the mixing performance of the mixer, was chosen as a model reaction. Initial investigations highlighted that the average particle size decreased from 32 to 23 to 20 nm as the inner diameter of the swirl mixers was decreased from 3.2 mm (Swirl mixer, SM-3.2) to 0.8 mm (Micro swirl mixer, MSM-0.8) to 0.5 mm (Micro swirl mixer, MSM-0.5), respectively. On the other hand, a similar decrease in the average particle size from 34 to 20 nm was observed with a decrease in the inner diameter of the T-shaped mixers from 1.3 mm (Tee union, T-1.3) to 0.3 mm (Micro tee union, T-0.3), respectively. Further, narrow particle size distributions were observed with a decrease in the inner diameter of each mixer. Furthermore, a computational fluid dynamics (CFD) simulation indicated an excellent mixing mechanism, which contributed to the improvement in the heating rate and the formation of nanoparticles of smaller size with a narrow particle size distribution. The result presented here indicates that the micro swirl mixers produce high-quality metal oxide nanoparticles. The size of the obtained particles with improved size distributions was comparable to that of the particles obtained using the T-shaped mixers, although the inner diameter of the swirl mixers was larger. Therefore, preliminary evidence suggests that the swirl flow mixers have the ability to produce rapid and homogeneous fluid mixing, thus controlling the particle size.

  5. Biocatalytic Synthesis of Acrylates in Supercritical Fluids: Tuning Enzyme Activity by Changing Pressure

    Science.gov (United States)

    Kamat, Sanjay V.; Iwaskewycz, Brian; Beckman, Eric J.; Russell, Alan J.

    1993-04-01

    Supercritical fluids are a unique class of non-aqueous media in which biocatalytic reactions can occur. The physical properties of supercritical fluids, which include gas-like diffusivities and liquid-like densities, can be predictably controlled with changing pressure. This paper describes how adjustment of pressure, with the subsequent predictable changes of the dielectric constant and Hildebrand solubility parameter for fluoroform, ethane, sulfur hexafluoride, and propane, can be used to manipulate the activity of lipase in the transesterification of methylmethacrylate with 2-ethyl-1-hexanol. Of particular interest is that the dielectric constant of supercritical fluoroform can be tuned from approximately 1 to 8, merely by increasing pressure from 850 to 4000 psi (from 5.9 to 28 MPa). The possibility now exists to predictably alter both the selectivity and the activity of a biocatalyst merely by changing pressure.

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

    International Nuclear Information System (INIS)

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

    2016-01-01

    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. - Highlights: • We synthesize nicotinic acid coated magnetite nanorods via hydrothermal technique • Effect of nicotinic acid concentration on the nanorods properties was significant • Nanorods maintained uniform shape with increased concentration of nicotinic acid • Alterations occurred in particle size, mineral phases and magnetics of coated samples.

  7. Comparative dynamics analysis on xonotlite spherical particles synthesized via hydrothermal synthesis

    Science.gov (United States)

    Liu, F.; Chen, S.; Lin, Q.; Wang, X. D.; Cao, J. X.

    2018-01-01

    The xonotlite crystals were synthesized via the hydrothermal synthesis manner from CaO and SiO2 as the raw materials with their Si/Ca molar ratio of 1.0. Comparative dynamics analysis on xonotlite spherical particles synthesized via hydrothermal synthesis process was explored in this paper. The accuracy of the dynamic equation of xonotlite spherical particles was verified by two methods, one was comparing the production rate of the xonotlite products calculated by the dynamic equation with the experimental values, and the other was comparing the apparent activation energies calculated by the dynamic equation with that calculated by the Kondo model. The results indicated that the production rates of the xonotlite spherical particles calculated by the dynamic equation were in good agreement with the experimental values and the apparent activation energy of the xonotlite spherical particles calculated by dynamic equation (84 kJ·mol-1) was close to that calculated by Kondo model (77 kJ·mol-1), verifying the high accuracy of the dynamic equation.

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

    Science.gov (United States)

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

    2011-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Attallah, Olivia A., E-mail: olivia.adly@hu.edu.eg [Center of Nanotechnology, Nile University, 12677 Giza (Egypt); Pharmaceutical Chemistry Department, Heliopolis University, 11777 El Salam, Cairo (Egypt); Girgis, E. [Solid State Physics Department, National Research Center, 12622 Dokki, Giza (Egypt); Advanced Materials and Nanotechnology Lab, CEAS, National Research Center, 12622 Dokki, Giza (Egypt); Abdel-Mottaleb, Mohamed M.S.A. [Center of Nanotechnology, Nile University, 12677 Giza (Egypt)

    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. - Highlights: • We synthesize nicotinic acid coated magnetite nanorods via hydrothermal technique • Effect of nicotinic acid concentration on the nanorods properties was significant • Nanorods maintained uniform shape with increased concentration of nicotinic acid • Alterations occurred in particle size, mineral phases and magnetics of coated samples.

  10. Synthesis of dittmarite/Mg(OH){sub 2} composite coating on AZ31 using hydrothermal treatment

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Qing, E-mail: qzhaoyuping@bit.edu.cn; Mahmood, Waqas; Zhu, Yanying

    2016-03-30

    Highlights: • Synthesis of dittmarite Mg(OH){sub 2} coating on AZ31 alloy by hydrothermal method. • The mechanism of composite coating growth and its characterizations. • The coating is corrosion resistant significantly. • Lack of hydroxyl deposition on the coating surface. • Strong adhesion between the coating and the substrate. • The synthesized coating meets the cytotoxicity standards. - Abstract: In this work, we have used hydrothermal method for the synthesis of dittmarite/Mg(OH){sub 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.

  11. Selective Fischer-Tropsch synthesis over an Al{sub 2}O{sub 3} supported cobalt catalyst in supercritical hexane

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Xiwen; Roberts, Christopher B. [Chemical Engineering Department, Auburn University, 230 Ross Hall, Auburn, AL 36849 (United States)

    2003-09-15

    Supercritical fluids (SCFs) offer several advantages as reaction media for catalytic reactions. These advantages include the ability to manipulate the reaction environment through simple changes in pressure to enhance solubility of reactants and products, to eliminate interphase transport limitations, and to integrate reaction and separation unit operations. Benefits derived from the SCF-phase Fischer-Tropsch synthesis (SCF-FTS) involve the gas-like diffusivities and liquid-like solubilities, which together combine the desirable features of the gas- and liquid-phase FT synthesis routes. In this paper, FT synthesis under SCF hexane conditions is examined in a continuous, high-pressure reactor by employing a traditional Co catalyst (15% Co-0.5% Pt/Al{sub 2}O{sub 3}). Steady-state operation was quickly achieved under SCF conditions and the SCF-FT process has a marked effect on the hydrocarbon product distribution with a shift to higher carbon number products owing to enhanced heat and mass transfer from the catalyst surface. In addition, an obvious difference in the olefin content was observed where the 1-olefin content in the SCF phase was always higher than in the gas phase. Based on the experimental observations, a mechanistic explanation is provided for the difference of the reaction behavior under supercritical and gas-phase environments. Enhanced olefins readsorption and increased availability of active sites in the supercritical state contribute to the increased olefin selectivity and chain growth probability in the supercritical phase. In addition, the effect of pressure tuning in the supercritical phase reaction was investigated as well as the effect of the supercritical medium on heat transfer and temperature distribution within the reactor.

  12. Synthesis of biodiesel fuel additives from glycerol using green chemistry and supercritical fluids

    Science.gov (United States)

    For every 3 moles of fatty acid esters produced, 1 mole of glycerol remains, ~11% of the biodiesel volume. One new method of glycerol use could be as a biodiesel fuel additive/extender using eco-friendly heterogeneous catalysts and supercritical fluids (SFs). SFs have advantages such as greater diff...

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

    Science.gov (United States)

    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

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

    Directory of Open Access Journals (Sweden)

    Hakimeh Pourabdollahi

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

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

    Science.gov (United States)

    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.

  16. Natural cotton as precursor for the refractory boron carbide—a hydrothermal synthesis and characterization

    Science.gov (United States)

    Saritha Devi, H. V.; Swapna, M. S.; Raj, Vimal; Ambadas, G.; Sankararaman, S.

    2018-01-01

    Boron carbide (B4C) is an excellent covalent carbide that finds applications in industries and nuclear power plants. The present synthesis methods of boron carbide are expensive and involve the use of toxic chemicals that adversely affect environment. In the present work, we report for the first time the use of the hydrothermal method for converting the cellulose from cotton as the carbon precursor for B4C. The carbon precursor is converted into functionalized porous carbonaceous material by hydrothermal treatment followed by sodium borohydride. It is further treated with boric acid to make it a B4C precursor. The precursor is characterized by UV-visible diffuse reflectance, Raman, Fourier transform infrared, photoluminescent and energy dispersive spectroscopy. The morphology and structure analysis is carried out using field emission scanning electron microscopy and x-ray diffraction techniques. The results of structural and optical characterization of the sample synthesized are compared with the commercial B4C. The thermal stability of the sample is studied by thermogravimetric analysis. The sample annealed at 700 °C is found to be B4C devoid of amorphous carbon with a yield of 44.7%. The analysis reveals the formation of boron carbide from the sample.

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

    Science.gov (United States)

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

    2017-07-01

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

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

    Science.gov (United States)

    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).

  19. Hydrothermal synthesis of two photoluminescent nitrogen-doped graphene quantum dots emitted green and khaki luminescence

    International Nuclear Information System (INIS)

    Zhu, Xiaohua; Zuo, Xiaoxi; Hu, Ruiping; Xiao, Xin; Liang, Yong; Nan, Junmin

    2014-01-01

    A simple and effective chemical synthesis of the photoluminescent nitrogen-doped graphene quantum dots (N-GQDs) biomaterial is reported. Using the hydrothermal treatment of graphene oxide (GO) in the presence of hydrogen peroxide (H 2 O 2 ) and ammonia, the N-GQDs are synthesized through H 2 O 2 exfoliating the GO into nanocrystals with lateral dimensions and ammonia passivating the generated active surface. Then, after a dialytic separation, two water-soluble N-GQDs with average size of about 2.1 nm/6.2 nm, which emit green/khaki luminescence and exhibit excitation dependent/independent photoluminescence (PL) behaviors, are obtained. In addition, it is also demonstrated that these two N-GQDs are stable over a broad pH range and have the upconversion PL property, showing this approach provides a simple and effective method to synthesize the functional N-GQDs. - Highlights: • Nitrogen-doped graphene quantum dots (N-GQDs) are prepared by hydrothermal routine. • Two N-GQDs with different size distribution emit green/khaki photoluminescence. • Two N-GQDs exhibit excitation-dependent/independent photoluminescence behaviors

  20. Natural precursor based hydrothermal synthesis of sodium carbide for reactor applications

    Science.gov (United States)

    Swapna, M. S.; Saritha Devi, H. V.; Sebastian, Riya; Ambadas, G.; Sankararaman, S.

    2017-12-01

    Carbides are a class of materials with high mechanical strength and refractory nature which finds a wide range of applications in industries and nuclear reactors. The existing synthesis methods of all types of carbides have problems in terms of use of toxic chemical precursors, high-cost, etc. Sodium carbide (Na2C2) which is an alkali metal carbide is the least explored one and also that there is no report of low-cost and low-temperature synthesis of sodium carbide using the eco-friendly, easily available natural precursors. In the present work, we report a simple low-cost, non-toxic hydrothermal synthesis of refractory sodium carbide using the natural precursor—Pandanus. The formation of sodium carbide along with boron carbide is evidenced by the structural and morphological characterizations. The sample thus synthesized is subjected to field emission scanning electron microscopy (FESEM), x-ray powder diffraction (XRD), ultraviolet (UV)—visible spectroscopy, Fourier transform infrared spectroscopy (FTIR), Raman, and photoluminescent (PL) spectroscopic techniques.

  1. An effective hydrothermal route for the synthesis of multiple PDDA-protected noble-metal nanostructures.

    Science.gov (United States)

    Chen, Hongjun; Wang, Yuling; Dong, Shaojun

    2007-12-10

    In this article, we demonstrate an effective hydrothermal route for the synthesis of multiple PDDA-protected (PDDA = poly(diallyl dimethylammonium) chloride) noble-metal (including silver, platinum, palladium, and gold) nanostructures in the absence of any seeds and surfactants, in which PDDA, an ordinary and water-soluble polyelectrolyte, acts as both a reducing and a stabilizing agent. Under optimal experimental conditions, Ag nanocubes, Pt and Pd nanopolyhedrons, and Au nanoplates can be obtained, which were characterized by transmission electron microscopy , scanning electron microscopy, energy-dispersive spectroscopy, and X-ray diffraction. More importantly, the nanostructures synthesized show potential applications in surface-enhanced Raman scattering and electrocatalysis, in which Ag nanocubes and Pt nanopolyhedrons were chosen as the examples, respectively.

  2. Hydrothermal synthesis of meso porous silica MCM-41 using commercial sodium silicate

    Energy Technology Data Exchange (ETDEWEB)

    Melendez O, H. I.; Mercado S, A.; Garcia C, L. A.; Castruita, G.; Perera M, Y A., E-mail: ivan_melendez380@hotmail.com [Centro de Investigacion en Quimica Aplicada, Bldv. Enrique Reyna Hermosillo No. 140, Saltillo 25294, Coahuila (Mexico)

    2013-08-01

    In this work, ordered meso porous silica MCM-41 was prepared by hydrothermal synthesis using industrial-grade sodium silicate (Na{sub 2}SiO{sub 3}) as silica source, hexadecyltrimethyl-ammonium bromide (CTAB) as template agent and ethyl acetate as ph regulator. The influence of CTAB/SiO{sub 2} molar ratio, reaction time, aging temperature, and co-surfactant type on the structural and morphological properties of the obtained silica was studied. The products were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and nitrogen adsorption-desorption isotherms. Ordered meso porous MCM-41 silica was obtained at 80 C by using a range of CTAB/SiO{sub 2} molar ratio from 0.35 to 0.71 and reaction times up to 72 h and isopropanol (i-Pr OH) as co-surfactant. (Author)

  3. Hydrothermal synthesis of meso porous silica MCM-41 using commercial sodium silicate

    International Nuclear Information System (INIS)

    Melendez O, H. I.; Mercado S, A.; Garcia C, L. A.; Castruita, G.; Perera M, Y A.

    2013-01-01

    In this work, ordered meso porous silica MCM-41 was prepared by hydrothermal synthesis using industrial-grade sodium silicate (Na 2 SiO 3 ) as silica source, hexadecyltrimethyl-ammonium bromide (CTAB) as template agent and ethyl acetate as ph regulator. The influence of CTAB/SiO 2 molar ratio, reaction time, aging temperature, and co-surfactant type on the structural and morphological properties of the obtained silica was studied. The products were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and nitrogen adsorption-desorption isotherms. Ordered meso porous MCM-41 silica was obtained at 80 C by using a range of CTAB/SiO 2 molar ratio from 0.35 to 0.71 and reaction times up to 72 h and isopropanol (i-Pr OH) as co-surfactant. (Author)

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

    Science.gov (United States)

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

    2017-03-01

    Iron oxide nanoparticles (IONPs) were synthesized through a simple low temperature hydrothermal approach to obtain with high saturation magnetization properties. Two series of iron precursors (sulfates and chlorides) were used in synthesis process by varying the reaction temperature at a constant pH. The X-ray diffraction pattern indicates the inverse spinel structure of the synthesized IONPs. The Field emission scanning electron microscopy and high resolution transmission electron microscopy studies revealed that the particles prepared using iron sulfate were consisting a mixer of spherical (16-40 nm) and rod (diameter 20-25 nm, length magnetization (MS) of 103.017 emu/g and low remanant magnetization (Mr) of 0.22 emu/g with coercivity (Hc) of 70.9 Oe, which may be attributed to the smaller magnetic domains (dm) and dead magnetic layer thickness (t).

  5. Hydrothermal Synthesis of Nanoclusters of ZnS Comprised on Nanowires.

    Science.gov (United States)

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

    2013-09-09

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

  6. Hydrothermal Synthesis of Nanoclusters of ZnS Comprised on Nanowires

    Directory of Open Access Journals (Sweden)

    Magnus Willander

    2013-09-01

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

  7. Continuous Hydrothermal Flow Synthesis of Functional Oxide Nanomaterials Used in Energy Conversion Devices

    DEFF Research Database (Denmark)

    Xu, Yu

    as materials are continuously produced, and the technology can be scaled-up to an industrial-relevant production capacity. The thesis starts with investigating the most appropriate mixer design for a novel two-stage reactor by computational fluid dynamics modelling. On basis of the modelling results, a two......Continuous hydrothermal flow synthesis (CHFS) was used to prepare functional oxide nanoparticles. Materials synthesized include NiO, Y-doped ZrO2, Gd-doped CeO2, LaCrO3 and Ni-substituted CoFe2O4. These types of oxides can be applied in several energy conversion devices, e.g. as active materials......, dense continuous layers (

  8. Synthesis of Polyhedral Magnetite Particles by Hydrothermal Process under High Pressure Condition

    Directory of Open Access Journals (Sweden)

    Siti Machmudah

    2016-12-01

    Full Text Available Magnetite particles were successfully generated by hydrothermal synthesis using water at subcritical conditions. By changing the temperature and pressure at subcritical water conditions, the thermodynamics and transport properties of the water can be controlled, thus enabling to manage the way of crystal formation, morphology, and particle size. In this work, the experiments were carried out at temperatures of 250 °C and 290 °C and a pressure of 10 MPa with a reactor made of SUS 316 in a batch system. The synthesized particles were dried in vacuum condition and characterized by SEM and XRD. The XRD patterns showed that magnetite particles were dominantly formed in the particle products with a black color. The results showed that the magnetite particles formed had diameters of around 60 nm in all experiments with irregular polyhedral shaped morphologies.

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

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Fausthon Fred da; Fernandes de Oliveira, Carlos Alberto; Lago Falcão, Eduardo Henrique [Laboratório de Terras Raras, Departamento de Química Fundamental, Universidade Federal de Pernambuco (DQF-UFPE), 50590-470 Recife, PE (Brazil); Gatto, Claudia Cristina [Laboratório de Síntese Inorgânica e Cristalografia, Instituto de Química, Universidade de Brasília (IQ-UnB), 70904-970 Brasilia, DF (Brazil); Bezerra da Costa, Nivan; Oliveira Freire, Ricardo [Pople Computational Chemistry Laboratory, Departamento de Química, Universidade Federal de Sergipe, São Cristóvão-SE 49100-000 (Brazil); Chojnacki, Jarosław [Department of Inorganic Chemistry, Gdansk University of Technology, 80-233 Gdansk (Poland); Alves Júnior, Severino, E-mail: salvesjr@ufpe.br [Laboratório de Terras Raras, Departamento de Química Fundamental, Universidade Federal de Pernambuco (DQF-UFPE), 50590-470 Recife, PE (Brazil)

    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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-02-15

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

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

    Science.gov (United States)

    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

  12. Supercritical fluids in chemical processes

    International Nuclear Information System (INIS)

    Hertz, A.; Charton, F.

    2011-01-01

    When the pressure and temperature of a fluid are simultaneously higher than their critical point values, the fluid is said to be supercritical. Supercritical fluids have unique physico-chemical properties, in particular they have specific gravity close to that of liquids and viscosity close to that of gases. Carbon dioxide CO 2 (P c = 73.8 bars, T c = 31 C. degrees) is the most widely used compound in supercritical processes. In the nuclear field, chemistry inspired by liquid phase extraction has been developed for the supercritical CO 2 used as a diluent in association with extractant systems such as organo-phosphorus compounds or β-dike-tones. The Japanese Super-DIREX (Supercritical fluid Direct Extraction) process exploits the supercritical CO 2 - tri-n-butyl phosphate - nitric acid chemical system to extract actinides from spent fuel. In the United States, the same chemical system is utilized in an industrial facility to recover enriched uranium from incineration ash. Supercritical water H 2 O (P c = 221 bars, T c = 374 C. degrees) exhibits solvation properties close to those of organic solvents and can solubilise organic compounds that are insoluble in liquid water. In the nuclear field, CEA is studying oxidation in supercritical water, also called hydrothermal oxidation, for the mineralization of contaminated organic solvents. (A.C.)

  13. Corrosion-deformation interactions in Inconel 718: application to stress corrosion in a supercritical aqueous medium and research of a material solution for the hydrothermal oxidation process

    International Nuclear Information System (INIS)

    Fournier, L.

    2000-01-01

    The aim of this study is to investigate the mechanisms responsible for stress corrosion cracking of nickel base superalloys in supercritical aerated water in order to determine a suitable material for the supercritical water oxidation (SCWO) reactors. For this purpose, alloy 718 is selected as a test material. We first focus on its 'hydrogen assisted cracking' behaviour at 25 deg C and on its 'oxidation assisted cracking behaviour' in the temperature range 400 deg C to 600 deg C. Then, its stress corrosion cracking behaviour in supercritical water is investigated for the first time by means of slow strain rate tensile tests (SSRT) performed on smooth specimens in de-ionised and aerated water at 400 deg C and 250 bars. Oxidation - deformation interactions are shown to control both the initiation and the propagation stages of alloy 718 stress corrosion cracks in supercritical water. We suggest that nickel base alloys without strengthening precipitates and with a high chromium content are suitable materials for the SCWO reactors. Such proposal is confirmed by SSRT performed on alloy 690 (28% Cr) specimens in de-ionised and aerated water at 400 deg C and 250 bars which do not reveal any susceptibility to stress corrosion cracking. (author)

  14. Properties of ceria doped with gadolinia via microwave-assisted hydrothermal synthesis

    International Nuclear Information System (INIS)

    Carregosa, J.D.C.; Oliveira, R.M.P.B.; Macedo, D.A.; Nascimento, R.M.

    2016-01-01

    The solid solution of CeO 2 doped with Gd 3+ (CGO) is a promising candidate for electrolyte in Solid Oxide Full Cells (SOFCs) operating in intermediate and low temperatures. The reduction of the working temperature of these energy conversion devices is the great technological challenge to its marketing. In this work, nanocrystalline powders of Ce 1-x Gd x O 2-x/2 with x=0, x=0.1 e x=0.2 were obtained via microwave-hydrothermal synthesis at low temperature and times of synthesis (10 and 20 min at 120° C). The powders were analyzed by TG-DTA, DRX and dilatometry. The results showed characteristic peaks of the cubic fluorite-type structure, referring to the cerium oxide (CeO 2 ), without the presence of secondary peaks. It was also observed that the samples processed at levels of 10 and 20 minutes showed distinct behaviors in contrast to the concentrations of Gd 3+ . (author)

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

    Directory of Open Access Journals (Sweden)

    Sylwia Kuśnieruk

    2016-11-01

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

  16. Synthesis of inorganic materials in a supercritical carbon dioxide medium. Application to ceramic cross-flow filtration membranes preparation

    International Nuclear Information System (INIS)

    Papet, Sebastien

    2000-01-01

    Membrane separations, using cross-flow mineral ceramic membranes, allows fractionation of aqueous solutions due to the molecular sieve effect and electrostatic charges. To obtain a high selectivity, preparation of new selective ceramic membranes is necessary. We propose in this document two different routes to prepare such cross-flow tubular mineral membranes. In the first exposed method, a ceramic material is used, titanium dioxide, synthesized in supercritical carbon dioxide by the hydrolysis of an organometallic precursor of the oxide. The influence of operating parameters is similar to what is observed during a liquid-phase synthesis (sol-gel process), and leads us to control the size and texture of the prepared particles. This material is then used to prepare mineral membrane with a compressed layer process. The particles are mixed with organic components to form a liquid suspension. A layer is then deposited on the internal surface of a tubular porous support by slip-casting. The layer is then dried and compressed on the support before sintering. The obtained membranes arc in the ultrafiltration range. A second process has been developed in this work. It consists on the hydrolysis, in a supercritical CO 2 medium, of a precursor of titanium dioxide infiltrated into the support. The obtained material is then both deposited on the support but also infiltrated into the porosity. This new method leads to obtain ultrafiltration membranes that retain molecules which molecular weight is round 4000 g.mol -1 . Furthermore, we studied mass transfer mechanisms in cross-flow filtration of aqueous solutions. An electrostatic model, based on generalized Nernst-Planck equation that takes into account electrostatic interactions between solutes and the ceramic material, lead us to obtain a good correlation between experimental results and the numerical simulation. (author) [fr

  17. Hydrothermal synthesis of 1D TiO2 nanostructures for dye sensitized solar cells

    International Nuclear Information System (INIS)

    Tacchini, I.; Ansón-Casaos, A.; Yu, Youhai; Martínez, M.T.; Lira-Cantu, M.

    2012-01-01

    Highlights: ► Hydrothermal synthesis allows the preparation of different 1D TiO 2 nanostructures easily. ► Nanotubular morphology demonstrates the highest photovoltaic efficiencies in dye sensitized cells (DSCs). ► Morphology at the nanoscale level is as decisive for DSC efficiency as it is TiO 2 crystal structure and surface area. - Abstract: Mono-dimensional titanium oxide nanostructures (multi-walled nanotubes and nanorods) were synthesized by the hydrothermal method and applied to the construction of dye sensitized solar cells (DSCs). First, nanotubes (TiNTs) and nanotubes loaded with titanium oxide nanoparticles (TiNT/NPs) were synthesized with specific surface areas of 253 m 2 /g and 304 m 2 /g, respectively. After that, thermal treatment of the nanotubes at 500 °C resulted in their transformation into the corresponding anatase nanorods (TiNT-Δ and TiNT/NPs-Δ samples). X-ray diffraction and Raman spectroscopy data indicated that titanium oxide in the pristine TiNT and TiNT/NP samples was converted into anatase phase TiO 2 during the heating. Additionally, specific surface areas and water adsorption capacities decreased after the heat treatment due to the sample agglomeration and the collapse of the inner nanotube channels. DSCs were fabricated with the nanotube TiNT and TiNT/NP samples and with the anatase nanorod TiNT-Δ and TiNT/NPs-Δ samples as well. The highest power conversion efficiency of η = 3.12% was obtained for the TiNT sample, despite its lower specific surface compared with the corresponding nanoparticle-loaded sample (TiNT/NP).

  18. Simulation, design and proof-of-concept of a two-stage continuous hydrothermal flow synthesis reactor for synthesis of functionalized nano-sized inorganic composite materials

    DEFF Research Database (Denmark)

    Zielke, Philipp; Xu, Yu; Simonsen, Søren Bredmose

    2016-01-01

    Computational fluid dynamics simulations were employed to evaluate several mixer geometries for a novel two-stage continuous hydrothermal flow synthesis reactor. The addition of a second stage holds the promise of allowing the synthesis of functionalized nano-materials as for example core......-shell or decorated particles. Based on the simulation results, a reactor system employing a confined jet mixer in the first and a counter-flow mixer in the second stage was designed and built. The two-stage functionality and synthesis capacity is shown on the example of single- and two-stage syntheses of pure...

  19. Hydrothermal synthesis and white light emission of cubic ZrO2:Eu3+ nanocrystals

    International Nuclear Information System (INIS)

    Meetei, Sanoujam Dhiren; Singh, Shougaijam Dorendrajit

    2014-01-01

    Highlights: • White light emitting cubic ZrO 2 :Eu 3+ nanocrystal is synthesized by hydrothermal technique. • Eu 3+ is used to stabilize crystalline phase and to get red counterpart of the white light. • Defect emission and Eu 3+ emission combined to give white light. • The white light emitted from this nanocrystal resembles vertical daylight of the Sun. • Lifetime corresponding to red counterpart of the sample is far longer than conventional white light emitters. -- Abstract: Production of white light has been a promising area of luminescence studies. In this work, white light emitting nanocrystals of cubic zirconia doped with Eu 3+ are synthesized by hydrothermal technique. The dopant Eu 3+ is used to stabilize crystalline phase to cubic and at the same time to get red counterpart of the white light. The synthesis procedure is simple and precursor required no further annealing for crystallization. X-ray diffraction patterns show the crystalline phase of ZrO 2 :Eu 3+ to be cubic and it is confirmed by Fourier Transform Infrared spectroscopy. From transmission electron microscopy images, size of the crystals is found to be ∼5 nm. Photoluminescence emission spectrum of the sample, on monitoring excitation at O 2− –Eu 3+ charge transfer state shows broad peak due to O 2− of the zirconia and that of Eu 3+ emission. Commission Internationale de l’éclairage co-ordinate of this nanocrystal (0.32, 0.34) is closed to that of the ideal white light (0.33, 0.33). Correlated color temperature of the white light (5894 K) is within the range of vertical daylight. Lifetime (1.32 ms) corresponding to 5 D 0 energy level of the Eu 3+ is found to be far longer than conventional red counterparts of white light emitters. It suggests that the ZrO 2 :Eu 3+ nanocrystals synthesized by hydrothermal technique may find applications in simulating the vertical daylight of the Sun

  20. Dissolution-Induced Nanowire Synthesis on Hot-Dip Galvanized Surface in Supercritical Carbon Dioxide.

    Science.gov (United States)

    Kaleva, Aaretti; Saarimaa, Ville; Heinonen, Saara; Nikkanen, Juha-Pekka; Markkula, Antti; Väisänen, Pasi; Levänen, Erkki

    2017-07-11

    In this study, we demonstrate a rapid treatment method for producing a needle-like nanowire structure on a hot-dip galvanized sheet at a temperature of 50 °C. The processing method involved only supercritical carbon dioxide and water to induce a reaction on the zinc surface, which resulted in growth of zinc hydroxycarbonate nanowires into flower-like shapes. This artificial patina nanostructure predicts high surface area and offers interesting opportunities for its use in industrial high-end applications. The nanowires can significantly improve paint adhesion and promote electrochemical stability for organic coatings, or be converted to ZnO nanostructures by calcining to be used in various semiconductor applications.

  1. Dissolution-Induced Nanowire Synthesis on Hot-Dip Galvanized Surface in Supercritical Carbon Dioxide

    Directory of Open Access Journals (Sweden)

    Aaretti Kaleva

    2017-07-01

    Full Text Available In this study, we demonstrate a rapid treatment method for producing a needle-like nanowire structure on a hot-dip galvanized sheet at a temperature of 50 °C. The processing method involved only supercritical carbon dioxide and water to induce a reaction on the zinc surface, which resulted in growth of zinc hydroxycarbonate nanowires into flower-like shapes. This artificial patina nanostructure predicts high surface area and offers interesting opportunities for its use in industrial high-end applications. The nanowires can significantly improve paint adhesion and promote electrochemical stability for organic coatings, or be converted to ZnO nanostructures by calcining to be used in various semiconductor applications.

  2. Development of Hydrotalcite Based Cobalt Catalyst by Hydrothermal and Co-precipitation Method for Fischer-Tropsch Synthesis

    Directory of Open Access Journals (Sweden)

    Muhammad Faizan Shareef

    2017-10-01

    Full Text Available This paper presents the effect of a synthesis method for cobalt catalyst supported on hydrotalcite material for Fischer-Tropsch synthesis. The hydrotalcite supported cobalt (HT-Co catalysts were synthesized by co-precipitation and hydrothermal method. The prepared catalysts were characterized by using various techniques like BET (Brunauer–Emmett–Teller, SEM (Scanning Electron Microscopy, TGA (Thermal Gravimetric Analysis, XRD (X-ray diffraction spectroscopy, and FTIR (Fourier Transform Infrared Spectroscopy. Fixed bed micro reactor was used to test the catalytic activity of prepared catalysts. The catalytic testing results demonstrated the performance of hydrotalcite based cobalt catalyst in Fischer-Tropsch synthesis with high selectivity for liquid products. The effect of synthesis method on the activity and selectivity of catalyst was also discussed. Copyright © 2017 BCREC Group. All rights reserved Received: 3rd November 2016; Revised: 26th February 2017; Accepted: 9th March 2017; Available online: 27th October 2017; Published regularly: December 2017 How to Cite: Sharif, M.S., Arslan, M., Iqbal, N., Ahmad, N., Noor, T. (2017. Development of Hydrotalcite Based Cobalt Catalyst by Hydrothermal and Co-precipitation Method for Fischer-Tropsch Synthesis. Bulletin of Chemical Reaction Engineering & Catalysis, 12(3: 357-363 (doi:10.9767/bcrec.12.3.762.357-363

  3. Hydrothermal synthesis and characterization of lead sulfide nanocubes through simple hydrothermal method in the presence of [bis(salicylate)lead(II)] as a new precursor

    Science.gov (United States)

    Emadi, Hamid; Salavati-Niasari, Masoud

    2013-02-01

    Well-defined single-crystalline lead sulfide nanostructures including nanocubes were synthesized in high yield by a simple hydrothermal solution route. Novel cube-shaped PbS nanocrystals have been achieved using [bis(salicylate)lead(II)]; [Pb(Hsal)2]; and L-cysteain, under the molar ratio [Pb(Hsal)2]/L-cysteain 1/1, at initial reaction temperature 180 °C, for 12 h in hydrothermal method. Based on the systematic studies on their shape evolution, a possible growth mechanism of these PbS nanocubes was proposed. The shapes of PbS nanocrystals were face centered cubic (fcc) structure. Under the current experimental conditions, it is possible to control the PbS shape evolution by tuning the molar ratio, the initial reaction temperature, and the reaction time. Based on the systematic studies on the shape evolution, this approach is expected to be employed for the control-shaped synthesis of other fcc structural semiconductor nanomaterials. The optical properties of obtained products were investigated by photoluminescence spectroscopy. The absorption edge of PbS nanostructures exhibit a blue-shift, which is attributed to the quantum confinement of charge carriers in the nanostructures and differences in shape and size.

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

    Science.gov (United States)

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

    2009-01-01

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

  5. Synthesis of zirconium carbide whiskers by a combination of microwave hydrothermal and carbothermal reduction

    Science.gov (United States)

    Li, Kezhi; Zhou, Xuan; Zhao, Zhigang; Chen, Chunyu; Wang, Changcong; Ren, Biyun; Zhang, Leilei

    2018-02-01

    Zirconium carbide (ZrC) whiskers were successfully synthesized by a combination of microwave hydrothermal (MH) and carbothermal reduction. The precursors of ZrC whiskers were produced by MH, subsequently carbothermally reduced to ZrC whiskers at 1100-1600 °C in an Ar atmosphere. Effects of the reduction temperature and precursors with various carbon/zirconium (C/Zr) molar ratios on the synthesis of ZrC whiskers were investigated. The results showed that the carbothermal reduction occurred at 1100 °C, and terminated at a relatively low temperature (1400 °C). When the reduction temperature was 1500 °C and the C/Zr molar ratio was 5:1, the ZrC whiskers with the largest aspect ratio and the most uniform distribution were produced. The whiskers exhibited the diameters of 0.1-2 μm and the lengths of 5-30 μm. The synthesized ZrC whiskers with a single crystalline phase displayed cylindrical and pagoda-like morphologies. The growth of ZrC whiskers was considered to be governed by the Ostwald ripening and S-L-S mechanism.

  6. Hydrothermal synthesis and characteristic photoluminescence of Er-doped SnO{sub 2} nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Tuan, Pham Van; Hieu, Le Trung; Nga, La Quynh [International Training Institute for Materials Science, Hanoi University of Science and Technology, No.1, Dai Co Viet, Hanoi (Viet Nam); Dung, Nguyen Duc [Advanced Institute of Science and Technology, Hanoi University of Science and Technology, No.1, Dai Co Viet, Hanoi (Viet Nam); Ha, Ngo Ngoc [International Training Institute for Materials Science, Hanoi University of Science and Technology, No.1, Dai Co Viet, Hanoi (Viet Nam); Khiem, Tran Ngoc, E-mail: khiem@itims.edu.vn [International Training Institute for Materials Science, Hanoi University of Science and Technology, No.1, Dai Co Viet, Hanoi (Viet Nam)

    2016-11-15

    We report the characteristic photoluminescence (PL) spectra of erbium ion (Er{sup 3+})-doped tin dioxide (SnO{sub 2})nanoparticles. The materials were prepared via hydrothermal method at 180 °C with in 20 h by using various Er{sup 3+} ion concentrations ranging from 0.0 to 1.0 at%. After the synthesis, the materials were characterized through X-ray diffraction and high-resolution transmission electron microscopy. Crystallite SnO{sub 2} and its average particle diameter of approximately 5 nm did not change with Er{sup 3+} ion dopant concentration. Photoluminescence spectra showed the characteristic light emission from the Er{sup 3+} ions. The PL excitation spectra referred to an efficient energy transfer to Er{sup 3+} ions in the presence of SnO{sub 2}nanoparticles. The most intense Er-related emission of SnO{sub 2}:Er{sup 3+} nanoparticles in near infrared region was found in samples containing an Er{sup 3+} ion concentration of 0.25 at%. Although the absorption bandgaps of the materials were identified at approximately 3.8 eV, we found that efficient excitation comes with low excitation energy band edge. Excitation is possibly involved in shallow defects in SnO{sub 2} nanoparticles.

  7. Hydrothermal route to VO2 (B) nanorods: controlled synthesis and characterization

    Science.gov (United States)

    Song, Shaokun; Huang, Qiwei; Zhu, Wanting

    2017-10-01

    One-dimensional vanadium dioxides have attracted intensive attention owing to their distinctive structure and novel applications in catalysis, high energy lithium-ion batteries, chemical sensors/actuators and electrochemical devices etc. In this paper, large-scale VO2 (B) nanorods have been successfully synthesized via a versatile and environment friendly hydrothermal strategy using V2O5 as vanadium source and carbohydrates/alcohols as reductant. The obtained samples are characterized by XRD, FT-IR, TEM, and XPS techniques to investigate the effects of chemical parameters such as reductants, temperature, and time of synthesis on the structure and morphology of products. Results show that pure B phase VO2 with homogeneous nanorod-like morphology can be prepared easily at 180 °C for 3 days with glycerol as reluctant. Typically, the nanorod-like products are 0.5-1 μm long and 50 nm width. Furthermore, it is also confirmed that the products are consisted of VO2, corresponding to the B phase. More importantly, this novel approach is efficient, free of any harmful solvents and surfactants. Therefore, this efficient, green, and cost-saving route will have great potential in the large-scale fabrication of 1D VO2 (B) nanorods from the economic and environmental point of view.

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

    Energy Technology Data Exchange (ETDEWEB)

    Cui, Hongmei, E-mail: hmcui@home.ipe.ac.cn [State Key Laboratory of Multiphase Complex Systems, Institute of Process Engineering, Chinese Academy of Sciences, 1 Zhongguancun Road, Haidian District 100190, Beijing (China); Research Institute of Synthetic Crystals, 1 Hongsong Road, Chaoyang District 100018, Beijing (China); Wu, Xiaofeng, E-mail: wxftsjc@mail.ipe.ac.cn [State Key Laboratory of Multiphase Complex Systems, Institute of Process Engineering, Chinese Academy of Sciences, 1 Zhongguancun Road, Haidian District 100190, Beijing (China); Chen, Yunfa, E-mail: yfchen@mail.ipe.ac.cn [State Key Laboratory of Multiphase Complex Systems, Institute of Process Engineering, Chinese Academy of Sciences, 1 Zhongguancun Road, Haidian District 100190, Beijing (China); Boughton, R.I. [Department of Physics and Astronomy, Bowling Green State University, Bowling Green 43403, OH (United States)

    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.

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

    International Nuclear Information System (INIS)

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

    2012-01-01

    Anatase TiO 2 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 TiO 2 consisted of well-defined spheres with size of 3-5 μm. The photocatalytic activity of spherical TiO 2 was determined by degradation of salicylic acid under visible light irradiation. It was revealed that the degradation rate of the spherical TiO 2 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 TiO 2 (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 TiO 2 (temperature: 150, time: 48 h).

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

    Science.gov (United States)

    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.

  11. Hydrothermal synthesis of zeolite T from kaolin using two different structure-directing agents

    Science.gov (United States)

    Arshad, Sazmal E.; Lutfor Rahman, M.; Sarkar, Shaheen M.; Yusslee, Eddy F.; Patuwan, Siti Z.

    2018-01-01

    Zeolite T was synthesized from the molar chemical composition of 1SiO2:0.04Al2O3:0.26Na2O:0.09K2O:14H2O in the form of a homogenous milky solution in the presence of the two different structure-directing agents TMAOH and TEAOH respectively. Modification of the composition of silica was undertaken using metakaolin from calcined kaolin at 750 °C for 4 h, while the molar composition of each different SDA was variated from 0.05, 0.10, 0.15, 0.20 and 0.25. The homogenous mixture was left at room temperature for 24 h before undergoing hydrothermal synthesis at 100 °C for 168 h. The synthesized samples were filtered and aged at 120 °C for 2 h and each sample was calcined at high temperatures (545 °C for TMAOH and 520 °C for TEAOH) for template removal before characterization using XRD and SEM. Crystallization of the zeolite T in its major form only took place at a molar ratio of 0.10 of TMAOH, while TEAOH showed the species evolution of zeolite T into zeolite L and W for other molar ratios.

  12. Improved seedless hydrothermal synthesis of dense and ultralong ZnO nanowires

    International Nuclear Information System (INIS)

    Tian Jinghua; Hu Jie; Li Sisi; Zhang Fan; Liu Jun; Shi Jian; Li Xin; Chen Yong; Tian Zhongqun

    2011-01-01

    Seedless hydrothermal synthesis has been improved by introducing an adequate content of ammonia into the nutrient solution, allowing the fabrication of dense and ultralong ZnO nanowire arrays over large areas on a substrate. The presence of ammonia in the nutrient solution facilitates the high density nucleation of ZnO on the substrate which is critical for the nanowire growth. In order to achieve an optimal growth, the growth conditions have been studied systematically as a function of ammonia content, growth temperature and incubation time. The effect of polyethyleneimine (PEI) has also been studied but shown to be of no benefit to the nucleation of ZnO. Ultradense and ultralong ZnO nanowires could be obtained under optimal growth conditions, showing no fused structure at the foot of the nanowire arrays. Due to different reaction kinetics, four growth regimes could be attributed, including the first fast growth, equilibrium phase, second fast growth and final erosion. Combining this simple method with optical lithography, ZnO nanowires could be grown selectively on patterned areas. In addition, the as-grown ZnO nanowires could be used for the fabrication of a piezoelectric nanogenerator. Compared to the device of ZnO nanowires made by other methods, a more than twice voltage output has been obtained, thereby proving an improved performance of our growth method.

  13. Synthesis of zinc oxide by microwave hydrothermal method for application to transesterification of soybean oil (biodiesel)

    Energy Technology Data Exchange (ETDEWEB)

    Quirino, Max Rocha [LABQUIM/Universidade Federal da Paraíba, Campus III, 58200-000, Bananeiras, PB (Brazil); Oliveira, Mateus José C. [DEMA/Universidade Federal de Campina Grande, Campina Grande, Campus I, 58429-900, Campina Grande, PB (Brazil); Keyson, Davy [DME/Universidade Federal da Paraíba, Campus – I, 58051-900, João Pessoa, PB (Brazil); Lucena, Guilherme Leocárdio, E-mail: guilhermelucena@cchsa.ufpb.br [LABQUIM/Universidade Federal da Paraíba, Campus III, 58200-000, Bananeiras, PB (Brazil); Oliveira, João Bosco L. [Universidade Federal do Rio Grande do Norte, Campus I, 59078-970, Natal, RN (Brazil); Gama, Lucianna [DEMA/Universidade Federal de Campina Grande, Campina Grande, Campus I, 58429-900, Campina Grande, PB (Brazil)

    2017-01-01

    ZnO nanostructures were synthesized by microwave hydrothermal treatment using two different mineralization agents (NaOH and NH{sub 4}OH), and were evaluated as catalysts for biodiesel synthesis. The materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and Brunauer-Emmett-Teller (BET) surface area analysis. The XRD patterns indicated the formation of the hexagonal wurtzite phase in both samples. SEM analysis showed completely different morphologies based on the mineralization agent employed. The ZnO nanostructures synthesized with NaOH (ZONa5 and ZONa5P) presented plate-like agglomerates, resulting in a quasi-spherical morphology, whereas the materials synthesized with NH{sub 4}OH (ZONH5 and ZONH5P) presented a flower-like morphology. The ZONa5P sample showed an activity of 77.82% for the catalytic conversion of soybean oil into biodiesel by transesterification using methanol. - Highlights: • ZnO was synthesized by MH method in only 5 min. • The powders morphology is completely influenced by mineralization agent. • ZONa5P showed activity of 77.82% for the conversion of soybean oil into biodiesel.

  14. Microwave-assisted hydrothermal synthesis of CePO4 nanostructures: Correlation between the structural and optical properties

    International Nuclear Information System (INIS)

    Palma-Ramírez, D.; Domínguez-Crespo, M.A.; Torres-Huerta, A.M.; Dorantes-Rosales, H.; Ramírez-Meneses, E.; Rodríguez, E.

    2015-01-01

    Highlights: • An enhancement in the hydrothermal synthesis for obtaining of CePO 4 is presented. • Microwave energy can replace the energy by convection for obtaining CePO 4 . • CePO 4 demonstrates to be an option to increase the optical properties of polymers. • Adjusting the pH, the sintering process is not necessary to obtain the desire phase. • CePO 4 morphologies undergo evolution from nanorods to semispherical nanoparticles. - Abstract: In this work, the microwave-assisted hydrothermal method is proposed as an alternative to the synthesis of cerium phosphate (CePO 4 ) nanostructures to evaluate the influence of different synthesis parameters on both the structural and optical properties. In order to reach this goal, two different sets of experiments were designed, varying the reaction temperature (130 and 180 °C), synthesis time (15 and 30 min) and sintering temperature (400 and 600 °C), maintaining a constant pH = 3. Thereafter, two experimental conditions were selected to assess changes in the properties of CePO 4 nanopowders with pH (1, 5, 9 and 11). The crystal structure and morphology of the nanostructures were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM), respectively. Diffuse reflectance properties of CePO 4 with different microstructures were studied. The results demonstrated that by using the microwave-assisted hydrothermal method, the shape, size and structural phase of CePO 4 can be modulated by using relatively low synthesis temperatures and short reaction times, and depending on pH, a sintering process is not needed to obtain either a desired phase or size. Under the selected experimental conditions, the materials underwent an evolution from nanorods to semispherical nanoparticles, accompanied by a phase transition from hexagonal to monoclinic

  15. Microwave-assisted hydrothermal synthesis of CePO{sub 4} nanostructures: Correlation between the structural and optical properties

    Energy Technology Data Exchange (ETDEWEB)

    Palma-Ramírez, D. [Instituto Politécnico Nacional, CICATA-Unidad Altamira, Km 14.5, Carretera Tampico-Puerto Industrial Altamira, C.P. 89600 Altamira, Tamps (Mexico); Domínguez-Crespo, M.A., E-mail: mdominguezc@ipn.mx [Instituto Politécnico Nacional, CICATA-Unidad Altamira, Km 14.5, Carretera Tampico-Puerto Industrial Altamira, C.P. 89600 Altamira, Tamps (Mexico); Torres-Huerta, A.M. [Instituto Politécnico Nacional, CICATA-Unidad Altamira, Km 14.5, Carretera Tampico-Puerto Industrial Altamira, C.P. 89600 Altamira, Tamps (Mexico); Dorantes-Rosales, H. [Instituto Politécnico Nacional, ESIQIE, Departamento de Metalurgia, C.P. 07300 México D.F. (Mexico); Ramírez-Meneses, E. [Universidad Iberoamericana, Departamento de Ingeniería y Ciencias Químicas, Prolongación Paseo de la Reforma 880, Lomas de Santa Fe, C.P. 01219 México D.F. (Mexico); Rodríguez, E. [Instituto Politécnico Nacional, CICATA-Unidad Altamira, Km 14.5, Carretera Tampico-Puerto Industrial Altamira, C.P. 89600 Altamira, Tamps (Mexico)

    2015-09-15

    Highlights: • An enhancement in the hydrothermal synthesis for obtaining of CePO{sub 4} is presented. • Microwave energy can replace the energy by convection for obtaining CePO{sub 4}. • CePO{sub 4} demonstrates to be an option to increase the optical properties of polymers. • Adjusting the pH, the sintering process is not necessary to obtain the desire phase. • CePO{sub 4} morphologies undergo evolution from nanorods to semispherical nanoparticles. - Abstract: In this work, the microwave-assisted hydrothermal method is proposed as an alternative to the synthesis of cerium phosphate (CePO{sub 4}) nanostructures to evaluate the influence of different synthesis parameters on both the structural and optical properties. In order to reach this goal, two different sets of experiments were designed, varying the reaction temperature (130 and 180 °C), synthesis time (15 and 30 min) and sintering temperature (400 and 600 °C), maintaining a constant pH = 3. Thereafter, two experimental conditions were selected to assess changes in the properties of CePO{sub 4} nanopowders with pH (1, 5, 9 and 11). The crystal structure and morphology of the nanostructures were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM), respectively. Diffuse reflectance properties of CePO{sub 4} with different microstructures were studied. The results demonstrated that by using the microwave-assisted hydrothermal method, the shape, size and structural phase of CePO{sub 4} can be modulated by using relatively low synthesis temperatures and short reaction times, and depending on pH, a sintering process is not needed to obtain either a desired phase or size. Under the selected experimental conditions, the materials underwent an evolution from nanorods to semispherical nanoparticles, accompanied by a phase transition from hexagonal to monoclinic.

  16. High-temperature synthesis of highly hydrothermal stable mesoporous silica and Fe-SiO2 using ionic liquid as a template

    International Nuclear Information System (INIS)

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

    2011-01-01

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

  17. Microwave-Hydrothermal Synthesis and Characterization of High-Purity Nb Doped BaTiO3 Nanocrystals

    Directory of Open Access Journals (Sweden)

    A. Khanfekr

    2014-01-01

    Full Text Available The synthesis of Nb doped BaTiO3 has been investigated under Microwave-Hydrothermal (MH conditions in the temperature of 150°C for only 2 h using C16H36O4Ti, BaH2O2.8H2O and NbCl5 as Ba, Ti and  Nb sources, respectively.  Typical experiments performed on MH processing have not yet reported for Nb doped BaTiO3.  In the MH process, the formation of high purity nano tetragonal Nb-BaTiO3 was strongly enhanced. New hydrothermal method was used instead of the previous solid state reaction for the BaTiO3±Nb2O3 system. The new method uses high pressure to create nano dimension particles in a lower time and temperature. In case of the phase evolution studies, the XRD pattern measurements and Raman spectroscopy were performed. TEM and FE-SEM images were taken for the detailed analysis of the particle size, surface and morphology.  Synthesis of Nb doped BaTiO3 with the Microwave-hydrothermal provides an advantage of fast crystallization and reduced crystal size when compared to existing methods.

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

    Science.gov (United States)

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

    2017-07-01

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

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

    Science.gov (United States)

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

    2015-01-01

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

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-03-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Tkalčec, Emilija, E-mail: etkalcec@fkit.hr [Faculty of Chemical Engineering and Technology, University of Zagreb, Marulićev trg 19, Zagreb (Croatia); Popović, Jasminka [Division of Materials Physics, Ruđer Bošković Institute, Bijenička 54, Zagreb (Croatia); Orlić, Sebastijan; Milardović, Stjepan; Ivanković, Hrvoje [Faculty of Chemical Engineering and Technology, University of Zagreb, Marulićev trg 19, Zagreb (Croatia)

    2014-09-01

    Phase composition, crystal structure and morphology of carbonated fluor/hydroxyapatite synthesized hydrothermally from aragonitic cuttlefish bones were studied by powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM) combined with energy dispersive X-ray spectroscopy (EDS). The product of synthesis has been characterized as carbonated fluor/hydroxyapatite with carbonate incorporated inside channel (A-type) and substituted for the PO{sub 4}{sup 3−} group (B-type). The vibration band at 874 cm{sup −1} assigned to bending (ν{sub 2}) mode undoubtedly confirmed carbonate substituted for PO{sub 4}{sup 3−} group, while the band at 880 cm{sup −1} was attributed to A-type carbonate substitution. The additional sharp and intense band at 865 cm{sup −1} considered as “non-apatitic” carbonate substitution is not assigned with certainty so far. Evolution of CO{sub 2} from tetrahedral (PO{sub 4}{sup 3−}) sites with the increase in heat-treatment temperature is evident by the changes in tetrahedral bond lengths and angles, as obtained by the Rietveld structure refinement. Also, changes in the isotropic temperature parameters for the 2a site point to A-type carbonate incorporation as well. - Highlights: • Thermal evolution of carbonated apatite from cuttlefish bones has been studied. • A-, B- and “non-apatitic”-type of carbonate in apatite structure was determined. • Carbonated fluor/hydroxyapatite transforms into pure fluorapatite at 1300 °C.

  3. Hydrothermal synthesis of new rare earth silicate fluorides: A novel class of polar materials

    Energy Technology Data Exchange (ETDEWEB)

    McMillen, Colin D., E-mail: cmcmill@clemson.edu [Department of Chemistry and Center for Optical Materials Science and Engineering Technologies (COMSET), Clemson University, 485 H.L. Hunter Laboratories, Clemson, SC 29634 (United States); Emirdag-Eanes, Mehtap, E-mail: mehtapemirdag@iyte.edu.tr [Department of Chemistry, Izmir Institute of Technology, Gulbahce koyu, Urla, Izmir 35430 (Turkey); Stritzinger, Jared T., E-mail: jstritz@clemson.edu [Department of Chemistry and Center for Optical Materials Science and Engineering Technologies (COMSET), Clemson University, 485 H.L. Hunter Laboratories, Clemson, SC 29634 (United States); Kolis, Joseph W., E-mail: kjoseph@clemson.edu [Department of Chemistry and Center for Optical Materials Science and Engineering Technologies (COMSET), Clemson University, 485 H.L. Hunter Laboratories, Clemson, SC 29634 (United States)

    2012-11-15

    Polar crystals provide an interesting avenue for materials research both in the structures they form and the properties they possess. This work describes the hydrothermal synthesis and structural characterization of three novel silicate fluorides. Compound (1), LiY{sub 3}(SiO{sub 4}){sub 2}F{sub 2} crystallizes in space group C2/c, with a=17.651(4) A, b=4.8868(10) A, c=11.625(2) A and {beta}=131.13(3) Degree-Sign . BaY{sub 2}(Si{sub 2}O{sub 7})F{sub 2} (2) crystallizes in space group P-1, with a=5.1576(10) A, b=6.8389(14) A, c=11.786(2) A, {alpha}=93.02(3) Degree-Sign , {beta}=102.05(3) Degree-Sign and {gamma}=111.55(3) Degree-Sign . Finally, the structure of Ba{sub 2}Y{sub 3}(SiO{sub 4}){sub 2}F{sub 5} (3) was determined in the polar orthorhombic space group Pba2, having unit cell parameters a=8.8864(18) A, b=12.764(3) A and c=5.0843(10) A. The structures are compared based on their building blocks and long range polarities. Aligned silicate tetrahedra segregated into a single layer in (3) impart the observed polarity. - Graphical abstract: The polar structure of Ba{sub 2}Y{sub 3}(SiO{sub 4}){sub 2}F{sub 5}. Highlights: Black-Right-Pointing-Pointer Natural yttrium silicate fluoride minerals are briefly reviewed. Black-Right-Pointing-Pointer The synthesis and structures of LiY{sub 3}(SiO{sub 4}){sub 2}F{sub 2}, BaY{sub 2}(Si{sub 2}O{sub 7})F{sub 2} and Ba{sub 2}Y{sub 3}(SiO{sub 4}){sub 2}F{sub 5} are discussed. Black-Right-Pointing-Pointer Ba{sub 2}Y{sub 3}(SiO{sub 4}){sub 2}F{sub 5} crystallizes in the polar space group Pba2. Black-Right-Pointing-Pointer Polarity occurs primarily through aligned silicate tetrahedra in a segregated layer.

  4. Microwave radiation hydrothermal synthesis and characterization of micro- and mesoporous composite molecular sieve Y/SBA-15

    Directory of Open Access Journals (Sweden)

    Wenyuan Wu

    2017-05-01

    Full Text Available A microwave radiation hydrothermal method to control synthesis of micro- and mesoporous Y/SBA-15 composite molecular sieves was reported. The synthesized SBA-15 and Y/SBA-15 were characterized by scanning electron microscopy (SEM and N2 adsorption–desorption. The three kinds of different concentrations of hydrochloric acid (0.75 M, 2 M and 3.25 M were used to investigate the effect on Y/SBA-15. The analysis results of the composite products indicated that the optimization synthesis condition employed zeolite type Y and TEOS as silicon sources under 0.75 M hydrochloric acid by the microwave radiation hydrothermal synthesis method. The N2 adsorption–desorption test results of micro–mesoporous composite molecular sieve type Y/SBA-15 in mesoporous extent indicated that SBET is 355.529 m2/g, D‾BET is 4.050 nm, and mesoporous aperture focuses on the distribution region of 5.3 nm. It was found that the received composite product has an appropriate proportion of smaller size, larger size pore structure and the thicker pore wall. In addition, its internal channels have a high degree of order and smooth flow in long-range channels.

  5. Controllable synthesis of α- and β-MnO2: cationic effect on hydrothermal crystallization

    International Nuclear Information System (INIS)

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

    2008-01-01

    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

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

    Science.gov (United States)

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

    2017-06-01

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

  7. Effects of hydrothermal synthetic conditions on the particle size of γ-AlO(OH) in sub and supercritical water using a flow reaction system

    International Nuclear Information System (INIS)

    Hakuta, Yukiya; Ura, Haruo; Hayashi, Hiromichi; Arai, Kunio

    2005-01-01

    In the present study, we synthesized boehmite (γ-AlO(OH)) fine particles hydrothermally at 350 deg. C and 400 deg. C using a flow reaction system. The influences of the synthetic parameters including temperature, pressure, starting Al(NO 3 ) 3 concentration, and pH of the starting solution, on the boehmite particle size were investigated. Products were characterized by X-ray diffractometry and transmission electron microscopy. According to XRD analyses, all the product were crystalline γ-AlO(OH). From the results of TEM observation, the morphology of γ-AlO(OH) particles obtained was rhombic or hexagonal plates with 70-470 nm of the average particle size. The particle size increased with an increase in the reaction temperature and the starting Al(NO 3 ) 3 concentration, while that decreased with an increase in the pH of the starting solution. Moreover, at 400 deg. C the particle size enlarged from 170 nm to 300 nm with increasing reaction pressure from 25 MPa to 40 MPa, while there is no dependency of reaction pressure on the particle size at 350 deg. C. Furthermore, the particle formation and growth mechanisms are discussed based on the solubility of γ-AlO(OH) under hydrothermal conditions

  8. The effects of synthesis parameters on the formation of PbI2 particles under DTAB-assisted hydrothermal process

    International Nuclear Information System (INIS)

    Zhu Gangqiang; Hojamberdiev, Mirabbos; Liu Peng; Peng Jianhong; Zhou Jianping; Bian Xiaobin; Huang Xijin

    2011-01-01

    Highlights: ► Submicron- and micron-sized PbI 2 particles were hydrothermally synthesized. ► Structural transformation form belt-like to rod- and microtube-like was observed. ► Phase-pure PbI 2 particles could be hydrothermally obtained at pH 2 particles. ► The optical band gap energy of PbI 2 was slightly affected by morphology. - Abstract: Submicron- and micron-sized lead iodide (PbI 2 ) particles with well-controlled morphologies were successfully fabricated via a low-temperature hydrothermal process assisted by dodecyltrimethylammonium bromide (DTAB) as cationic surfactant. The as-synthesized powders were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and UV–vis spectroscopy. The effects of synthesis parameters (temperature, time, pH, and surfactant amount) were systematically investigated. The obtained results showed that the submicron structure was belt-like at 100–120 °C, transformed to rod-like by increasing temperature to 140 °C and it became a microtube-like at 160–200 °C. By changing the pH of the synthesizing solution, it was found that a pure PbI 2 phase could be obtained below 7. With the addition of increasing amount of surfactant, microparticles were converted to microrods → submicron belts → microtubes. The time-dependent experimental results revealed that the dissolution–recrystallization and dissolution–recrystallization–self-oriented-attachment were considered to be the possible mechanisms for the formation of the belt- and tube-like PbI 2 submicron- and micron-sized particles, respectively. The optical properties of the PbI 2 particles synthesized at 100–200 °C for 8 h under hydrothermal conditions were also studied.

  9. One-step hydrothermal synthesis of three-dimensional porous graphene aerogels/sulfur nanocrystals for lithium–sulfur batteries

    International Nuclear Information System (INIS)

    Jiang, Yong; Lu, Mengna; Ling, Xuetao; Jiao, Zheng; Chen, Lingli; Chen, Lu; Hu, Pengfei; Zhao, Bing

    2015-01-01

    Highlights: • 3D porous GA/S nanocrystals are prepared by a one-step hydrothermal method. • The structure is affected by hydrothermal temperature and liquid sulfur’s viscosity. • The hybrid delivers a capacity of 716.2 mA h g −1 after 50 cycles at 100 mA g −1 . • The nanosized S, strong adsorbability and intimate contact of GNS are main factors. - Abstract: Lithium–sulfur (Li–S) batteries are receiving significant attention as a new energy source because of its high theoretical capacity and specific energy. However, the low sulfur loading and large particles (usually in submicron dimension) in the cathode greatly offset its advantage in high energy density and lead to the instability of the cathode and rapid capacity decay. Herein, we introduce a one-step hydrothermal synthesis of three-dimensional porous graphene aerogels/sulfur nanocrystals to suppress the rapid fading of sulfur electrode. It is found that the hydrothermal temperature and viscosity of liquid sulfur have significant effects on particle size and loading mass of sulfur nanocrystals, graphitization degree of graphene and chemical bonding between sulfur and oxygen-containing groups of graphene. The hybrid could deliver a specific capacity of 716.2 mA h g −1 after 50 cycles at a current density of 100 mA g −1 and reversible capacity of 517.9 mA h g −1 at 1 A g −1 . The performance we demonstrate herein suggests that Li–S battery may provide an opportunity for development of rechargeable battery systems

  10. Functionalized TiO2nanoparticles by single-step hydrothermal synthesis: the role of the silane coupling agents.

    Science.gov (United States)

    Dalod, Antoine R M; Henriksen, Lars; Grande, Tor; Einarsrud, Mari-Ann

    2017-01-01

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

  11. A facile one-step hydrothermal synthesis of HfO2/graphene nanocomposite and its physio-chemical properties

    Science.gov (United States)

    Sagadevan, Suresh; Zaman Chowdhury, Zaira; Johan, Mohd. Rafie Bin; Rafique, Rahman F.

    2018-03-01

    A facile one-step hydrothermal synthesis of Hafnium oxide/Graphene (HfO2/Gr) Nanocomposite was successfully synthesized. The crystallinity index and the overall phase transformation process during the synthesis process was observed using x-ray diffraction (XRD) pattern. The surface morphology of the prepared composite was analyzed using Scanning electron microscopy (SEM). Transmission electron microscopy studies (HR-TEM) were conducted to measure the particle sizes. The presence of different types of functional groups was confirmed using FT Raman spectroscopy. UV–Visible spectrum analysis with optical ingestion was conducted to observe the optical properties of the prepared sample. The dielectric properties and conductivity of the prepared sample were investigated whereby the frequencies and the temperatures were altered. The results showed that both the phenomenon of the dielectric consistent and the dielectric loss were frequency and temperature dependent. The thermal conductivity behavior of the prepared samples was checked by calculating AC conductivity values at various temperatures.

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

    Science.gov (United States)

    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.

  13. A catechol-like phenolic ligand-functionalized hydrothermal carbon: One-pot synthesis, characterization and sorption behavior toward uranium

    Energy Technology Data Exchange (ETDEWEB)

    Li, Bo; Ma, Lijian; Tian, Yin; Yang, Xiaodan; Li, Juan; Bai, Chiyao; Yang, Xiaoyu; Zhang, Shuang; Li, Shoujian, E-mail: sjli000616@scu.edu.cn; Jin, Yongdong, E-mail: jinyongdong@scu.edu.cn

    2014-04-01

    Highlights: • A new catechol-like ligand-functionalized hydrothermal carbon sorbent is synthesized. • A combination of bayberry tannin and glyoxal is firstly used as starting materials. • Simple, economically viable and environment-friendly synthesis method. • The sorbent exhibits high sorption capacity and distinct selectivity for uranium. - Abstract: We proposed a new approach for preparing an efficient uranium-selective solid phase extractant (HTC-btg) by choosing bayberry tannin as the main building block and especially glyoxal as crosslinking agent via a simple, economic, and green one-pot hydrothermal synthesis. The results of characterization and analysis show that after addition of glyoxal into only bayberry tannin-based hydrothermal reaction system, the as-synthesized HTC-btg displayed higher thermal stability, larger specific surface area and more than doubled surface phenolic hydroxyl groups. The sorption behavior of the sorbents toward uranium under various conditions was investigated in detail and the results indicated that the process is fast, endothermic, spontaneous, and pseudo-second-order chemisorption. The U(VI) sorption capacity reached up to 307.3 mg g{sup −1} under the current experimental conditions. The selective sorption in a specially designed multi-ion solution containing 12 co-existing cations over the range of pH 1.0–4.5 shown that the amount of uranium sorbed accounts for about 53% of the total sorption amount at pH 4.5 and distinctively about 85%, unreported so far to our knowledge, at pH 2.0. Finally, a possible mechanism involving interaction between uranyl ions and phenolic hydroxyl groups on HTC-btg was proposed.

  14. Morphology-controlled hydrothermal synthesis of MnCO3 hierarchical superstructures with Schiff base as stabilizer

    International Nuclear Information System (INIS)

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

    2011-01-01

    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: → The most interesting in this work is the use of the greenhouse gases CO 2 in atmosphere as carbonate ions source to precipitate with Mn 2+ for producing MnCO 3 crystals. → This work is the first report related to the small organic molecule Schiff base as shape guiding-agent to produce different MnCO 3 hierarchical superstructures. → We are controllable synthesis of the MnCO 3 hierarchical superstructures such as chrysanthemum, straw-bundle, dumbbell and sphere-like microcrystals. → The as-prepared MnCO 3 could be used precursor to fabricate the Mn 2 O 3 hierarchical superstructures after thermal decomposition at high temperature. -- Abstract: MnCO 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 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 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 3 superstructures was proposed based on the rod-dumbbell-sphere model. Furthermore, the MnCO 3 as precursor could be further successfully transferred to Mn 2 O 3 microstructure after heating in the atmosphere at 500 o C, and the morphology of the Mn 2 O 3 was directly determined by that of the MnCO 3 precursor.

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

    Science.gov (United States)

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

    2017-09-01

    Vanadium dioxide (VO 2 ) is a widely studied inorganic phase change material, which has a reversible phase transition from semiconducting monoclinic to metallic rutile phase at a critical temperature of τ c ≈ 68 °C. The abrupt decrease of infrared transmittance in the metallic phase makes VO 2 a potential candidate for thermochromic energy efficient windows to cut down building energy consumption. However, there are three long-standing issues that hindered its application in energy efficient windows: high τ c , low luminous transmittance (T lum ), and undesirable solar modulation ability (ΔT sol ). Many approaches, including nano-thermochromism, porous films, biomimetic surface reconstruction, gridded structures, antireflective overcoatings, etc, have been proposed to tackle these issues. The first approach-nano-thermochromism-which is to integrate VO 2 nanoparticles in a transparent matrix, outperforms the rest; while the thermochromic performance is determined by particle size, stoichiometry, and crystallinity. A hydrothermal method is the most common method to fabricate high-quality VO 2 nanoparticles, and has its own advantages of large-scale synthesis and precise phase control of VO 2 . This Review focuses on hydrothermal synthesis, physical properties of VO 2 polymorphs, and their transformation to thermochromic VO 2 (M), and discusses the advantages, challenges, and prospects of VO 2 (M) in energy-efficient smart windows application. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Hydrothermal Synthesis and Mechanism of Unusual Zigzag Ag2Te and Ag2Te/C Core-Shell Nanostructures

    Directory of Open Access Journals (Sweden)

    Saima Manzoor

    2014-01-01

    Full Text Available A single step surfactant-assisted hydrothermal route has been developed for the synthesis of zigzag silver telluride nanowires with diameter of 50–60 nm and length of several tens of micrometers. Silver nitrate (AgNO3 and sodium tellurite (Na2TeO3, are the precursors and polyvinylpyrrolidone (PVP is used as surfactant in the presence of the reducing agent, that is, hydrazine hydrate (N2H4·H2O. In addition to the zigzag nanowires a facile hydrothermal reduction-carbonization route is proposed for the preparation of uniform core-shell Ag2Te/C nanowires. In case of Ag2Te/C synthesis process the same precursors are employed for Ag and Te along with the ethylene glycol used as reducing agent and glucose as the carbonizing agent. Morphological and compositional properties of the prepared products are analyzed with the help of scanning electron microscopy, transmission electron microscopy, and energy dispersive X-ray spectroscopy, respectively. The detailed formation mechanism of the zigzag morphology and reduction-carbonization growth mechanism for core-shell nanowires are illustrated on the bases of experimental results.

  17. Hydrothermal synthesis of polyethylenimine-protected high luminescent Pt-nanoclusters and their application to the detection of nitroimidazoles

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Na [State Key Laboratory of Supramolecular Structure and Materials, College of Chemistry, Jilin University, Changchun, 130012 (China); College of Materials Science and Engineering, Jilin Institute of Chemical Technology, Jilin, 132022 (China); Li, Hong-Wei, E-mail: lihongwei@jlu.edu.cn [State Key Laboratory of Supramolecular Structure and Materials, College of Chemistry, Jilin University, Changchun, 130012 (China); Wu, Yuqing, E-mail: yqwu@jlu.edu.cn [State Key Laboratory of Supramolecular Structure and Materials, College of Chemistry, Jilin University, Changchun, 130012 (China)

    2017-03-15

    A novel one-step hydrothermal synthesis of highly fluorescent platinum nanoclusters protected by polyethylenimine (Pt-NCs@PEI) is described. The products are characterized well by UV–vis absorption, fluorescence spectra, X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) imaging. The Pt-NCs@PEI possess high quantum yield at 28%, which is the relatively high one among the reported Pt-NCs; especially, the synthesis is in one-step and the reaction time is much shorter (<1 h) than the related methods. In addition, the Pt-NCs@PEI have large Stocks-shift (∼150 nm), high tolerability to the extreme pH and high ionic strengths, and excellent photo-stability under UV–vis irradiation, lay the foundation for the practical bio-applications. Finally, the obtained Pt-NCs@PEI are used to determine trace amount of metronidazole (MTZ) in buffer solution in showing a linear response over a concentration range of 0.25–300 μM and a low detection limit of 0.1 μM. Furthermore, the related investigation on response mechanism will be helpful to design and synthesize new metal nanoclusters as fluorescent probe to detect the trace amount of harmful medicine residuum as nitroimidazoles in human body. - Highlights: • This paper provides the first hydrothermal synthesis of platinum nanoclusters. • The prepared polyethylenimine-protected platinum nanoclusters possess high quantum yield of 28%. • A new method to detect trace amount of metronidazole in urine is proposed.

  18. Hydrothermal synthesis of polyethylenimine-protected high luminescent Pt-nanoclusters and their application to the detection of nitroimidazoles

    International Nuclear Information System (INIS)

    Xu, Na; Li, Hong-Wei; Wu, Yuqing

    2017-01-01

    A novel one-step hydrothermal synthesis of highly fluorescent platinum nanoclusters protected by polyethylenimine (Pt-NCs@PEI) is described. The products are characterized well by UV–vis absorption, fluorescence spectra, X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) imaging. The Pt-NCs@PEI possess high quantum yield at 28%, which is the relatively high one among the reported Pt-NCs; especially, the synthesis is in one-step and the reaction time is much shorter (<1 h) than the related methods. In addition, the Pt-NCs@PEI have large Stocks-shift (∼150 nm), high tolerability to the extreme pH and high ionic strengths, and excellent photo-stability under UV–vis irradiation, lay the foundation for the practical bio-applications. Finally, the obtained Pt-NCs@PEI are used to determine trace amount of metronidazole (MTZ) in buffer solution in showing a linear response over a concentration range of 0.25–300 μM and a low detection limit of 0.1 μM. Furthermore, the related investigation on response mechanism will be helpful to design and synthesize new metal nanoclusters as fluorescent probe to detect the trace amount of harmful medicine residuum as nitroimidazoles in human body. - Highlights: • This paper provides the first hydrothermal synthesis of platinum nanoclusters. • The prepared polyethylenimine-protected platinum nanoclusters possess high quantum yield of 28%. • A new method to detect trace amount of metronidazole in urine is proposed.

  19. Nanostructured Materials: Symthesis in Supercritical Fluids

    Energy Technology Data Exchange (ETDEWEB)

    Lin, Yuehe; Ye, Xiangrong; Wai, Chien M.

    2009-03-24

    This chapter summarizes the recent developent of synthesis and characterization of nanostructured materials synthesized in supercritical fluids. Nanocomposite catalysts such as Pt and Pd on carbon nanotube support have been synthesized and used for fuel cell applications.

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

  1. Synthesis of nickel oxide - zirconia composites by coprecipitation route followed by hydrothermal treatment

    International Nuclear Information System (INIS)

    Yoshito, Walter Kenji; Ussui, Valter; Lazar, Dolores Ribeiro Ricci; Paschoal, Jose Octavio Armani

    2009-01-01

    Nickel oxide-yttria stabilized zirconia (NiO-YSZ) for use as solid oxide fuel cell anode were synthesized by coprecipitation to obtain amorphous zirconia and crystallized β-nickel gels of the corresponding metal hydroxides. Hydrothermal treatment at 200°C and 220 psi from 2 up to 16 hours, under stirring, was performed to produce nanocrystalline powder. The as-synthesized powders were uniaxially pressed and sintered in air. Powders were characterized by X-ray diffraction, laser scattering, scanning and transmission electron microscopy (SEM/TEM), gas adsorption technique (BET) and TGDTA thermal analysis. Ceramic samples were characterized by dilatometric analysis and density measurements by Archimedes method. The characteristics of hydrothermally synthesized powders and compacts were compared to those produced without temperature and pressure application. Crystalline powders were obtained after hydrothermal process, excluding the calcination step from this route. The specific surface area of powders decreases with increasing time of hydrothermal treatment while the agglomerate mean size is not affected by this parameter. (author)

  2. Hydrothermal Synthesis and Characterization of 3R Polytypes of Mg-Al Layered Double Hydroxides

    NARCIS (Netherlands)

    Budhysutanto, W.N.

    2010-01-01

    Layered Double Hydroxides (LDH) is a unique group of clays that have an anionic exchange capability. This research explored the hydrothermal method as an alternative method to synthesize Mg-Al LDH. It is a simple and more environmentally friendly compared to the conventional method of

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

    Science.gov (United States)

    Duan, Qiuyan; Chen, Haiyan

    2017-06-01

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

  4. Hydrothermal synthesis of NiFe2O4 nano-particles: structural ...

    Indian Academy of Sciences (India)

    crystallites with an average diameter of 8.9 nm are synthesized via hydrothermal method. ..... Parameter. Value. Literature. Reference. Ms (emu g. −1. ) 57.6. 54.8. 10. A (cm2). 1551.1. —. —. Hc (G). 65.1. 59.4. 10. Mr (emu g. −1. ) 0.714. 9.8. 2. Mr/Ms.

  5. One-step hydrothermal synthesis of flower-like CoS ...

    Indian Academy of Sciences (India)

    2018-03-29

    Mar 29, 2018 ... Abstract. Flower-like CoS hierarchitectures were successfully synthesized through a hydrothermal route in the presence of ethylenediamine as ligand and structure-directing agent. The structure and morphology of the products were characterized by X-ray diffraction, transmission electron microscopy, field ...

  6. Sol-gel/hydrothermal synthesis of mixed metal oxide of Titanium and ...

    African Journals Online (AJOL)

    Mixed metal oxides of titanium and zinc nanocomposites were prepared through sol-gel method under hydrothermal condition using titanium oxy-(1, 2 - pentadione) and zinc acetate without hazardous additives. The resulting composites were characterized by X-Ray Diffractometer (XRD), Scanning Electron Microscope ...

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

    Science.gov (United States)

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

    2017-08-01

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

  8. Synthesis of nano-crystalline NiFe2O4 powders in subcritical and supercritical ethanol

    Czech Academy of Sciences Publication Activity Database

    Ćosović, A.; Žák, Tomáš; Glisić, S.; Sokić, M.; Lazarević, S.; Ćosović, V.; Orlović, A.

    2016-01-01

    Roč. 113, JUL (2016), s. 96-105 ISSN 0896-8446 R&D Projects: GA MŠk(CZ) ED1.1.00/02.0068 Institutional support: RVO:68081723 Keywords : supercritical * subcritical * nano-crystalline powders * nickel ferrite * metal oxide * magnetic properties Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.991, year: 2016

  9. Enhanced performance of LiFePO4 through hydrothermal synthesis coupled with carbon coating and cupric ion doping

    International Nuclear Information System (INIS)

    Pei Bo; Wang Qiang; Zhang Weixin; Yang Zeheng; Chen Min

    2011-01-01

    Highlights: → Hydrothermal reaction has been adopted to synthesize LiFePO 4 with a narrow size distribution. → LiFePO 4 was modified with carbon coating and cupric cation (Cu 2+ ) doping simultaneously. → Electrochemical properties of LiFePO 4 were improved by carbon coating and cupric cation doping. - Abstract: A hydrothermal reaction has been adopted to synthesize pure LiFePO 4 first, which was then modified with carbon coating and cupric ion (Cu 2+ ) doping simultaneously through a post-heat treatment. X-ray diffraction patterns, transmission electron microscopy and scanning electron microscopy images along with energy dispersive spectroscopy mappings have verified the homogeneous existence of coated carbon and doped Cu 2+ in LiFePO 4 particles with phospho-olivine structure and an average size of 400 nm. The electrochemical performances of the material have been studied by cyclic voltammetry, electrochemical impedance spectroscopy and galvanostatic charge-discharge measurements. The carbon-coated and Cu 2+ -doped LiFePO 4 sample (LFCu5/C) exhibited an enhanced electronic conductivity of 2.05 x 10 -3 S cm -1 , a specific discharge capacity of 158 mAh g -1 at 50 mA g -1 , a capacity retention of 96.4% after 50 cycles, a decreased charge transfer resistance of 79.4 Ω and superior electrode reaction reversibility. The present synthesis route is promising in making the hydrothermal method more practical for preparation of the LiFePO 4 material and enhancement of electrochemical properties.

  10. Complexing and hydrothermal ore deposition

    CERN Document Server

    Helgeson, Harold C

    1964-01-01

    Complexing and Hydrothermal Ore Deposition provides a synthesis of fact, theory, and interpretative speculation on hydrothermal ore-forming solutions. This book summarizes information and theory of the internal chemistry of aqueous electrolyte solutions accumulated in previous years. The scope of the discussion is limited to those aspects of particular interest to the geologist working on the problem of hydrothermal ore genesis. Wherever feasible, fundamental principles are reviewed. Portions of this text are devoted to calculations of specific hydrothermal equilibriums in multicompone

  11. Facile hydrothermal synthesis and luminescent properties of Sm3+/Eu3+ codoped GdPO4 phosphors

    Science.gov (United States)

    Yang, Junfeng; Xiong, Hailong; Dong, Jianchao; Yang, Chunming; Gan, Shucai; Zou, Lianchun

    2017-12-01

    Well-defined GdPO4 nanocrystals were successfully prepared through the facile hydrothermal synthesis route followed by a heat treatment. The microstructure, morphologies and photoluminescence properties of as-prepared samples were investigated via X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), fourier transform infrared spectroscopy (FT-IR), photoluminescence (PL) spectroscopy and luminescence decay, which were significantly affected by the reaction conditions (phosphorus source, acidity of hydrothermal process and surfactants). It is found that Sodium dodecyl sulfate (SDS) as a shape modifier has the dynamic effect by adjusting the growth rate of different facets, resulting in morphology transformation of GdPO4·H2O from the nanowire (without SDS) to the nanorod (with SDS). Strong yellow-orange emissions could be obtained in Sm3+ and Eu3+ ions codoped GdPO4 phosphors under ultraviolet light irradiation. Moreover, the energy transfer mechanism from Sm3+ to Eu3+ has been studied and proved to be a dipole-dipole interaction mechanism. These results show this yellow-orange-emitting phosphors material may have potential applications in field-emission displays.

  12. Synthesis of metal-doped Mn-Zn ferrite from the leaching solutions of vanadium slag using hydrothermal method

    Science.gov (United States)

    Liu, Shiyuan; Wang, Lijun; Chou, Kuochih

    2018-03-01

    Using vanadium slag as raw material, Metal-doped Mn-Zn ferrites were synthesized by multi-step processes including chlorination of iron and manganese by NH4Cl, selective oxidation of Fe cation, and hydrothermal synthesis. The phase composition and magnetic properties of synthesized metal-doped Mn-Zn ferrite were characterized by X-ray powder diffraction, Raman spectroscopy, transmission electron microscopy (TEM), X-ray photon spectra (XPS) and physical property measurement. It was found that Mn/Zn mole ratio significantly affected the magnetic properties and ZnCl2 content significantly influenced the purity of the phase of ferrite. Synthesized metal-doped Mn-Zn ferrite, exhibiting a larger saturation magnetization (Ms = 60.01 emu/g) and lower coercivity (Hc = 8.9 Oe), was obtained when the hydrothermal temperature was controlled at 200 °C for 12 h with a Mn/Zn mole ratio of 4. The effect of ZnCl2 content, Mn/Zn mole ratio and temperature on magnetic properties of the synthesized metal-doped Mn-Zn ferrite were systemically investigated. This process provided a new insight to utilize resources in the aim of obtaining functional materials.

  13. SYNTHESIS OF ZEOLITE SOCONY MOBIL FROM BLUE SILICA GEL AND RICE HUSK ASH AS CATALYSTS FOR HYDROTHERMAL LIQUEFACTION

    Directory of Open Access Journals (Sweden)

    SUYITNO

    2015-08-01

    Full Text Available Renewable biofuels produced by the hydrothermal liquefaction of rice husks have received much attention because of rapid increases in fuel consumption and corresponding declines in fossil fuel resources. To increase biofuel yields, template-free syntheses of Zeolite Socony Mobil (ZSM catalysts based on blue silica gel and rice husk ash as silica sources were studied. After ZSM synthesis in a closed reactor at 170°C, the crystallinity and crystalline diameters of the products were determined by X-ray diffraction, affording values of 56.33%– 65.81% and 64.3–68.5 nm, respectively. The hydrothermal liquefaction of rice husks with or without a catalyst was conducted in a closed reactor (1200 mm length × 100 mm diameter at 275°C for 45 min. The light biofuel was separated from the ethanol solvent and heavy biofuel via vacuum evaporation. The ZSM catalysts increased the biofuel yields by 2.9%–6.0%. The light biofuels exhibited heating values, flash points, and viscosities of approximately 4.2–4.3 kcal·g−1, 19°C, and 1.48–1.52 cSt, respectively. However, further studies are required to enhance the activity of the ZSMs and increase the quality of the biofuels.

  14. Synthesis of cerium oxide (CeO2) with high surface area through microwave assisted hydrothermal method

    International Nuclear Information System (INIS)

    Oliveira, M.J.C. de; Neiva, L.S.; Gama, L.; Oliveira, J.B.

    2011-01-01

    The objective of this research is synthesize nanoparticles with high surface area of Ceria (CeO 2 ) catalyst by a microwave hydrothermal method. For that it was used a 5% concentration in weight of [Ce(NO 3 ) 3. 6H 2 O] and 10 mL of [NaOH (5M)] under processing conditions in the equipment: maximum temperature of 150 deg C for 60 min with heating rate of 15 C /min. The resulting sample was characterized by XRD, SEM and BET method. It was observed that the Ceria particles are presented spatially in cubic structure, with crystallite size of 10 nm and surface area of 112 m²/g. Through the pore size distribution it was possible to observe that these were in mesoporous size, ranging from 3 to 30 nm. The possibility of obtaining catalysts with nanometer scale and high surface area by beans of microwave hydrothermal method, which involves low energy (low temperatures) and short synthesis time, makes this method very interesting and promising. (author)

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

    Science.gov (United States)

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

    2017-06-01

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

  16. Direct Energy Supply to the Reaction Mixture during Microwave-Assisted Hydrothermal and Combustion Synthesis of Inorganic Materials

    Directory of Open Access Journals (Sweden)

    Roberto Rosa

    2014-05-01

    Full Text Available The use of microwaves to perform inorganic synthesis allows the direct transfer of electromagnetic energy inside the reaction mixture, independently of the temperature manifested therein. The conversion of microwave (MW radiation into heat is useful in overcoming the activation energy barriers associated with chemical transformations, but the use of microwaves can be further extended to higher temperatures, thus creating unusual high-energy environments. In devising synthetic methodologies to engineered nanomaterials, hydrothermal synthesis and solution combustion synthesis can be used as reference systems to illustrate effects related to microwave irradiation. In the first case, energy is transferred to the entire reaction volume, causing a homogeneous temperature rise within a closed vessel in a few minutes, hence assuring uniform crystal growth at the nanometer scale. In the second case, strong exothermic combustion syntheses can benefit from the application of microwaves to convey energy to the reaction not only during the ignition step, but also while it is occurring and even after its completion. In both approaches, however, the direct interaction of microwaves with the reaction mixture can lead to practically gradient-less heating profiles, on the basis of which the main observed characteristics and properties of the aforementioned reactions and products can be explained.

  17. Easy and fast preparation of TiO{sub 2} - based nanostructures using microwave assisted hydrothermal synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Bregadiolli, Bruna Andressa, E-mail: brunabregadiolli@fc.unesp.br [Universidade Estadual Paulista Julio de Mesquita Filho (UNESP), Bauru, SP (Brazil); Fernandes, Silvia Leticia; Graeff, Carlos Frederico de Oliveira [Universidade Estadual Paulista de Mesquita Filho (UNESP), Araraquara, SP (Brazil)

    2017-07-15

    TiO{sub 2} derivatives with distinct morphologies have been successfully obtained by microwave assisted hydrothermal synthesis in acidic and alkaline medium using mild conditions. Titanium tetraisopropoxide (TTIP) was used as precursor in different environmental conditions under low temperatures, inferior to 150 °C, and short synthesis times, from 2 to 60 min. X ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and N{sub 2} adsorption at 77 K (BET) were used to characterize the microstructural properties of the oxides. In the acidic synthesis the reaction time and temperature are not accompanied by significant changes in the structure of the material. However, in the basic conditions, the concentration of Na{sup +} ions strongly influences the particle morphology and growth. The morphology of the nanoparticles shows irregular spheres in acidic conditions, while in alkaline medium, needle like structures are formed as well as aggregated nanotube-like structures synthesized in only 30 min. Besides the difference in the morphology and structure, in both systems, high surface area was obtained. (author)

  18. MZnFe{sub 2}O{sub 4} (M = Ni, Mn) cubic superparamagnetic nanoparticles obtained by hydrothermal synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Freire, R. M. [Universidade Federal do Ceara-UFC, Grupo de Quimica de Materiais Avancados (GQMAT)- Departamento de Quimica Analitica e Fisico-Quimica (Brazil); Ribeiro, T. S.; Vasconcelos, I. F. [Universidade Federal do Ceara, Departamento de Engenharia Metalurgica e de Materiais (Brazil); Denardin, J. C. [Universidad de Santiago de Chile, USACH, Departamento de Fisica (Chile); Barros, E. B. [Universidade Federal do Ceara-UFC, Departamento de Fisica (Brazil); Mele, Giuseppe [Universita del Salento, Dipartimento di Ingegneria dell' Innovazione (Italy); Carbone, L. [IPCF-CNR, UOS Pisa (Italy); Mazzetto, S. E.; Fechine, P. B. A., E-mail: fechine@ufc.br [Universidade Federal do Ceara-UFC, Grupo de Quimica de Materiais Avancados (GQMAT)- Departamento de Quimica Analitica e Fisico-Quimica (Brazil)

    2013-05-15

    MZnFe{sub 2}O{sub 4} (M = Ni or Mn) cubic nanoparticles have been prepared by hydrothermal synthesis in mild conditions and short time without any procedure of calcinations. The structural and magnetic properties of the mixed ferrites were investigated by X-ray diffraction, Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, Moessbauer spectroscopy, vibrating sample magnetometer, and Transmission electron microscopy (TEM). X-ray analysis showed peaks characteristics of the spinel phase. The average diameter of the nanoparticles observed by TEM measurements was approximately between 4 and 10 nm. Spectroscopy study of the spinel structure was performed based on Group Theory. The predicted bands were observed in FTIR and Raman spectrum. The magnetic parameters and Moessbauer spectroscopy were measured at room temperature and superparamagnetic behavior was observed for mixed ferrites. This kind of nanoparticles can be used as precursor in drug delivery systems, magnetic hyperthermia, ferrofluids, or magnetic imaging contrast agents.

  19. Hydrothermal synthesis of size-dependent Pt in Pt/MWCNTs nanocomposites for methanol electro-oxidation

    International Nuclear Information System (INIS)

    Chen Liang; Lu Gongxuan

    2008-01-01

    A hydrothermal method has been developed to prepare size-controlled Pt nanoparticles dispersed highly on multiwalled carbon nanotubes (Pt/MWCNTs). It was found that the size of Pt nanoparticles was strongly dependent on the solution pH in synthesis. The Pt nanoparticles with mean size of 3.0, 4.2 and 9.1 nm were obtained at pHs 13, 12 and 10 separately. After Pt/MWCNTs composites were fabricated, the different properties of cyclic voltammetry and chronoamperometry in electro-oxidation of methanol were found. The results showed that the smaller diameter Pt deposited Pt/MWCNTs nanocomposites exhibited higher electrocatalytic activity for methanol oxidation. By characterization of X-ray diffraction (XRD), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS), size-dependent activities were identified

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

    Energy Technology Data Exchange (ETDEWEB)

    Rueff, Jean-Michel, E-mail: jean-michel.rueff@ensicaen.fr [Laboratoire CRISMAT, CNRS UMR 6508, ENSICAEN, 6 bd du Maréchal Juin, F-14050 Caen Cedex (France); Poienar, Maria [National Institute for Research and Development in Electrochemistry and Condensed Matter, Plautius Andronescu Str Nr. 1, 300224 Timisoara (Romania); Guesdon, Anne; Martin, Christine; Maignan, Antoine [Laboratoire CRISMAT, CNRS UMR 6508, ENSICAEN, 6 bd du Maréchal Juin, F-14050 Caen Cedex (France); Jaffrès, Paul-Alain [Université de Brest, Université Européenne de Bretagne, CNRS UMR 6521, CEMCA, SFR 148 ScInBios, 6 Avenue Victor Le Gorgeu, 29238 Brest (France)

    2016-04-15

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

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

    Directory of Open Access Journals (Sweden)

    Patcharaporn Tippayawat

    2016-10-01

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

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

    Science.gov (United States)

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

    2016-01-01

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

  3. Hydrothermal synthesis and crystal structure of CsFe23(HPO4)2(PO4)(H2O)

    International Nuclear Information System (INIS)

    Anisimova, N.Yu.; Ilyukhin, A.B.; Chudinova, N.N.; Serafin, M.

    2001-01-01

    The double acid iron-cesium orthophosphate CsFe 2 3 (HPO 4 ) 2 (PO 4 )(H 2 O) was prepared by hydrothermal synthesis (from the Fe 2 O 3 , Cs 2 CO 3 and H 3 PO 4 mixture at 290 Deg C during 1 h following by cooling to 25 Deg C). Its crystal structure (a = 5.021(3), b = 15.80(1), c = 13.646(8), β 94.49(4) Deg, sp. gr. P2 1 /n, Z = 4) was analyzed by X-ray diffraction. The structure is formed by the orthophosphate tetrahedrons and the FeO 6 octahedrons, the water molecule is coordinated by the iron atom [ru

  4. Synthesis and characterization of silica mesoporous material produced by hydrothermal continues pH adjusting path way

    Directory of Open Access Journals (Sweden)

    A. Salemi Golezani

    2016-08-01

    Full Text Available Mesoporous silica molecular sieves MCM-41 were synthesized under hydrothermal conditions. For this purpose, a solution with a molar coefficient of water, cetyltri-methyl ammonium bromide surfactants as template and sodium silicate as the source of SiO2 are used. Phase formation, morphology and gas absorption properties were investigated by XRD and BET analysis, respectively. The results showed that silica mesoporous material has been successfully synthesized. A favorable special surface and porosity volume together with regular arrangement of nano metric-hexagonal porosities were obtained from this synthesis. Thickness of the wall and average diameter of the pores are 0.8 nm and 4 nm, respectively.

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

    Science.gov (United States)

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

    Directory of Open Access Journals (Sweden)

    Quanguo Li

    2013-01-01

    Full Text Available 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.

  7. Hydrothermal synthesis of PEDOT/rGO composite for supercapacitor applications

    Science.gov (United States)

    Ahmed, Sultan; Rafat, M.

    2018-01-01

    In this study, PEDOT/rGO composite has been successfully synthesized using hydrothermal method. Precursor solution of EDOT monomer was mixed with a predetermined solution of graphene oxide (GO). The resultant mixture was then hydrothermally treated. Surface morphology, crystal structure vibrational response and thermal stability have been studied using standard characterization techniques: field-emission scanning electron microscopy, X-ray diffraction, Raman spectroscopy and thermo-gravimetric analysis. The observed results confirm that the required composite of PEDOT/rGO has indeed been synthesized. Electrochemical properties of the synthesized product were studied in 6 M KOH aqueous solution, using characterization techniques such as: cyclic voltammetry, electrochemical impedance spectroscopy and galvanostatic charge-discharge measurements. The results show a high value of specific capacitance (102.8 F g-1) at 10 mV s-1, indicating that the composite can be profitably used for energy storage devices.

  8. Hydrothermal Synthesis of SBA-15 Using Sodium Silicate Derived from Coal Gangue

    Directory of Open Access Journals (Sweden)

    Jing Wang

    2013-01-01

    Full Text Available Well-ordered SBA-15 was prepared with a hydrothermal route by sodium silicate derived from coal gangue. The as-prepared sample was analyzed by SAXRD, BET, TEM, and SEM, respectively. The results indicate that at a low hydrothermal temperature of 100∘C the well-ordered mesoporous SBA-15 could be synthesized. The surface area, pore volume, and pore size of the sample are 552 m2/g, 0.54 cm3/g, and 7.0 nm, respectively. It is suggested that coal gangue could be used in obtaining an Si source to prepare mesoporous materials, such as SBA-15.

  9. Hydrothermal synthesis of CdTe quantum dots–TiO2–graphene hybrid

    International Nuclear Information System (INIS)

    Liu, Jinghua; Li, Xin

    2014-01-01

    CdTe–TiO 2 –graphene nanocomposites were successfully synthesized via a simple and relatively general hydrothermal method. During the hydrothermal environment, GO was reduced to reduced graphene oxide (RGO), accompanying with the anchoring of TiO 2 nanoparticles on the surface of RGO. In the following process, CdTe quantum dots (QDs) were then in situ grown on the carbon basal planes. The morphologies and structural properties of the as-prepared composites were characterized by X-ray diffraction, Raman spectroscopy, transmission electron microscopy and fluorescent spectroscopy. It is hoped that our current work could pave a way towards the fabrication of QDs–TiO 2 –RGO hybrid materials.

  10. Synthesis and characterization on titanium dioxide prepared by precipitation and hydrothermal treatment

    International Nuclear Information System (INIS)

    Santos, Andre V.P. dos; Yoshito, Walter K.; Lazar, Dolores R.R.; Ussui, Valter

    2012-01-01

    Surface properties of titanium dioxide (titania) are outstanding among ceramic materials and enables uses as catalysts, photoelectrochemical devices, solar cells and others. In many of these applications, it is necessary to keep the anatase phase, that is stable only in low temperatures (<400 deg C). In the present work, the influence of hydrothermal treatment on physical characteristics and crystal structure of titania powders synthesized by precipitation was investigated. Characterizations of obtained powders were carried out by X-ray diffraction, surface area analysis by N2 gas sorption (BET) and microstructure of powders and ceramics were analyzed by scanning electron microscopy. As prepared powders were formed as cylindrical pellets by uniaxial pressing and sintered at 1500 deg C for 01 hour. Results showed that anatase phase without formation of rutile phase can be formed in hydrothermally treated samples . Rutile phase is predominant in calcined and/or sintered samples (author)

  11. Synthesis of Titanium Dioxide nanoparticles via sucrose ester micelle-mediated hydrothermal processing route

    International Nuclear Information System (INIS)

    Anwar, N.S.; Kassim, A.; Lim, H.N.; Zakarya, S.A.; Huang, N.M.

    2010-01-01

    Titanium dioxide nanoparticles were synthesized via low-temperature sucrose ester micelle-mediated hydrothermal processing route using titanium isopropoxide as the precursor. X-ray diffractometer revealed that the samples possessed a mixed crystalline phases consisting of anatase and brookite in which anatase was the main phase. Upon increasing the hydrothermal reaction temperature, the degree of crystallinity of the nanoparticles improved and their morphology transformed from bundles of needles to rods and to spheres. Photo catalytic behaviour of the as-synthesized nanoparticles was investigated by photodegradation of methylene blue solution in an ultraviolet A irradiating photo reactor. The as-synthesized nanoparticles exhibited higher photo catalytic performance as compared to the commercial counterpart. (author)

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

    International Nuclear Information System (INIS)

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

    2010-01-01

    NiO microspheres were successfully obtained by calcining the Ni(OH) 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.

  13. Hydrothermal synthesis and characterization of sea urchin-like nickel and cobalt selenides nanocrystals

    Energy Technology Data Exchange (ETDEWEB)

    Liu Xiaohe [Department of Inorganic Materials, Central South University, Changsha, Hunan 410083 (China) and School of Metallurgical Science and Engineering, Central South University, Changsha, Hunan 410083 (China)]. E-mail: liuxh@mail.csu.edu.cn; Zhang Ning [Department of Inorganic Materials, Central South University, Changsha, Hunan 410083 (China); Yi Ran [Department of Inorganic Materials, Central South University, Changsha, Hunan 410083 (China); Qiu Guanzhou [Department of Inorganic Materials, Central South University, Changsha, Hunan 410083 (China); Yan Aiguo [Department of Inorganic Materials, Central South University, Changsha, Hunan 410083 (China); Wu Hongyi [Department of Inorganic Materials, Central South University, Changsha, Hunan 410083 (China); Meng Dapeng [Department of Inorganic Materials, Central South University, Changsha, Hunan 410083 (China); Tang, Motang [School of Metallurgical Science and Engineering, Central South University, Changsha, Hunan 410083 (China)

    2007-05-25

    Sea urchin-like nanorod-based nickel and cobalt selenides nanocrystals have been selective synthesized via a hydrothermal reduction route in which hydrated nickel chloride and hydrated cobalt chloride were employed to supply Ni and Co source and aqueous hydrazine (N{sub 2}H{sub 4}.H{sub 2}O) was used as reducing agent. The composition, morphology, and structure of final products could be easily controlled by adjusting the molar ratios of reactants and process parameters such as hydrothermal time. The morphology and phase structure of the final products have been investigated by X-ray diffraction, transmission electron microscopy, and scanning electron microscopy. The probable formation mechanism of the sea urchin-like nanorod-based nickel and cobalt selenides nanocrystals was discussed on the basis of the experimental results.

  14. Synthesis of boehmite by hydrothermal treatment used as inorganic binder for alumina powder

    International Nuclear Information System (INIS)

    Lima, M.B.; Tercini, M.B.; Yoshimura, H.N.

    2012-01-01

    Presently, due to the concerns with the environment, it has been developed studies to replace the organic binder by an inorganic binder for forming of ceramic powders, in order to avoiding the generation of polluting gases during sintering (firing). A potential alternative is the use of boehmite, produced by hydrothermal treatment on the surfaces of the alumina powder, previously ground in a ball mill using zirconia milling media to produce hydrated phases on alumina powder which are converted to boehmite. In the treated alumina powders, it was observed the formation of boehmite phase by X-ray diffraction analysis and Fourier transformed infrared (FTIR) spectroscopy, demonstrating the efficiency of boehmite formation during the hydrothermal treatment at 150°C for 3 hours.(author)

  15. Single step hydrothermal based synthesis of M(II)Sb2O6 (M = Cd ...

    Indian Academy of Sciences (India)

    Abstract. Experiments involving single step hydrothermal reactions of the divalent metal (Zn2+, Cd2+, Pb2+,. Cu2+, Ni2+ and Mn2+) salts with ilmenite NaSbO3 yielded pure divalent antimonates in the case of CdSb2O6 crys- tallizing in the PbSb2O6 type structure and ZnSb2O6 crystallizing in the trirutile structure type.

  16. Hydrothermal synthesis and upconversion luminescent properties of YVO4:Yb3+,Er3+ nanoparticles

    International Nuclear Information System (INIS)

    Liang, Yanjie; Chui, Pengfei; Sun, Xiaoning; Zhao, Yan; Cheng, Fuming; Sun, Kangning

    2013-01-01

    Graphical abstract: YVO 4 :Yb 3+ ,Er 3+ nanoparticles have been successfully prepared via a facile hydrothermal technique in the presence of citric acid as a complexing agent followed by a subsequent heat treatment process. The PL intensity of the sample increases with the increase of annealing temperature and excitation power. Under the excitation of a 980 nm diode laser, the samples show bright green luminescence. Highlights: ► YVO 4 :Yb 3+ ,Er 3+ nanoparticles were prepared by a hydrothermal approach. ► Bright green luminescence is observed under the excitation of a 980 nm laser diode. ► The PL intensity increases with the increase of annealing temperature. ► Energy transfer properties between Yb 3+ ion and Er 3+ ion were analyzed. -- Abstract: In this paper, YVO 4 :Yb 3+ ,Er 3+ nanoparticles have been successfully prepared via a facile hydrothermal technique in the presence of citric acid as a complexing agent followed by a subsequent heat treatment process. The nanostructures, morphologies and upconversion luminescent properties of the as-prepared YVO 4 :Yb 3+ ,Er 3+ upconverting nanoparticles were investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM) and photoluminescent (PL) spectra. XRD results indicate that all the diffraction peaks of samples can be well indexed to the tetragonal phase of YVO 4 . TEM images demonstrate that the samples synthesized hydrothermally consist of granular-like nanoparticles ranging in size from about 30 to 50 nm. After being calcined at 500–800 °C for 2 h, the grain sizes of nanoparticles increase slightly. Additionally, the as-prepared nanoparticles show bright green luminescence corresponding to the 2 H 11/2 → 4 I 15/2 and 4 S 3/2 → 4 I 15/2 transitions of Er 3+ ions under the excitation of a 980 nm diode laser, which might find potential applications in fields such as phosphor powders, infrared detection and display devices

  17. Synthesis of tungsten oxide nanoparticles using a hydrothermal method at ambient pressure

    DEFF Research Database (Denmark)

    Ahmadi, Majid; Younesi, Reza; Guinel, Maxime J-F

    2014-01-01

    ) nanoparticles were synthesized using a simple and inexpensive low temperature and low pressure hydrothermal (HT) method. The precursor solution used for the HT process was prepared by adding hydrochloric acid to diluted sodium tungstate solutions (Na2WO4 center dot 2H(2)O) at temperatures below 5 degrees C....... The products were characterized using powder x-ray diffraction, transmission electron microscopy (including electron energy-loss spectroscopy and electron diffraction), and x-ray photoelectron spectroscopy....

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

    Directory of Open Access Journals (Sweden)

    Shintaro Ueno

    2015-03-01

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

  19. Hydrothermal synthesis of barium germanate microrods and photocatalytic degradation performance for methyl blue

    Energy Technology Data Exchange (ETDEWEB)

    Pei, L.Z., E-mail: lzpei@ahut.edu.cn [Key Lab of Materials Science and Processing of Anhui Province, School of Materials Science and Engineering, Anhui University of Technology, Ma’anshan, Anhui 243002 (China); Wang, S.; Xie, Y.K.; Yu, H.Y. [Key Lab of Materials Science and Processing of Anhui Province, School of Materials Science and Engineering, Anhui University of Technology, Ma’anshan, Anhui 243002 (China); Guo, Y.H. [Department of Materials Science, Fudan University, Shanghai 200433 (China)

    2014-02-25

    Highlights: • Barium germanate microrods have been synthesized by a simple hydrothermal process. • The size of the barium germanate microrods can be controlled by growth conditions. • Barium germanate microrods exhibit good photocatalytic activities for methyl blue. -- Abstract: Barium germanate microrods were prepared by a facile hydrothermal process without any surfactants. X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared (FTIR) and photoluminescence spectra were used to characterize the structure, morphology, size and optical properties of the barium germanate microrods. XRD and SEM observations show that the microrods with hexagonal BaGe{sub 4}O{sub 9} phase have the diameter of 500 nm to 1.5 μm. The size of the barium germanate microrods can be tuned by controlling the hydrothermal temperature, reaction time and surfactants. The influence factors including the irradiation time, content of the barium germanate microrods and MB concentration on the photocatalytic degradation of methylene blue (MB) have been analyzed. The barium germanate microrods show a MB degradation ratio of 83.49% after the irradiation time for 30 min using 1.25 mg/ml barium germanate microrods in 10 mgL{sup −1} MB solution.

  20. Controlled synthesis of graphene sheets with tunable sizes by hydrothermal cutting

    International Nuclear Information System (INIS)

    Ma Chen; Chen Zhongxin; Fang Ming; Lu Hongbin

    2012-01-01

    We report a hydrothermal method that directly reduces graphene oxide (GO) into graphene nanosheets (GNs) with different sizes. In the presence of NaOH and hydrazine, the hydrothermal reaction at 80 °C resulted in the formation of GNs with a lateral size of ∼1 μm but the size of GNs decreased to ∼300 and ∼100 nm upon increasing the reaction temperature to 150 and 200 °C, respectively. The morphology of the resulting GNs was observed by atomic force microscopy and transmission electron microscopy. The thickness of GNs is basically <3 nm, indicates the GNs stack together in a few-layer manner. XRD, XPS, FTIR, and Raman spectroscopy were used to characterize the structural changes before and after reduction. The results suggested that the defect stability in GO and reduced GNs could be responsible for the temperature dependence of the size of reduced GNs.Graphical AbstractA hydrothermal method is proposed to simultaneously reduce and cut graphene oxide into graphene sheets with different sizes in a controlled manner, in which the reaction temperature as a critical parameter is used to control the size of resulting graphene sheets.

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

    Energy Technology Data Exchange (ETDEWEB)

    Anuwattana, Rewadee [Environmental Technology Division, School of Energy and Materials, King Mongkut' s University of Technology Thonburi, Bangkok 10140 (Thailand); Khummongkol, Pojanie, E-mail: Pojanie.khu@kmutt.ac.th [Environmental Technology Division, School of Energy and Materials, King Mongkut' s University of Technology Thonburi, Bangkok 10140 (Thailand)

    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 {sup o}C for 1-9 h with different H{sub 2}O/SiO{sub 2} ratios. The result shows that higher H{sub 2}O/SiO{sub 2} ratio increases the rate of crystallization. The largest amount of crystallinity for Na-A was found at 3 h. 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{sup 4+} and Al{sup 3+} in 3 M NaOH were investigated during the hydrothermal reaction.

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

    Science.gov (United States)

    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.

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

    International Nuclear Information System (INIS)

    Anuwattana, Rewadee; Khummongkol, Pojanie

    2009-01-01

    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 o C for 1-9 h with different H 2 O/SiO 2 ratios. The result shows that higher H 2 O/SiO 2 ratio increases the rate of crystallization. The largest amount of crystallinity for Na-A was found at 3 h. 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 3 M NaOH were investigated during the hydrothermal reaction.

  4. Synthesis and Electrochemical Performance of LiMnPO4 by Hydrothermal Method

    Directory of Open Access Journals (Sweden)

    Daichi Fujimoto

    2014-01-01

    Full Text Available LiMnPO4 with olivinestructure which is the promising candidate for high voltage cathode material was synthesized by hydrothermal method. In order to synthesize high purity and well-defined LiMnPO4, several precursors for Li, Mn, and P sources and hydrothermal reaction parameters including temperature and [H2O]/[Mn] value are optimized. By analyzing the structure, Mn valence, morphology, and chemical ratio via XRD, XPS, Raman, SEM, and ICP LiMnPO4 synthesized from manganese acetate tetrahydrate have single phase of LiMnPO4 without impurity and showed charge and discharge reaction caused by Mn2+/Mn3+ redox. Specific capacity of synthesized LiMnPO4 grew up during cycling. Moreover, when hydrothermal temperature was set at 150°C and [H2O]/[Mn] value was set at 15, discharge capacity as high as 70 mAh/g was obtained at 1/20  C rate.

  5. Hydrothermal synthesis of core–shell TiO2 to enhance the photocatalytic hydrogen evolution

    International Nuclear Information System (INIS)

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

    2016-01-01

    Graphical abstract: Core–shell TiO 2 with interior cavity was synthesized by a hydrothermal approach to enhance the photocatalytic performance. - Highlights: • Core–shell TiO 2 with interior cavity can be synthesized by hydrothermal approach. • Multiple reflection of incident light in cavity can increase the absorption. • Rutile can optimize the bandgap and delay the charge recombination. - Abstract: A hydrothermal approach was designed to synthesize core–shell TiO 2 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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Uchiyama, Hiroaki, E-mail: h_uchi@kansai-u.ac.jp; 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.

  7. Supercritical fluid technologies for ceramic-processing applications

    International Nuclear Information System (INIS)

    Matson, D.W.; Smith, R.D.

    1989-01-01

    This paper reports on the applications of supercritical fluid technologies for ceramic processing. The physical and chemical properties of these densified gases are summarized and related to their use as solvents and processing media. Several areas are identified in which specific ceramic processes benefit from the unique properties of supercritical fluids. The rapid expansion of supercritical fluid solutions provides a technique for producing fine uniform powders and thin films of widely varying materials. Supercritical drying technologies allow the formation of highly porous aerogel products with potentially wide application. Hydrothermal processes leading to the formation of large single crystals and microcrystalline powders can also be extended into the supercritical regime of water. Additional applications and potential applications are identified in the areas of extraction of binders and other additives from ceramic compacts, densification of porous ceramics, the formation of powders in supercritical micro-emulsions, and in preceramic polymer processing

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

    Energy Technology Data Exchange (ETDEWEB)

    Hu, He; Xu, Jie-yan; Yang, Hong; Liang, Jie [Department of Chemistry, Shanghai Normal University, No. 100, Guilin Road, Shanghai 200234 (China); Yang, Shiping, E-mail: shipingy@shnu.edu.cn [Department of Chemistry, Shanghai Normal University, No. 100, Guilin Road, Shanghai 200234 (China); Wu, Huixia [Department of Chemistry, Shanghai Normal University, No. 100, Guilin Road, Shanghai 200234 (China)

    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.

  9. A process to enhance the specific surface area and capacitance of hydrothermally reduced graphene oxide

    KAUST Repository

    Alazmi, Amira

    2016-08-26

    The impact of post-synthesis processing in reduced graphene oxide materials for supercapacitor electrodes has been analyzed. A comparative study of vacuum, freeze and critical point drying was carried out for hydrothermally reduced graphene oxide demonstrating that the optimization of the specific surface area and preservation of the porous network are critical to maximize its supercapacitance performance. As described below, using a supercritical fluid as the drying medium, unprecedented values of the specific surface area (364 m2 g−1) and supercapacitance (441 F g−1) for this class of materials have been achieved.

  10. Clean synthesis of molecular recognition polymeric materials with chiral sensing capability using supercritical fluid technology. Application as HPLC stationary phases.

    Science.gov (United States)

    da Silva, Mara Soares; Vão, Eva R; Temtem, Márcio; Mafra, Luís; Caldeira, Jorge; Aguiar-Ricardo, Ana; Casimiro, Teresa

    2010-03-15

    Molecularly imprinted polymers (MIPs) of poly(ethylene glycol dimethacrylate) and poly(N-isopropylacrylamide-co-ethylene glycol dimethacrylate) were synthesized for the first time in supercritical carbon dioxide (scCO(2)), using Boc-L-tryptophan as template. Supercritical fluid technology provides a clean and one-step synthetic route for the preparation of affinity polymeric materials with sensing capability for specific molecules. The polymeric materials were tested as stationary HPLC phases for the enantiomeric separation of L- and D-tryptophan. HPLC results prove that the synthesized MIPs are able to recognize the template molecule towards its enantiomer which opens up potential applications in chromatographic chiral separation. (c) 2009 Elsevier B.V. All rights reserved.

  11. Synthesis and characterization of Zn3Ta2O8 nanomaterials by hydrothermal method

    International Nuclear Information System (INIS)

    Bîrdeanu, M.; Bîrdeanu, A.-V.; Gruia, A.S.; Fagadar-Cosma, E.; Avram, C.N.

    2013-01-01

    Graphical abstract: The results of an experimental program that was focused on obtaining the Zn 3 Ta 2 O 8 nanocrystalline synthesized by hydrothermal method using tantalum (V) oxide and zinc nitrate, the results of the nanomaterial’s structure characterization and the optical spectral properties of such nanomaterials that were thoroughly investigated. Also, the experimental results are compared with ab initio calculations of electronic properties of Zn 3 Ta 2 O 8 . Highlights: •Zn 3 Ta 2 O 8 nanomaterials were synthesized by hydrothermal method and characterized. •The obtained nanomaterials has excellent phosphor, optical and morphological properties. •The material can be used in designing high performance optoelectronical devices. -- Abstract: Zn 3 Ta 2 O 8 has been synthesized by hydrothermal method using tantalum (V) oxide and zinc nitrate. The crystal structure and microstructure, phase composition and the absorption of Zn 3 Ta 2 O 8 nanomaterials were characterized by X-ray diffraction, FT/IR measurements, UV–VIS measurements, PL measurements, SEM and AFM techniques and BET analysis. XRD results show the single phase of Zn 3 Ta 2 O 8 and the average particle size that is 52 nm. This narrow nanometer size was also confirmed by AFM measurements. BET analysis revealed that the nanomaterials are mesoporous. The PL spectra show the blue luminescence of Ta 2 Zn 3 O 8 . Besides, in the present work we report ab initio calculations regarding electronic properties of Zn 3 Ta 2 O 8 ; the theoretical results are compared with the experimental ones

  12. Hydrothermal Synthesis of ZnO/SnO2 Nanoparticles with High Photocatalytic Activity

    OpenAIRE

    Azam Anaraki Firooz; Ali Reza Mahjoub; Abbas Ali Khodadadi

    2011-01-01

    The paper reports the preparation and photocatalytic activity of ZnO/SnO2 and SnO2 nanoparticles. These nanoparticles were synthesized by hydrothermal method. The products were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Their grain sizes are about 50-100 nm. The photocatalytic activities of these materials were investigated for congo red removal from aqueous solution under UV light irradiation. It was shown that the use of ZnO/SnO2 as...

  13. Two-step hydrothermal synthesis of Ru-Sn oxide composites for electrochemical supercapacitors

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Chi-Chang; Chang, Kuo-Hsin; Wang, Chen-Ching [Department of Chemical Engineering, National Chung Cheng University, Chia-Yi 621 (China)

    2007-03-20

    A two-step hydrothermal process was developed to synthesize hydrous 30RuO{sub 2}-70SnO{sub 2} composites with much better capacitive performances than those fabricated through the normal hydrothermal process, co-annealing method, or modified sol-gel procedure. A very high specific capacitance of RuO{sub 2} (C{sub S,Ru}), ca. 1150 F g{sup -1}, was obtained when this composite was synthesized via this two-step hydrothermal process with annealing in air at 150 C for 2 h. The voltammetric currents of this annealed composite were found to be quasi-linearly proportional to the scan rate of CV (up to 500 mV s{sup -1}), demonstrating its excellent power property. From Raman, UV-vis spectroscopic and TEM analyses, the reduction in mean particulate size is clearly found for this two-step oxide composite, attributable to the co-precipitation of (Ru{sub {delta}}Sn{sub 1-{delta}})O{sub 2}.xH{sub 2}O onto partially dissolved SnO{sub 2}.xH{sub 2}O and the formation of (Ru{sub {delta}}Sn{sub 1-{delta}})O{sub 2}.xH{sub 2}O crystallites in the second step. This effect significantly promotes the utilization of RuO{sub 2} (i.e., very high C{sub S,Ru}). The excellent capacitive performances, very similar to that of RuO{sub 2}.xH{sub 2}O, suggest the deposition of RuO{sub 2}-enriched (Ru{sub {delta}}Sn{sub 1-{delta}})O{sub 2}.xH{sub 2}O onto SnO{sub 2}.xH{sub 2}O seeds as well as the individual formation of (Ru{sub {delta}}Sn{sub 1-{delta}})O{sub 2}.xH{sub 2}O crystallites in the second hydrothermal step. (author)

  14. Thioglycolic acid (TGA) assisted hydrothermal synthesis of SnS nanorods and nanosheets

    International Nuclear Information System (INIS)

    Biswas, Subhajit; Kar, Soumitra; Chaudhuri, Subhadra

    2007-01-01

    Nanorods and nanosheets of tin sulfide (SnS) were synthesized by a novel thioglycolic acid (TGA) assisted hydrothermal process. The as prepared nanostructures were characterized by X-ray diffraction (XRD) study, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). XRD study reveals the formation of well-crystallized orthorhombic structure of SnS. Diameter of the SnS nanorods varied within 30-100 nm. High-resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED) patterns identify the single crystalline nature for the SnS nanocrystals. The mechanism for the TGA assisted growth for the nanosheets and nanorods have been discussed

  15. Hydrothermal Synthesis and Electrochemical Performance of Manganese Oxide (Na-OMS-2) Nanorods.

    Science.gov (United States)

    Zhang, Qing; Xu, Shan; Zheng, Hao; Luo, Zhaohui; Liu, Kang; Wang, Wei; Li, Guohua; Wang, Shiquan; Liu, Jianwen; Feng, Chuanqi

    2017-02-01

    Sodium octahedral molecular sieve nanorods (Na-OMS-2) were prepared through a facile hydrothermal method. The effects of reaction temperature and duration on particle sizes of the products were investigated. The electrochemical performance of samples was studied by constant current charge–discharge tests as cathode material for Li-ion batteries (LIBs). The initial discharge capacity of Na-OMS-2 is 123.4 mAh g−1 and the capacity retention was 123.9 mAh g−1 after 100 cycles. The result demonstrates that Na-OMS-2 cathode material behaves a good cycling stability.

  16. Controlled hydrothermal synthesis of CeO{sub 2} nanospheres and their excellent magnetic properties

    Energy Technology Data Exchange (ETDEWEB)

    Niu, Xiaofei [Suzhou University, Anhui Key Laboratory of Spintronics and Nanomaterials Research, Suzhou, Anhui (China)

    2017-04-15

    Monodisperse spherical CeO{sub 2} nanostructures with irregular and rough surfaces have successfully been synthesized via a facile hydrothermal technology. XRD, SEM, XPS, Raman scattering, and M-H curves were employed to characterize the samples. The results showed that the spherical CeO{sub 2} nanostructures have a cubic fluorite structure and that there are Ce{sup 3+} ions and oxygen vacancies in the surface of the samples. The M-H curve of CeO{sub 2} nanospheres exhibits excellent room-temperature ferromagnetism (RT-FM), which is likely ascribed to the effects of the Ce{sup 3+} ions and oxygen vacancies. (orig.)

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

    Science.gov (United States)

    Uchiyama, Hiroaki; Nakanishi, Shunsuke; Kozuka, Hiromitsu

    2014-09-01

    Crystalline SnO particles were obtained from Sn6O4(OH)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.

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

    Science.gov (United States)

    Niu, Xiaofei

    2017-04-01

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

  19. Hydrothermal Synthesis of Bi2S3 Nanostructures and ABS-Based Polymeric Nanocomposite

    Directory of Open Access Journals (Sweden)

    D. Ghanbari

    2014-04-01

    Full Text Available Bismuth sulfide nano-rods and nano-flowers were synthesized via a hydrothermal reaction at a relatively low temperature. Thioglycolic acid is used as sulfur source and capping agent simultaneously. Bi2S3 nanostructures were then added to acrylonitrile-butadiene-styrene (ABS copolymer. The thermal stability behavior of ABS filled with bismuth sulfide nano-rods were investigated by thermogravimetric analysis (TGA. Nanostructures were characterized by X-ray diffraction (XRD, scanning electron microscopy (SEM and atomic force microscopy (AFM. The flame retardancy behavior of ABS-Bi2S3 was studied by UL-94 analysis.

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

    Science.gov (United States)

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

    2006-11-23

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

  1. Hydrothermal synthesis of ZnSe:Cu quantum dots and their luminescent mechanism study by first-principles

    Energy Technology Data Exchange (ETDEWEB)

    Liang, Qingshuang; Bai, Yijia; Han, Lin; Deng, Xiaolong [State Key Laboratory of Rare Earth Resources Utilization, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China); Graduate School, Chinese Academy of Sciences, Beijing 10049 (China); Wu, Xiaojie [State Key Laboratory of Rare Earth Resources Utilization, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China); Wang, Zhongchang [WPI Research Center, Advanced Institute for Materials Research, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai 980-8577 (Japan); Liu, Xiaojuan, E-mail: lxjuan@ciac.jl.cn [State Key Laboratory of Rare Earth Resources Utilization, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China); Meng, Jian, E-mail: jmeng@ciac.jl.cn [State Key Laboratory of Rare Earth Resources Utilization, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China)

    2013-11-15

    An one-pot synthesis of aqueous ZnSe:Cu nanocrystals (NCs) is realized in aqueous solution by a facile yet efficient hydrothermal technique. The dopant emission spectrum of the NCs is tunable, spanning a wide range from 438 to 543 nm. Room-temperature quantum yield for the NCs prepared at the optimal conditions reaches as high as 20% without any post-treatment. The ZnSe:Cu NCs prepared in a neutral aqueous solution (pH=8) are remarkably stable and exhibit comparatively high photoluminescent quantum yield (PL QY) as high as 17%. First-principles pseudopotential calculations using plane-wave basis functions have been performed. The formation energies of copper ions occupied in the interstitial octahedron and substitutional tetrahedral Zn{sup 2+} sites have been calculated. The occupation of copper ions in the interstitial octahedral site is found to be more thermodynamics-facilitated by −0.98 eV. The density of state analysis indicates that the Cu-related emission is primary dominated by the substitutional tetrahedral Cu ions, and the large dopant related emission width of ZnSe:Cu NCs originated from the corresponding Cu 3d impurity band. Highlights: • One-pot synthesis of aqueous ZnSe:Cu nanocrystals with tunable emission and high QY%. • ZnSe:Cu NCs exhibit high QY% at neutral pH suitable for biological application. • The microscopic mechanism underlying Cu-related emission has been provided.

  2. Hydrothermal synthesis and characterization of a binuclear complex and a coordination

    Directory of Open Access Journals (Sweden)

    Reza Mohamadinasab

    2010-06-01

    Full Text Available Two new copper complexes [(bipy(pydcCu(μ-OCO-pydcCu(bipy(H2O].3.5H¬2O (1 and {[(μ2-C2O4(2,2'-bipyCu].2H2O}n (2 (pydcH2 = pyridine-2,6-dicarboxylilic acid, bipy = 2,2'-bipyridine have been hydrothermally synthesized. Both complexes were characterized by IR spectroscopy, elemental analysis and single crystal X-ray diffraction studies. Complex 1 consists of two independent neutral molecules. In every moiety, metal ion center is in a distorted octahedral geometry. Coordination polymer (2 has been prepared from the reaction of bis-(cyclohexanone-oxal-dihydrazone,2,2'-bipyridine and Cu(NO32 in basic solution and under hydrothermal condition. The results showed that the bis-(cyclohexanone-oxal-dihydrazone was converted to oxalate ion under heating and basic pH. Each metal ion center in 2 is in a distorted octahedral geometry and is coordinated by four oxygen atoms of two bridged oxalate ions and two nitrogen atoms of 2,2'-bipyridine molecules. In the crystal structure of 2, some H-bonds and π-π interaction cause formation of a 3D network.

  3. Synthesis of ZnO nanoparticles using a hydrothermal method and a study its optical activity.

    Science.gov (United States)

    Bharti, Dattatraya B; Bharati, A V

    2017-05-01

    ZnO nanoparticles (NPs) with a granular morphology were synthesized using a hydrothermal method. Structural analysis revealed that ZnO NPs had a single crystal wurtzite hexagonal structure. Solvent polarity was responsible for varying and controlling their size and morphology. The process was very trouble free and scalable. In addition, it could be used for fundamental studies on tunable morphology formation. This hydrothermal method showed different morphology with different co-surfactants such as a floral-like or wire-like belt sheet structures etc. Based on their surface morphology, the same material had different applications as a catalyst in various organic reactions and also could be used as a photocatalyst and fuel cell, solar cell or in semiconductors etc. X-ray diffraction (XRD), scanning electron microscopy (SEM), ultraviolet-visible spectroscopy and photoluminescence of the resulting product was performed to study its purity, morphology and size, plus its optical properties via measurement of band gap energy and light absorbance. Copyright © 2016 John Wiley & Sons, Ltd.

  4. Synthesis of anatase mesoporous by using cyclodextrin as a pore forming template via hydrothermal treatment

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Joo Hee; An, So Young; Jang, Soe Hyun; Lee, Jun Woo; Chung, Jae Woo [Dept. of Organic Materials and Fiber Engineering, Soongsil University, Seoul (Korea, Republic of)

    2015-06-15

    Porous titanium dioxide with an average pore diameter of several nanometers and a narrow pore size distribution was prepared by using cyclodextrin (CD) in a sol–gel reaction of titanium precursor. After the reaction, a hydrothermal treatment was performed, and a WAXD analysis shows that the hydrothermal treatment successfully induces an anatase crystalline structure in TiO{sub 2} . The combined results from TGA, FT-IR, N{sub 2} adsorption–desorption isotherm, TEM, and SEM analyses show that the CD act as a pore forming template to form TiO{sub 2} with a wormhole-type pore and a large specific surface area. Furthermore, the ratio of the CD/Ti precursor affects the porosity and the morphology of the mesoporous TiO{sub 2} . In contrast, TiO{sub 2} prepared without CD does not exhibit a porous structure. The formation of these porous structures is a result of the self-assembly of Ti species around the CD molecules, TiO{sub 2} growth, and pore-forming by the removal of CD.

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

    International Nuclear Information System (INIS)

    Xu Jiasheng; Xue Dongfeng

    2007-01-01

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

  6. Investigation of the Optimal Parameters in Hydrothermal Method for the Synthesis of ZnO Nanorods

    Directory of Open Access Journals (Sweden)

    Ying-Chung Chen

    2014-01-01

    Full Text Available We investigated a two-step method to deposit the ZnO-based nanostructure films, including nanorods and nanoflowers. In the first step, sputtering method was used to deposit the ZnO films on SiO2/Si substrates as the seed layer. In the second step, Zn(NO32–6H2O and C6H12N4 were used as precursors and hydrothermal process was used as the method to synthesize the ZnO films. After that, the ZnO films were measured by an X-ray diffraction pattern and a FESEM to analyze their crystallization and morphology. We had found that the ZnO films had three different morphologies synthesized on ZnO/SiO2/Si substrates, including irregular-plate structure films, nanorod films, and beautiful chrysanthemum-like clusters (nanoflower films. We would prove that the face direction of ZnO/SiO2/Si substrates in the hydrothermal bottle and deposition time were two important factors to influence the synthesized results of the ZnO films.

  7. Hydrothermal synthesis of Ni{sub 2}P nanoparticle and its hydrodesulfurization of dibenzothiophene

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Qi; Han, Yang; Huang, Xiang, E-mail: materials@ouc.edu.cn; Dai, Jinhui; Tian, Jintao; Zhu, Zhibin; Yue, Li [Ocean University of China, Institute of Materials Science and Engineering (China)

    2017-04-15

    Nanosized nickel phosphide (Ni{sub 2}P) has been synthesized via hydrothermal reaction with environmental-friendly red phosphorus and nickel chloride. The reaction mechanism has been studied by measurement techniques of IC, XRD ,TEM, EDS, and XPS. The results showed that the particle sizes of as-prepared Ni{sub 2}P are in nanoscale ranging from 10 to 30 nm. In hydrothermal reaction, red phosphorus reacts with water to its oxyacids, especially its hypophosphorous acid (or hypophosphite) which can reduce nickel chloride to nickel, and then metallic nickel will penetrate into the rest of red phosphorus to generate nano-Ni{sub 2}P. Furthermore, the catalytic performance of as-synthesized Ni{sub 2}P for the hydrodesulfurization of dibenzothiophene has been tested. It has been shown that the HDS reaction process over Ni{sub 2}P catalyst agrees well with the pseudo-first order kinetic equation, and the HDS conversion can reach up to 43.83% in 5 h with a stable increasing catalytic activity during the whole examination process.

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

    Energy Technology Data Exchange (ETDEWEB)

    Ravishankar, T.N. [Centre for Nano and Material Sciences, Jain University, Jakkasandra, Kanakapura (T) (India); Nagaraju, G., E-mail: nagarajugn@rediffmail.com [Centre for Nano and Material Sciences, Jain University, Jakkasandra, Kanakapura (T) (India); Department of Chemistry, Siddaganga Institute of Technology, Tumkur, Karnataka (India); Dupont, Jairton [School of Chemistry, University of Nottingham, University Park, NG7 2RD Nottingham (United Kingdom)

    2016-06-15

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

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

    Science.gov (United States)

    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.

  10. Hydrothermal Synthesis, Characterization, and Optical Properties of Ce Doped Bi2MoO6 Nanoplates

    Directory of Open Access Journals (Sweden)

    Anukorn Phuruangrat

    2014-01-01

    Full Text Available Undoped and Ce doped Bi2MoO6 samples were synthesized by hydrothermal reaction at 180°C for 20 h. Phase, morphology, atomic vibration, and optical properties were characterized by X-ray powder diffraction (XRD, X-ray photoelectron spectroscopy (XPS, Raman spectrophotometry, Fourier transform infrared (FTIR spectroscopy, scanning electron microscopy (SEM, transmission electron microscopy (TEM, selected area electron diffraction (SAED, and UV-visible spectroscopy. In this research, the products were orthorhombic Bi2MoO6 nanoplates with the growth direction along the [0b0], including the asymmetric and symmetric stretching and bending modes of Bi–O and Mo–O. Undoped and Ce doped Bi2MoO6 samples show a strong absorption in the UV region.

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

    Energy Technology Data Exchange (ETDEWEB)

    Huirache-Acuna, R., E-mail: rafael_huirache@yahoo.it [CFATA-UNAM, Boulevard Juriquilla 3001, Juriquilla Queretaro, 76230 (Mexico); Universidad La Salle Morelia, Av. Universidad 500, Mpio. Tarimbaro Mich., 58880 (Mexico); Paraguay-Delgado, F. [Centro de Investigacion en Materiales Avanzados, S.C. CIMAV, Laboratorio Nacional de Nanotecnologia-Chihuahua, Miguel de Cervantes 120, Complejo Industrial Chihuahua, Chih., 31109 (Mexico); Albiter, M.A.; Lara-Romero, J. [Facultad de Ingenieria Quimica, Universidad Michoacana de San Nicolas de Hidalgo, Morelia Mich., 58000 (Mexico); Martinez-Sanchez, R. [Centro de Investigacion en Materiales Avanzados, S.C. CIMAV, Laboratorio Nacional de Nanotecnologia-Chihuahua, Miguel de Cervantes 120, Complejo Industrial Chihuahua, Chih., 31109 (Mexico)

    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.

  12. Synthesis and characterization of WO3 nanostructures prepared by an aged-hydrothermal method

    International Nuclear Information System (INIS)

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

    2009-01-01

    Nanostructures of tungsten trioxide (WO 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 BET ) were measured by using the BET method. The lengths of the WO 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.

  13. Tetrapropylammonium ion influence on the synthesis of Pt Ru/carbon hybrids by hydrothermal carbonization

    International Nuclear Information System (INIS)

    Tusi, M.M.; Polanco, N.S.O.; Brandalise, M.; Correa, O.V.; Silva, A.C.; Oliveira Neto, A.; Linardi, M.; Spinace, E.V.

    2010-01-01

    PtRu/Carbon hybrid materials were prepared by hydrothermal carbonization using starch as carbon source and reducing agent and H 2 PtCl 6 .6H 2 O e RuCl 3 .xH 2 O as metals source and catalyst of the carbonization process. The materials were prepared in the following conditions: without pH adjustment, in the absence and in the presence of tetrapropylammonium chloride (TPACl), and adjusting the pH using potassium hydroxide (KOH) or tetrapropylammonium hydroxide (TPAOH). The obtained materials were treated under argon atmosphere at 900 deg C and characterized by SEM/EDX, BET isotherm, XRD and TEM. The electro-oxidation of methanol was studied by chronoamperometry. The material prepared using TPAOH showed the best performance for methanol electro-oxidation. (author)

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

    Science.gov (United States)

    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.

  15. Hydrothermal synthesis and structure of a new layered zincophosphate intercalated with 3-Methylaminopropylamine cations

    Directory of Open Access Journals (Sweden)

    NEVENKA RAJIC

    2005-04-01

    Full Text Available A novel layered zincophosphate (ZnPO–MPA was prepared by hydrothermal crystallization using 3-methylaminopropylamine (MPA as a structure-directing agent. The structure consists of macroanion [Zn2P3O8(OH3]2- layers which are built up of 4-membered ring channels. The channels (of about 3.7 Å diameter arise through the connection of the neighbouring rings by two oxygen bridges. The negative charge of the layers is compensated by diprotonated MPA molecules which are stacked parallel to the ring channels. ZnPO–MPA is stable up to 300 °C. At higher temperatures MPA decomposition begins followed by a dehydration, which occurs through condensation of the framework hydroxyl groups. The activation energy of the MPA decomposition is high due to the fact that the layers and MPA cations are held together by strong hydrogen bonds.

  16. Red, green, and blue lanthanum phosphate phosphors obtained via surfactant-controlled hydrothermal synthesis

    International Nuclear Information System (INIS)

    Sousa Filho, Paulo C. de; Serra, Osvaldo A.

    2009-01-01

    A new solution route for the obtainment of highly pure luminescent rare-earth orthophosphates in hydrothermal conditions was developed. By starting from soluble precursors (lanthanide tripolyphosphato complexes, i.e. with P 3 O 10 5- as a complexing agent and as an orthophosphate source) and by applying surfactants in a water/toluene medium, the precipitations are confined to reverse micelle structures, thus yielding nanosized and homogeneous orthophosphates. The method was employed to obtain lanthanide-activated lanthanum phosphates, which can be applied as red (LaPO 4 :Eu 3+ ), green (LaPO 4 :Ce 3+ ,Tb 3+ ) and blue (LaPO 4 :Tm 3+ ) phosphors. The produced materials were analyzed by powder X-ray diffractometry, scanning electron microscopy, infrared spectroscopy and luminescence spectroscopy (emission, excitation, lifetimes and chromaticity coordinates).

  17. High-Yielding Green Hydrothermal Synthesis of Ruthenium Nanoparticles and Their Characterization.

    Science.gov (United States)

    Dikhtiarenko, Alla; Khainakov, Sergei A; Khaynakova, Olena; García, José R; Gimeno, José

    2016-06-01

    Using hydrothermal techniques, a novel synthetic approach to prepare ruthenium nanoparticles has been developed. At 180 degrees C and under autogenous pressure, starting from an aqueous solution of ruthenium trichloride, the method yielded nanoparticles whose form and size both depended on the reducing agent: sodium citrate (hexagonal shaped nanocrystals, 1-20 nm), ascorbic acid (spherical nanoparticles, 3-5 nm) and succinic acid (spherical nanoparticles, 1-120 nm). Depending on the reaction variables, the nature and concentration of partially reduced species determines the characteristics of the final products. HRTEM image analysis along with the simulation techniques were stabilized preferential growth of nanoparticles on specific directions. Ruthenium samples have been investigated by Temperature-Programmed Reduction (TPR) showing that the reduction temperature of nanoparticles is correlated to their nanocrystalline size.

  18. Hydrothermal synthesis of Ca3Bi8O15 rods and their visible light photocatalytic properties

    International Nuclear Information System (INIS)

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

    2014-01-01

    Graphical abstract: The novel Ca 3 Bi 8 O 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 3 Bi 8 O 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 3 Bi 8 O 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 3 Bi 8 O 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 2 · − and ·OH

  19. Hydrothermal synthesis of hexagonal CeO{sub 2} nanosheets and their room temperature ferromagnetism

    Energy Technology Data Exchange (ETDEWEB)

    Meng, Fanming, E-mail: mrmeng@ahu.edu.cn [School of Physics and Materials Science, Anhui University, Hefei 230601 (China); Key Laboratory of Materials Modification by Laser, Ion and Electron Beams, Dalian University of Technology, Ministry of Education, Dalian 116024 (China); Zhang, Cheng; Fan, Zhenghua; Gong, Jinfeng; Li, Aixia; Ding, Zongling; Tang, Huaibao; Zhang, Miao; Wu, Guifang [School of Physics and Materials Science, Anhui University, Hefei 230601 (China)

    2015-10-25

    Hexagonal CeO{sub 2} nanosheets of 40–50 nm in thickness and 300–400 nm in side-length have been successfully synthesized via controlling the morphology of CeCO{sub 3}OH precursors by a facile hydrothermal technique using CeCl{sub 3}·7H{sub 2}O as cerium source, ammonium hydrogen carbonate as precipitants, and ethylenediamine as complexant. The reaction time and the amount of CeCl{sub 3}·7H{sub 2}O and ethylenediamine were systematically investigated. The as-synthesized hexagonal CeO{sub 2} nanosheets were examined by XRD, SEM, TEM, XPS, Raman scattering and magnetization measurements. It is found that the amount of CeCl{sub 3}·7H{sub 2}O and ethylenediamine are key parameters for controlling the final morphology. The hexagonal CeO{sub 2} nanosheets have a fluorite cubic structure and there are Ce{sup 3+} ions and oxygen vacancies in surface of samples. The synthesized CeO{sub 2} shows excellent room temperature optical properties. M–H curve exhibits excellent room-temperature ferromagnetism (RTFM) with saturation magnetization (M{sub s}) of 3.02 × 10{sup −2} emu/g, residual magnetization (M{sub r}) of 0.68 × 10{sup −2} emu/g and coercivity (H{sub c}) of 210 Oe, which is likely attributed to the effects of the Ce{sup 3+} ions and oxygen vacancies. - Highlights: • Hexagonal CeO{sub 2} nanosheets with superexerllent RTFM are synthesized by a facile hydrothermal method. • RTFM mechanism of CeO{sub 2} nanosheets can be attributed to the influences of oxygen vacancies and Ce{sup 3+} ions. • A defect driven dissolution–recrystallization mechanism is suggested to explain the transformation from nanowires to nanosheets.

  20. Hydrothermal synthesis of YBO3:Tb3+ microflowers and their luminescence properties

    International Nuclear Information System (INIS)

    Yang Lan; Zhou Liqun; Chen Xiange; Liu Xiaolan; Hua Pei; Shi Yan; Yue Xiaoguang; Tang Ziwei; Huang Ying

    2011-01-01

    Research highlights: → We report an efficient surfactant-free hydrothermal approach to synthesize hexagonal YBO 3 :Tb 3+ with novel self-assembled 3D architectures. The as-obtained samples present flowerlike agglomerates composed of nanoflakes with thickness of 20 nm and high crystallinity in 180 o C. The reaction mechanism has been considered as a dissolution/precipitation mechanism; the self-assembly evolution process has been proposed on homocentric layer-by-layer growth style. The luminescent properties of the flowerlike YBO 3 :Tb 3+ composed of nanoflakes have also been reported and investigated. - Abstract: Three-dimensional flowerlike YBO 3 :Tb 3+ phosphors have been successfully prepared by an efficient surfactant-free hydrothermal process directly without further sintering treatment. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray (EDS) spectrometry, selected area electron diffraction (SAED), photoluminescence (PL) spectra were used to characterize the samples. The as-obtained samples present flowerlike agglomerates composed of nanoflakes with thickness of 20 nm and high crystallinity in spite of the moderate reaction temperature of 180 o C. The reaction mechanism has been considered as a dissolution/precipitation mechanism; the self-assembly evolution process has been proposed on homocentric layer-by-layer growth style. The different luminescent intensity with different molar ratio of Y-Tb [Y:Tb = 8:2; 7:3; 6:4; 5:5; 4:6], YBO 3 :Tb 3+ phosphors exhibit different light (white, red, green) under ultraviolet excitation, which might find potential applications in the fields such as light display systems and optoelectronic devices.

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

    Czech Academy of Sciences Publication Activity Database

    Pashková, Veronika; Sklenák, Štěpán; Klein, Petr; Urbanová, Martina; Dědeček, Jiří

    2016-01-01

    Roč. 22, č. 12 (2016), s. 3937-3941 ISSN 1521-3765 R&D Projects: GA ČR GA15-13876S Institutional support: RVO:61388955 Keywords : ZSM-5 * synthesis * zeolites Subject RIV: CF - Physical ; Theoretical Chemistry

  2. Incorporation of Al at ZSM-5 hydrothermal synthesis. Tuning of Al pairs in the framework

    Czech Academy of Sciences Publication Activity Database

    Pashková, Veronika; Klein, Petr; Dědeček, Jiří; Tokarová, V.; Wichterlová, Blanka

    2015-01-01

    Roč. 202, JAN 2015 (2015), s. 138-146 ISSN 1387-1811 R&D Projects: GA ČR GAP106/11/0624 EU Projects: European Commission(XE) 229183 Institutional support: RVO:61388955 Keywords : ZSM-5 * zeolite synthesis * Al distribution Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 3.349, year: 2015

  3. Hydrothermal synthesis of size-controllable Yttrium Orthovanadate (YVO4) nanoparticles and its application in photocatalytic degradation of direct blue dye

    International Nuclear Information System (INIS)

    Mohamed, R.M.; Harraz, F.A.; Mkhalid, I.A.

    2012-01-01

    Graphical abstract: XRD patterns of YVO 4 nanopowders prepared at different hydrothermal times; where Y 1 = 4 h, Y 2 = 8 h, Y 3 = 12 h and Y 4 = 24 h. Highlights: ► Size control of Yttrium Orthovanadate. ► Hydrothermal synthesis. ► Removal of direct blue dye. - Abstract: Sized-controlled YVO 4 nanoparticles have been synthesized by a simple hydrothermal method by changing hydrothermal time from 4 to 24 h. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), specific surface area (Brunauer–Emmett–Teller (BET)), and ultraviolet–visible spectroscopy (UV–vis) measurements. The results showed that the size of as-synthesized YVO 4 nanoparticles was in the range of 11–40 nm and was extremely dependent on the hydrothermal time. Photocatalytic measurement showed that the YVO 4 nanoparticles with particle size of about 11 nm (prepared by 4 h hydrothermal time) possess superior photocatalytic properties in the decolorization of direct blue dye. Due to simple preparation, high photocatalytic oxidation of direct blue dye and low cost, the YVO 4 photocatalyst is a potential candidate for pollutants removal and will find wide application in the coming future in photocatalytic oxidation processes. The overall kinetics of photodegradation of direct blue dye using YVO 4 nanopowders photocatalyst was found to be of first order. The photocatalyst could be easily removed from the reaction mixture and its recyclability with no loss of activity was possible for six times. The catalytic performance was found to decrease by 5% after run number six.

  4. One-Step Hydrothermal Synthesis of Small TiO₂ Porous Nanoparticles for Efficient Degradation of Organic Dyes.

    Science.gov (United States)

    Zhang, Jing; Wang, Donghai; Zhang, Haijiao

    2018-05-01

    In the work, small TiO2 porous nanoparticles with an average size of 60 nm have been prepared by a simple, eco-friendly, and one-step hydrothermal method. The TiO2 products are achieved by only using tetrabutyl titanate (TBOT), tetrapropylammonium hydroxide (TPAOH), and water as the starting materials. Various techniques such as SEM, TEM, HRTEM, XRD, Raman, and BET are used to characterize the surface morphology and structural features of products. The growth parameters including reaction time, titanium source and temperature of thermal treatment are systematically investigated. In the synthesis, TPAOH plays a decisive role as structure-directing agent for the formation of desirable TiO2 nanostructure. The photocatalytic tests manifest that the TiO2 nanoparticles annealed at 450 °C shows an outstanding photocatalytic activity for degradation of methyl orange (MO) and rhodamine B (RhB), which is comparable to Degussa P25. The superior performance may mainly come from the contributions of their small particle size and unique nanostructure.

  5. Experimental design for determination of effective parameters in hydrothermal synthesis of TiO{sub 2}-derived nanotubes

    Energy Technology Data Exchange (ETDEWEB)

    Safaei, M.; Sarraf-Mamoory, R. [Materials Engineering Department, Tarbiat Modares University, Tehran (Iran, Islamic Republic of); Rashidzadeh, M. [Catalysis Research Center, Research Institute of Petroleum Industry, Tehran (Iran, Islamic Republic of); Manteghian, M. [Chemical Engineering Department, Tarbiat Modares University, Tehran (Iran, Islamic Republic of)

    2010-11-15

    In this paper, a screening approach, involving the use of Plackett-Burman experimental design, permitted the evaluation of the effects of 8 parameters from hydrothermal synthesis of TiO{sub 2} derived nanotubes such as raw materials surface area, m{sub TiO2}, filling factor, temperature, time, aging, stirring, and HCl concentration on the surface area of products. The study highlights the role of filling factor, stirring, temperature, raw materials, and time conditions on surface area of responses. TEM micrographs showed that the morphologies for high, medium, and low surface areas of products are nanotubes, nanowires, and nanospheres, respectively. The N{sub 2} adsorption-desorption isotherms and pore size distributions showed that with decreasing surface area, the area of the hysteresis loops and gas volumes of N{sub 2} adsorbed are decreased. Also, the hysteresis loops shift to the region of higher relative pressure. Therefore, An increase in average pore size and a decrease in pore volume reduced surface area of product (copyright 2010 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  6. Microwave assisted hydrothermal synthesis of Ag/AgCl/WO3 photocatalyst and its photocatalytic activity under simulated solar light

    International Nuclear Information System (INIS)

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

    2013-01-01

    Simulated solar light responsive Ag/AgCl/WO 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 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: ► Successful synthesis of Ag/AgCl/WO 3 nanocomposite. ► Photocatalytic experiment was performed under simulated solar light. ► Nanocomposite photocatalyst was very active as compared to WO 3 commercial powder. ► SPR effect due to Ag nanoparticles enhanced the photocatalytic activity.

  7. Hydrothermal synthesis of one-dimensional tungsten oxide nanostructures using cobalt ammonium sulfate as a structure-directing agent

    International Nuclear Information System (INIS)

    Rajagopal, Shanmugasundaram; Lee, Hae-Min; Kim, Chang-Koo; Lee, Kangtaek

    2013-01-01

    Hydrothermal synthesis of one-dimensional tungsten oxide nanostructures was performed using cobalt ammonium sulfate as a structure-directing agent, and the effect of the concentration of cobalt ammonium sulfate on the characteristics of the tungsten oxide nanostructures was investigated. XRD measurements showed that hexagonal tungsten oxide (h-WO 3 ) structures were obtained at a higher concentration of cobalt ammonium sulfate (0.2 M), while cubic tungsten oxide (c-WO 3 ) structures were obtained at a lower concentration of cobalt ammonium sulfate (0.01M). Mixed structures of h-WO 3 and c-WO 3 were observed at an intermediate concentration of cobalt ammonium sulfate. Morphological studies revealed that h-WO 3 appeared as nanowires with a diameter of about 40 nm and an average length of 1 µm. c-WO 3 was shaped in pillar-like nanorods with a diameter of about 30 nm. A red-shift in the UV/Vis absorption peak was observed with different phases of tungsten oxide nanostructures

  8. Synthesis and Characterization of Si Oxide Coated Nano Ceria by Hydrolysis, and Hydrothermal Treatment at Low Temperature

    Directory of Open Access Journals (Sweden)

    Kong M.

    2017-06-01

    Full Text Available The purpose of this work was to the application of Si oxide coatings. This study deals with the preparation of ceria (CeO2 nanoparticles coating with SiO2 by water glass and hydrolysis reaction. First, the low temperature hydro-reactions were carried out at 30~100°C. Second, Silicon oxide-coated Nano compounds were obtained by the catalyzing synthesis. CeO2 Nano-powders have been successfully synthesized by means of the hydrothermal method, in a low temperature range of 100~200°C. In order to investigate the structure and morphology of the Nano-powders, scanning electron microscopy (SEM and X-ray diffraction (XRD were employed. The XRD results revealed the amorphous nature of silica nanoparticles. To analyze the quantity and properties of the compounds coated with Si oxide, transmission electron microscopy (TEM in conjunction with electron dispersive spectroscopy was used. Finally, it is suggested that the simple growth process is more favorable mechanism than the solution/aggregation process.

  9. Facile Hydrothermal Synthesis and Enhanced Methane Sensing Properties of Pt-Decorated ZnO Nanosheets.

    Science.gov (United States)

    Zhou, Qu; Hong, Changxiang; Li, Zhiguang; Peng, Shudi; Wu, Gaolin; Wang, Qian; Zhang, Qingyan; Xu, Lingna

    2018-05-01

    Pure and Pt-decorated ZnO nanosheets were synthesized via a facile and environment-friendly hydrothermal process, and characterized by X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FESEM) and energy dispersive X-ray spectroscopy (EDS), respectively. Side-heated chemical gas sensors were fabricated with the synthesized ZnO based powders and their sensing properties to methane CH4, an important characteristic hydrocarbon contaminant extracted from power transformer oil with overheating or discharging fault, were systemically investigated. Interestingly, Pt decoration not only obviously increased the gas response of sensor fabricated with the synthesized ZnO nanosheets to CH4, but also effectively reduced its optimum operating temperature. Its highest response to 50 ppm of CH4 was about 63.45 at 240 °C, which was about two times larger when compared with the pure one. Meanwhile, the Pt-decorated ZnO nanosheets sensor exhibited shorter response-recovery characteristic, good linearity in low concentration range and excellent stability towards CH4. Those superior sensing features indicate the synthesized Pt-decorated ZnO nanosheets is a promising candidate for fabricating high-performance CH4 sensor.

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

    Science.gov (United States)

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

    2017-08-01

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

  11. Hydrothermal synthesis, structural and thermal characterizations of three open-framework gallium phosphites

    Science.gov (United States)

    Hamchaoui, Farida; Alonzo, Véronique; Marlart, Isabelle; Auguste, Sandy; Galven, Cyrille; Rebbah, Houria; Le Fur, Eric

    2017-11-01

    Three new gallium phosphites A[Ga(HPO3)2], where A = K (1), NH4 (2), Rb (3), have been synthesized by using mild hydrothermal conditions under autogeneous pressure. Their structures have been determined by single-crystal X-ray diffraction. These compounds crystallize in the hexagonal P63mc space group with a = 5.2567 (2) Å and c = 12.2582 (3) Å for 1, a = 5.2576 (2) Å and c = 12.9113 (4) Å for 2, a = 5.27020 (10) Å and c = 12.7619 (5) Å for 3, with Z = 2 in the three phases. The three compounds are isostructural and exhibit the same framework topology, consisting of a layered structure stacked along the c-axis with the A+ cations located in the interlayer spaces. The [Ga(HPO3)2]- sheets contain GaO6 octahedra interconnected by phosphite units through sharing vertices. Thermal analysis under air atmosphere shows a large range stability for alkali cations containing compounds with decomposition starting around 750 K leading to phosphate phases. Under nitrogen, a disproportionation of the phosphite into red phosphorus and phosphates is expected, accompanied by a release of H2.

  12. Synthesis and Photocatalytic Activity of Iron Doped CdS by Hydrothermal Method

    Directory of Open Access Journals (Sweden)

    LIU Yang-long

    2017-10-01

    Full Text Available Fe-doped cadmium sulfide was prepared by hydrothermal method in aqueous solution using cadmium nitrate, ferric nitrate and thiourea as raw materials. The samples were characterized by SEM, XRD, EDS and XPS. The photocatalytic degradation of methylene blue (MB in aqueous solution was used as a target reaction to evaluate their photocatalytic activity. The experimental results show that the reaction temperature has a great effect on the morphology of cadmium sulfide, and spherical, flowerlike, clustered and rodlike cadmium sulfide are obtained in various reaction temperatures. Among them, the photocatalytic activity of flowerlike CdS is observed to be better than other CdS materials. The XRD indicates that Fe-doped cadmium sulfide is hexagonal crystal structure when the reaction temperature is 160℃. The experimental results also indicate that Fe-doped can obviously improve the photocatalytic activity of cadmium sulfide and when the doping ratio of Fe to Cd is 1:10, the photocatalytic effect is the best of all.

  13. Hydrothermal synthesis of 2D MoS 2 nanosheets for electrocatalytic hydrogen evolution reaction

    KAUST Repository

    Muralikrishna, S.

    2015-10-20

    Nanostructured molybdenum disulfide (MoS) is a very promising catalyst for producing molecular hydrogen by electrochemical methods. Herein, we have designed and synthesized highly electocatalytically active 2D MoS nanosheets (NS) from molybdenum trioxide (MoO) by a facile hydrothermal method and have compared their electrocatalytic activities for hydrogen evolution reaction (HER). The electrochemical characterization was performed using linear sweep voltammetry (LSV) in acidic medium. The MoS NS show a HER onset potential at about 80 mV vs. reversible hydrogen electrode (RHE) which is much lower than MoO (300 mV). The MoS NS and MoO show a current density of 25 mA cm and 0.3 mA cm, respectively at an overpotential of 280 mV vs. RHE. The MoS NS showed an 83 times higher current density when compared to MoO. The Tafel slopes of the MoS NS and MoO were about 90 mV per dec and 110 mV per dec respectively. This suggests that MoS NS are a better electrocatalyst when compared to MoO and follow the Volmer-Heyrovsky mechanism for HER.

  14. Optical and Magnetic Properties of Fe Doped ZnO Nanoparticles Obtained by Hydrothermal Synthesis

    Directory of Open Access Journals (Sweden)

    Xiaojuan Wu

    2014-01-01

    Full Text Available Diluted magnetic semiconductors Zn1-xFexO nanoparticles with different doping concentration (x=0, 0.01, 0.05, 0.10, and 0.20 were successfully synthesized by hydrothermal method. The crystal structure, morphology, and optical and magnetic properties of the samples were characterized by X-ray diffraction (XRD, energy dispersive spectrometer (EDS, high-resolution transmission electron microscopy (HRTEM, Raman scattering spectra (Raman, photoluminescence spectra (PL, and the vibrating sample magnetometer (VSM. The experiment results show that all samples synthesized by this method possess hexagonal wurtzite crystal structure with good crystallization, no other impurity phases are observed, and the morphology of the sample shows the presence of ellipsoidal nanoparticles. All the Fe3+ successfully substituted for the lattice site of Zn2+ and generates single-phase Zn1-xFexO. Raman spectra shows that the peak shifts to higher frequency. PL spectra exhibit a slight blue shift and the UV emission is annihilated with the increase of Fe3+ concentration. Magnetic measurements indicated that Fe-doped ZnO samples exhibit ferromagnetic behavior at room temperature and the saturation magnetization is enhanced with the increase of iron doping content.

  15. Hydrothermal synthesis and optical properties of hexagonal tungsten oxide nanocrystals assisted by ammonium tartrate

    Energy Technology Data Exchange (ETDEWEB)

    Pang, Hua-Feng; Li, Zhi-Jie [Department of Applied Physics, University of Electronic Science and Technology of China, Chengdu (China); Xiang, Xia; Zu, Xiao-Tao [Department of Applied Physics, University of Electronic Science and Technology of China, Chengdu (China); International Center for Material Physics, Chinese Academy of Sciences, Shenyang (China); Fu, Yong-Qing [Thin Film Center, Scottish Universities of Physics Alliance (SUPA), University of the West of Scotland, Paisley (United Kingdom)

    2012-03-15

    Crystals of hexagonal tungsten oxides (hex-WO{sub 3}) have been synthesized using hydrothermal method at 150 C, assisted by the capping reagent of ammonium tartrate (AT). The XRD and EDX results reveal that the lattice distortion exists in all the samples, possibly due to the defects and the intercalation of the residual sodium ions. Different crystal shapes including plate-like, urchin-like, and particle structures were obtained by varying concentration of AT and pH values in the precursor solution. Beside the absorption action of the NH{sub 4}{sup +} and Na{sup +} ions, the capping effect can be reinforced by the hydrogen bonding from the tartrate groups in the crystallization process. The bandgap energies were modulated by the size of the nanostructured hex-WO{sub 3} crystals due to quantum confinement effect, which increases from 2.74 to 3.04 eV. Based on the analysis of the photoluminescence and X-ray photoelectron spectroscopy, the enhancement of the blue emission of the nanocrystals is assigned as a result of a complex of the local intercalation of the residual sodium ions and the oxygen vacancies or defects. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  16. Hydrothermal Synthesis of Nitrogen-Doped Titanium Dioxide and Evaluation of Its Visible Light Photocatalytic Activity

    Directory of Open Access Journals (Sweden)

    Junjie Qian

    2012-01-01

    Full Text Available Nitrogen-doped titanium dioxide (N-doped TiO2 photocatalyst was synthesized from nanotube titanic acid (denoted as NTA; molecular formula H2Ti2O5·H2O precursor via a hydrothermal route in ammonia solution. As-synthesized N-doped TiO2 catalysts were characterized by means of X-ray diffraction, transmission electron microscopy, diffuse reflectance spectrometry, X-ray photoelectron spectroscopy, electron spin resonance spectrometry and Fourier transform infrared spectrometry. It was found that nanotube ammonium titanate (NAT was produced as an intermediate during the preparation of N-doped TiO2 from NTA, as evidenced by the N1s X-ray photoelectron spectroscopic peak of NH4 + at 401.7 eV. The catalyst showed much higher activities to the degradation of methylene blue and p-chlorophenol under visible light irradiation than Degussa P25. This could be attributed to the enhanced absorption of N-doped TiO2 in visible light region associated with the formation of single-electron-trapped oxygen vacancies and the inhibition of recombination of photo-generated electron-hole pair by doped nitrogen.

  17. Hydrothermal synthesis of hydrated vanadium oxide nanobelts using poly (ethylene oxide) as a template

    Energy Technology Data Exchange (ETDEWEB)

    Subba Reddy, Ch.V.; Mho, Sun-il [Division of Energy Systems Research, Ajou University, Suwon 443-749 (Korea); Kalluru, Rajamohan R.; Williams, Quinton L. [Department of Physics, Atmospheric Sciences and Geosciences, 1400, J R Lynch Street, Jackson State University, Jackson, MS 39217-17660 (United States)

    2008-05-01

    With the aim of obtaining nanodevices as batteries, sensors and fuel cells, we prepared V{sub 2}O{sub 5} and V{sub 3}O{sub 7}.H{sub 2}O nanobelts by a simple hydrothermal process using poly (ethylene oxide) (PEO) as a template. The yielding percentage of the nanomaterial is less in polymer-free V{sub 2}O{sub 5} nanobelts and material size is also big. It is apparent that PEO used V{sub 3}O{sub 7}.H{sub 2}O form a continuous and relatively homogeneous matrix with a clearly 1-5 {mu}m long and 50-150 nm diameter nanobelts morphology. The SEM micrographs suggest that there is no bulk deposition of polymer on the surface of the nano-crystallites. Strong interaction between the vanadyl group and the polymer during the formation process has been identified by the shifts of the vanadyl vibration peaks. The CV curve of the electrode made of the V{sub 3}O{sub 7}.H{sub 2}O nanobelts have higher current densities than the CV curve of the electrode made of V{sub 2}O{sub 5} nanobelts. (author)

  18. Hydrothermal synthesis and crystal structure of a new lanthanum(III coordination polymer with fumaric acid

    Directory of Open Access Journals (Sweden)

    Hayet Anana

    2015-05-01

    Full Text Available The title compound, poly[diaquatris(μ4-but-2-enedioato(μ2-but-2-enedioic aciddilanthanum(III], [La2(C4H2O43(C4H4O4(H2O2]n, was synthesized by the reaction of lanthanum chloride pentahydrate with fumaric acid under hydrothermal conditions. The asymmetric unit comprises an LaIII cation, one and a half fumarate dianions (L2−, one a half-molecule of fumaric acid (H2L and one coordinated water molecule. Each LaIII cation has the same nine-coordinate environment and is surrounded by eight O atoms from seven distinct fumarate moieties, including one protonated fumarate unit and one water molecule in a distorted tricapped trigonal–prismatic environment. The LaO8(H2O polyhedra centres are edge-shared through three carboxylate bridges of the fumarate ligand, forming chains in three dimensions to construct the MOF. The crystal structure is stabilized by O—H...O hydrogen-bond interactions between the coordinated water molecule and the carboxylate O atoms, and also between oxygen atoms of fumaric acid

  19. Hydrothermal Synthesis and Hydrogen Sensing Properties of Nanostructured SnO2 with Different Morphologies

    Directory of Open Access Journals (Sweden)

    Weigen Chen

    2014-01-01

    Full Text Available In this work, nanoscale SnO2 with various geometrical morphologies, including pine needle-like, sphere-like, sheet-like, grape-like nanostructures, was prepared via a facile hydrothermal process. Microstructures and morphologies of all the as-synthesized products were characterized by X-ray diffraction (XRD and field emission scanning electron microscopy (FESEM. Meanwhile, the specific surface areas of the as-prepared SnO2 nanostructures were determined by Brunauer-Emmett-Teller (BET analysis. Gas sensors were fabricated and their gas sensing properties towards hydrogen were systematically investigated. The results indicate pine needle-like SnO2 structure exhibits exclusive better gas sensing performances to hydrogen than the other morphologies, which can be attributed to its novel shape with a large specific surface area. Such an unexpected morphology is a promising candidate for the use of SnO2 as a gas sensing material in future hydrogen sensor applications.

  20. Rapid microwave hydrothermal synthesis of GaOOH nanorods with photocatalytic activity toward aromatic compounds

    International Nuclear Information System (INIS)

    Sun Meng; Li Danzhen; Zhang Wenjuan; Fu Xianzhi; Shao Yu; Li Wenjuan; Xiao Guangcan; He Yunhui

    2010-01-01

    GaOOH nanorods were synthesized from Ga(NO 3 ) 3 via a facile microwave hydrothermal method. The obtained sample was characterized by x-ray diffraction, N 2 sorption-desorption, UV-vis diffuse reflectance spectroscopy, transmission electron microscopy, electron spin resonance, and x-ray photoelectron spectroscopy. The results revealed that the as-synthesized sample was consisted of rod-like particles. It possessed a surface area of 14.3 m 2 g -1 , and a band gap of 4.75 eV. The photocatalytic property of GaOOH nanorods was evaluated by the degradation of aromatic compounds (such as benzene and toluene) in an O 2 gas stream under ultraviolet (UV) light illumination. The results demonstrated that GaOOH nanorods exhibited superior photocatalytic activity and stability as compared to commercial TiO 2 (P25, Degussa Co.) in both benzene and toluene degradation. In the extended (35 h) reaction test toward benzene, GaOOH maintained a high activity, and no obvious deactivation was observed. A possible mechanism of the photocatalysis over GaOOH is proposed.

  1. Hydrothermal Synthesis of Zeolitic Imidazolate Frameworks-8 (ZIF-8) Crystals with Controllable Size and Morphology

    KAUST Repository

    Lestari, Gabriella

    2012-05-01

    Zeolitic imidazolate frameworks (ZIFs) is a new class of metal-organic frameworks (MOFs) with zeolite-like properties such as permanent porosity, uniform pore size, and exceptional thermal and chemical stability. Until recently, ZIF materials have been mostly synthesized by solvothermal method. In this thesis, further analysis to tune the size and morphology of ZIF-8 is done upon our group’s recent success in preparing ZIF-8 crystals in pure aqueous solutions. Compositional parameters (molar ratio of 2-methylimidazole/Zn2+, type of zinc salt reagents, reagent concentrations, addition of surfactants) as well as process parameters (temperature and time) were systematically investigated. Upon characterizations of as-synthesized samples by X-ray powder diffraction, thermal gravimetric analysis, N2 adsorption, and field-emission scanning electron microscope, the results show that the particle size and morphology of ZIF-8 crystals are extremely sensitive to the compotional parameters of reagent concentration and addition of surfactants. The particle size and morphology of hydrothermally synthesized ZIF-8 crystals can be finely tuned; with the size ranging from 90 nm to 4 μm and the shape from truncated cubic to rhombic dodecahedron.

  2. Hydrothermal Synthesis and Tunable Multicolor Upconversion Emission of Cubic Phase Y2O3 Nanoparticles

    Directory of Open Access Journals (Sweden)

    Haibo Wang

    2013-01-01

    Full Text Available Highly crystalline body-centered cubic structure Y2O3 with lanthanide (Ln codopants (Ln = Yb3+/Er3+ and Yb3+/Ho3+ has been synthesized via a moderate hydrothermal method in combination with a subsequent calcination. The structure and morphology of Y(OH3 precursors and Y2O3 nanoparticles were characterized by X-ray diffraction and transmission electron microscopy. The results reveal that the Y2O3 nanoparticles possess cubic phase and form the quasispherical structure. The upconversion luminescence properties of Y2O3 nanoparticles doped with different Ln3+ (Yb3+/ Er3+ and Yb3+/ Ho3+ ions were well investigated under the 980 nm excitation. The results show that the Yb3+/Er3+ and Yb3+/Ho3+ codoped Y2O3 nanoparticles exhibit strong red and light yellow upconversion emissions, respectively. It is expected that these Y2O3 nanoparticles with tunable multicolor output and intense red upconversion emission may have potential application in color displays and biolabels.

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

    Science.gov (United States)

    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.

  4. Hydrothermal synthesis, structure, and catalytic properties of UO2Sb2O4

    International Nuclear Information System (INIS)

    Sykora, Richard E.; King, Joseph E.; Illies, Andreas J.; Albrecht-Schmitt, Thomas E.

    2004-01-01

    A new uranyl antimonite, UO 2 Sb 2 O 4 (1), has been prepared from the hydrothermal reaction of UO 3 with Sb 2 O 3 and KCl. The structure of 1 consists of neutral two-dimensional ∞ 2 [UO 2 Sb 2 O 4 ] layers. The U(VI) centers are ligated by two trans oxo ligands and four square pyramidal antimonite anions. In addition, the U(VI) also forms long contacts with two additional oxygen atoms that are distorted by 12.7(2) degree sign out of the equatorial plane perpendicular to the uranyl unit. These long interactions are significant owing to evidence supplied by bond valence sum calculations. The two-dimensional layers found in 1 are built from one-dimensional chains formed from edge-sharing UO 6 octahedra that run along the b-axis, and are linked together by [Sb 2 O 4 ] 2- chains. A flow microreactor system has been used to study the catalytic activity of 1, and these results show that it can be used as a catalyst in the conversion of propene and O 2 to acrolein. Crystallographic data: 1, monoclinic, space group C2/m, a=13.490(2) A, b=4.0034(6) A, c=5.1419(8) A, β=104.165(3) deg., Z=2, MoKα, λ=0.71073, R(F)=1.74% for 30 parameters with 365 reflections with I>2σ(I)

  5. Synthesis of nanoparticles of barium strontium titanate using hydrothermal microwave method

    International Nuclear Information System (INIS)

    Silva, R.A.; Souza, A.E.; Teixeira, S.R.; Moreira, M.L.; Volanti, D.P.; Longo, E.

    2009-01-01

    Nanoparticles of barium strontium titanate Ba x Sr 1 - x TiO 3 (BST) had been prepared, with x = 0.5, using the hydrothermal method attended by microwaves (HTMW). A solution was prepared using deionized water, barium chloride (BaCl 2 .2H 2 O), strontium chloride (SrCl 2 .6H 2 O), titanium (IV) isopropoxide (C 12 H28O 4 Ti) and potassium hydroxide (KOH). Afterward the solution was heated to 140 deg C in a microwave oven, at a heating rate of 140 deg C/min, and maintained at this temperature for 40 min, under a pressure of 3 to 4 bar. X-ray diffraction (DRX) and field emission scanning electron microscopy (FE-SEM) had been used in the particles characterization. DRX was used to identify the crystallized phases and the images taken from (FE-SEM) show that the material has a wide particle-size distribution with most of them between 10 and 30 nm. (author)

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

    Science.gov (United States)

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

    2015-03-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Min; Li, Wenjuan, E-mail: liwenjuan2801@163.com; Du, Yong; Kong, Defen; Wang, Ze; Meng, Yi; Sun, Xiaolan; Yan, Tingjiang; Kong, Desheng; You, Jinmao [Qufu Normal University, Shandong Province Key Laboratory of Life-Organic Analysis (China)

    2016-11-15

    Bismuth ferrite, Fenton-like catalysts have been successfully synthesized via simple hydrothermal methods without any templates. Through changing the molar ratio of Bi/Fe, the two main phases BiFeO{sub 3} and Bi{sub 25}FeO{sub 40} can be synthesized under different temperatures. Furthermore, different morphologies of the BiFeO{sub 3} phase can be adjusted by changing different concentrations of HNO{sub 3} and NaOH which were used to dissolve the reactants and adjust the pH values in the prepared process. When the concentration of HNO{sub 3}/NaOH was 8/12 M, some uniform cylindrical bodies with equal height (1 μm) and width (0.6 μm) were obtained, which have not been reported before. The uniform structures exhibited better activities in the photoassisted Fenton-like oxidation process for the degradation of rhodamine B (RhB) under visible light irradiation (420 nm < λ < 800 nm). Through the detection of the degradation mechanism, it showed that the concerted effect of the catalysts and H{sub 2}O{sub 2} can increase the generation of the charge carriers and accelerate the photogenerated charge transfer between the catalysts and dyes. The BiFeO{sub 3} samples also showed magnetic properties at room temperature, which may have potential applications in multiferroic or magnetoelectric sensors and devices.

  8. Synthesis and growth mechanism of sponge-like nickel using a hydrothermal method

    Science.gov (United States)

    Shao, Bin; Yin, Xueguo; Hua, Weidong; Ma, Yilong; Sun, Jianchun; Li, Chunhong; Chen, Dengming; Guo, Donglin; Li, Kejian

    2018-05-01

    Sponge-like nickel composed of micro-chains with a diameter of 1-5 μm was selectively synthesized by the hydrothermal method, using sodium hydroxide (NaOH) as the alkaline reagent, aqueous hydrazine as reducing agent and citric acid as a coordination agent. The time-dependent samples prepared at different NaOH concentrations were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and Fourier transform infrared spectrometer (FTIR). The results showed that the agglomerates of nickel citrate hydrazine complex nanoplates were first precipitated and then reduced to prickly nickel micro-chains at a lower NaOH concentration, which played a role in the further formation of sponge-like nickel. Also, the probable growth mechanism of the sponge-like nickel was proposed. The magnetic properties of sponge-like nickel were studied using a vibrating sample magnetometer. The sponge-like nickel exhibited a ferromagnetic behavior with a saturation magnetization value of 43.8 emu g-1 and a coercivity value of 120.7 Oe.

  9. Controlled Hydrothermal Synthesis, Optical and Magnetic Properties of Monodisperse Leaf-Like CeO₂ Nanosheets.

    Science.gov (United States)

    Niu, Xiaofei; Zhang, Xiuxiang; Liu, Yan

    2018-04-01

    The monodisperse leaf-like CeO2 nanosheets of about 40 nm in thickness have been successfully synthesized by a simple hydrothermal route. SEM, XRD, FT-IR, TG-DSC, XPS, Raman scattering, Photoluminescence (PL) spectra and M-H curves were employed to characterize the samples. The results showed that all the CeO2 samples had a cubic fluorite structure and there are Ce3+ ions and oxygen vacancies in the surface of samples. Based on the SEM patterns, a clear morphology transformation from leaf-like to heart-shaped, and then to triangular prism-like structure was observed. The magnetic and photoluminescence measurements displayed that all the samples have excellent ferromagnetism and optical properties at room temperature and the ferromagnetism and optical properties increase along with the rise of NH4HCO3 concentration, which can be reasonably explained for the affects of the morphology of samples, the concentration of oxygen vacancies and Ce3+ ions.

  10. Facile hydrothermal synthesis of mesoporous In2O3 nanoparticles with superior formaldehyde-sensing properties

    Science.gov (United States)

    Zhang, Su; Song, Peng; Yang, Zhongxi; Wang, Qi

    2018-03-01

    Mesoporous In2O3 nanoparticles were successfully synthesized via a facile, template free, and low-cost hydrothermal method. Their morphology and structure were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), differential thermal and thermogravimetry analysis (DSC-TG), and N2 adsorption-desorption analyses. The results reveal that mesoporous In2O3 nanoparticles with a size range of 40-60 nm, possess plenty of pores, and average pore size is about 5 nm. Importantly, the mesoporous structure, large specific surface area, and small size endow the mesoporous In2O3 nanoparticles with highly sensing performance for formaldehyde detection. The response value to 10 ppm HCHO is 20 at an operating temperature of 280 °C, and the response and recovery time are 4 and 8 s, respectively. It is expected that the mesoporous In2O3 nanoparticles with large specific surface area and excellent sensing properties will become a promising functional material in monitoring and detecting formaldehyde.

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

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

    Science.gov (United States)

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

    2015-01-01

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

  13. Hydrothermal synthesis and characterization of hydroxyapatite and fluorhydroxyapatite nano-size powders

    International Nuclear Information System (INIS)

    Montazeri, Leila; Javadpour, Jafar; Shokrgozar, Mohammad Ali; Bonakdar, Shahin; Javadian, Sayfoddin

    2010-01-01

    Pure hydroxyapatite (HAp) and fluoride-containing apatite powders (FHAp) were synthesized using a hydrothermal method. The powders were assessed by x-ray diffraction (XRD), Fourier transform infrared (FTIR), scanning electron microscope (SEM) and F-selective electrode. X-ray diffraction results revealed the formation of single phase apatite structure for all the compositions synthesized in this work. However, the addition of a fluoride ion led to a systematic shift in the (3 0 0) peak of the XRD pattern as well as modifications in the FTIR spectra. It was found that the efficiency of fluoride ion incorporation decreased with the increase in the fluoride ion content. Fluorine incorporation efficiency was around 60% for most of the FHAp samples prepared in the current study. Smaller and less agglomerated particles were obtained by fluorine substitution. The bioactivity of the powder samples with different fluoride contents was compared by performing cell proliferation, alkaline phosphatase (ALP) and Alizarin red staining assays. Human osteoblast cells were used to assess the cellular responses to the powder samples in this study. Results demonstrated a strong dependence of different cell activities on the level of fluoridation.

  14. Synthesis of anhydrous K2TiOF4 via a mild hydrothermal method

    Science.gov (United States)

    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. Continuous synthesis of Oleyl Oleate in supercritical carbon oxide using solid p-Toluenesulfonic Acid as catalyst

    International Nuclear Information System (INIS)

    Ghaziaskar, H.; Ikushima, Y.

    2000-01-01

    Supercritical carbon dioxide (Sc-CO 2 ) was used as solvent to synthesize oleyl oleate as an analog of Jojoba oil from oleic acid and oleyl alcohol with high conversion (100%) of the acid into ester in a short time of 100 min. Utilizing a low cost solid catalyst, p-toluenesulfonic acid monohydrate , the esterification reaction was performed, without any prior preparation step, in a flow mode, at a pressure of 147 bar and a temperature of 60 d eg C. This method seems industrially suitable for the production of oleyl oleate. The solubility of a mixture of oleyl alcohol and oleic acid in Sc-CO 2 were also measured to calculate the alcohol to acid ratio and the esterification yield

  16. CdS-sensitized TiO2 nanocorals: hydrothermal synthesis, characterization, application.

    Science.gov (United States)

    Mali, S S; Desai, S K; Dalavi, D S; Betty, C A; Bhosale, P N; Patil, P S

    2011-10-01

    Cadmium sulfide (CdS) nanoparticle-sensitized titanium oxide nanocorals (TNC) were synthesized using a two-step deposition process. The TiO(2) nanocorals were grown on the conducting glass substrates (FTO) using A hydrothermal process and CdS nanoparticles were loaded on TNC using successive ionic layer adsorption and reaction (SILAR) method. The TiO(2), CdS and TiO(2)-CdS samples were characterized by optical absorption, X-ray diffraction (XRD), FT-Raman, FT-IR, scanning electron microscopy (SEM) and contact angle. Further, their photoelectrochemical (PEC) performance was tested in NaOH, Na(2)S-NaOH-S and Na(2)S electrolytes, respectively. When CdS nanoparticles are coated on TNCs, the optical absorption is found to be enhanced and band edge is red-shifted towards visible region. The TiO(2)-CdS sample exhibits improved photoelectrochemical (PEC) performance with maximum short circuit current of (J(sc)) 1.04 mA cm(-2). After applying these TiO(2)-CdS electrodes in photovoltaic cells, the photocurrent was found to be enhanced by 2.7 and 32.5 times, as compared with those of bare CdS and TiO(2) nanocorals films electrodes respectively. Also, the power conversion efficiency of TiO(2)-CdS electrodes is 0.72%, which is enhanced by about 16 and 29 times for TiO(2), CdS samples. This journal is © The Royal Society of Chemistry and Owner Societies 2011

  17. Synthesis of ZnSn(OH){sub 6} regular octahedrons by a simple hydrothermal process

    Energy Technology Data Exchange (ETDEWEB)

    Yu, Xiujun; Lu, Hongxia; Zhao, Yunlong; Chen, Deliang; Fan, Bingbing; Wang, Hailong; Yang, Daoyuan; Xu, Hongliang [School of Materials Science and Engineering, Zhengzhou University (China); Li, Qi [School of Information Engineering, Zhengzhou University (China); Zhang, Rui [School of Materials Science and Engineering, Zhengzhou University (China); Zhengzhou Institute of Aeronautical Industry Management, Zhengzhou (China)

    2011-10-15

    ZnSn(OH){sub 6} regular octahedrons were successfully synthesized through a simple hydrothermal method using an aqueous solution containing ZnO flower-like structures, SnCl{sub 4}.5H{sub 2}O, and NaOH. Phase structure, morphology and microstructure of the samples were investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Parameters in preparation process such as the ratios of Sn{sup 4+}/OH{sup -}, the molar ratio of Zn/Sn and reaction time were discussed. Results show that the obtained samples are comprised of ZnSn(OH){sub 6} regular octahedrons with about 2 {mu}m in side length and ZnSn(OH){sub 6} urchins-like structures. ZnSn(OH){sub 6} urchins-like structures preferentially grow on the edges and corners of regular octahedrons. Morphology of the products is susceptible to the ratios of Sn{sup 4+}/OH{sup -}. A relatively low concentration of OH{sup -} is favored to obtain ZnSn(OH){sub 6} regular octahedrons with urchins-like structures on the surface, while a high concentration of OH{sup -} results in a handful of regular octahedrons without urchins-like structures on the surface. When the molar ratio of Zn/Sn changes to 1:2 or 2:1, the edges and corners of regular octahedrons become coarse and urchins-like structures disappear from the surface. More urchins-like structures form on the surface of regular octahedrons and the edges and corners of regular octahedrons become coarsened with the increase of reaction time. Moreover, the possible mechanism for ZnSn(OH){sub 6} regular octahedrons is discussed. (copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  18. Hydrothermal synthesis of mixed zinc–cobalt ferrite nanoparticles: structural and magnetic properties

    Energy Technology Data Exchange (ETDEWEB)

    Coppola, P. [Univ. de Brasília, Complex Fluids Group, Instituto de Química (Brazil); Silva, F. G. da [Univ. de Brasília, Laboratório de Nanociência Ambiental e Aplicada - LNAA, Faculdade UnB Planaltina (Brazil); Gomide, G.; Paula, F. L. O. [Univ. de Brasília, Complex Fluids Group, Instituto de Física (Brazil); Campos, A. F. C. [Univ. de Brasília, Laboratório de Nanociência Ambiental e Aplicada - LNAA, Faculdade UnB Planaltina (Brazil); Perzynski, R. [Sorbonne Universités, UPMC Univ. Paris 06, CNRS, Laboratoire PHENIX (France); Kern, C. [Univ. de Brasília, Complex Fluids Group, Instituto de Química (Brazil); Depeyrot, J. [Univ. de Brasília, Complex Fluids Group, Instituto de Física (Brazil); Aquino, R., E-mail: reaquino@unb.br [Univ. de Brasília, Laboratório de Nanociência Ambiental e Aplicada - LNAA, Faculdade UnB Planaltina (Brazil)

    2016-05-15

    We synthesize Zn-substituted cobalt ferrite (Zn{sub x}Co{sub 1−x}Fe{sub 2}O{sub 4}, with 0 ≤ x ≤ 1) magnetic nanoparticles by a hydrothermal co-precipitation method in alkaline medium. The chemical composition is evaluated by atomic absorption spectroscopy and energy-dispersive X-ray spectroscopy techniques. The structure and morphology of the nanopaticles are investigated by X-ray diffraction (XRD) and transmission electron microscopy (TEM), respectively. XRD Rietveld refinements reveal the cation distribution among the tetrahedral (A) and octahedral (B) sites. It shows that up to x ~0.5 zinc ions occupy preferably A-sites, above which Zn ions begin also a gradual occupancy of B-sites. TEM images show nanoparticles with different shapes varying from spheres, cubes, to octahedrons. Hysteresis loop properties are studied at 300 and 5 K. These properties are strongly influenced by the Zn and Co proportion in the nanoparticle composition. At 300 K, only samples with high Co content present hysteresis. At 5 K, the reduced remanent magnetization ratio (M{sub R}/M{sub S}) and the coercivity (H{sub C}) suggest that nanoparticles with x < 0.5 have cubic anisotropy. A kink on the hysteresis loop, close to the remanence, is observed at low temperature. This feature is presumably associated to interplay between hard and soft anisotropy regimes in the powder samples.Graphical Abstract.

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

    Science.gov (United States)

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

    2016-03-14

    (27) Al 3Q MAS NMR and UV/Vis spectroscopy with bare Co(II) ions as probes of Al pairs in the zeolite framework were employed to analyze the location of framework Al atoms in the channel system of zeolite ZSM-5. Furthermore, the effect of Na(+) ions together with tetrapropylammonium cation (TPA(+)) in the ZSM-5 synthesis gel on the location of Al in the channel system was investigated. Zeolites prepared using exclusively TPA(+) as a structure-directing agent (i.e., in the absence of Na(+) ions) led to 55-90% of Al atoms located at the channel intersection, regardless the presence or absence of Al pairs [Al-O-(Si-O)2 -Al sequences in one ring] in the zeolite framework. The presence of Na(+) ions in the synthesis gel did not modify the Al location at the channel intersection (55-95% of Al atoms) and led only to changes in i) the distribution of framework Al atoms between Al pairs (decrease) and single isolated Al atoms (increase), and ii) the siting of Al in distinguishable framework tetrahedral sites. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Synthesis and characterization of Ni-CeO2 catalysts by the hydrothermal method

    International Nuclear Information System (INIS)

    Lazcano O, I.

    2013-01-01

    At the present time the necessity exists to reduce the level of atmospheric pollutants, because these are the main originators of such problems as: the greenhouse effect, acid rain, global heating, among others and that are affecting the human being seriously. In this context, is necessary to look for new solutions that contribute to the improvement of the problems without appealing to limitations in the energy production, because this would imply a non only delay in the economic development, but also in the cultural, technological and of research in our country. An alternative for the energy solution is the use of renewable fuels, because they will decrease the production costs with the time, as well as to diminish the dependence of the fossil fuels, contributing this way to the improvement of the environment quality. The use of the hydrogen as an alternating fuel to the petroleum, is intends as energy solution. The objective of the present work is to develop Ni-CeO 2 catalysts through the hydrothermal method for the hydrogen production starting from the partial oxidation reaction of methanol for the clean fuel generation that does not produce polluting emissions to the environment. As well as, to determine the importance of the metallic load in the catalytic activity for which catalysts to 1 and 2% in weight of Ni were prepared. To achieve these objective different techniques were used to characterize the prepared catalysts, as: Temperature Programmed Reduction to evidence the metal-support interaction, Scanning Electron Microscopy (Sem) to determine the morphology of the catalysts, Surface Area (Bet) with respect to the adsorption-desorption of N 2 and X-Rays Diffraction (XRD) to know the crystalline structure of the catalysts. Also the catalytic properties (activity and selectivity) were studied under the reaction: CH 3 OH + 1/2 O 2 obtaining as products to the CO 2 + 2H 2 , with the help of the multi-tasks equipment Rig-100 that operated to temperatures among

  1. Ferrites nanoparticles MFe2O4 (M = Ni and Zn: hydrothermal synthesis and magnetic properties

    Directory of Open Access Journals (Sweden)

    Pérez Mazariego, J. L.

    2008-06-01

    Full Text Available MFe2O4 (M = Ni and Zn nanoparticles were prepared by the hydrothermal method. The obtained samples were characterized by X-ray and electron diffraction, Scanning and Transmission Electron Microscopy and Mössbauer spectroscopy. The transmission images show homogeneous shape and particle size ranging from 10 to 40 nm, depending on the nature of the M cation. Mössbauer spectroscopy yields to a ratio of occupancy between the A and B sites of 0.7 in the case of NiFe2O4 oxide. DC magnetization (2-300 K measurements reveal a superparamagnetic behaviour for the ZnFe2O4 sample with a blocking temperature of 20 K. By contrast, in the case of the NiFe2O4 ferrite the blocking temperature appears to be above 300 K and at lower temperature, it shows a ferrimagnetic behaviour arising from the superexchange interactions that take place in this inverse spinel. Mössbauer spectroscopy results confirm the bulk magnetic measurements.Se han preparado mediante el método hidrotermal nanopartículas de ferritas MFe2O4 (M = Ni, Zn. Las muestras obtenidas fueron caracterizadas mediante difracción de rayos X y electrones, microscopía electrónica de transmisión y barrido y espectroscopia Mössbauer. Las imágenes de transmisión muestran partículas de forma y tamaño homogéneo de 10 a 40 nm según la naturaleza del catión M. La espectroscopia Mössbauer revela una relación de ocupación entre los sitios A y B por los átomos de hierro de 0.7 en el caso del óxido NiFe2O4. Las medidas de magnetización DC (2 – 300 K muestran un comportamiento superparamagnético para la muestra ZnFe2O4 con una temperatura de bloqueo de 20 K. En el caso de las nanopartículas de NiFe2O4 la temperatura de bloqueo parece estar por encima de los 300 K mostrando por debajo de la misma, comportamiento ferrimagnético provocado por las interacciones de superintercambio que tienen lugar en esta espinela inversa. Los resultados de espectroscopia Mössbauer confirman los datos de las

  2. In situ one-step hydrothermal synthesis of oxygen-containing groups-modified g-C3N4 for the improved photocatalytic H2-evolution performance

    Science.gov (United States)

    Wu, Xinhe; Chen, Fengyun; Wang, Xuefei; Yu, Huogen

    2018-01-01

    Surface modification of g-C3N4 is one of the most effective strategies to boost its photocatalytic H2-evolution performance via promoting the interfacial catalytic reactions. In this study, an in situ one-step hydrothermal method was developed to prepare the oxygen-containing groups-modified g-C3N4 (OG/g-C3N4) by a facile and green hydrothermal treatment of bulk g-C3N4 in pure water without any additives. It was found that the hydrothermal treatment (180 °C) not only could greatly increase the specific surface area (from 2.3 to 69.8 m2 g-1), but also caused the formation of oxygen-containing groups (sbnd OH and Cdbnd O) on the OG/g-C3N4 surface, via the interlayer delamination and intralayer depolymerization of bulk g-C3N4. Photocatalytic experimental results indicated that after hydrothermal treatment, the resultant OG/g-C3N4 samples showed an obviously improved H2-evolution performance. Especially, when the hydrothermal time was 6 h, the resultant OG/g-C3N4(6 h) exhibited the highest photocatalytic activity, which was clearly higher than that of the bulk g-C3N4 by a factor of ca. 7. In addition to the higher specific surface area, the enhanced H2-evolution rate of OG/g-C3N4 photocatalysts can be mainly attributed to the formation of oxygen-containing groups, which possibly works as the effective H2-evolution active sites. Considering the facie and green synthesis method, the present work may provide a new insight for the development of highly efficient photocatalytic materials.

  3. Hydrothermal Synthesis of Zeolite from Coal Class F Fly Ash. Influence of Temperature

    Directory of Open Access Journals (Sweden)

    Goñi, S.

    2010-06-01

    Full Text Available The influence of temperature of alkaline hydrothermal treatment on the conversion in zeolite of Spanish coal low calcium-fly ash (ASTM class F is presented in this work. Zeolite Na-P1 gismondine type (Na6Al6Si10O32.12H2O was formed at the temperature of 100ºC, which transformed in zeolite; analcime-C type (Na(Si2AlO6H2O and sodalite (1.08 Na2O.Al2O3.1.68SiO2.1.8H2O at 200ºC together with traces of tobermorite-11Å (Ca5(OH2Si6O16.4H2O. At this temperature the 100% of the fly ash reaction was allowed. An equivalent study was carried out in water as reference. The zeolite conversion of the fly ash was characterized by X ray diffraction (XRD, FT infrared (FTIR spectroscopy, surface area (BET-N2 and thermal analyses.

    En este trabajo se presenta el papel que juega la temperatura durante el tratamiento hidrotermal en medio alcalino para convertir una ceniza volante de bajo contenido en cal (clase F, según la norma ASTM en zeolita. Durante este tratamiento a la temperatura de 100ºC se forma Zeolita Na-P1 tipo gismondina (Na6Al6Si10O32.12H2O; al elevar la temperatura a 200ºC, dicha zeolita se transforma en zeolita Analcima C (Na(Si2AlO6H2O y en fase sodalita (1.08 Na2O.Al2O3.1.68SiO2.1.8H2O junto con trazas de tobermorita-11Å (Ca5(OH2Si6O16.4H2O. A esta temperatura y en estas condiciones se ha conseguido un 100% de reacción. Un estudio equivalente se ha llevado a cabo empleando agua como medio de referencia. La conversión de ceniza volante en zeolita se ha caracterizado mediante técnicas, como difracción de Rayos X (DRX, espectroscopia

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

    Energy Technology Data Exchange (ETDEWEB)

    Rizzuti, Antonino [Politecnico di Bari, Dipartimento di Ingegneria Civile, Ambientale, del Territorio, Edile e di Chimica (Italy); Dassisti, Michele [Politecnico di Bari, Dipartimento di Meccanica, Management e Matematica (Italy); Mastrorilli, Piero, E-mail: p.mastrorilli@poliba.it [Politecnico di Bari, Dipartimento di Ingegneria Civile, Ambientale, del Territorio, Edile e di Chimica (Italy); Sportelli, Maria C.; Cioffi, Nicola; Picca, Rosaria A. [Università di Bari, Dipartimento di Chimica (Italy); Agostinelli, Elisabetta; Varvaro, Gaspare [Consiglio Nazionale delle Ricerche, Istituto di Struttura della Materia (Italy); Caliandro, Rocco [Consiglio Nazionale delle Ricerche, Istituto di Cristallografia (Italy)

    2015-10-15

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

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

    Science.gov (United States)

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

    2015-10-01

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

  6. Study of the synthesis of TiO2 layers on macroporous ceramic supports in supercritical (SC) CO2 for processing radioactive aqueous effluents in dynamic mode

    International Nuclear Information System (INIS)

    Duchateau, Maxime

    2014-01-01

    Public and military nuclear industry generates a significant amount of radioactive liquid waste which must be treated before being released into the environment. Decontamination methods alternative to the industrial techniques (evaporation, chemical treatment) are being developed, such as column treatments or coupled filtration/sorption processes. Current researches mainly focus on the development and shaping of specific sorbents. In this context, the objectives of this thesis were first to study the synthesis of TiO 2 layers on macroporous ceramic supports in supercritical (SC) CO 2 and then to evaluate their potential for radionuclide extraction in these alternative processes. A robust synthesis method has been developed, based on the thermal decomposition of titanium isopropoxide in SC CO 2 in the temperature range between 150 C and 350 C. Nano-structured TiO 2 films were formed on the macroporous supports (ceramic foams, tubular α-alumina supports) with good adhesion, already at 150 C. The effect of the synthesis temperature on sorbents physico-chemical characteristics and sorption properties has been studied with TiO 2 powders prepared under the same conditions as the supported films. The best sorption performance were observed for the powder prepared at 150 C, owing to its higher density of surface sites in comparison with powders prepared at either 250 C or 350 C. Consequently, this synthesis temperature (150 C) was selected for a detailed study of the composite sorbents (TiO 2 /support), in order to assess their sorption performance in continuous treatment processes. The sorption experiments have shown that a column of alumina macroporous foam (Φpore = 400μm) coated with TiO 2 was suitable for processing effluents in dynamic mode with high throughputs. Both macro-pore sizes and column height were revealed as important parameters to be controlled. For the coupled filtration/sorption treatment, TiO 2 membranes exhibit good mechanical strength and are able

  7. Sol–gel synthesis of highly TiO2 aerogel photocatalyst via high temperature supercritical drying

    Directory of Open Access Journals (Sweden)

    Rebah Moussaoui

    2017-09-01

    Full Text Available Nanocrystalline powders of TiO2 xerogel and aerogel were prepared by using acid-modified sol–gel approach. For TiO2 aerogel material (TA, the solvent was high temperature supercritically extracted at 300 °C and 100 bars. However, the TiO2 xerogel material (TX was dried at 200 °C and ambient pressure. The effects of the drying processes on the crystalline structure, phase transformation and grain growth were determined by Raman spectroscopy, SAED and X-ray diffraction (XRD analyses using Rietveld refinement method. The TiO2 aerogel was composed of anatase crystalline structure. The TiO2 xerogel material was composed of anatase, brookite and small amount of amorphous phase with anatase as dominant phase. The TX sample still contains a relatively high concentration of carbon than that of TA, indicating the amorphous character of TiO2 xerogel. These materials were applied as catalyst for the degradation of indigo carmine in aqueous medium. Photo-degradation ability of TA and TX was compared to the TiO2 commercial Degussa P25. The photo-catalytic results showed that the degradation efficiency was in the order TA > P25 > TX. The photo-degradation of indigo carmine followed pseudo first order reaction kinetics.

  8. Supercritical CO2 Assisted Synthesis of EDTA-Fe3O4 Nanocomposite with High Adsorption Capacity for Hexavalent Chromium

    Directory of Open Access Journals (Sweden)

    Gunjan Bisht

    2016-01-01

    Full Text Available Efficiency of EDTA functionalized nanoparticles in adsorption of chromium (VI from water was investigated in this study. Magnetic iron oxide nanoparticles (IONPs were synthesized by a simple chemical coprecipitation route and EDTA coating onto IONPs was attained via supercritical carbon dioxide (Sc CO2, a technology with green sustainable properties. The obtained nanoparticles were then characterized by UV-Visible spectroscopy, Fourier transform infrared spectroscopy (FTIR, X-ray powder diffraction (XRD, transmission electron microscopy (TEM, scanning electron microscopy (SEM, and vibrating magnetometric analysis (VSM. The synthesized nanoparticle and its modified variant were evaluated as adsorbent for chromium (VI removal from water through batch adsorption technique and the effect of analytic concentration; contact time and adsorbent concentration were studied at pH 2. The results showed higher removal efficiency for modified magnetic iron oxide nanoparticles (MIONPs (i.e., 99.9% than their nonmodified variant IONPs, that is, 34.06% for the same concentration after 18 hours of incubation. Also maximum adsorption capacity (qe = 452.26 mg/g of MIONPs attained can be related to their preparation in Sc CO2 as qe calculated from IONPs, that is, 170.33 mg/g, is lower than that of MIONPs. The adsorption data fit well with Freundlich isotherm equation while kinetic adsorption studies of chromium (VI were modeled by pseudo-second-order model.

  9. Continuous-flow Heck synthesis of 4-methoxybiphenyl and methyl 4-methoxycinnamate in supercritical carbon dioxide expanded solvent solutions

    Directory of Open Access Journals (Sweden)

    Phei Li Lau

    2013-12-01

    Full Text Available The palladium metal catalysed Heck reaction of 4-iodoanisole with styrene or methyl acrylate has been studied in a continuous plug flow reactor (PFR using supercritical carbon dioxide (scCO2 as the solvent, with THF and methanol as modifiers. The catalyst was 2% palladium on silica and the base was diisopropylethylamine due to its solubility in the reaction solvent. No phosphine co-catalysts were used so the work-up procedure was simplified and the green credentials of the reaction were enhanced. The reactions were studied as a function of temperature, pressure and flow rate and in the case of the reaction with styrene compared against a standard, stirred autoclave reaction. Conversion was determined and, in the case of the reaction with styrene, the isomeric product distribution was monitored by GC. In the case of the reaction with methyl acrylate the reactor was scaled from a 1.0 mm to 3.9 mm internal diameter and the conversion and turnover frequency determined. The results show that the Heck reaction can be effectively performed in scCO2 under continuous flow conditions with a palladium metal, phosphine-free catalyst, but care must be taken when selecting the reaction temperature in order to ensure the appropriate isomer distribution is achieved. Higher reaction temperatures were found to enhance formation of the branched terminal alkene isomer as opposed to the linear trans-isomer.

  10. Continuous-flow Heck synthesis of 4-methoxybiphenyl and methyl 4-methoxycinnamate in supercritical carbon dioxide expanded solvent solutions.

    Science.gov (United States)

    Lau, Phei Li; Allen, Ray W K; Styring, Peter

    2013-01-01

    The palladium metal catalysed Heck reaction of 4-iodoanisole with styrene or methyl acrylate has been studied in a continuous plug flow reactor (PFR) using supercritical carbon dioxide (scCO2) as the solvent, with THF and methanol as modifiers. The catalyst was 2% palladium on silica and the base was diisopropylethylamine due to its solubility in the reaction solvent. No phosphine co-catalysts were used so the work-up procedure was simplified and the green credentials of the reaction were enhanced. The reactions were studied as a function of temperature, pressure and flow rate and in the case of the reaction with styrene compared against a standard, stirred autoclave reaction. Conversion was determined and, in the case of the reaction with styrene, the isomeric product distribution was monitored by GC. In the case of the reaction with methyl acrylate the reactor was scaled from a 1.0 mm to 3.9 mm internal diameter and the conversion and turnover frequency determined. The results show that the Heck reaction can be effectively performed in scCO2 under continuous flow conditions with a palladium metal, phosphine-free catalyst, but care must be taken when selecting the reaction temperature in order to ensure the appropriate isomer distribution is achieved. Higher reaction temperatures were found to enhance formation of the branched terminal alkene isomer as opposed to the linear trans-isomer.

  11. Immobilization of CALB on activated chitosan: Application to enzymatic synthesis in supercritical and near-critical carbon dioxide

    Directory of Open Access Journals (Sweden)

    José C.S. dos Santos

    2017-03-01

    Full Text Available The objective of this new paper was to evaluate the enzymatic esterification reaction conducted in supercritical or near-critical CO2, catalyzed by immobilized lipase B from Candida antarctica (CALB. The biocatalyst was prepared through the immobilization of CALB by covalent attachment using chitosan sequentially activated with Glycidol, ethylenediamine (EDA and glutaraldehyde as support. In order to determine the best operational conditions of the esterification reaction (1: 1 (alcohol–acid; biocatalyst content, 10% (by substrate mass; 45 °C, an experimental design (23 was conducted to evaluate the effects of the following parameters: alcohol to oil molar ratios, reaction time and temperature. The maximum loading of chitosan was 20 mg protein/g support, and the thermal and solvent stability of the new biocatalyst was higher than that of the CALB-GX (by a 26-fold factor, CALB-OC (by a 53-fold factor and Novozym 435 (by a 3-fold factor. The maximum conversion was 46.9% at a temperature of 29.9 °C, ethanol to oleic acid molar ratio equal to 4.50:1, and a reaction time of 6.5 h. Additionally, the removal of water from the medium, by using molecular sieves, promoted a 16.0% increase in the conversion of oleic acid into ethyl esters.

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

    Science.gov (United States)

    Kacimi, Larbi; Cyr, Martin; Clastres, Pierre

    2010-09-15

    The objective of this study was the synthesis of alpha'(L)-C(2)S (Ca(2)SiO(4)) belite cement, starting from fly-ash of system CaO-SiO(2)-Al(2)O(3)-SO(3), and using the hydrothermal method in alkaline solution. The lime deficit in these ashes was compensated by the addition of slaked lime from lime bagging workshops. The hydrothermal treatment of the mixture was carried out in demineralized water, NaOH or KOH solution, continually stirred at a temperature below 100 degrees C and atmospheric pressure. The dehydration and calcination of the mixtures at temperatures between 800 and 1100 degrees C allowed alpha'(L)-C(2)S-rich cement to be obtained. The optimization of the synthesis parameters (temperature and time of stirring, pH of solution, temperature and duration of mixture burning) was also studied. The phase formation during various synthesis stages was studied by X-ray diffraction (XRD). Other techniques, such as SEM and EDX, were used to characterize the cement minerals. The results obtained showed that these ashes could form belite cement composed of only one dicalcium silicate phase (alpha'(L)-C(2)S). Copyright 2010 Elsevier B.V. All rights reserved.

  13. Synthesis and characterization of the aluminium phosphates modified with ammonium, calcium and molybdenum by hydrothermal method

    Directory of Open Access Journals (Sweden)

    Łuczka Kinga

    2016-06-01

    Full Text Available Synthesis and characterization of the aluminum phosphates modified with ammonium, calcium and molybdenum were conducted. The influence of process parameters (reactive pressure and molar ratios in the reaction mixture were studied. The contents of the individual components in the products were in the range of: 10.97–17.31 wt% Al, 2.65–13.32 wt% Ca, 0.70–3.11 wt% Mo, 4.36–8.38 wt% NH3, and 35.12–50.54 wt% P2O5. The materials obtained in the experiments were characterized by various physicochemical parameters. The absorption oil number was in the range from 67 to 89 of oil/100 g of product, the surface area was within the range of 4–76 m2/g, whereas the average particle size of products reached 282–370 nm. The Tafel tests revealed comparable anticorrosive properties of aluminum phosphates modified with ammonium, calcium, molybdenum in comparison with commercial phosphate.

  14. Synthesis of ruthenium(II) complexes containing hydroxymethylphosphines and their catalytic activities for hydrogenation of supercritical carbon dioxide.

    Science.gov (United States)

    Kayaki, Yoshihito; Shimokawatoko, Yoshiki; Ikariya, Takao

    2007-07-09

    Ligand substitution of RuCl2[P(C6H5)3]3 and Cp*RuCl(isoprene) (Cp*=1,2,3,4,5-pentamethylcyclopentadienyl) complexes with hydroxymethylphosphines was investigated to develop new catalyst systems for CO2 hydrogenation. A reaction of P(C6H5)2CH2OH with RuCl2[P(C6H5)3]3 in CH2Cl2 gave Ru(H)Cl(CO)[P(C6H5)2CH2OH]3 (1), which was characterized by NMR spectroscopy and X-ray crystallographic analysis. An isotope labeling experiment using P(C6H5)213CH2OH indicated that the carbonyl moiety in complex 1 originated from formaldehyde formed by degradation of the hydroxymethylphosphine. Elimination of formaldehyde from PCy2CH2OH (Cy=cyclohexyl) was also promoted by treatment of RuCl2[P(C6H5)3]3 in ethanol to give RuCl2(PHCy2)4 under mild conditions. On the other hand, the substitution reaction using Cp*RuCl(isoprene) with the hydroxymethylphosphine ligands proceeded smoothly with formation of Cp*RuCl(L)2 [2a-2c; L=P(C6H5)2CH2OH, PCy(CH2OH)2, and P(CH2OH)3] in good yields. The isolable hydroxymethylphosphine complexes 1 and 2 efficiently catalyzed the hydrogenative amidation of supercritical carbon dioxide (scCO2) to N,N-dimethylformamide (DMF).

  15. Solvation in supercritical water

    International Nuclear Information System (INIS)

    Cochran, H.D.; Cummings, P.T.; Karaborni, S.

    1991-01-01

    The aim of this work is to determine the solvation structure in supercritical water composed with that in ambient water and in simple supercritical solvents. Molecular dynamics studies have been undertaken of systems that model ionic sodium and chloride, atomic argon, and molecular methanol in supercritical aqueous solutions using the simple point charge model of Berendsen for water. Because of the strong interactions between water and ions, ionic solutes are strongly attractive in supercritical water, forming large clusters of water molecules around each ion. Methanol is found to be a weakly-attractive solute in supercritical water. The cluster of excess water molecules surrounding a dissolved ion or polar molecule in supercritical aqueous solutions is comparable to the solvent clusters surrounding attractive solutes in simple supercritical fluids. Likewise, the deficit of water molecules surrounding a dissolved argon atom in supercritical aqueous solutions is comparable to that surrounding repulsive solutes in simple supercritical fluids. The number of hydrogen bonds per water molecule in supercritical water was found to be about one third the number in ambient water. The number of hydrogen bonds per water molecule surrounding a central particle in supercritical water was only mildly affected by the identify of the central particle--atom, molecule, or ion. These results should be helpful in developing a qualitative understanding of important processes that occur in supercritical water. 29 refs., 6 figs

  16. Geological model of supercritical geothermal reservoir related to subduction system

    Science.gov (United States)

    Tsuchiya, Noriyoshi

    2017-04-01

    Following the Great East Japan Earthquake and the accident at the Fukushima Daiichi Nuclear power station on 3.11 (11th March) 2011, geothermal energy came to be considered one of the most promising sources of renewable energy for the future in Japan. The temperatures of geothermal fields operating in Japan range from 200 to 300 °C (average 250 °C), and the depths range from 1000 to 2000 m (average 1500 m). In conventional geothermal reservoirs, the mechanical behavior of the rocks is presumed to be brittle, and convection of the hydrothermal fluid through existing network is the main method of circulation in the reservoir. In order to minimize induced seismicity, a rock mass that is "beyond brittle" is one possible candidate, because the rock mechanics of "beyond brittle" material is one of plastic deformation rather than brittle failure. Supercritical geothermal resources could be evaluated in terms of present volcanic activities, thermal structure, dimension of hydrothermal circulation, properties of fracture system, depth of heat source, depth of brittle factures zone, dimension of geothermal reservoir. On the basis of the GIS, potential of supercritical geothermal resources could be characterized into the following four categories. 1. Promising: surface manifestation d shallow high temperature, 2 Probability: high geothermal gradient, 3 Possibility: Aseismic zone which indicates an existence of melt, 4 Potential : low velocity zone which indicates magma input. Base on geophysical data for geothermal reservoirs, we have propose adequate tectonic model of development of the supercritical geothermal reservoirs. To understand the geological model of a supercritical geothermal reservoir, granite-porphyry system, which had been formed in subduction zone, was investigated as a natural analog of the supercritical geothermal energy system. Quartz veins, hydrothermal breccia veins, and glassy veins are observed in a granitic body. The glassy veins formed at 500-550

  17. Controlled synthesis of La1−xSrxCrO3 nanoparticles by hydrothermal method with nonionic surfactant and their ORR activity in alkaline medium

    International Nuclear Information System (INIS)

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

    2013-01-01

    Graphical abstract: We demonstrate that Sr-doped LaCrO 3 nanoparticles were successfully prepared by the hydrothermal synthesis method using the nonionic surfactant Triton X-100 and the applicability of La 1−x Sr x CrO 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 3 nanoparticles were successfully prepared by the hydrothermal method using the nonionic surfactant. • Homogeneously shaped and sized Sr-doped LaCrO 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 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 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

  18. Synthesis of biomorphological mesoporous TiO2 templated by mimicking bamboo membrane in supercritical CO2.

    Science.gov (United States)

    Li, Jinhong; Shi, Xiaoying; Wang, Lijuan; Liu, Fei

    2007-11-01

    A new approach is presented for preparing biomorphological mesoporous TiO2 templated by mimicking bamboo inner shell membrane via supercritical CO2 (SCCO2) transportation through titanium tetrabutyloxide (TTBO). The analysis of wide-angle X-ray powder diffraction (XRD) showed the prepared TiO2 in phase of anatase, and the small-angle XRD revealed the presence of mesopores without periodicity. The product exhibited the shape of crinkled films and extended in two dimensions up to centimeters. The electron microscopic observation showed that the TiO2 films were around 200 nm in thickness, and across the films there were numerous round or ellipse-shaped mesopores, being 10-50 nm in diameter, which were formed by the close packing of TiO2 particles. High-resolution transmission electron microscope (HRTEM) displayed that the single TiO2 particle size was about 12.5 nm. The UV-vis absorption spectrum was transparent in the wavelength of 320-350 nm for suspensions of the prepared mesoporous TiO2 in ethanol at the concentration of 5.0 mg/l. The mesoporous TiO2 prepared with the aid of SCCO2 exhibited an obvious blue shift compared with the TiO2 prepared by sol-gel infiltration. The possible mechanism for the formation of the mesoporous TiO2 is summarized into a biomimetic mineralization pathway. First, TTBO was transported to the membrane surface via SCCO2, and then condensed. Hydrolysis reactions between the functional groups of organic membrane and TTBO took place to form the nuclear TiO2, and the TiO2 seeds grew around the organic membrane into TiO2 mesoporous materials. The approach provides a low-cost and efficient route for the production of ceramics nanomaterials with unique structural features, which may have potential application in designing UV-selective shielding devices [S. Zhao, X.H. Wang, S.B. Xin, Q. Jiang, X.P. Liang, Rare Metal Mater. Eng. 35 (2006) 508-510].

  19. Influence of reaction time and synthesis temperature on the physical properties of ZnO nanoparticles synthesized by the hydrothermal method

    Science.gov (United States)

    Wasly, H. S.; El-Sadek, M. S. Abd; Henini, Mohamed

    2018-01-01

    Influence of synthesis temperature and reaction time on the structural and optical properties of ZnO nanoparticles synthesized by the hydrothermal method was investigated using X-ray diffraction (XRD), high resolution transmission electron microscopy (HR-TEM), energy-dispersive X-ray, Fourier transform infra-red spectroscopy, and UV-visible and fluorescence spectroscopy. The XRD pattern and HR-TEM images confirmed the presence of crystalline hexagonal wurtzite ZnO nanoparticles with average crystallite size in the range 30-40 nm. Their energy gap determined by fluorescence was found to depend on the synthesis temperature and reaction time with values in the range 2.90-3.78 eV. Thermal analysis, thermogravimetric and the differential scanning calorimetry were used to study the thermal reactions and weight loss with heat of the prepared ZnO nanoparticles.

  20. Factors influencing formation of highly dispersed BaTiO3 nanospheres with uniform sizes in static hydrothermal synthesis

    International Nuclear Information System (INIS)

    Gao, Jiabing; Shi, Haiyue; Dong, Huina; Zhang, Rui; Chen, Deliang

    2015-01-01

    Highly dispersed BaTiO 3 nanospheres with uniform sizes have important applications in micro/nanoscale functional devices. To achieve well-dispersed spherical BaTiO 3 nanocrystals, we carried out as reported in this paper the systematic investigation on the factors that influence the formation of BaTiO 3 nanospheres by the static hydrothermal process, including the NaOH concentrations [NaOH], molar Ba/Ti ratios (R Ba/Ti ), hydrothermal temperatures, and durations, with an emphasis on understanding the related mechanisms. Barium nitrate and TiO 2 sols derived from tetrabutyl titanate were used as the starting materials. The as-synthesized BaTiO 3 samples were characterized by X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray analysis, thermogravimetry, differential thermal analysis, and FT-IR spectra. The highly dispersed BaTiO 3 nanospheres (76 ± 13 nm) were achieved under the optimum hydrothermal conditions at 200 °C for 10 h: [NaOH] = 2.0 mol L −1 and R Ba/Ti  = 1.5. Higher NaOH concentrations, higher Ba/Ti ratios, higher hydrothermal temperatures, and longer hydrothermal durations are favorable in forming BaTiO 3 nanospheres with larger fractions of tetragonal phase and higher yields; but too long hydrothermal durations resulted in abnormal growth and reduced the uniformity in particle sizes. The possible formation mechanisms for BaTiO 3 nanocrystals under the static hydrothermal conditions were investigated

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

    Science.gov (United States)

    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

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

    Science.gov (United States)

    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.

  3. Hydrothermal synthesis of PtRu on CNT/SnO2 composite as anode catalyst for methanol oxidation fuel cell

    International Nuclear Information System (INIS)

    Kakati, Nitul; Maiti, Jatindranath; Jee, Seung Hyun; Lee, Seok Hee; Yoon, Young Soo

    2011-01-01

    Graphical abstract: Display Omitted Highlights: → CNTs are homogeneously covered by the porous SnO 2 layer which enhanced the electronic property of the catalyst support as well as the catalyst and fuel interaction. → PtRu/SnO 2 /CNT catalyst shows an electrochemically active surface area of 81.84 m 2 g Pt -1 and a mass activity of 890mAmg Pt -1 . → Hydrothermal synthesis offers small particle size as well as well dispersion of the catalyst nanoparticles. → Addition of SnO 2 with PtRu provides an additional route for OH ads formation and hence accelerates methanol oxidation. - Abstract: An electrocatalyst support comprising of carbon nanotube and tin oxide (CNT/SnO 2 ) was prepared by an ethylene glycol mediated synthesis procedure and proposed as an improved catalyst support for direct methanol fuel cell. CNTs are covered by the porous SnO 2 layer which is homogeneously distributed over CNT surface. PtRu alloy nanoparticles were deposited over this composite material by a hydrothermal synthesis method. The CNT/SnO 2 composite and its supported PtRu catalyst (PtRu/SnO 2 /CNT) were characterized by X-ray diffraction, field emission scanning electron microscopy and transmission electron microscopy. The electrocatalytic activity of PtRu/SnO 2 /CNT catalyst for methanol oxidation has been studied by cyclic voltammetry, impedance spectroscopy and chronoamperometry. The results were compared with Pt/SnO 2 /CNT and PtRu/CNT catalysts synthesized by the same procedure. PtRu/SnO 2 /CNT catalyst shows an electrochemically active surface area of 81.84 m 2 g Pt -1 and a mass activity of 890mAmg Pt -1 . The presence of SnO 2 layer over CNT can further improve the electrocatalytic activity of PtRu alloy nanoparticles for methanol oxidation.

  4. In-situ hydrothermal synthesis of three-dimensional MnO2-CNT nanocomposites and their electrochemical properties

    International Nuclear Information System (INIS)

    Teng, Fei; Santhanagopalan, Sunand; Wang, Ying; Meng, Dennis Desheng

    2010-01-01

    Three-dimensional (3-D) MnO 2 -carbon nanotube (CNT) nanocomposites were prepared by a simple one-pot hydrothermal method. An electrode was then prepared with these nanocomposites. For comparative investigation, MnO 2 microspheres were also hydrothermally prepared without adding CNTs. The as-synthesized MnO 2 microspheres were then mechanically mixed with CNTs to prepare a subsequent electrode. The samples were characterized by electron microscopy, X-ray diffraction, and electrochemical methods. It has been revealed that a 3-D conductive network of CNTs was formed with microspheres of MnO 2 nanorods interwoven with and connected by CNTs. As a result, the hydrothermally mixed MnO 2 -CNT electrode showed a higher specific capacitance than the mechanically mixed electrode. It has therefore been concluded that the hydrothermal mixing method yields a more homogeneous product that is better suited to take full advantages of both the high capacitance of MnO 2 and the high electrical conductivity of CNTs. The 3-D MnO 2 -CNT nanocomposites reported herein have provided a promising electrode material for supercapacitors and other electrochemical energy storage/conversion devices.

  5. Hydrothermal synthesis and electrochemical properties of nano-sized Co-Sn alloy anodes for lithium ion batteries

    International Nuclear Information System (INIS)

    He Jianchao; Zhao Hailei; Wang Jing; Wang Jie; Chen Jingbo

    2010-01-01

    Research highlights: → Nano-sized Co-Sn alloys were synthesized by hydrothermal route. → Li 2 O and CoSn can buffer the large volume change associated with lithiation of Sn. → A two-step reaction mechanism of CoSn 2 alloy during cycling was confirmed. - Abstract: Nano-sized Co-Sn alloys with a certain amount of Sn oxides used as potential anode materials for lithium ion batteries were synthesized by hydrothermal route. The effects of hydrothermal conditions and post annealing on the phase compositions and the electrochemical properties of synthesized powders were characterized by means of X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM) with energy dispersive spectra (EDS) analysis and galvanostatic cycling tests. Prolonging the dwelling time at the same hydrothermal temperature can increase the content of Sn oxides, which will lead to a high initial irreversible capacity loss but a better cycling stability owing to the buffer effect of irreversible product Li 2 O. Heat-treatment can increase the crystallinity and cause the presence of a certain amount of inert CoSn component, which both have positive impact on the cycling stability of Co-Sn electrode. By comparison with the lithiation/delithiation processes of metal Sn, a two-step mechanism of CoSn 2 alloy during cycling was confirmed.

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

    Science.gov (United States)

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

    2015-01-01

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

  7. Hydrothermal Synthesis of Bi6S2O15 Nanowires: Structural, in situ EXAFS, and Humidity-Sensing Studies

    DEFF Research Database (Denmark)

    Zhou, Y.; Grunwaldt, Jan-Dierk; Krumeich, F.

    2010-01-01

    Sensing oxysulfates: A new type of bismuth oxysulfate nanowire emerges from the straightforward hydrothermal reaction of Bi2O3 and K2SO4. The formation pathway of this versatile material is monitored with in situ QEXAFS techniques. The high-aspect-ratio nanorods display promising features...

  8. Radiolytic and electron-transfer reactions in supercritical CO2

    International Nuclear Information System (INIS)

    Bartels, D. M.; Dimitrijevic, N. M.; Jonah, C. D.; Takahashi, K.

    2000-01-01

    Using supercritical fluids as solvents is useful for both practical and theoretical reasons. It has been proposed to use supercritical CO 2 as a solvent for synthesis because it eliminates the air pollution arising from other solvents. The properties of supercritical fluids can be easily varied with only modest changes in temperature and density, so they provide a way of testing theories of chemical reactions. It has also been proposed to use supercritical fluids for the treatment of hazardous mixed waste. For these reasons the authors have studied the production of radiolytic species in supercritical CO 2 and have measured their reactivity as a function of density. They have shown that the C 2 O 4 + is formed. They also have shown that the electron transfer reactions of dimethylaniline to C 2 O 4 + and CO 2 (e - ) to benzoquinone are diffusion controlled over a considerable density range

  9. Hydrothermal synthesis, characterization and composition-dependent magnetic properties of LaFe1-xCrxO3 system (0≤x≤1)

    International Nuclear Information System (INIS)

    Hu Weiwei; Chen Yan; Yuan Hongming; Zhang Ganghua; Li Guanghua; Pang Guangsheng; Feng Shouhua

    2010-01-01

    Hydrothermal synthesis, characterization and magnetic properties of a series of ABO 3 -perovskites LaFe 1-x Cr x O 3 (0≤x≤1) are reported. The alkalinity in initial reaction mixtures plays a critical role in controlling the designed stoichiometry of the final compositions. Their magnetic properties are strongly dependent on the compositions and a maximum magnetic moment is found for the sample at x=0.5. Weak ferromagnetic interaction observed for the samples from x=0 to 0.9 arises from the presence of Fe-O-Fe antisymmetric exchange and Fe-O-Cr superexchange interaction. The weak ferromagnetism as well as the linear variation of the lattice parameters implies the possible random distribution of Fe and Cr ions in B sites of the perovskites. The evolution of magnetic ordering transition temperatures has a close relationship with substituent ratios, for the competition of antiferromagnetism and ferromagnetism. The saturated magnetic moment shows a great improvement compared with that for the samples synthesized by solid state method. - Graphical abstract: A series of perovskites LaFe 1-x Cr x O 3 (0≤x≤1) were synthesized by mild hydrothermal method and characterized by their weak ferromagnetism due to the possible random distribution of Fe and Cr ions in B sites of the perovskites. The magnetic property of the perovskites is strongly dependent upon the compositions and a maximum magnetic moment is found for LaFe 1-x Cr x O 3 at x=0.5.

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

    Science.gov (United States)

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

    2017-08-01

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

  11. Depletion of a brine layer at the base of ridge-crest hydrothermal systems

    NARCIS (Netherlands)

    Schoofs, Stan; Hansen, Ulrich

    2000-01-01

    The variable salinity of fluid venting from mid-ocean ridges is indicative of mixing between hydrothermal seawater and fluids that have undergone supercritical phase separation. In order to study the stability of a brine-saturated layer that may form in the lowermost part of the hydrothermal

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

    Science.gov (United States)

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

    2017-07-01

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

  13. Ultrafast microwave hydrothermal synthesis and characterization of Bi1-xLaxFeO3 micronized particles

    DEFF Research Database (Denmark)

    Ponzoni, C.; Cannio, M.; Boccaccini, Dino

    2015-01-01

    In this work a microwave assisted hydrothermal method is applied to successfully synthesize lanthanum doped bismuth ferrites (BLFO, Bi1-xLaxFeO3 where x = 0, 0.15, 0.30 and 0.45). The growth mechanism of the Bi1-xLaxFeO3 crystallites is discussed in detail. The existence of the single-phase perov......In this work a microwave assisted hydrothermal method is applied to successfully synthesize lanthanum doped bismuth ferrites (BLFO, Bi1-xLaxFeO3 where x = 0, 0.15, 0.30 and 0.45). The growth mechanism of the Bi1-xLaxFeO3 crystallites is discussed in detail. The existence of the single...

  14. Shape-controlled synthesis and properties of manganese sulfide microcrystals via a biomolecule-assisted hydrothermal process

    Energy Technology Data Exchange (ETDEWEB)

    Jiang Jinghui; Yu Runnan; Zhu Jianyu; Yi Ran; Qiu Guanzhou [School of Resources Processing and Bioengineering, Central South University, Changsha, Hunan 410083 (China); He Yuehui [State Key Laboratory of Powder Metallurgy, Central South University, Changsha, Hunan 410083 (China); Liu Xiaohe, E-mail: liuxh@mail.csu.edu.cn [School of Resources Processing and Bioengineering, Central South University, Changsha, Hunan 410083 (China); State Key Laboratory of Powder Metallurgy, Central South University, Changsha, Hunan 410083 (China)

    2009-06-15

    An effective biomolecule-assisted synthetic route has been successfully developed to prepare {gamma}-manganese sulfide (MnS) microtubes under hydrothermal conditions. In the synthetic system, soluble hydrated manganese chloride was employed to supply Mn source and L-cysteine was used as precipitator and complexing reagent. Sea urchin-like {gamma}-MnS and octahedron-like {alpha}-MnS microcrystals could also be selectively obtained by adjusting the process parameters such as hydrothermal temperature and reaction time. The phase structures, morphologies and properties of the as-prepared products were investigated in detail by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersion spectroscopy (EDS), and photoluminescence spectra (PL). The photoluminescence studies exhibited the correlations between the morphology, size, and shape structure of MnS microcrystals and its optical properties. The formation mechanisms of manganese sulfide microcrystals were discussed based on the experimental results.

  15. Reaction kinetics of cellulose hydrolysis in subcritical and supercritical water

    Science.gov (United States)

    Olanrewaju, Kazeem Bode

    The uncertainties in the continuous supply of fossil fuels from the crisis-ridden oil-rich region of the world is fast shifting focus on the need to utilize cellulosic biomass and develop more efficient technologies for its conversion to fuels and chemicals. One such technology is the rapid degradation of cellulose in supercritical water without the need for an enzyme or inorganic catalyst such as acid. This project focused on the study of reaction kinetics of cellulose hydrolysis in subcritical and supercritical water. Cellulose reactions at hydrothermal conditions can proceed via the homogeneous route involving dissolution and hydrolysis or the heterogeneous path of surface hydrolysis. The work is divided into three main parts. First, the detailed kinetic analysis of cellulose reactions in micro- and tubular reactors was conducted. Reaction kinetics models were applied, and kinetics parameters at both subcritical and supercritical conditions were evaluated. The second major task was the evaluation of yields of water soluble hydrolysates obtained from the hydrolysis of cellulose and starch in hydrothermal reactors. Lastly, changes in molecular weight distribution due to hydrothermolytic degradation of cellulose were investigated. These changes were also simulated based on different modes of scission, and the pattern generated from simulation was compared with the distribution pattern from experiments. For a better understanding of the reaction kinetics of cellulose in subcritical and supercritical water, a series of reactions was conducted in the microreactor. Hydrolysis of cellulose was performed at subcritical temperatures ranging from 270 to 340 °C (tau = 0.40--0.88 s). For the dissolution of cellulose, the reaction was conducted at supercritical temperatures ranging from 375 to 395 °C (tau = 0.27--0.44 s). The operating pressure for the reactions at both subcritical and supercritical conditions was 5000 psig. The results show that the rate-limiting step in

  16. Hydrothermal Synthesis and Structural Characterization of NiO/SnO2 Composites and Hydrogen Sensing Properties

    OpenAIRE

    Wei, Chao; Bo, Bin; Tao, Fengbo; Lu, Yuncai; Peng, Shudi; Song, Wei; Zhou, Qu

    2015-01-01

    Pure SnO2 and NiO doped SnO2 nanostructures were successfully synthesized via a simple and environment-friendly hydrothermal method. X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), and X-ray photoelectron spectra (XPS) were used to investigate the crystalline structures, surface morphologies and microstructures, and element components and their valences of the as-synthesized samples. Furthermore, planar chemical gas sensors based...

  17. Hydrothermal synthetic strategies of inorganic semiconducting nanostructures.

    Science.gov (United States)

    Shi, Weidong; Song, Shuyan; Zhang, Hongjie

    2013-07-07

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

  18. Self-assembly of hollow MoS{sub 2} microflakes by one-pot hydrothermal synthesis for efficient electrocatalytic hydrogen evolution

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Aishi; Cui, Renjie; He, Yanna; Wang, Qi [Key Laboratory for Organic Electronics and Information Displays & Institute of Advanced Materials (IAM), Jiangsu National Synergetic Innovation Center for Advanced Materials (SICAM), Nanjing University of Posts & Telecommunications, Nanjing 210023 (China); Zhang, Jian, E-mail: iamjzhang@njupt.edu.cn [Key Laboratory for Organic Electronics and Information Displays & Institute of Advanced Materials (IAM), Jiangsu National Synergetic Innovation Center for Advanced Materials (SICAM), Nanjing University of Posts & Telecommunications, Nanjing 210023 (China); Yang, Jianping [School of Science, Nanjing University of Posts and Telecommunications (NUPT), Nanjing 210023 (China); Li, Xing’ao, E-mail: lxahbmy@126.com [Key Laboratory for Organic Electronics and Information Displays & Institute of Advanced Materials (IAM), Jiangsu National Synergetic Innovation Center for Advanced Materials (SICAM), Nanjing University of Posts & Telecommunications, Nanjing 210023 (China); School of Science, Nanjing University of Posts and Telecommunications (NUPT), Nanjing 210023 (China)

    2017-07-31

    Highlights: • A new hollow MoS{sub 2} microflakes are prepared by hydrothermal synthesis firstly. • SEM and TEM study show the structural nature of hollow microflakes in depth. • The unique hollow structures have large surface area owing to the cavity. • The hollow microflakes show better HER performance than their solid counterparts. - Abstract: Molybdenum disulfide (MoS{sub 2}) has emerged as a promising non-precious metal catalyst for hydrogen evolution reaction (HER) in recent years. Some strategies including nanotechnology as well as atom doping have been employed in the preparing of electrocatalysts for high-activity and stability. To the best of our knowledge, hollow MoS{sub 2} microflakes assembled from ultrathin nanosheets have not been prepared previously. In this work, a simple, facile and environmentally friendly hydrothermal synthesis was utilized for the fabrication of hollow MoS{sub 2} microflakes for the first time. The unique hollow structures have fascinating properties, such as the large surface and low density. The morphology and structure of MoS{sub 2} microflakes were confirmed by XRD, SEM, TEM and Raman. The composition of these materials was identified by the X-ray photoelectron spectroscopy. Notably, the as-prepared hollow MoS{sub 2} microflakes showed better electrocatalytic activity than other samples. The hollow flake-like structure can not only increase the active edge sites owing to the large specific surface area, but also enhance the electron transport to improve the electrocatalytic activity. Benefiting from these factors, the hollow MoS{sub 2} microflakes exhibited electrocatalytic activity and excellent stability with a low overpotential about 85 mV and a Tafel slope of 59 mV per decade.

  19. Platelet-like hexagonal SrFe{sub 12}O{sub 19} particles: Hydrothermal synthesis and their orientation in a magnetic field

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Tao; Peng, Xiaoling, E-mail: pxlqingliu@cjlu.edu.cn; Li, Jing; Yang, Yanting; Xu, Jingcai; Wang, Panfeng; Jin, Dingfeng; Jin, Hongxiao; Hong, Bo; Wang, Xinqing; Ge, Hongliang

    2016-08-15

    Platelet-like hexagonal SrFe{sub 12}O{sub 19} particles were prepared by hydrothermal synthesis, and the effects of molar ratio of Fe/Sr (R{sub Fe/Sr}) on the phase compositions, morphologies and magnetic properties of as-prepared samples were investigated. The optimum R{sub Fe/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 SrFe{sub 12}O{sub 19} 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){sub max} can be effectively adjusted by given a suitable magnetic field. - Highlights: • We prepared platelet-like hexagonal SrFe{sub 12}O{sub 19} particles by hydrothermal synthesis. • The platelet-like particles arrange with the platelet perpendicular to the magnetic field direction. • The magnetocrystalline anisotropy plays a leading role in the changing effective anisotropy with the rapidly growing shape anisotropy. • The SrFe{sub 12}O{sub 19} (BH){sub max} can be effectively adjusted after magnetic orientation.

  20. Selective hydrothermal synthesis of BiOBr microflowers and Bi2O3 shuttles with concave surfaces

    International Nuclear Information System (INIS)

    Xiao Peipei; Zhu Lingling; Zhu Yongchun; Qian Yitai

    2011-01-01

    Through controlling the amount of NaOH added, BiOBr and Bi 2 O 3 with different shapes were hydrothermally synthesized in the reaction system of Bi(NO 3 ) 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 2 O 3 shuttles with concave surfaces were obtained. The length of these shuttles was 100 μm and the diameter at the middle of these shuttles was 50 μm. The photocatalytic activity of as-prepared BiOBr microflowers was evaluated by the degradation of methyl orange (MO) under visible-light irradiation (λ>420 nm), which was up to 96% within 90 min. - Graphical abstract: Through controlling the amount of NaOH added, BiOBr microflowers and Bi 2 O 3 shuttles with concave surfaces were hydrothermally synthesized in the reaction system of Bi(NO 3 ) 3 -hexadecyl trimethyl ammonium bromide (CTAB)-NaOH. Highlights: → BiOBr microflowers constructed of nanoflakes were synthesized hydrothermally. → Bi 2 O 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.

  1. Simple hydrothermal synthesis and sintering of Na0.5Bi0.5TiO3 nanowires

    International Nuclear Information System (INIS)

    Jiang Xiangping; Lin Mei; Tu Na; Chen Chao; Zhou Shulan; Zhan Hongquan

    2011-01-01

    Highlights: → Single-crystalline NBT nanowires were synthesized using a simple hydrothermal route. → Reaction time can significantly influence the growth behavior of powders. → 1D growth mechanism of NBT corresponds to the dissolution-recrystallization mechanism. → NBT ceramics derived from nanowires showed typical characteristics of relax or ferroelectrics. - Abstract: Single-crystalline Na 0.5 Bi 0.5 TiO 3 (NBT) nanowires, with diameters of 100 nm and lengths of about 4 μm, were synthesized by using a simple hydrothermal method. Phase composition, morphology and microstructure of the as-prepared powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscope (TEM). The effects of reaction temperature and reaction time on precipitation of the NBT nanowires were investigated. It was found that reaction time significantly influenced the growth behavior of the powders in the hydrothermal system. Based on the experimental results, the one-dimensional (1D) growth mechanism of the NBT was governed by a dissolution-recrystallization mechanism. NBT ceramics derived from the nanowires showed typical characteristics of relaxor ferroelectrics, with diffuseness exponent γ of as high as 1.73.

  2. Generic supercritical water technology; Generic technology to shite no chorinkaisui riyo gijutsu

    Energy Technology Data Exchange (ETDEWEB)

    Arai, K.; Ajiri, M.; Inomata, H.; Smith, R.; Hakuta, Y. [Tohoku University, Sendai (Japan). Faculty of Engineering; Yokoyama, C. [Tohoku University, Sendai (Japan). The Institute forChemical Reaction Science; Chin, L. [New Energy and Industrial Technology Development Organization, Tokyo, (Japan)

    1997-02-01

    This paper describes the measurement and analysis for clarifying solution structure of supercritical water and exhibition mechanism of solvent functions. It also describes the development of new processes using supercritical water as reaction solvent. The PVT measurements were conducted in the supercritical region using pure water and NaCl aqueous solution, to confirm the reduction of molar volume of the electrolyte solution. The hydration structure was examined in the supercritical aqueous solution by the molecular dynamic simulation. As a result, presence of hydrogen bond structure, where the contribution of two branching hydrogen bond can not be ignored, was suggested under the supercritical condition. Characteristics of supercritical aqueous solutions are analyzed through in-situ Raman and scattered X-ray spectral measurements. Moreover, this paper introduces developments of some processes in the supercritical water, such as decomposition of wasted polymers, recovery of chemical materials, reforming of heavy hydrocarbons by contact hydrogenation, and synthesis of fine powders of metal oxide by reaction crystallization.

  3. Hydrothermal minerals

    Digital Repository Service at National Institute of Oceanography (India)

    Nath, B.N.

    and in sedimented rifts adjacent to continental margins. The hydrothermal deposits mainly occur in the tectonically active regions, where plates shift and spread creating fissures in the seafloor. Mineralization at the spreading ridges is the result of sea-floor... processes. Submarine hydrothermal circulation in the oceanic crust and its activity on the ocean floor are fundamental processes controlling the transfer of energy and material from the lithosphere to the hydrosphere. Thermally induced circulation...

  4. Synthesis, characterization and optical property of shrimps-like nanostructures of MnO2 by hydrothermal route.

    Science.gov (United States)

    Toufiq, Arbab Mohammad; Wang, Fengping; Javed, Qurat-ul-ain

    2013-04-01

    Hexagonal MnO2 shrimps like nanostructures have been successfully synthesized through a facile hydrothermal route at a temperature of 175 degrees C. The synthesized MnO2 nanostructures were characterized by the X-Ray Diffraction, Scanning Electron Microscopy, Energy Dispersive X-Ray spectroscopy, Transmission Electron Microscopy, High Resolution Transmission Electron Microscopy, Selected Area Electron Diffraction and UV-visible spectroscopy. UV-vis spectrophotometer was used to determine the absorption behaviour of shrimps like nanostructures. Direct optical band gap of 1.65 eV was acquired by using Davis-Mott model. The UV-visible spectrum exhibited the prominent absorption in visible region.

  5. Hydrothermal synthesis of hierarchical flower-like ZnO nanostructure and its enhanced ethanol gas-sensing properties

    Science.gov (United States)

    Zhu, Ling; Li, Yanqiong; Zeng, Wen

    2018-01-01

    ZnO nanoparticles, nanoplates and nanoflowers have been successfully synthesized via a facile hydrothermal route, and their microstructures and gas-sensing properties to ethanol were investigated. Among all the nanostructures, the nanoplates-assembled nanoflowers exhibited significantly higher gas-sensing performances than the others, which may ascribe to their hierarchical architectures with large specific area and abundant spaces for gas diffusion. Furthermore, we surprisingly found that the concentration of surfactant CTAB used had an essential effect on the ultimate morphology of the hierarchical nanoflowers. We hoped our findings could be in favor of further investigations on the fabrication of perfect hierarchical architectures.

  6. Template-less surfactant-free hydrothermal synthesis NiO nanoflowers and their photoelectrochemical hydrogen production

    KAUST Repository

    Qurashi, Ahsanulhaq

    2015-12-01

    A facile direct surfactant-free template-less hydrothermal method is employed for the growth of high surface-area NiO nanoflowers made up of complex and assembled nanosheets network.Field emission scanning electron microscopy revealed that each nanosheet is about 50-60nm thick. Detailed structural analysis reveals single-crystalline nature of NiO nanoflowers with cubic crystal structure. The optical absorption bands in the wavelength range of 350-800nm illustrated in terms of ligand field theory. The photoelectrochemical (PEC), water splitting performance on the NiO nanoflowers were also investigated. © 2015 Hydrogen Energy Publications, LLC.

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

    Energy Technology Data Exchange (ETDEWEB)

    Azzez, Shrook A., E-mail: shurouq44@yahoo.com [Institutes of Nano-Optoelectronic Research and Technology Laboratory (INOR), Ministry of Science and Technology, Baghdad (Iraq); Hassan, Z.; Alimanesh, M.; Rasheed, Hiba S.; Sabah, Fayroz A.; Abdulateef, Sinan A. [Institutes of Nano-Optoelectronic Research and Technology Laboratory (INOR), Ministry of Science and Technology, Baghdad (Iraq); Hassan, J. J. [Department of Physics, College of Science, University of Basrah, Basrah (Iraq)

    2016-07-06

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

  8. Biomolecule-Assisted Hydrothermal Synthesis and Self-Assembly of Bi2Te3 Nanostring-Cluster Hierarchical Structure

    DEFF Research Database (Denmark)

    Mi, Jianli; Lock, Nina; Sun, Ting

    2010-01-01

    A simple biomolecule-assisted hydrothermal approach has been developed for the fabrication of Bi2Te3 thermoelectric nanomaterials. The product has a nanostring-cluster hierarchical structure which is composed of ordered and aligned platelet-like crystals. The platelets are100 nm in diameter...... the concentration of NaOH, which plays a crucial role on the formation mechanism of Bi2Te3. An even smaller polycrystalline Bi2Te3 superstructure composed of polycrystalline nanorods with some nanoplatelets attached to the nanorods is achieved at lower NaOH concentration. The room temperature thermoelectric...

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

    Science.gov (United States)

    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.

  10. Properties of ceria doped with gadolinia via microwave-assisted hydrothermal synthesis; Propriedades de ceria dopada com gadolinia via sintese hidrotermal assistida por micro-ondas

    Energy Technology Data Exchange (ETDEWEB)

    Carregosa, J.D.C.; Oliveira, R.M.P.B. [Universidade Federal de Sergipe (UFS), Sao Cristovao, SE (Brazil); Macedo, D.A. [Universidade Federal da Paraiba (UFPB), Joao Pessoa, PB (Brazil); Nascimento, R.M., E-mail: jdcovello@hotmail.com [Universidade Federal do Rio Grande do Norte (UFRN), Natal, RN (Brazil)

    2016-07-01

    The solid solution of CeO{sub 2} doped with Gd{sup 3+} (CGO) is a promising candidate for electrolyte in Solid Oxide Full Cells (SOFCs) operating in intermediate and low temperatures. The reduction of the working temperature of these energy conversion devices is the great technological challenge to its marketing. In this work, nanocrystalline powders of Ce{sub 1-x}Gd{sub x}O{sub 2-x/2} with x=0, x=0.1 e x=0.2 were obtained via microwave-hydrothermal synthesis at low temperature and times of synthesis (10 and 20 min at 120° C). The powders were analyzed by TG-DTA, DRX and dilatometry. The results showed characteristic peaks of the cubic fluorite-type structure, referring to the cerium oxide (CeO{sub 2}), without the presence of secondary peaks. It was also observed that the samples processed at levels of 10 and 20 minutes showed distinct behaviors in contrast to the concentrations of Gd{sup 3+}. (author)

  11. Synthesis of highly disperse tetragonal BaTiO3 nanoparticles with core–shell by a hydrothermal method

    Directory of Open Access Journals (Sweden)

    Jinhui Li

    2017-12-01

    Full Text Available In order to synthesize of high-dispersion and tetragonal BaTiO3 (BT nanoparticle, a hydrothermal method is used in a mixture of chloride metal sources and KOH with polyvinylpyrrolidone (PVP. The properties of BT–PVPs prepared by different reaction temperature and time are investigated via XRD, FE-SEM, DLS, FT-IR, and TEM to clarify the changes of the crystal phase, dispersion, and particle structure. The reaction is finished at 230 °C for 24 h and the critical reaction condition for that the crystal phase of the obtained BT particle changed from the cubic to the tetragonal is found to be 190 °C fixed in reaction time 24 h, and 9 h. During reaction the PVP on the BT surface decomposed to different form, and the PVP plays the role of dispersant in aqueous solution. By the hydrothermal condition of 230 °C for 24 h almost monodisperse BT–PVP with sizes of 83 nm and tetragonality (c/a of 1.0062 were synthesized. The structure of nanoparticle, core (BT–shell (PVP was investigated by FT-IR and direct observed by TEM and the mechanism of particle growth and dispersion was discussed.

  12. Hydrothermal synthesis, structure, heterogeneous catalytic activity and photoluminescent properties of a novel homoleptic Sm(III)-organic framework

    Energy Technology Data Exchange (ETDEWEB)

    Ay, Burak [Department of Chemistry, Arts and Science Faculty,Çukurova University, 01330 Adana (Turkey); Yildiz, Emel, E-mail: eeyildiz@cu.edu.tr [Department of Chemistry, Arts and Science Faculty,Çukurova University, 01330 Adana (Turkey); Felts, Ashley C.; Abboud, Khalil A. [Department of Chemistry, University of Florida, Gainesville, FL 32611 (United States)

    2016-12-15

    A novel metal-organic framework, (H{sub 2}pip){sub n}[Sm{sub 2}(pydc){sub 4}(H{sub 2}O){sub 2}]{sub n} (1) (H{sub 2}pydc=2,6-pyridinedicarboxylic acid, H{sub 2}pip=piperazine) has been synthesized under hydrothermal conditions and characterized by the elemental analysis, inductively coupled plasma (ICP) spectrometer, fourier transform infrared (FT-IR) spectra, thermogravimetric analysis (TGA), single crystal X-ray diffraction analysis and powder X-ray diffraction (PXRD). The structure of 1 was determined to be three-dimensional, linked along Sm-O-Sm chains. The asymmetric unit consisted of one singly anionic fragment consisting of Sm(III) coordinated to two H{sub 2}pydc ligands and one water, and one half of a protonated H{sub 2}pip, which sits on an inversion center. 1 exhibited luminescence emission bands at 534 nm at room temperature when excited at 440 nm. Its thermal behavior and catalytic performance were investigated and the selectivity was measured as 100% for the oxidation of thymol to thymoquinone. - Graphical abstract: A novel 3D lanthanide-organic framework has been synthesized under hydrothermal conditions. The thermal behavior and catalytic performance of 1 were investigated and its selectivity was measured as 100% for the oxidation of thymol to thymoquinone.

  13. Development of high energy density supercapacitor through hydrothermal synthesis of RGO/nano-structured cobalt sulphide composites.

    Science.gov (United States)

    Jana, Milan; Saha, Sanjit; Samanta, Pranab; Murmu, Naresh Chandra; Kim, Nam Hoon; Kuila, Tapas; Lee, Joong Hee

    2015-02-20

    Co9S8/reduced graphene oxide (RGO) composites were prepared on nickel foam substrate through hydrothermal reaction and used directly as supercapacitor electrode. The field emission scanning electron microscopy analysis of the composites showed the formation of Co9S8 nano-rods on the RGO surfaces. The average crystal size of the Co9S8 nano rods grown on the RGO sheets were ∼25-36 nm as calculated from x-ray diffraction analysis. The reduction of graphene oxide (GO) was confirmed by Raman and x-ray photoelectron spectroscopy analysis. The electrical conductivity of the Co9S8/RGO composite was recorded as 1690 S m(-1) at room temperature, which is much higher than that of pure GO further confirming the hydrothermal reduction of GO. Cyclic voltammetry, galvanostatic charge-discharge and electrochemical impedance spectroscopy were investigated to check the electrochemical performances of the Co9S8/RGO composites. The Co9S8/RGO composites supported on nickel foam showed very high specific capacitance (Sc)(1349 F g(-1) at a current density of 2.2 A g(-1)), energy density (68.6 W h kg(-1)) and power density (1319 W kg(-1)) in 6 M KOH electrolyte. The retention in Sc of the composite electrode was found to be ∼96% after 1000 charge-discharge cycles.

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

    Science.gov (United States)

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

    2017-09-01

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

  15. Hydrothermal synthesis of HoMn{sub 2}O{sub 5} nanorods and their size-dependent magnetic properties

    Energy Technology Data Exchange (ETDEWEB)

    Lv, Yichao; Wu, Songping, E-mail: chwsp@scut.edu.cn; Xu, Rui

    2017-03-01

    The HoMn{sub 2}O{sub 5} nanorods were synthesized by a surfactant-assisted hydrothermal process. The length of nanorods is readily controllable with basically constant diameter. HoMn{sub 2}O{sub 5} nanorods show recognizable divagation at T{sub N}(Ho) of 13 K between FC and ZFC curve due to the contribution of the magnetic ordering of holmium. Size-dependent magnetic properties (i.e. a critical length for magnetization) of HoMn{sub 2}O{sub 5} nanorods can be ascribed to the competition between surface strain and uncompensated spin at the surface. - Highlights: • HoMn{sub 2}O{sub 5} nanorods were synthesized by a surfactant-assisted hydrothermal route. • HoMn{sub 2}O{sub 5} nanorods show recognizable divagation at T{sub N}(Ho) of 13 K between FC and ZFC. • Size-dependent magnetic properties of HoMn{sub 2}O{sub 5} nanorods can be observed.

  16. Synthesis of zinc aluminate with high surface area by microwave hydrothermal method applied in the transesterification of soybean oil (biodiesel)

    Energy Technology Data Exchange (ETDEWEB)

    Quirino, M.R. [Chemistry Laboratory of Federal University of Paraiba (LABQUIM), Campus III, 58200-000 Bananeiras, PB (Brazil); Oliveira, M.J.C. [Academic Unit of Materials Engineering, UFCG, Campina Grande Campus I, 58429-900 Campina Grande, PB (Brazil); Keyson, D. [Laboratory of study in Science, DME, Federal University of Paraíba, Campus I, 58051-900 João Pessoa, PB (Brazil); Lucena, G.L., E-mail: guilherme_leo1@yahoo.com.br [Chemistry Laboratory of Federal University of Paraiba (LABQUIM), Campus III, 58200-000 Bananeiras, PB (Brazil); Oliveira, J.B.L. [Federal University of Rio Grande do Norte, UFRN, Campus I, 59078-970 Natal, RN (Brazil); Gama, L. [Academic Unit of Materials Engineering, UFCG, Campina Grande Campus I, 58429-900 Campina Grande, PB (Brazil)

    2016-02-15

    Highlights: • ZnAl{sub 2}O{sub 4} spinel was synthesized by the microwave hydrothermal method in only 15 or 30 min. • The powders show high specific surface area. • ZAT{sub b}15 showed activity of 52.22% for the conversion of soybean oil into biodiesel. - Abstract: Zinc aluminate is a material with high thermal stability and high mechanical strength that, owing to these properties, is used as a catalyst or support. In this work, zinc aluminate spinel was synthesized by the microwave hydrothermal method in only 15 or 30 min at a low temperature (150 °C) without templates, using only Al(NO{sub 3}){sub 3}·9H{sub 2}O, Zn(NO{sub 3}){sub 2}·6H{sub 2}O, and urea as precursors and applied in the transesterification of soybean oil. X-ray diffraction analysis showed that ZnAl{sub 2}O{sub 4} had a cubic structure without secondary phases. The nitrogen adsorption measurements (BET) revealed a high surface area (266.57 m{sup 2} g{sup −1}) for the nanopowder synthesized in 15 min. This powder showed activity of 52.22% for the catalytic conversion of soybean oil into biodiesel by transesterification.

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

    Energy Technology Data Exchange (ETDEWEB)

    Mirnajafizadeh, Fatemeh; Ramsey, Deborah; McAlpine, Shelli [School of Chemistry, University of New South Wales, Sydney, NSW 2052 (Australia); Wang, Fan; Reece, Peter [School of Physics, University of New South Wales, Sydney, NSW 2052 (Australia); Stride, John Arron, E-mail: j.stride@unsw.edu.au [School of Chemistry, University of New South Wales, Sydney, NSW 2052 (Australia); Bragg Institute, Australian Nuclear Science and Technology Organisation, PMB 1, Menai, NSW 2234 (Australia)

    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 0.5 g/L, which makes them of potential use in biological imaging applications. - Highlights: • Highly luminescent ZnSe(S) QDs were synthesized using a simple, one-step hydrothermal method. • The as-synthesized QDs were found to be nontoxic in the presence of biological cells. • The QDs were stable in biological media with identical emission profile to that in water.

  18. The ethylene glycol template assisted hydrothermal synthesis of Co{sub 3}O{sub 4} nanowires; structural characterization and their application as glucose non-enzymatic sensor

    Energy Technology Data Exchange (ETDEWEB)

    Khun, K., E-mail: kimleang.khun@liu.se [Department of Science and Technology, Linköping University, SE-60174 Norrköping (Sweden); Ibupoto, Z.H. [Dr M.A. Kazi Institute of Chemistry, University of Sindh Jamshoro, Sindh Jamshoro (Pakistan); Liu, X. [Department of Physics, Chemistry and Biology, Linköping University, 58183 Linköping (Sweden); Beni, V. [Biosensors and Biolelectronics Centre, Department of Physics, Chemistry and Biology, Linköping University, 58183 Linköping (Sweden); Willander, M. [Department of Science and Technology, Linköping University, SE-60174 Norrköping (Sweden)

    2015-04-15

    Highlights: • Ethylene glycol assisted Co{sub 3}O{sub 4} nanowires were synthesized by hydrothermal method. • The grown Co{sub 3}O{sub 4} nanowires were used for sensitive non-enzymatic glucose sensor. • The proposed glucose sensor shows a wide linear range with fast response. • The Co{sub 3}O{sub 4} modified electrode is a highly specific enzyme-less glucose sensor. - Abstract: In the work reported herein the ethylene glycol template assisted hydrothermal synthesis, onto Au substrate, of thin and highly dense cobalt oxide (Co{sub 3}O{sub 4}) nanowires and their characterization and their application for non-enzymatic glucose sensing are reported. The structure and composition of Co{sub 3}O{sub 4} nanowires have been fully characterized using scanning electron microscopy, X-ray diffraction, high resolution transmission electron microscopy and X-ray photoelectron spectroscopy. The synthesized Co{sub 3}O{sub 4} nanowires resulted to have high purity and showed diameter of approximately 10 nm. The prepared Co{sub 3}O{sub 4} nanowires coated gold electrodes were applied to the non-enzymatic detection of glucose. The developed sensor showed high sensitivity (4.58 × 10{sup 1} μA mM{sup −1} cm{sup −2}), a wide linear range of concentration (1.00 × 10{sup −4}–1.2 × 10{sup 1} mM) and a detection limit of 2.65 × 10{sup −5} mM. The developed glucose sensor has also shown to be very stable and selective over interferents such as uric acid and ascorbic acid. Furthermore, the proposed fabrication process was shown to be highly reproducible response (over nine electrodes)

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

    International Nuclear Information System (INIS)

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

    2011-01-01

    Hydrothermal synthesis process of tobermorite (5CaO.6SiO 2 .5H 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 2 .5H 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.

  20. Facile one-step hydrothermal synthesis and luminescence properties of Eu{sup 3+}-doped NaGd(WO{sub 4}){sub 2} nanophosphors

    Energy Technology Data Exchange (ETDEWEB)

    Jiang, Zehan; Cai, Peiqing; Chen, Cuili; Pu, Xipeng; Kim, Sun Il, E-mail: sikim@pknu.ac.kr; Jin Seo, Hyo, E-mail: hjseo@pknu.ac.kr

    2017-06-01

    Eu{sup 3+}-doped NaGd(WO{sub 4}){sub 2} nanophosphors were synthesized via a facile one-step hydrothermal method without any surfactants or a further heat treatment. X-ray powder diffraction (XRD), scanning electron microscope (SEM), fourier transform infrared spectroscopy (FT-IR), the photoluminescence (PL) excitation and emission spectra, and decay curves were used to characterize NaGd(WO{sub 4}){sub 2}:Eu{sup 3+} phosphors. The results show that the Eu{sup 3+}-concentration has little influence on the structure and morphology of the as-synthesized samples. However, pH value plays a vital role on the structure and morphology of NaGd(WO{sub 4}){sub 2}. The well-crystallized sheet-like NaGd(WO{sub 4}){sub 2} phosphors can be obtained only at pH = 5–7. On the basis of the time-dependent synthesis, a possible growth mechanism of sheet-like architectures is proposed. The luminescence properties of NaGd{sub 1-x}Eu{sub x}(WO{sub 4}){sub 2} (0 ≤ x ≤ 1) are investigated. It is found that the charge transfer band of Eu{sup 3+} shifts to lower energy and broadens with increasing the Eu{sup 3+}-concentration. - Highlights: • NaGd(WO{sub 4}){sub 2}:Eu{sup 3+} nanosheets were synthesized by facile one-step hydrothermal method. • Luminescence properties of NaGd(WO{sub 4}){sub 2}:Eu{sup 3+} phosphor were firstly reported. • The CT band of Eu{sup 3+} depends strongly on Eu{sup 3+}-concentrations.

  1. Geological Model of Supercritical Geothermal Reservoir on the Top of the Magma Chamber

    Science.gov (United States)

    Tsuchiya, N.

    2017-12-01

    We are conducting supercritical geothermal project, and deep drilling project named as "JBBP: Japan Beyond Brittle Project" The temperatures of geothermal fields operating in Japan range from 200 to 300 °C (average 250 °C), and the depths range from 1000 to 2000 m (average 1500 m). In conventional geothermal reservoirs, the mechanical behavior of the rocks is presumed to be brittle, and convection of the hydrothermal fluid through existing network is the main method of circulation in the reservoir. In order to minimize induced seismicity, a rock mass that is "beyond brittle" is one possible candidate, because the rock mechanics of "beyond brittle" material is one of plastic deformation rather than brittle failure. To understand the geological model of a supercritical geothermal reservoir, granite-porphyry system, which had been formed in subduction zone, was investigated as a natural analog of the supercritical geothermal energy system. Quartz veins, hydrothermal breccia veins, and glassy veins are observed in a granitic body. The glassy veins formed at 500-550 °C under lithostatic pressures, and then pressures dropped drastically. The solubility of silica also dropped, resulting in formation of quartz veins under a hydrostatic pressure regime. Connections between the lithostatic and hydrostatic pressure regimes were key to the formation of the hydrothermal breccia veins, and the granite-porphyry system provides useful information for creation of fracture clouds in supercritical geothermal reservoirs. A granite-porphyry system, associated with hydrothermal activity and mineralization, provides a suitable natural analog for studying a deep-seated geothermal reservoir where stockwork fracture systems are created in the presence of supercritical geothermal fluids. I describe fracture networks and their formation mechanisms using petrology and fluid inclusion studies in order to understand this "beyond brittle" supercritical geothermal reservoir, and a geological

  2. Hydrothermal synthesis of α-Ni(OH){sub 2} and its conversion to NiO with electrochemical properties

    Energy Technology Data Exchange (ETDEWEB)

    Cai, Yong; Ma, Jianmin, E-mail: nanoelechem@hnu.edu.cn; Wang, Taihong, E-mail: thwang@hnu.edu.cn

    2014-01-05

    Highlights: • α-Ni(OH){sub 2} microspheres have been synthesized with triethanolamine. • The formation mechanism of α-Ni(OH){sub 2} microspheres is suggested. • NiO deriving from α-Ni(OH){sub 2} microspheres exhibits better electrochemical performances. -- Abstract: The paper reports the fabrication of microscale NiO matrixes with enhanced electrochemical properties through annealing the corresponding chrysanthemum-like α-Ni(OH){sub 2} microspheres. The precursor α-Ni(OH){sub 2} can be synthesized by a hydrothermal method using triethanolamine as the alkaline source. The formation mechanism of chrysanthemum-like α-Ni(OH){sub 2} microspheres is properly discussed. Furthermore, the electrochemical experiments demonstrate that the microscale NiO matrixes show superior electrochemical behavior in lithium-ion batteries due to their unique structures.

  3. One-pot hydrothermal synthesis of heterostructured ZnO/ZnS nanorod arrays with high ethanol-sensing properties.

    Science.gov (United States)

    Gao, Peng; Wang, Longqiang; Wang, Ying; Chen, Yujin; Wang, Xiaona; Zhang, Guoli

    2012-04-10

    ZnO/ZnS heterostructured nanorod arrays with uniform diameter and length were synthesized from zinc substrates in a one-pot procedure by using a simple hydrothermal method. Structural characterization by HRTEM indicated that the heterostructured nanorods were composed of parallel segments of wurtzite-type ZnO and zinc-blende ZnS, with a distinct interface along the axial direction, which revealed the epitaxial relationship, ZnO (1010) and ZnS (111). The as-prepared ZnO/ZnS nanorods showed only two green emissions at around 523 nm and 576 nm. We also found that the nanorods exhibited high sensitivity to ethanol at relatively low temperatures, owing to their smaller size and structure. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Synthesis of Barium Titanate (BT) Nano Particles via Hydrothermal Route for the Production of BT-Polymer Nanocomposite

    Science.gov (United States)

    Habib, A.; Haubner, R.; Jakopic, G.; Stelzer, N.

    2007-08-01

    Barium titanate (high-k dielectric material) nano-powders (approx. 30 nm to 60 nm) were synthesised using hydrothermal route under moderate conditions. Effect of temperature and time was studied using transmission electron microscopy (TEM), scanning electron microscopy (SEM) and X-ray diffraction techniques. Obtained barium titanate nano-powders were dispersed in thermoplastic polymethyl methacrylate (PMMA) to get homogeneous dispersions. Thin layers were obtained using these dispersions to achieve BaTiO3 endorsed polymer layers by dip-coating for improved polymer insulators on various substrates e.g., glass, and Au sputtered silicon wafers. SEM and focused ion beam (FIB) techniques were used to study the dispersion of barium titanate nano-particles in PMMA. The layers obtained showed homogenous distribution of BaTiO3 nano particles with no agglomeration.

  5. Hydrothermal Synthesis and Electrochemical Properties of CoS2-Reduced Graphene Oxide Nanocomposite for Supercapacitor Application

    Science.gov (United States)

    Venkateshalu, Sandhya; Rangappa, Dinesh; Grace, Andrews Nirmala

    A Cobalt disulfide-reduced graphene oxide (CoS2-RGO) nanocomposite was prepared by a simple hydrothermal method and the prepared nanocomposite was characterized using various techniques like XRD, SEM and FTIR. The results of these techniques indicated the uniform deposition of CoS2 nanoparticles on Graphene sheets. Further, the prepared nanocomposites were tested for its activity towards energy storage and the test results showed a specific capacitance of 28F/g in an aqueous 20% KOH electrolyte at a current density of 0.5A/g. All these materials showed highly reversible charge-discharge cycles. The overall electrochemical performance of this composite is shown to be drastically improved when compared to bare CoS2 nanoparticles. Thus with the good electrochemical properties, CoS2-RGO nanocomposites could be effectively used as an electrode material for supercapacitors.

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

    Science.gov (United States)

    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.

  7. Mechanochemical Effects on the Synthesis of Copper Orthophosphate and cyclo-Tetraphosphate Bulks by the Hydrothermal Hot Pressing Method

    Directory of Open Access Journals (Sweden)

    Isao Tanaka

    2009-01-01

    Full Text Available Copper orthophosphate, Cu3(PO42, and cyclo-tetraphosphates, Cu2P4O12, were synthesized using phosphoric acid and basic copper carbonate, and then treated with a planetary mill for up to 360 minutes. The un-milled and milled samples were characterized by X-ray diffraction (XRD and Fourier transform infrared (FT-IR spectroscopy. SEM images, particle size distribution, specific surface area, UV-Vis reflectance spectra were also used to evaluate the materials. The un-milled and milled materials were used to fabricate copper phosphate bulks by a hydrothermal hot pressing method. The influence of powder condition on the sintering behavior of the copper phosphates was studied.

  8. CTAB-Assisted Hydrothermal Synthesis of WO3 Hierarchical Porous Structures and Investigation of Their Sensing Properties

    Directory of Open Access Journals (Sweden)

    Dan Meng

    2015-01-01

    Full Text Available WO3 hierarchical porous structures were successfully synthesized via cetyltrimethylammonium bromide- (CTAB- assisted hydrothermal method. The structure and morphology were investigated using scanning electron microscope, X-ray diffractometer, transmission electron microscopy, X-ray photoelectron spectra, Brunauer-Emmett-Teller nitrogen adsorption-desorption, and thermogravimetry and differential thermal analysis. The result demonstrated that WO3 hierarchical porous structures with an orthorhombic structure were constructed by a number of nanoparticles about 50–100 nm in diameters. The H2 gas sensing measurements showed that well-defined WO3 hierarchical porous structures with a large specific surface area exhibited the higher sensitivity compared with products without CTAB at all operating temperatures. Moreover, the reversible and fast response to H2 gas and good selectivity were obtained. The results indicated that the WO3 hierarchical porous structures are promising materials for gas sensors.

  9. Hydrothermal synthesis and corrosion behavior of the protective coating on Mg-2Zn-Mn-Ca-Ce alloy

    Directory of Open Access Journals (Sweden)

    Dan Song

    2016-12-01

    Full Text Available Protective coatings were synthesized on the Mg-2Zn-Mn-Ca-Ce Mg alloy through the hydrothermal method with de-ionized water as the reagent. The coatings were composed of Mg hydroxide, generally uniform and compact. Hydrogen evolution tests and electrochemical tests in the Hanks’ solution demonstrated that the Mg(OH2 coatings effectively decreased the bio-degradation rate of the Mg alloy substrate. Microstructure observation showed that the coating formation on the secondary phases was more difficult than that on the α-Mg matrix, which led to micro cracks and pores on the secondary phases after drying. Over synthesizing time, the coating layer on secondary phases gradually becomes more compact and uniform. Meanwhile, owing to the thicker and more compact coatings, the corrosion resistance and protective efficiency were significantly improved with longer synthesizing time as well.

  10. Synthesis and Antibacterial Activity of Rutile-TiO2 ‎Nano Powder Prepared by Hydrothermal Process ‎

    Directory of Open Access Journals (Sweden)

    Rashed T. Rasheed ‎

    2017-11-01

    Full Text Available Rutile titanium dioxide (r-TiO2 Nano powder has been synthesized by hydrothermal method in autoclave. The reaction took place between titanium tetrachloride (TiCI4 and mixture solution consisted of deionized water and ethanol, in the ratio (3:7 respectively. The product has been dried and annealed at 400°C. The structure, morphology and the particle size of the Nano powder were investigated by X-ray Diffraction, Scanning Electron Microscopy (SEM, Atomic Force Microscope (AFM, FT-IR and UV/visible spectroscopy measurements. The effect of r-TiO2 on gram-negative bacteria Escherichia coli (E. coli and gram-positive bacteria Staphylococcus aurous (S. aureus has been studied. This study showed that rutile TiO2 Nano powder has efficient antibacterial activity, and can use as an antibacterial agent for different purposes

  11. Hydrothermal Synthesis of Pt-, Fe-, and Zn-doped SnO2 Nanospheres and Carbon Monoxide Sensing Properties

    Directory of Open Access Journals (Sweden)

    Weigen Chen

    2013-01-01

    Full Text Available Pure and M-doped (M = Pt, Fe, and Zn SnO2 nanospheres were successfully synthesized via a simple and facile hydrothermal method and characterized by X-ray powder diffraction, field-emission scanning electron microscopy, and energy dispersive spectroscopy. Chemical gas sensors were fabricated based on the as-synthesized nanostructures, and carbon monoxide sensing properties were systematically measured. Compared to pure, Fe-, and Zn-doped SnO2 nanospheres, the Pt-doped SnO2 nanospheres sensor exhibits higher sensitivity, lower operating temperature, more rapid response and recovery, better stability, and excellent selectivity. In addition, a theoretical study based on the first principles calculation was conducted. All results demonstrate the potential of Pt dopant for improving the gas sensing properties of SnO2-based sensors to carbon monoxide.

  12. Hydrothermal synthesis and electrochemical properties of Li₃V₂(PO₄)₃/C-based composites for lithium-ion batteries.

    Science.gov (United States)

    Sun, Chunwen; Rajasekhara, Shreyas; Dong, Youzhong; Goodenough, John B

    2011-09-01

    To improve performance at higher rates, we developed a hydrothermal method to prepare carbon-coated monoclinic lithium vanadium phosphate (Li(3)V(2)(PO(4))(3)) powder to be used as a cathode material for Li-ion batteries. The structural, morphological and electrochemical properties were characterized by X-ray diffraction (XRD), scanning and transmission electron microscopy (SEM and TEM), and galvanostatic charge-discharge cycling. A superior cycle and rate behavior are demonstrated for Li(3)V(1.85)Sc(0.15)(PO(4))(3)/C and Li(2.96)Ca(0.02)V(2)(PO(4))(3)/C electrodes at charge-discharge current rates above 5C.

  13. Supercritical Airfoil Coordinates

    Data.gov (United States)

    National Aeronautics and Space Administration — Rectangular Supercritical Wing (Ricketts) - design and measured locations are provided in an Excel file RSW_airfoil_coordinates_ricketts.xls . One sheet is with Non...

  14. Hydrothermal synthesis and crystal structure of a new lithium copper bismuth oxide, LiCuBiO{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Kumada, Nobuhiro, E-mail: kumada@yamanashi.ac.jp [Center for Crystal Science and Technology, University of Yamanashi, Miyamae-cho 7-32, Kofu 400-8511 (Japan); Nakamura, Ayumi [Center for Crystal Science and Technology, University of Yamanashi, Miyamae-cho 7-32, Kofu 400-8511 (Japan); Miura, Akira [Center for Crystal Science and Technology, University of Yamanashi, Miyamae-cho 7-32, Kofu 400-8511 (Japan); Faculty of Engineering, Hokkaido University, Kita 13, Nishi 8, Kita-ku, Sapporo 060-8628 (Japan); Takei, Takahiro [Center for Crystal Science and Technology, University of Yamanashi, Miyamae-cho 7-32, Kofu 400-8511 (Japan); Azuma, Masaki; Yamamoto, Hajime [Laboratory for Materials and Structures, Tokyo Institute of Technology, 4259 Nagatsuta, Midori-ku Yokohama, Kanagawa 226-8503 (Japan); Magome, Eisuke; Moriyoshi, Chikako; Kuroiwa, Yoshihiro [Department of Physical Science, Hiroshima University, 1-3-1 Kagamiyama, Higashihiroshima, Hiroshima 739-8526 (Japan)

    2017-01-15

    A new lithium copper bismuth oxide, LiCuBiO{sub 4} was prepared by hydrothermal reaction using NaBiO{sub 3}0.1*4H{sub 2}O. The crystal structural model of this compound was refined by using synchrotron X-ray powder diffraction data. This bismuthate has the LiCuSbO{sub 4} related structure with the orthorhombic cell (Space group: Pnma) of a=10.9096(9), b=5.8113(5) and c=5.0073(4) Å, and the final R-factors were R{sub wp}=4.84 and R{sub p}=3.58%. This compound is the first example of a lithium copper bismuthate containing Bi{sup 5+}. An antiferromagnetic ordering of Cu{sup 2+} moment was observed at 6 K. - Graphical abstract: In the crystal structure of LiCuBiO{sub 4} all metal atoms are coordinated octahedrally by six O atoms and LiO{sub 6} and CuO{sub 6} octahedra form the one-dimensional chains by edge-sharing along the b-axis. The LiO{sub 6} and CuO{sub 6} chains form the layer by face-sharing in the bc plane. The Bi atoms are placed in that interlayer and BiO{sub 6} octahedra are edge-sharing with LiO{sub 6} and CuO{sub 6} octahedra. - Highlights: • A new lithium copper bismuth oxide, LiCuBiO{sub 4} is prepared by hydrothermal reaction. • The crystal structure of LiCuBiO{sub 4} is closely related with that of LiCuSbO{sub 4}. • This new compound exhibits an antiferromagnetic ordering of Cu{sup 2+} moment at 6 K.

  15. Ultrafast microwave hydrothermal synthesis and characterization of Bi1−xLaxFeO3 micronized particles

    International Nuclear Information System (INIS)

    Ponzoni, C.; Cannio, M.; Boccaccini, D.N.; Bahl, C.R.H.; Agersted, K.; Leonelli, C.

    2015-01-01

    In this work a microwave assisted hydrothermal method is applied to successfully synthesize lanthanum doped bismuth ferrites (BLFO, Bi 1−x La x FeO 3 where x = 0, 0.15, 0.30 and 0.45). The growth mechanism of the Bi 1−x La x FeO 3 crystallites is discussed in detail. The existence of the single-phase perovskite structure for all the doped samples is confirmed by the X-ray powder diffraction patterns. A peak shift, observed at lower angle with increasing La doping concentration, indicates that the BiFeO 3 lattice is doped. The results of TG/DTA show a shift in the transition temperature from 805 °C to 815 °C as function of the La-doping for all the doped powders. At higher levels of La doping, i.e. x = 0.30 and 0.45, significant weight losses occur above 860 °C suggesting a change in the physical and chemical properties. Finally, magnetic measurements are carried out at room temperature for pure BiFeO 3 and Bi 0.85 La 0.15 FeO 3 . The results indicate that the materials are both weakly ferromagnetic, with no significant hysteresis in the curves. - Graphical abstract: Display Omitted - Highlights: • MW hydrothermal method applied to synthesize Bi 1−x La x FeO 3 , x = 0, 0.15, 0.30, 0.45. • A single-phase perovskite structure for all the samples was confirmed by XRD. • A T c shift in La doped BiFeO 3 DTA was observed as function of the La-doping. • Magnetic measurements indicate that the materials are weakly ferromagnetic

  16. Hydrothermal synthesis of CdTe QDs: Their luminescence quenching in the presence of bio-molecules and observation of bistable memory effect in CdTe QD/PEDOT:PSS heterostructure

    International Nuclear Information System (INIS)

    Khatei, Jayakrishna; Koteswara Rao, K.S.R.

    2011-01-01

    Highlights: · CdTe QD has been prepared by modified hydrothermal method in room ambient. · Luminescence quenching of CdTe QDs in the presence of bio-molecules demonstrated. · The CdTe QDs shows memory effect (electrical bistability). - Abstract: We report one-pot hydrothermal synthesis of nearly mono-disperse 3-mercaptopropionic acid capped water-soluble cadmium telluride (CdTe) quantum dots (QDs) using an air stable Te source. The optical and electrical characteristics were also studied here. It was shown that the hydrothermal synthesis could be tuned to synthesize nano structures of uniform size close to nanometers. The emissions of the CdTe QDs thus synthesized were in the range of 500-700 nm by varying the duration of synthesis. The full width at half maximum (FWHM) of the emission peaks is relatively narrow (40-90 nm), which indicates a nearly uniform distribution of QD size. The structural and optical properties of the QDs were characterized by transmission electron microscopy (TEM), photoluminescence (PL) and Ultraviolet-visible (UV-Vis) spectroscopy. The photoluminescence quenching of CdTe QDs in the presence of L-cysteine and DNA confirms its biocompatibility and its utility for biosensing applications. The room temperature current-voltage characteristics of QD film on ITO coated glass substrate show an electrically induced switching between states with high and low conductivities. The phenomenon is explained on the basis of charge confinement in quantum dots.

  17. Hydrothermal Processes

    Science.gov (United States)

    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

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

    Energy Technology Data Exchange (ETDEWEB)

    Torre-Fernández, Laura; Khainakova, Olena A. [Departamentos de Química Física y Analítica y Química Orgánica e Inorgánica, Universidad de Oviedo-CINN, 33006 Oviedo (Spain); Espina, Aránzazu [Servicios Científico Técnicos, Universidad de Oviedo, 33006 Oviedo (Spain); Amghouz, Zakariae, E-mail: amghouz.uo@uniovi.es [Servicios Científico Técnicos, Universidad de Oviedo, 33006 Oviedo (Spain); Khainakov, Sergei A. [Servicios Científico Técnicos, Universidad de Oviedo, 33006 Oviedo (Spain); Alfonso, Belén F.; Blanco, Jesús A. [Departamento de Física, Universidad de Oviedo, 33007 Oviedo (Spain); García, José R.; García-Granda, Santiago [Departamentos de Química Física y Analítica y Química Orgánica e Inorgánica, Universidad de Oviedo-CINN, 33006 Oviedo (Spain)

    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

  19. Hydrothermal Growth of Polyscale Crystals

    Science.gov (United States)

    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.

  20. Synthesis of barium titanate crystalline nanoparticles using hydrothermal microwave method; Obtencao de nanoparticulas cristalinas de titanato de bario usando metodo hidrotermal assistido por microondas

    Energy Technology Data Exchange (ETDEWEB)

    Souza, A.E.; Silva, R.A.; Teixeira, S.R. [Universidade Estadual Paulista (DFQB/FCT/UNESP), Presidente Prudente, SP (Brazil). Dept. de Fisica, Quimica e Biologia. Lab. de Compositos e Ceramicas Funcionais; Moreira, M.L. [Universidade Federal de Sao Carlos (LiEC/UFSCAR), SP (Brazil). Lab. Interdisciplinar de Eletroquimica e Ceramica; Volanti, D.P.; Longo, E. [Universidade Estadual Paulista (LiEC/UNESP), Araraquara, SP (Brazil). Lab. Interdisciplinar de Eletroquimica e Ceramica

    2009-07-01

    The hydrothermal microwave method (HTMW) was used in the synthesis of barium titanate (BaTiO{sub 3}) nanoparticles. The solution was prepared in deionized water by using titanium (IV) isopropoxide (C{sub 12}H{sub 28}O{sub 4}Ti), barium chloride (BaCl{sub 2}.2H{sub 2}O) and potassium hydroxide (KOH). Afterwards it was heated in an adapted conventional microwave oven. The system is composed of a temperature controller with thermocouple, a hermetic camera of reaction made of teflon, a manometer and a safety valve. The solution was heated to 140 deg C, at a 140 deg C/min heating rate, and maintained at this temperature for 40 minutes. The obtained ceramic powder was characterized by using X-ray diffraction (XRD) and field emission scanning electron microscopy (FE-SEM). The XRD data confirms the formation of a high crystalline ceramic material with perovskite structure. The FE-SEM images reveal morphologies with dimensions varying from 27 to 54 nm. (author)

  1. One-step hydrothermal synthesis of sandwich-type NiCo2S4@reduced graphene oxide composite as active electrode material for supercapacitors

    Science.gov (United States)

    Wang, Fangping; Li, Guifang; Zhou, Qianqian; Zheng, Jinfeng; Yang, Caixia; Wang, Qizhao

    2017-12-01

    A facile one step hydrothermal process is developed for the synthesis of NiCo2S4@reduced graphene oxide (NiCo2S4@RGO) composite as electrode for electrochemical supercapacitors. This NiCo2S4@RGO electrode exhibits an ultrahigh specific capacitance of 2003 F g-1 at 1 A g-1 and 1726 F g-1 at 20 A g-1 (86.0% capacitance retention from 1 A g-1 to 20 A g-1), excellent cycling stabilities (86.0% retention after 3500 cycles). Moreover, an asymmetric supercapacitor is successfully assembled by using NiCo2S4@RGO nanoparticle as the positive electrode and active carbon(AC) as the negative electrode in 2 M KOH electrolyte. The fabricated NiCo2S4@RGO//AC asymmetric supercapacitor exhibits a high energy density of 21.9 Wh kg-1 at a power density of 417.1 W kg-1 and still remains an impressive energy density of 13.5 Wh kg-1 at a large power density of 2700 W kg-1. The results demonstrate that the NiCo2S4@RGO composite is a promising electrode material as supercapacitors in energy storage.

  2. A two-step hydrothermal synthesis approach to synthesize NiCo2S4/NiS hollow nanospheres for high-performance asymmetric supercapacitors

    Science.gov (United States)

    Xu, Rui; Lin, Jianming; Wu, Jihuai; Huang, Miaoliang; Fan, Leqing; He, Xin; Wang, Yiting; Xu, Zedong

    2017-11-01

    In this work, a high-performance asymmetric supercapacitor device based on NiCo2S4/NiS hollow nanospheres as the positive electrode and the porous activated carbon as the negative electrode was successfully fabricated via a facile two-step hydrothermal synthesis approach. This NiCo2S4/NiS//activated carbon asymmetric supercapacitor achieved a high energy density of 43.7 Wh kg-1 at a power density of 160 W kg-1, an encouraging specific capacitance of 123 F g-1 at a current density of 1 mA cm-2, as well as a long-term performance with capacitance degradation of 5.2% after 3000 consecutive cycles at 1 mA cm-2. Moreover, the NiCo2S4/NiS electrode also demonstrated an excellent specific capacitance (1947.5 F g-1 at 3 mA cm-2) and an outstanding cycling stability (retaining 90.3% after 1000 cycles). The remarkable electrochemical performances may be attributed to the effect of NiS doping on NiCo2S4 which could enlarge the surface area and increase the surface roughness.

  3. High-throughput continuous hydrothermal flow synthesis of Zn-Ce oxides: unprecedented solubility of Zn in the nanoparticle fluorite lattice.

    Science.gov (United States)

    Kellici, Suela; Gong, Kenan; Lin, Tian; Brown, Sonal; Clark, Robin J H; Vickers, Martin; Cockcroft, Jeremy K; Middelkoop, Vesna; Barnes, Paul; Perkins, James M; Tighe, Christopher J; Darr, Jawwad A

    2010-09-28

    High-throughput continuous hydrothermal flow synthesis has been used as a rapid and efficient synthetic route to produce a range of crystalline nanopowders in the Ce-Zn oxide binary system. High-resolution powder X-ray diffraction data were obtained for both as-prepared and heat-treated (850 degrees C for 10 h in air) samples using the new robotic beamline I11, located at Diamond Light Source. The influence of the sample composition on the crystal structure and on the optical and physical properties was studied. All the nanomaterials were characterized using Raman spectroscopy, UV-visible spectrophotometry, Brunauer-Emmett-Teller surface area and elemental analysis (via energy-dispersive X-ray spectroscopy). Initially, for 'as-prepared' Ce(1-x)Zn(x)O(y), a phase-pure cerium oxide (fluorite) structure was obtained for nominal values of x=0.1 and 0.2. Biphasic mixtures were obtained for nominal values of x in the range of 0.3-0.9 (inclusive). High-resolution transmission electron microscopy images revealed that the phase-pure nano-CeO(2) (x=0) consisted of ca 3.7 nm well-defined nanoparticles. The nanomaterials produced herein generally had high surface areas (greater than 150 m(2) g(-1)) and possessed combinations of particle properties (e.g. bandgap, crystallinity, size, etc.) that were unobtainable or difficult to achieve by other more conventional synthetic methods.

  4. MOF-derived Cu-Pd/nanoporous carbon composite as an efficient catalyst for hydrogen evolution reaction: A comparison between hydrothermal and electrochemical synthesis

    Science.gov (United States)

    Mandegarzad, Sakineh; Raoof, Jahan Bakhsh; Hosseini, Sayed Reza; Ojani, Reza

    2018-04-01

    In this study, a novel catalyst based on Cu-Pd bimetallic nanoparticles supported on nanoporous carbon composite (NPCC) is successfully fabricated through three-step process and used as an electrocatalyst towards hydrogen evolution reaction (HER). At the first step, MOF-199 is synthesized via two distinct strategies; (1) hydrothermal (HT) and (2) electrochemical (EC). Next, the synthesized MOF-199 is used as a template in order to prepare Cu/NPCC by direct carbonization under N2 atmosphere followed by galvanic replacement reaction of Cu metals by PdII ions. All the prepared materials are characterized by X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDS), scanning electron microscopy (SEM), and nitrogen adsorption/desorption measurements. The effect of synthesis method of MOF-199 on the electrocatalytic activity of the final product towards HER is investigated. The electrochemical measurements indicate that Cu-Pd/NPCC derived from the MOF prepared by EC method (Cu-Pd/NPCC/EC) exhibits an enhanced catalytic activity towards HER in H2SO4 solution than the Cu-Pd/NPCC/HT. This improvement may be attributed to using of supporting electrolyte in the preparation of Cu-Pd/NPCC/EC.

  5. Template-free hydrothermal synthesis of beaded nanochain bundles of ZnO and their application as photoanode in dye-sensitized solar cells

    Science.gov (United States)

    Ballal, Reshma; Shinde, Manish; Waghadkar, Yogesh; Arbuj, Sudhir; Rane, Sunit; Chauhan, Ratna

    2018-02-01

    ZnO shows promising candidature as photoanode material for dye-sensitized solar cells (DSSCs) due to its high bulk electron mobility and easily tailorable geometrical structures. The objective of this study is to facilitate the development of highly porous hierarchical ZnO for enhanced power conversion efficiency in dye-sensitized solar cells (DSSC) due to its greater dye adsorption. This study investigated the influence of reaction temperatures of 120 °C (sample Z-1) and 180 °C (sample Z-2) in hydrothermal synthesis on structural, morphological and optical properties of resultant ZnO nanostructures and their performance as photoanode material in DSSCs. The synthesized beaded nanochain bundles of ZnO, with multilayered and highly ordered texture, have diameters of several micrometers. Structural and morphological analysis shows that the ZnO beaded nanochain-like architectures possess wurtzite crystalline nature. These morphological improvements (beaded nanochains) of ZnO were found to exhibit higher dye loading and conversion efficiency due to increase in the surface area while reducing charge recombination. The maximum conversion efficiency was obtained with Z-1 and Z-2 is 2.95 and 3.56% with photocurrent of 7.73 and 9.24 mA/cm2, respectively. The obtained results pertaining to the DSSC performance studies were corroborated by the impedance spectroscopy data.

  6. The green hydrothermal synthesis of nanostructured Cu2ZnSnSe4 as solar cell material and study of their structural, optical and morphological properties

    Science.gov (United States)

    Vanalakar, S. A.; Agawane, G. L.; Kamble, A. S.; Patil, P. S.; Kim, J. H.

    2017-12-01

    Cu2ZnSnSe4 (CZTSe) has attracted intensive attention as an absorber material for the thin-film solar cells due to its high absorption coefficient, direct band gap, low toxicity, and abundance of its constituent elements. In this study nanostructured CZTSe nanoparticles are prepared via green hydrothermal synthesis without using toxic solvents, organic amines, catalysts or noxious chemicals. The structural, optical, and morphological properties of CZTSe nanostructured powder were studied using X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), UV-vis absorption spectroscopy, and transmission electron microscope (TEM) techniques. Raman peaks at 170, 195, and 232 cm-1 confirm the formation of pure phase CZTSe nanostructured particles. In addition, the EDS and XPS results confirm the appropriate chemical purity of the annealed CZTSe nanoparticles. Meanwhile, the TEM analysis showed the presence of phase pure oval like CZTSe particle with size of about 80-140 nm. The UV-Vis-NIR absorption spectra analysis showed that the optical band gap of CZTSe nanostructured particles is about 1.14 eV. This band gap energy is close to the optimum value of a photovoltaic solar cell absorber material.

  7. Synthesis and Characterization of WO3/Graphene Nanocomposites for Enhanced Photocatalytic Activities by One-Step In-Situ Hydrothermal Reaction

    Directory of Open Access Journals (Sweden)

    Xiaoxiao Hu

    2018-01-01

    Full Text Available Tungsten trioxide (WO3 nanorods are synthesized on the surface of graphene (GR sheets by using a one-step in-situ hydrothermal method employing sodium tungstate (Na2WO4·2H2O and graphene oxide (GO as precursors. The resulting WO3/GR nanocomposites are characterized by X-ray diffraction, Raman spectroscopy, transmission electron microscopy, scanning electron microscopy and X-ray photoelectron spectroscopy. The results confirm that the interface between WO3 nanorod and graphene contains chemical bonds. The enhanced optical absorption properties are measured by UV-vis diffuse reflectance spectra. The photocatalytic activity of the WO3/GR nanocomposites under visible light is evaluated by the photodegradation of methylene blue, where the degradation rate of WO3/GR nanocomposites is shown to be double that of pure WO3. This is attributed to the synergistic effect of graphene and the WO3 nanorod, which greatly enhances the photocatalytic performance of the prepared sample, reduces the recombination of the photogenerated electron-hole pairs and increases the visible light absorption efficiency. Finally, the photocatalytic mechanism of the WO3/GR nanocomposites is presented. The synthesis of the prepared sample is convenient, direct and environmentally friendly. The study reports a highly efficient composite photocatalyst for the degradation of contaminants that can be applied to cleaning up the environment.

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

    Science.gov (United States)

    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.

  9. Hydrothermal synthesis and enhanced photocatalytic activity of mixed-phase TiO2 powders with controllable anatase/rutile ratio

    Science.gov (United States)

    Wang, Qi; Qiao, Zhi; Jiang, Peng; Kuang, Jianlei; Liu, Wenxiu; Cao, Wenbin

    2018-03-01

    In this study, mixed-phase TiO2 powders were novelly synthesized via a facile and mild hydrothermal method without any post-heat treatment. TiOSO4 and peroxide titanic acid (PTA) were used as inorganic titanium sources, while no special solvent or additive were introduced. The XRD and TEM results showed the mixed-phase TiO2 powders were composed of anatase and rutile phases, and the PTA sol played an important role on forming the rutile nucleus. The proportion of rutile in the mixed-phase TiO2 could be easily controlled in the range of 0%-70.5% by changing the amount of PTA sol used in the synthesis process. The UV-Visible absorption spectra indicated the prepared mixed-phase TiO2 showed enhanced visible light absorption with the increase of rutile ratio. The photodegradation experiments revealed the mixed-phase TiO2 exhibited the best photocatalytic activity at the rutile ratio of 41.5%, while a higher or lower rutile ratio both resulted in the decrease of photocatalytic activity.

  10. Self-assembly of hollow MoS2 microflakes by one-pot hydrothermal synthesis for efficient electrocatalytic hydrogen evolution

    Science.gov (United States)

    Chen, Aishi; Cui, Renjie; He, Yanna; Wang, Qi; Zhang, Jian; Yang, Jianping; Li, Xing'ao

    2017-07-01

    Molybdenum disulfide (MoS2) has emerged as a promising non-precious metal catalyst for hydrogen evolution reaction (HER) in recent years. Some strategies including nanotechnology as well as atom doping have been employed in the preparing of electrocatalysts for high-activity and stability. To the best of our knowledge, hollow MoS2 microflakes assembled from ultrathin nanosheets have not been prepared previously. In this work, a simple, facile and environmentally friendly hydrothermal synthesis was utilized for the fabrication of hollow MoS2 microflakes for the first time. The unique hollow structures have fascinating properties, such as the large surface and low density. The morphology and structure of MoS2 microflakes were confirmed by XRD, SEM, TEM and Raman. The composition of these materials was identified by the X-ray photoelectron spectroscopy. Notably, the as-prepared hollow MoS2 microflakes showed better electrocatalytic activity than other samples. The hollow flake-like structure can not only increase the active edge sites owing to the large specific surface area, but also enhance the electron transport to improve the electrocatalytic activity. Benefiting from these factors, the hollow MoS2 microflakes exhibited electrocatalytic activity and excellent stability with a low overpotential about 85 mV and a Tafel slope of 59 mV per decade.

  11. In-Situ Hydrothermal Synthesis of Bi-Bi2O2CO3 Heterojunction Photocatalyst with Enhanced Visible Light Photocatalytic Activity

    Science.gov (United States)

    Kar, Prasenjit; Maji, Tuhin Kumar; Nandi, Ramesh; Lemmens, Peter; Pal, Samir Kumar

    2017-04-01

    Bismuth containing nanomaterials recently received increasing attention with respect to environmental applications because of their low cost, high stability and nontoxicity. In this work, Bi-Bi2O2CO3 heterojunctions were fabricated by in-situ decoration of Bi nanoparticles on Bi2O2CO3 nanosheets via a simple hydrothermal synthesis approach. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high-resolution TEM (HRTEM) were used to confirm the morphology of the nanosheet-like heterostructure of the Bi-Bi2O2CO3 composite. Detailed ultrafast electronic spectroscopy reveals that the in-situ decoration of Bi nanoparticles on Bi2O2CO3 nanosheets exhibit a dramatically enhanced electron-hole pair separation rate, which results in an extraordinarily high photocatalytic activity for the degradation of a model organic dye, methylene blue (MB) under visible light illumination. Cycling experiments revealed a good photochemical stability of the Bi-Bi2O2CO3 heterojunction under repeated irradiation. Photocurrent measurements further indicated that the heterojunction incredibly enhanced the charge generation and suppressed the charge recombination of photogenerated electron-hole pairs.

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

    International Nuclear Information System (INIS)

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

    2011-01-01

    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, N 2 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.

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

    International Nuclear Information System (INIS)

    Guan, Lei; Wang, Ying

    2015-01-01

    A novel cobalt phosphonate, [Co(HL)(H 2 O) 3 ] n (1) (L=N(CH 2 PO 3 H) 3 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 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

  14. Hydrothermal synthesis, characterization, photocatalytic activity and dye-sensitized solar cell performance of mesoporous anatase TiO2 nanopowders

    International Nuclear Information System (INIS)

    Pavasupree, Sorapong; Jitputti, Jaturong; Ngamsinlapasathian, Supachai; Yoshikawa, Susumu

    2008-01-01

    Mesoporous anatase TiO 2 nanopowder was synthesized by hydrothermal method at 130 deg. C for 12 h. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected-area electron diffraction (SAED), HRTEM, and Brunauer-Emmett-Teller (BET) surface area. The as-synthesized sample with narrow pore size distribution had average pore diameter about 3-4 nm. The specific BET surface area of the as-synthesized sample was about 193 m 2 /g. Mesoporous anatase TiO 2 nanopowders (prepared by this study) showed higher photocatalytic activity than the nanorods TiO 2 , nanofibers TiO 2 mesoporous TiO 2 , and commercial TiO 2 nanoparticles (P-25, JRC-01, and JRC-03). The solar energy conversion efficiency (η) of the cell using the mesoporous anatase TiO 2 was about 6.30% with the short-circuit current density (Jsc) of 13.28 mA/cm 2 , the open-circuit voltage (Voc) of 0.702 V and the fill factor (ff) of 0.676; while η of the cell using P-25 reached 5.82% with Jsc of 12.74 mA/cm 2 , Voc of 0.704 V and ff of 0.649

  15. Synthesis of CaCu3Ti4O12 by modified Sol-gel method with Hydrothermal process

    Science.gov (United States)

    Masingboon, C.; Rungruang, S.

    2017-09-01

    CaCu3Ti4O12 powders were synthesized by modified Sol-gel method with Hydrothermal process using Ca(NO3)2· 4H2O, Cu(NO3)2·3H2O, Ti(OC3H7)4 and freshly extracted egg white (ovalbumin) in aqueous medium. The precursor was calcined at 800, 900 and 1000 °C in air for 8 h to obtain nanocrystalline powders of CaCu3Ti4O12. The calcined CaCu3Ti4O12 powders were characterized by XRD, TEM and EDX. The XRD results indicated that all calcined samples have a typical perovskite CaCu3Ti4O12 structure and a small amount of CaTiO3, CuO and TiO2. TEM micrographs showed particle size 100 - 500 nm and EDX results showed elements of CaCu3Ti4O12 powders have calcium, copper, titanium and oxygen.

  16. Hydrothermal synthesis of Mn-doped ZnCo2O4 electrode material for high-performance supercapacitor

    Science.gov (United States)

    Mary, A. Juliet Christina; Bose, A. Chandra

    2017-12-01

    Mn-doped ZnCo2O4 nanoparticle has been synthesized by hydrothermal method without adding any surfactants. Structural, morphological and electrochemical performances have been studied for the pure and various concentration of Mn-doped ZnCo2O4 nanoparticles. XRD and Raman studies demonstrate the crystalline structure of the material. Specific capacitance of the 10 wt% Mn doped ZnCo2O4 nanomaterial is analysed using the three-electrode system. 10 wt% Mn-doped ZnCo2O4 has a maximum capacitance of 707.4 F g-1 at a current density of 0.5 A g-1. Coulombic efficiency of the material is 96.3% for 500 cycles in the KOH electrolyte medium. A two-electrode device using 10 wt% Mn-doped ZnCo2O4 exhibits the highest specific capacitance of 6.5 F g-1 at a current density of 0.03 A g-1 which is the suitable material for supercapacitor application.

  17. Hydrothermal synthesis and crystal Structure of a new coordination polymer: [Zn1(deta(btec(H2O2]n

    Directory of Open Access Journals (Sweden)

    Manel Halouani

    2013-05-01

    Full Text Available A new metal–organic compound [Zn1(deta(btec(H2O2]n where (deta= Diethylenetriamine and (btec= benzenetetracarboxylic acid (I was hydrothermally synthesized from an aqueous solution of Zn(NO32 6H2O, (deta and (btec. Compound I crystallizes in the monoclinic system with the P21/c space group. The unit cell parameters are a= 9.6716(5Å, b= 14.3776(8Å, c= 13.5306(8Å, β= 105.311(3°, Z= 4, V= 1814.71(18 Å3 and Dx= 1.657 g/cm3. The refinement converged into R= 0.045, Rw= 0.048. The structure, determined by single crystal X-ray diffraction, consists of a network of ZnO4 centers, tetrahedrally coordinated by pyromellitate anions giving rise to a two-dimensional sheet structure. The connectivity resembles a 4-connected network in which each Zn atom is connected to four btec anions and each btec anion is linked to four Zn2+ ions.

  18. One-Pot Template-Free Hydrothermal Synthesis of Monoclinic Hollow Microspheres and Their Enhanced Visible-Light Photocatalytic Activity

    Directory of Open Access Journals (Sweden)

    Bei Cheng

    2012-01-01

    Full Text Available Monoclinic-phase BiVO4 hollow microspheres with diameters of about 2–4 μm have been successfully fabricated in high yield by a one-pot template-free hydrothermal route. The reaction duration and urea concentration are shown to play important roles in the formation of the BiVO4 hollow microspheres. X-ray diffraction, scanning electron microscopy, nitrogen adsorption-desorption isotherms, fourier transform infrared spectrometry, and UV-visible diffuse reflectance spectroscopy are used to characterize the products. The results show that all the as-prepared BiVO4 samples have monoclinic phase structure and exhibit good crystallinity. A formation mechanism for the BiVO4 hollow spherical structure via a localized Ostwald ripening is proposed based on the experimental observations. In addition, studies of the photocatalytic properties by exposure to visible light irradiation demonstrate that the as-obtained BiVO4 hollow spheres show potential photocatalytic application. Hydroxyl radicals (•OH are not detected on the surface of visible-light-illuminated BiVO4 by the photoluminescence technique, suggesting that •OH is not the dominant photooxidant and photogenerated hole could directly take part in photocatalytic reaction. The prepared BiVO4 hollow spheres are also of great interest in pigment, catalysis, separation technology, biomedical engineering, and nanotechnology.

  19. Synthesis and characterization of SrFe{sub 12}O{sub 19} powder obtained by hydrothermal process

    Energy Technology Data Exchange (ETDEWEB)

    Jean, Malick, E-mail: malick.jean@univ-rouen.f [Groupe de Physique des Materiaux, UMR CNRS 6634, Universite de Rouen, 76801 St Etienne du Rouvray (France); Nachbaur, Virginie; Bran, Julien; Le Breton, Jean-Marie [Groupe de Physique des Materiaux, UMR CNRS 6634, Universite de Rouen, 76801 St Etienne du Rouvray (France)

    2010-04-30

    We have synthesized strontium hexaferrite particles in an alkaline medium using a hydrothermal process at 180 {sup o}C. Our results show that to obtain a quasi-single SrFe{sub 12}O{sub 19} phase, the Fe/Sr ratio in the initial solution must be equal to 8. However, the powders obtained contain traces of {alpha}-Fe{sub 2}O{sub 3} and SrCO{sub 3}. The SrFe{sub 12}O{sub 19} hexaferrite particles are hexagonal-shaped platelets about 2 {mu}m wide and 40 nm thick. When heated to 1000 {sup o}C, SrCO{sub 3} reacts with SrFe{sub 12}O{sub 19} to give Sr{sub 4}Fe{sub 6}O{sub 13}. According to XRD analysis, Moessbauer spectrometry and magnetic measurements, the magnetization axis of the single-phase SrFe{sub 12}O{sub 19} particle is perpendicular to the platelets. For an Fe/Sr ratio higher than 8, the {alpha}-Fe{sub 2}O{sub 3} phase becomes the major phase and for a ratio lower than 8, the amount of SrCO{sub 3} increases. For an Fe/Sr ratio equal to 5, the formation of the Sr{sub 3}Fe{sub 2}(OH){sub 12} phase is also observed.

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

    Science.gov (United States)

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

    2015-01-30

    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.

  1. Hydrothermal Synthesis and Structural Characterization of NiO/SnO2 Composites and Hydrogen Sensing Properties

    Directory of Open Access Journals (Sweden)

    Chao Wei

    2015-01-01

    Full Text Available Pure SnO2 and NiO doped SnO2 nanostructures were successfully synthesized via a simple and environment-friendly hydrothermal method. X-ray powder diffraction (XRD, scanning electron microscopy (SEM, energy dispersive X-ray spectroscopy (EDS, and X-ray photoelectron spectra (XPS were used to investigate the crystalline structures, surface morphologies and microstructures, and element components and their valences of the as-synthesized samples. Furthermore, planar chemical gas sensors based on the synthesized pure SnO2 and NiO/SnO2 composites were fabricated and their sensing performances to hydrogen, an important fault characteristic gas dissolved in power transformer oil, were investigated in detail. Gas sensing experiments indicate that the NiO/SnO2 composites showed much higher gas response and lower working temperature than those of pure SnO2, which could be ascribed to the formation of p-n heterojunctions between p-type NiO and n-type SnO2. These results demonstrate that the as-synthesized NiO/SnO2 composites a promising hydrogen sensing material.

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

    Science.gov (United States)

    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. Carbon Nitride Decorated Ball-Flower like Co3O4 Hybrid Composite: Hydrothermal Synthesis and Ethanol Gas Sensing Application

    Directory of Open Access Journals (Sweden)

    Yuxiao Gong

    2018-02-01

    Full Text Available Recently, semiconducting metal oxide (SMO gas sensors have attracted the attention of researchers for high conductivity, labile features by environment, low cost, easy preparation, etc. However, traditional SMOs have some defects such as higher operating temperature and lower response value, which greatly limit their application in the field of gas sensor. In this work, the carbon nitride decorated ball-flower like Co3O4 composite was successfully synthesized via a facile hydrothermal method, the composition and morphology of the as-synthesized samples were studied by the techniques of X-ray powder diffraction (XRD, Field-emission scanning electron microscopy (FESEM, Transmission electron microscopy (TEM, Fourier transform infrared spectrometer (FT-IR and N2-sorption. As a consequence, the pure Co3O4 and the carbon nitride decorated Co3O4 both possess ball-flower like structure, and the as-synthesized carbon nitride decorated Co3O4 composite exhibits significant sensing properties to ethanol which is 1.6 times higher than that of pure Co3O4, furthermore, the composite possesses high selectivity and stability towards ethanol detection.

  4. Hydrothermal synthesis, crystal structures, and luminescent properties of a series of new lanthanide oxalatophosphonates with a layer architecture.

    Science.gov (United States)

    Zhu, Yan-Yu; Sun, Zhen-Gang; Tong, Fei; Liu, Zhong-Min; Huang, Cui-Ying; Wang, Wei-Nan; Jiao, Cheng-Qi; Wang, Cheng-Lin; Li, Chao; Chen, Kai

    2011-05-28

    Eleven new lanthanide oxalatophosphonate hybrids with a 2D layered structures, namely, [Ln(H(3)L)(C(2)O(4))]·2H(2)O (Ln = La-Dy, Er and Y, H(4)L = C(6)H(5)CH(2)N(CH(2)PO(3)H(2))(2)), have been synthesized under hydrothermal conditions and structurally characterized by X-ray single-crystal diffraction, X-ray powder diffraction, infrared spectroscopy, elemental analysis and thermogravimetric analysis. Compounds 1-11 are isomorphous and they exhibit a 2D framework structure. Two {LnO(8)} polyhedra and four {CPO(3)} tetrahedra are interconnected into a unit via corner-sharing, and the so-built units are bridged by the oxalate anions into a layer. The result of connections in this manner is the formation of a 24-atom window. The thermal stabilities and guest desorption-sorption properties of compounds 1-11 have been investigated. The luminescent properties of compounds 5, 6, 8 and 9 have also been studied.

  5. Facile Hydrothermal Synthesis of Monodispersed MoS2 Ultrathin Nanosheets Assisted by Ionic Liquid Brij56

    Directory of Open Access Journals (Sweden)

    Guan-Qun Han

    2015-01-01

    Full Text Available Monodispersed MoS2 ultrathin nanosheets have been successfully fabricated by a facile hydrothermal process assisted by ionic liquid Brij56. The effect of Brij56 on the morphology and structure of MoS2 has been obviously observed. XRD shows that the as-prepared MoS2 assisted by Brij56 has the weak and broad peak of (002 planes, which implies the small size and well dispersed structure of MoS2 nanosheets. TEM and SEM images reveal that MoS2 ultrathin nanosheets have small size and few stacking layers with the adding of Brij56. HRTEM images prove that MoS2 appears to have a highly monodispersed morphology and to be monolayer ultrathin nanosheets with the length about 5–8 nm, which can provide more exposed rims and edges as active sites for hydrogen evolution reaction. Brij56 has played a crucial role in preparing monodispersed MoS2 ultrathin nanosheets as excellent electrocatalysts. The growth mechanism of monodispersed MoS2 has been discussed in detail.

  6. Hydrothermal Synthesis and Up-Conversion Luminescence of Yb3+/Ho3+ Co-doped Y6WO12 Nanocrystals

    Science.gov (United States)

    Rao, Weifeng; Zhu, Qiansheng; Ren, Qiang; Wu, Chenchen; Miao, Juhong

    2017-08-01

    Yb3+/Ho3+ co-doped Y6WO12 nanocrystals with different concentrations of Ho3+ ions have been synthesized through a facile hydrothermal method followed by a subsequent heat treatment. The nanostructures, morphologies, and up-conversion luminescent properties of the as-prepared Y6WO12:Yb3+/Ho3+ nanocrystals were investigated by powder x-ray diffraction (XRD), scanning electron microscopy (SEM), and photoluminescence spectra. XRD results indicate that all the diffraction peaks of the samples match well with the cubic phase of Y6WO12. SEM images demonstrate that the samples consist of spherical-like nanoparticles ranging in size from about 30 nm to 50 nm, which increases slightly with the increase of sintering temperature. Under the excitation of a 980 nm diode laser, the as-prepared nanocrystals show bight red and green luminescence, which is attributed to the transition of 5F5 → 5I8 and 5F4, 5S2 → 5I8 of Ho3+, respectively. With the elevation of the heat treatment temperature from 700°C to 900°C, the up-conversion emission intensity goes up significantly. Additionally, the decay lifetimes data follow a bi-exponential nature. Both the emission intensity (red and green) and their corresponding decay lifetimes increase with increasing Ho3+ concentration, maximizing at 1.0 mol.%, and then decrease, which is mainly attributed to the concentration quenching effect.

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

    Science.gov (United States)

    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.

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

    Directory of Open Access Journals (Sweden)

    Ezzaldeen Younes Jomma

    2016-02-01

    Full Text Available 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.

  9. Hydrothermal synthesis of single-walled carbon nanotube–TiO{sub 2} hybrid and its photocatalytic activity

    Energy Technology Data Exchange (ETDEWEB)

    Dai, Ke, E-mail: dk@mail.hzau.edu.cn [College of Resources and Environment, Huazhong Agricultural University, Wuhan 430070 (China); Zhang, Xiaohu; Fan, Ke; Peng, Tianyou [College of Chemistry and Molecular Science, Wuhan University, Wuhan 430072 (China); Wei, Bingqing [Department of Mechanical Engineering, University of Delaware, Newark, DE 19716 (United States)

    2013-04-01

    A single-walled carbon nanotube (SWCNT)–TiO{sub 2} hybrid was prepared hydrothermally by direct growth of TiO{sub 2} nanoparticles on the surface of functionalized SWCNTs to develop highly efficient photocatalysts. The SWCNT–TiO{sub 2} hybrid was characterized by X-ray diffraction, electron microscopy, N{sub 2}-adsorption analysis, FT-IR, Raman, and UV–vis spectroscopy. The photocatalytic activity of the SWCNT–TiO{sub 2} hybrid was examined by the photocatalytic degradation of pirimicarb. Although the SWCNT–TiO{sub 2} hybrid exhibits no visible-light-induced activity, the photocatalytic degradation efficiency of pirimicarb over TiO{sub 2} can be increased significantly with the introduction of SWCNTs (2–3 times) because SWCNTs can act as electron conductors that hinder the recombination of photo-generated electrons and holes. Compared with a multi-walled carbon nanotube–TiO{sub 2} hybrid, it can be found that the electronic configurations of carbon nanotubes significantly affect the photocatalytic activity of carbon nanotube–TiO{sub 2} hybrid. Metal-typed SWCNTs act more as an electrical conductor than a photosensitizer, which efficiently suppress charge recombination, improve interfacial charge transfer, and improve the photoactivity.

  10. Synthesis and Characterization of Flower-Like Bundles of ZnO Nanosheets by a Surfactant-Free Hydrothermal Process

    Directory of Open Access Journals (Sweden)

    Jijun Qiu

    2014-01-01

    Full Text Available Flower-like bundles of ZnO nanosheets have been prepared by using preheating hydrothermal process without any surfactants. The flower-like bundles consist of many thin and uniform hexagonal-structured ZnO nanosheets, with a thickness of 50 nm. The selected area electronic diffraction (SAED and high-resolution transmission electron microscope (HRTEM images indicate that the ZnO nanosheets are single crystal in nature. The growth mechanism of the flower-like bundles of ZnO nanosheets is discussed based on the morphology evolution with growth times and reaction conditions. It is believed that the formation of flower-like bundles of ZnO nanosheets is related to the shielding effect of OH− ions and the self-assembly process, which is dominated by a preheating time. Room temperature photoluminescence spectra results show that the annealing atmosphere strongly affects the visible emission band, which is sensitive to intrinsic and surface defects, especially oxygen interstitials, in flower-like bundles of ZnO nanosheets.

  11. Hydrothermal synthesis, magnetic and electromagnetic properties of hexagonal Fe{sub 3}O{sub 4} microplates

    Energy Technology Data Exchange (ETDEWEB)

    Ma, Fei-Xiang [School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China); MOE Key Laboratory of Micro-system and Micro-structures Manufacturing, Harbin Institute of Technology, Harbin 150080 (China); Sun, Xue-Yin [School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China); He, Kai [Department of Materials Science and Engineering, University of Maryland, College Park, MD 20742 (United States); Jiang, Jian-Tang [School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China); Zhen, Liang [School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China); MOE Key Laboratory of Micro-system and Micro-structures Manufacturing, Harbin Institute of Technology, Harbin 150080 (China); Xu, Cheng-Yan, E-mail: cy_xu@hit.edu.cn [School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China); MOE Key Laboratory of Micro-system and Micro-structures Manufacturing, Harbin Institute of Technology, Harbin 150080 (China)

    2014-06-01

    Magnetite (Fe{sub 3}O{sub 4}), with an inverse spinel structure, grows naturally in octahedral shape with eight equivalent {111} crystallographic planes. Here we demonstrated the successful morphology tuning of Fe{sub 3}O{sub 4} microcrystal from the dominant octahedral shape to planar microplate shape by a facile hydrothermal method. The top and bottom surfaces of Fe{sub 3}O{sub 4} microplates obtained under strongly alkaline and reductive conditions were bounded by {111} facets, and the formation of {111} twin planes was thought to be accountable for the anisotropic morphologies. The obtained Fe{sub 3}O{sub 4} microplates delivered saturation magnetization (M{sub s}) of 96.6 emu/g and coercivity (H{sub c}) of 50 Oe. We also measured the electromagnetic properties of Fe{sub 3}O{sub 4} microplates for possible applications as filler for electromagnetic wave absorption coatings. - Highlights: • Single-crystal Fe{sub 3}O{sub 4} microplates with well-defined hexagonal shapes were successfully prepared. • Formation of twin planes was accountable for the anisotropic growth of Fe{sub 3}O{sub 4} microplates. • Fe{sub 3}O{sub 4} microplates showed potential applications as filler for EMA coatings.

  12. Hydrothermal synthesis, structural characteristics, and enhanced photocatalysis of SnO(2)/alpha-Fe(2)O(3) semiconductor nanoheterostructures.

    Science.gov (United States)

    Niu, Mutong; Huang, Feng; Cui, Lifeng; Huang, Ping; Yu, Yunlong; Wang, Yuansheng

    2010-02-23

    Branched SnO(2)/alpha-Fe(2)O(3) semiconductor nanoheterostructures (SNHs) of high purity were synthesized by a low-cost and environmentally friendly hydrothermal strategy, through crystallographic-oriented epitaxial growth of the SnO(2) nanorods onto the alpha-Fe(2)O(3) nanospindles and nanocubes, respectively. It was demonstrated that the SnO(2) nanorods would change their preferential growth direction on the varied alpha-Fe(2)O(3) precursors with distinct crystallographic surface, driven by decrease in the distortion energy induced by lattice mismatch at the interfaces. All of the prepared SNHs were of high purity, ascribing to the successful preinhibition of the SnO(2) homonucleation in the reaction system. Significantly, some of the SnO(2)/alpha-Fe(2)O(3) SNHs exhibited excellent visible light or UV photocatalytic abilities, remarkably superior to their alpha-Fe(2)O(3) precursors, mainly owing to the effective electron-hole separation at the SnO(2)/alpha-Fe(2)O(3) interfaces.

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

    Science.gov (United States)

    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.

  14. Hydrothermal synthesis of In2S3/g-C3N4 heterojunctions with enhanced photocatalytic activity.

    Science.gov (United States)

    Xing, Chaosheng; Wu, Zhudong; Jiang, Deli; Chen, Min

    2014-11-01

    Graphitic carbon nitride (g-C3N4) was hybridized by In2S3 to form a novel In2S3/g-C3N4 heterojunction photocatalyst via a hydrothermal method. TEM and HRTEM results reveal that In2S3 nanoparticles and g-C3N4 closely contact with each other to form an intimate interface. The as-obtained In2S3/g-C3N4 heterojunctions exhibit higher photocatalytic activity than those of pure g-C3N4 and In2S3 for the photodegradation of rhodamine B (RhB) under visible light irradiation. The enhanced photocatalytic performance of In2S3/g-C3N4 heterojunctions could be attributed to its wide absorption in the visible region and efficient electron-hole separation. On the basis of radical scavenger experiments, superoxide radicals and holes are suggested to play a critical role in RhB degradation over In2S3/g-C3N4 heterojunctions. Copyright © 2014 Elsevier Inc. All rights reserved.

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Zhao Qinfu [Department of Pharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No.103, Wenhua Road, Shenyang 110016 (China); Wang Tianyi [Department of Clinical Pharmacy, School of Pharmacy, Shenyang Pharmaceutical University, No.103, Wenhua Road, Shenyang 110016 (China); Wang Jing [Department of Physical Chemistry, School of Basic Science, Shenyang Pharmaceutical University, No.103, Wenhua Road, Shenyang 110016 (China); Zheng Li; Jiang, Tongying; Cheng Gang [Department of Pharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No.103, Wenhua Road, Shenyang 110016 (China); Wang Siling, E-mail: silingwang@syphu.edu.cn [Department of Pharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No.103, Wenhua Road, Shenyang 110016 (China)

    2011-09-15

    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, N{sub 2} 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. Hydrothermal synthesis and characterization of micro/nanostructured ZnSn(OH){sub 6}/ZnO composite architectures

    Energy Technology Data Exchange (ETDEWEB)

    Yu, Xiujun; Lu, Hongxia; Zhao, Yunlong; Zhang, Liwei; Fan, Bingbing; Chen, Deliang; Wang, Hailong; Xu, Hongliang [School of Materials Science and Engineering, Zhengzhou University, Zhengzhou 450002 (China); Li, Qi [School of Information Engineering, Zhengzhou University, Zhengzhou 450002 (China); Zhang, Rui [School of Materials Science and Engineering, Zhengzhou University, Zhengzhou 450002 (China); Zhengzhou Institute of Aeronautical Industry Management, Zhengzhou 450015 (China)

    2011-11-15

    Micro/nanostructured ZnSn(OH){sub 6}/ZnO composite architectures were synthesized through a simple one-step hydrothermal method. Phase structure and morphology of the products were characterized by using X-ray diffraction (XRD), scanning electron microscope (SEM) and transmission electron microscope (TEM). ZnSn(OH){sub 6} microcubes and ZnO nanorods with uniform size were interconnected to form the micro/nanostructured architectures. ZnO nanorods preferentially grow at edges and corners of the microcubes. Morphology of the products was susceptible to concentration of the reactants. With increasing reactant concentration, the ZnO nanorods grown on the surfaces of ZnSn(OH){sub 6} microcubes disappeared. Meanwhile, the smooth surfaces of the ZnSn(OH){sub 6} microcubes become coarsened and were etched to spherical outlines. Growth mechanism of the micro/nanostructured ZnSn(OH){sub 6}/ZnO composite architectures was discussed and thermal decomposition properties of the micro/nanostructured ZnSn(OH){sub 6}/ZnO composite architectures at high temperature were examined. (copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  18. Hydrothermal Synthesis of Al/Cr-doped V6O13 as Cathode Material for Lithium-ion Battery

    Directory of Open Access Journals (Sweden)

    Yuan Qi

    2017-01-01

    Full Text Available Pure V6O13 and Al/Cr-doped V6O13 were synthesized via a hydrothermal route using C2H2O4·2H2O, V2O5, Al(NO33·9H2O and Cr(NO33·9H2O as raw materials. The products were characterized by XRD, SEM, EDS. Doping proven to be an effective method to improve the samples discharge specific capacity and cycle performance. Doping samples electrochemical performance were better than pure V6O13, the initial discharge specific capacity of sample 0.02 and 0.06 were 311mAh/g and 337mAh/g larger than pure V6O13 sample (241 mAh/g. The capacity retention of samples 0.00, 0.02, 0.06 was 32.0%, 44.69%, 28.78% after 100 cycles, respectively. The increased electrochemical performance originated from the enhanced of electrical conductivity and adhered together by stacking region in an regular arrangement with every unit.

  19. Microbial-Physical Synthesis of Fe and Fe3O4 Magnetic Nanoparticles Using Aspergillus niger YESM1 and Supercritical Condition of Ethanol

    Directory of Open Access Journals (Sweden)

    Mai Abdeen

    2016-01-01

    Full Text Available Magnetic Fe and Fe3O4 (magnetite nanoparticles are successfully synthesized using Aspergillus niger YESM 1 and supercritical condition of liquids. Aspergillus niger is used for decomposition of FeSO4 and FeCl3 to FeS and Fe2O3, respectively. The produced particles are exposed to supercritical condition of ethanol for 1 hour at 300°C and pressure of 850 psi. The phase structure and the morphology measurements yield pure iron and major Fe3O4 spherical nanoparticles with average size of 18 and 50 nm, respectively. The crystal size amounts to 9 nm for Fe and 8 nm for Fe3O4. The magnetic properties are measured to exhibit superparamagnetic- and ferromagnetic-like behaviors for Fe and Fe3O4 nanoparticles, respectively. The saturation magnetization amounts to 112 and 68 emu/g for Fe and Fe3O4, respectively. The obtained results open new route for using the biophysical method for large-scale production of highly magnetic nanoparticles to be used for biomedical applications.

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

    Science.gov (United States)

    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. Copyright © 2016. Published by Elsevier B.V.

  1. Single step hydrothermal synthesis of carbon nanodot decorated V2O5 nanobelts as hybrid conducting material for supercapacitor application

    Science.gov (United States)

    Narayanan, Remya

    2017-09-01

    Carbon nanodot (C-dot) decorated V2O5 (C-dot@V2O5) nanobelts are synthesized by single step, low cost hydrothermal route at low temperature by using V2O5 and glucose as precursors. We have not added any extra organic solvents or surfactants which are commonly used for the preparation of different nanostructures of V2O5. Electron microscopy analyses demonstrate that C-dot is entrapped inside V2O5 nanobelts which in turn enhance the conductivity and ion propagation property of this composite material. The C-dot@V2O5 nanobelts exhibit an excellent three electrode electrochemical performance in 1 M Na2SO4 and which showed a specific capacitance of 270 F g-1 at 1 A g-1, which is 4.5 times higher than the pristine V2O5 electrode. The electrochemical energy storage capacity of this hybrid is investigated towards solid state supercapacitor application also for the first time by employing electrophoretically deposited C-dot as the counter electrode and Li based gel as the electrolyte. The hybrid material delivers an energy density of 60 W h kg-1 and a reasonably high power density of 4.1 kW kg-1 at 5 A g-1 and good cycling stability and capacitance retention of about 87% was observed even after 5000 cycles. Above mentioned results clearly show that C-dot embedded hybrid, nanostructured transition metal oxides has great potential towards fabrication of electrodes for energy storage devices.

  2. Static in-situ hydrothermal synthesis of small pore zeolite SSZ-16 (AFX) using heated and pre-aged synthesis mixtures

    Czech Academy of Sciences Publication Activity Database

    Hrabánek, Pavel; Zikánová, Arlette; Supiňková, Taťána; Drahokoupil, Jan; Fíla, V.; Lhotka, M.; Dragounová, H.; Laufek, František; Brabec, Libor; Jirka, Ivan; Bernauer, B.; Prokopová, Olga; Martin-Gil, V.; Kočiřík, Milan

    2016-01-01

    Roč. 228, JUL 2016 (2016), s. 107-115 ISSN 1387-1811 R&D Projects: GA ČR(CZ) GAP204/11/1206 Institutional support: RVO:61388955 ; RVO:68378271 Keywords : zeolite * synthesis * AFX Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 3.615, year: 2016

  3. Supercritical fuel injection system

    Science.gov (United States)

    Marek, C. J.; Cooper, L. P. (Inventor)

    1980-01-01

    a fuel injection system for gas turbines is described including a pair of high pressure pumps. The pumps provide fuel and a carrier fluid such as air at pressures above the critical pressure of the fuel. A supercritical mixing chamber mixes the fuel and carrier fluid and the mixture is sprayed into a combustion chamber. The use of fuel and a carrier fluid at supercritical pressures promotes rapid mixing of the fuel in the combustion chamber so as to reduce the formation of pollutants and promote cleaner burning.

  4. Hydrothermal synthesis, structure, Raman spectroscopy, and self-irradiation studies of 248Cm(IO3)3

    International Nuclear Information System (INIS)

    Sykora, Richard E.; Assefa, Zerihun; Haire, Richard G.; Albrecht-Schmitt, Thomas E.

    2004-01-01

    The study of curium iodate, Cm(IO 3 ) 3 , was undertaken as part of a systematic investigation of the 4f- and 5f-elements' iodates. The reaction of 248 CmCl 3 with aqueous H 5 IO 6 under mild hydrothermal conditions results in the reduction of IO 6 5- to IO 3 - anions, and the subsequent formation of Cm(IO 3 ) 3 single crystals. Crystallographic data are: (193K, MoKα, λ=0.71073A): monoclinic, space group P2 1 /c, a=7.2014(7)A, b=8.5062(9)A, c=13.4622(14)A, β=100.142(2) o , V=811.76(14), Z=4, R(F)=2.11%, Rw(Fo2)=4.43% for 119 parameters with 1917 reflections with I>2σ(I). The structure consists of Cm 3+ cations bound by iodate anions to form [Cm(IO 3 ) 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 -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 3 ) 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, β=100.021(2) o , V=818.3(2)

  5. Hydrothermal Liquefaction of Biomass

    Energy Technology Data Exchange (ETDEWEB)

    Elliott, Douglas C.

    2010-12-10

    Hydrothermal liquefaction technology is describes in its relationship to fast pyrolysis of biomass. The scope of work at PNNL is discussed and some intial results are presented. HydroThermal Liquefaction (HTL), called high-pressure liquefaction in earlier years, is an alternative process for conversion of biomass into liquid products. Some experts consider it to be pyrolysis in solvent phase. It is typically performed at about 350 C and 200 atm pressure such that the water carrier for biomass slurry is maintained in a liquid phase, i.e. below super-critical conditions. In some applications catalysts and/or reducing gases have been added to the system with the expectation of producing higher yields of higher quality products. Slurry agents ('carriers') evaluated have included water, various hydrocarbon oils and recycled bio-oil. High-pressure pumping of biomass slurry has been a major limitation in the process development. Process research in this field faded away in the 1990s except for the HydroThermal Upgrading (HTU) effort in the Netherlands, but has new resurgence with other renewable fuels in light of the increased oil prices and climate change concerns. Research restarted at Pacific Northwest National Laboratory (PNNL) in 2007 with a project, 'HydroThermal Liquefaction of Agricultural and Biorefinery Residues' with partners Archer-Daniels-Midland Company and ConocoPhillips. Through bench-scale experimentation in a continuous-flow system this project investigated the bio-oil yield and quality that could be achieved from a range of biomass feedstocks and derivatives. The project was completed earlier this year with the issuance of the final report. HydroThermal Liquefaction research continues within the National Advanced Biofuels Consortium with the effort focused at PNNL. The bench-scale reactor is being used for conversion of lignocellulosic biomass including pine forest residue and corn stover. A complementary project is an international

  6. Synthesis and Magnetic Properties of Nearly Monodisperse CoFe2O4Nanoparticles Through a Simple Hydrothermal Condition

    Directory of Open Access Journals (Sweden)

    Li Xing-Hua

    2010-01-01

    Full Text Available Abstract Nearly monodisperse cobalt ferrite (CoFe2O4 nanoparticles without any size-selection process have been prepared through an alluring method in an oleylamine/ethanol/water system. Well-defined nanospheres with an average size of 5.5 nm have been synthesized using metal chloride as the law materials and oleic amine as the capping agent, through a general liquid–solid-solution (LSS process. Magnetic measurement indicates that the particles exhibit a very high coercivity at 10 K and perform superparamagnetism at room temperature which is further illuminated by ZFC/FC curves. These superparamagnetic cobalt ferrite nanomaterials are considered to have potential application in the fields of biomedicine. The synthesis method is possible to be a general approach for the preparation of other pure binary and ternary compounds.

  7. One-pot hydrothermal synthesis of zirconium dioxide nanoparticles decorated reduced graphene oxide composite as high performance electrochemical sensing and biosensing platform

    International Nuclear Information System (INIS)

    Teymourian, Hazhir; Salimi, Abdollah; Firoozi, Somayeh; Korani, Aazam; Soltanian, Saied

    2014-01-01

    Graphical abstract: - Highlights: • One pot hydrothermal synthesis used for preparing of ZrO 2 NPs reduced graphene oxide. • Electrocatalytic activity of ZrO 2 /rGO improved in compared to ZrO 2 based C- materials. • ZrO 2 NPs/rGO modified GCE was used for electrocatalytic reduction of O 2 and H 2 O 2 . • ZrO 2 NPs/rGO/GCE shows excellent ability to simultaneous detection of AA,UA and DP. • With immobilization of GOX onto ZrO 2 NPs/rGO a sensitive glucose biosensor fabricated. - Abstract: We report on the synthesis of zirconium dioxide-reduced graphene oxide composite (ZrO 2 -rGO) and its application as a novel architecture for electrochemical sensing and biosensing purposes. ZrO 2 -rGO hybrid is synthesized through a simple one-step hydrothermal route, where the reduction of GO and the in-situ generation of ZrO 2 nanoparticles (NPs) occurred simultaneously. Characterization of the resultant hybrid material using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and Raman spectroscopy clearly indicated the homogeneous dispersion of ZrO 2 NPs with particle sizes of ∼5 nm on rGO sheets. The potential application of ZrO 2 -rGO modified glassy carbon electrode (ZrO 2 -rGO/GC) for electroanalytical purposes was demonstrated by using several important electroactive compounds as representative examples (i.e., O 2 , hydrogen peroxide (H 2 O 2 ), glucose, ascorbic acid (AA), dopamine (DA) and uric acid (UA)). Electrochemical control experiments by using different composites of ZrO 2 /graphite, ZrO 2 /Active Carbon and ZrO 2 electrodeposited on activated GC electrode revealed that the ZrO 2 -rGO composite possessed superior electrocatalytic activitiy towards the catalytic reduction of O 2 and H 2 O 2 at more reduced overpotentials. The linear range of H 2 O 2 concentration was from 0.10 to 1340 μM with the detection limit of 20 nM (S/N = 3). Furthermore, via immobilization of glucose oxidase (GOx) enzyme onto the

  8. Facile hydrothermal synthesis and characterization of cesium-doped PbI2 nanostructures for optoelectronic, radiation detection and photocatalytic applications

    Science.gov (United States)

    Shkir, Mohd; AlFaify, S.; Yahia, I. S.; Hamdy, Mohamed S.; Ganesh, V.; Algarni, H.

    2017-10-01

    Low-temperature hydrothermal-assisted synthesis of pure and cesium (Cs) (1, 3, 5, 7 and 10 wt%) doped lead iodide (PbI2) nanorods and nanosheets have been achieved successfully for the first time. The structural and vibrational studies confirm the formation of a 2H-polytypic PbI2 predominantly. Scanning electron microscope analysis confirms the formation of well-aligned nanorods of average size 100 nm at low concentration and nanosheets of average thicknesses in the range of 20-40 nm at higher concentrations of Cs doping. The presence of Cs doping was confirmed by energy dispersive X-ray study. Ultra-violet-visible absorbance spectra were recorded, and energy gap was calculated in the range of 3.33 to 3.45 eV for pure and Cs-doped PbI2 nanostructures which is higher than the bulk value (i.e., 2.27 eV) due to quantum confinement effect. Dielectric constant, loss, and AC conductivity studies have been done. Enhancement in Gamma linear absorption coefficient due to Cs doping confirms the suitability of prepared nanostructures for radiation detection applications. Furthermore, the photocatalytic performance of the synthesized nanostructures was evaluated in the decolorization of methyl green (MG) and methyl orange (MO) under the illumination of visible light (λ > 420 nm). The observed photocatalytic activity for 5 and 7 wt% Cs-doped PbI2 was observed to be more than pure PbI2 and also > 10 times higher than the commercially available photocatalysts. The results suggest that the prepared nanostructures are highly applicable in optoelectronic, radiation detection and many other applications. [Figure not available: see fulltext.

  9. Photocatalytic performance of Cu-doped TiO2 nanofibers treated by the hydrothermal synthesis and air-thermal treatment

    Science.gov (United States)

    Wu, Ming-Chung; Wu, Po-Yeh; Lin, Ting-Han; Lin, Tz-Feng

    2018-02-01

    Series of transition metal-doped TiO2 (metal/TiO2) is prepared by combining the hydrothermal synthesis and air-thermal treatment without any reduction process. The selected transition metal precursors, including Ag, Au, Co, Cr, Cu, Fe, Ni, Pd, Pt, Y, and Zn, were individually doped into TiO2 nanofibers to evaluate the photocatalytic degradation activity and photocatalytic hydrogen generation. Consider the photocatalytic performance of these synthesized metal/TiO2 under UV-A irradiation, copper doped TiO2 nanofibers (Cu/TiO2 NFs) was chosen for further study due to its extraordinary reactivity. Systematical studies were spread to optimize the doping concentration and the calcination condition for much higher photocatalytic activity Cu/TiO2 NFs. In the photocatalytic degradation test, 0.5 mol%-Cu/TiO2 NFs calcined at 650 °C exhibits the highest activity, which is even higher than commercial TiO2-AEROXIDE® TiO2 P25 under UV-A irradiation. The synthesized 0.5 mol%-Cu/TiO2-650 NFs also have the capability in the photocatalytic hydrogen production. The hydrogen evolution rates are 200 μmol/g·h under UV-A irradiation and 280 μmol/g·h under UV-B irradiation. The density of state calculated by CASTEP for Cu/TiO2 indicates that Cu doping contributes to the states near valence band edge and narrows the band gap. The disclosed process in this study is industrial safe, convenient and cost-effective. We further produce a significant amount of TiO2-based catalysts without any hydrogen reduction treatment.

  10. In situ hydrothermal synthesis of g-C3N4/TiO2 heterojunction photocatalysts with high specific surface area for Rhodamine B degradation

    Science.gov (United States)

    Hao, Ruirui; Wang, Guohong; Jiang, Chuanjia; Tang, Hua; Xu, Qingchuan

    2017-07-01

    Semiconductor-based photocatalysis is a promising method for degradation of environmental pollutants, but the activity of most widely used photocatalysts such as titania (TiO2) is still unsatisfactory under visible light. Herein, we synthesized a highly efficient visible-light-responsive heterojunction catalysts based on graphitic carbon nitride (g-C3N4) and TiO2. The g-C3N4/TiO2 heterojunction composites with high specific surface area were prepared via in situ hydrothermal synthesis followed by calcination, using titanium tetrachloride (TiCl4) and melamine as precursors. Interesting, HCl from the hydrolysis of TiCl4 served as the proton source to acidify the melamine. The g-C3N4/TiO2 heterojunction composites exhibited higher photocatalytic performance for decomposition of Rhodamine B (RhB) than pure g-C3N4 or TiO2 under visible light irradiation. The high activity can be ascribed to the high specific surface area (up to 115.6 m2 g-1) of the g-C3N4/TiO2 composites and a synergistic heterojunction structure between TiO2 and g-C3N4. Moreover, the photocatalytic performances of the g-C3N4/TiO2 composites rely on the content of melamine in the synthesis precursors: with an optimum melamine content (3 g for 0.5 mL of TiCl4), the sample showed the highest photocatalytic performance, which is superior to pure TiO2 and g-C3N4 by a factor of 18.7 and 3.5, respectively. Active species trapping experiments revealed that superoxide radicals and photogenerated holes played crucial roles in the photocatalytic reactions. The results will provide new ideas for the smart design and development of g-C3N4-based highly active photocatalysts with ultrahigh specific surface area for environmental and energy applications.

  11. One-pot hydrothermal synthesis and characterization of CoFe{sub 2}O{sub 4} nanoparticles and its application as magnetically recoverable catalyst in oxidation of alcohols by periodic acid

    Energy Technology Data Exchange (ETDEWEB)

    Paul, Bappi; Purkayastha, Debraj Dhar; Dhar, Siddhartha Sankar, E-mail: ssd_iitg@hotmail.com

    2016-09-15

    A novel and facile approach for one-pot synthesis of spinel cobalt ferrite (CoFe{sub 2}O{sub 4}) nanoparticles (NPs) is presented here. The synthesis involves homogeneous chemical precipitation followed by hydrothermal heating, using tributylamine (TBA) as a hydroxylating agent. Polyethylene glycol (PEG) 4000 was used as surfactant. As-synthesized CoFe{sub 2}O{sub 4} NPs were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), N{sub 2} adsorption-desorption isotherm (BET) and vibrating sample magnetometry (VSM). TEM image showed formation of spherical particles of sizes 2–30 nm. These NPs were used as magnetically recoverable catalyst in oxidation of alcohols to their corresponding aldehydes by periodic acid. This oxidative procedure is found to be highly efficient affording products in very high yield and selectivity. The easy magnetic separation of the catalyst and efficient reusability are key features of this methodology. - Highlights: • Hydrothermal synthesis of CoFe{sub 2}O{sub 4} NPs with (C{sub 4}H{sub 9}){sub 3}N as hydroxylating agent. • The TEM images showed the particles to be spherical in shape with sizes 2–30 nm. • CoFe{sub 2}O{sub 4} was used as recyclable catalyst for oxidation of alcohols by periodic acid.

  12. Synthesis and antimicrobial evaluation of nanostructures ZrO2:AG against staphylococcus aureus by hydrothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Nova, C.V.; Reis, K.H.; Galico, D.A.; Venturini, J.; Pontes, F.M.L.; Pinheiro, A.L. [Universidade Estadual Paulista Julio de Mesquita Filho (UNESP), SP (Brazil); Longo, E. [Universidade Estadual de Campinas (UNICAMP), SP (Brazil)

    2016-07-01

    Nanostructures of zirconia (ZrO2) has shown great prominence in the area of advanced materials and shows excellent properties such as chemical stability, mechanical strength, electrical and optical properties. When certain metals are supported on the compound, such as Fe, Ag, Au and Al, a potentiation of some properties, such as bactericide and fungicide can occur. Thus, this work deals with the synthesis and characterization of ZrO2 and ZrO2:Ag (1% and 10 % of Ag) nanostructures and the study of the influence of the antimicrobial activity against Staphylococcus aureus. X-ray powder diffractograms of the zirconia and silver with zirconia shown the formation of well defined peaks of tetragonal zirconia in all the samples. Although the ZrO2:Ag (10 % of Ag) shown the characteristics peaks of cubic silver, these peaks do not appear in ZrO2:Ag (1 % of Ag) due to the small amount of silver in comparison with zirconium. The crystal size was estimated by the Scherrer equation and the calculated values for zirconia were 12.84, 12.27 and 12.61 nm for ZrO2, ZrO2 : Ag (1%) and ZrO2 : Ag (10%) respectively and the silver crystal size was 8,09 nm. Diffuse reflectance of the silver particles shown a broad plasmon band at 405 and 424 nm for the ZrO2 : Ag (1%) and ZrO2 : Ag (10%). Antimicrobial assay demonstrated that ZrO2 showed a bacteriostatic effect (61 %) and the inclusion of the silver in the ZrO2 matrix enhanced this effect to 65-72 %. Both particles with different silver content shown similar effect {[ZrO2:Ag 1%] = [ZrO2:Ag 10%]>[ZrO2]}.(author)

  13. Use of supercritical carbon dioxide extraction

    Energy Technology Data Exchange (ETDEWEB)

    Taniguchi, Masayuki (Niigata Univ., Faculty of Engineering, Niigata, (Japan))

    1989-09-25

    Supercritical fluid extraction is a novel diffusion and separation technique which exploits simultaneously the increase of vapor pressure and the difference of chemical affinities of fluids near the critical point. A solvent which is used as the supercritical fluid has the following features: the critical point exists in the position of relatively ease of handling, the solvent is applicable to the extraction of a physiological active substance of thermal instability. Carbon dioxide as the solvent is non-flammable, non-corrosive, non-toxic, cheap, and readily available of high purity. The results of studies on the use of supercritical carbon dioxide (SC-CO{sub 2}) as a solvent for natural products in the fermentation and food industries, were collected. SC-CO{sub 2} extraction are used in many fields, examples for the application are as follows: removal of organic solvents from antibiotics; extraction of vegetable oils contained in wheat germ oil, high quality mustard seeds, rice bran and so on; brewing of sake using rice and rice-koji; use as a non-aqueous medium for the synthesis of precursors of the Aspartame; and use in sterilization. 66 refs., 17 figs., 21 tabs.

  14. Depletion of a brine layer at the base of ridge-crest hydrothermal systems

    OpenAIRE

    Schoofs, Stan; Hansen, Ulrich

    2000-01-01

    The variable salinity of fluid venting from mid-ocean ridges is indicative of mixing between hydrothermal seawater and fluids that have undergone supercritical phase separation. In order to study the stability of a brine-saturated layer that may form in the lowermost part of the hydrothermal system, we have performed numerical simulations of a system that has returned into the subcritical regime. For typical geological parameters, it is shown that the interface between the brine layer and the...

  15. Study of the synthesis and self-assembly of CO2-philic copolymers with complexing groups: application to decontamination in supercritical CO2 medium

    International Nuclear Information System (INIS)

    Ribaut, T.

    2009-10-01

    In the frame of sustainable development, a priority is to decrease the volume of nuclear wastes. The use of supercritical carbon dioxide (scCO 2 ) could allow to solve this problem. The aim of this study is to extract an ionic or particle cobalt contamination deposited on textile lab coats. The strategy uses CO 2 -philic/CO 2 -phobic copolymers soluble in scCO 2 and containing complexing groups. This approach combines the use of amphiphilic copolymers for steric stabilization of particles, of surfactants able to self-assemble to promote extraction and of ligands. Controlled radical polymerization is used to synthesize fluorinated gradient or block copolymers. Cloud point curves of the copolymers are determined experimentally in scCO 2 . Prediction of polymer/scCO 2 phase diagrams was assessed by Perturbed-Chain Statistical Associating Fluid Theory (PC-SAFT) modeling. Gradient copolymers appear more advantageous than block copolymers due to their solubility in much milder conditions of pressure and temperature. Small-angle neutron scattering (SANS) allowed us to evidence the pressure-induced aggregation of the gradient copolymers in scCO 2 . Their interface properties were demonstrated: they allow to form water-in-CO 2 microemulsions and to stabilize cobalt hydroxide dispersions in scCO 2 . Lastly, in presence of a very low quantity of water, Co 2+ ions were removed with a rate of 37 % from a cotton/polyester matrix by a gradient copolymer. (author)

  16. Synthesis of an excellent electrocatalyst for oxygen reduction reaction with supercritical fluid: Graphene cellular monolith with ultrafine and highly dispersive multimetallic nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Yazhou; Cheng, Xiaonong; Yen, Clive H.; Wai, Chien M.; Wang, Chongmin; Yang, Juan; Lin, Yuehe

    2017-04-01

    Graphene cellular monolith (GCM) can be used as an excellent support for nanoparticles in widespread applications. However, it's still a great challenge to deposit the desirable nanoparticles in GCM that have small size, controllable structure, composition, and high dispersion using the current methods. Here we demonstrate a green, efficient and large-scale method to address this challenge using supercritical fluid (SCF). By this superior method, graphene hydrogel can be transferred into GCM while being deposited with ultrafine and highly dispersive nanoparticles. Specifically, the bimetallic PtFe/GCM and the trimetallic PtFeCo/GCM catalysts are successfully synthesized, and their electrocatalytic performances toward oxygen reduction reaction (ORR) are also studied. The resultant PtFe/GCM shows the significant enhancement in ORR activity, including a factor of 8.47 enhancement in mass activity (0.72 A mgPt-1), and a factor of 7.67 enhancement in specific activity (0.92 mA cm-2), comparing with those of the commercial Pt/C catalyst (0.085 A mgPt-1, 0.12 mA cm-2). Importantly, by introducing the Co, the trimetallic PtFeCo/GCM exhibits the further improved ORR activities (1.28 A mgPt-1, 1.80 mA cm-2). The high ORR activity is probably attributed to the alloying structure, ultrafine size, highly dispersive, well-defined, and a better interface with 3D porous graphene support.

  17. Synthesis of Spongy-Like Mesoporous Hydroxyapatite from Raw Waste Eggshells for Enhanced Dissolution of Ibuprofen Loaded via Supercritical CO2

    Science.gov (United States)

    Ibrahim, Abdul-Rauf; Li, Xiangyun; Zhou, Yulan; Huang, Yan; Chen, Wenwen; Wang, Hongtao; Li, Jun

    2015-01-01

    The use of cheaper and recyclable biomaterials (like eggshells) to synthesize high purity hydroxyapatite (HAp) with better properties (small particle size, large surface area and pore volume) for applications (in environmental remediation, bone augmentation and replacement, and drug delivery systems) is vital since high-purity synthetic calcium sources are expensive. In this work, pure and mesoporous HAp nanopowder with large pore volume (1.4 cm3/g) and surface area (284.1 m2/g) was produced from raw eggshells at room temperature using a simple two-step procedure. The control of precursor droplets could stabilize the pH value of the reaction solution, because of the size of the needle (of the syringe pump used for precursor additions) leading to production of HAp with high surface area and pore size. The as-produced HAp revealed high ibuprofen (as a model drug) loading (1.38 g/g HAp), enhanced dissolution and controllable release of the drug via solute-saturated supercritical carbon dioxide. PMID:25860950

  18. Supercritical fluids processing: emerging opportunities

    International Nuclear Information System (INIS)

    Kovaly, K.A.

    1985-01-01

    This publication on the emerging opportunities of supercritical fluids processing reveals the latest research findings and development trends in this field. These findings and development trends are highlighted, and the results of applications of technology to the business of supercritical fluids are reported. Applications of supercritical fluids to chemical intermediates, environmental applications, chemical reactions, food and biochemistry processing, and fuels processing are discussed in some detail

  19. 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

    Energy Technology Data Exchange (ETDEWEB)

    Choi, Bo Hyun; Park, Shin-Ae [Energy System Major, School of Mechanical Engineering, Pusan National University, Busan 609-735 (Korea, Republic of); Park, Bong Kyu [GIFT Center, Pusan National University, Busan, 609-735 (Korea, Republic of); Chun, Ho Hwan, E-mail: chunahh@pusan.ac.kr [Global Core Research Center for Ships and Offshore Plants(GCRC-SOP), Pusan National University, Busan, 609-735 (Korea, Republic of); Kim, Yong-Tae, E-mail: yongtae@pusan.ac.kr [Energy System Major, School of Mechanical Engineering, Pusan National University, Busan 609-735 (Korea, Republic of)

    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.

  20. Supercritical fluids cleaning

    Energy Technology Data Exchange (ETDEWEB)

    Butner, S.; Hjeresen, D.; Silva, L.; Spall, D.; Stephenson, R.

    1991-01-01

    This paper discusses a proposed multi-party research and development program which seeks to develop supercritical fluid cleaning technology as an alternative to existing solvent cleaning applications. While SCF extraction technology has been in commercial use for several years, the use of these fluids as cleaning agents poses several new technical challenges. Problems inherent in the commercialization of SCF technology include: the cleaning efficacy and compatibility of supercritical working fluids with the parts to be cleaned must be assessed for a variety of materials and components; process parameters and equipment design Have been optimized for extractive applications and must be reconsidered for application to cleaning; and co-solvents and entrainers must be identified to facilitate the removal of polar inorganic and organic contaminants, which are often not well solvated in supercritical systems. The proposed research and development program would address these issues and lead to the development and commercialization of viable SCF-based technology for precision cleaning applications. This paper provides the technical background, program scope, and delineates the responsibilities of each principal participant in the program.

  1. Ultrasonic and hydrothermal mediated synthesis routes for functionalized Mg-Al LDH: Comparison study on surface morphology, basic site strength, cyclic sorption efficiency and effectiveness.

    Science.gov (United States)

    Ezeh, Collins I; Tomatis, Marco; Yang, Xiaogang; He, Jun; Sun, Chenggong

    2018-01-01

    Amine functionalized layered double hydroxide (LDHs) adsorbents prepared using three different routes: co-precipitation, sono-chemical and ultrasonic-assisted high pressure hydrothermal. The prepared adsorbent samples were characterized using X-ray diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), Scanning electron microscope-Energy dispersive X-ray spectroscopy (SEM-EDX), Temperature Programmed Desorption (TPD), Brunauer-Emmett-Teller (BET), and Thermogravimetric analysis (TGA), respectively. The performance of the prepared adsorbents was tested in a controlled thermal-swing adsorption process to measure its adsorption capacity, regeneration and cyclic efficiencies subsequently. The characterisation results were compared with those obtained using the conventional preparation routes but taking into account of the impact of sonochemical and hydrothermal pre-treatment on textural properties, adsorption capacity, regeneration and cyclic efficiencies. Textural results depicts a surge in surface area of the adsorbent synthesised by hydrothermal route (311m 2 /g) from 25 to 171m 2 /g for conventional and ultrasonic routes respectively. Additionally, it has been revealed from the present study that adsorbents prepared using ultrasonic-assisted hydrothermal route exhibit a better CO 2 uptake capacity than that prepared using sonochemical and conventional routes. Thus, the ultrasonic-assisted hydrothermal treatment can effectively promote the adsorption capacity of the adsorbent. This is probably due to the decrease of moderate (M-O) and weak (OH - groups) basic sites with subsequent surge in the number of strong basic sites (O 2- ) resulting from the hydrothermal process. Moreover, the cyclic adsorption efficiency of the ultrasonic mediated process was found to be 76% compared with 60% for conventional and 53% for hydrothermal routes, respectively. According to the kinetic model analysis, adsorption mechanism is mostly dominated by physisorption before amine

  2. Hydrothermal synthesis of Ti oxide nanostructures and TiO2:SnO2 heterostructures applied to the photodegradation of rhodamine B

    International Nuclear Information System (INIS)

    Mourão, Henrique A.J.L.; Junior, Waldir Avansi; Ribeiro, Caue

    2012-01-01

    The present study describes the synthesis, characterization and testing of the photocatalytic potential of TiO 2 nanoparticles (NPs), TiO 2 :SnO 2 heterostructures and potassium titanate nanotubes (TNTs) obtained by the alkaline hydrothermal method. The materials were characterized by X-ray diffraction (XRD), energy-dispersive X-ray (EDX) spectroscopy, surface area estimated from the N 2 physisorption isotherm (BET), X-ray absorption near-edge structure (XANES) spectroscopy, scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), scanning transmission electron microscopy (STEM) and Fourier transform near-infrared (FT-NIR) spectroscopy, among other methods. Photocatalytic potential was assessed by rhodamine B dye photodegradation under UVC radiation. The properties of the materials were shown to depend on the KOH concentration. Potassium TNTs with high surface area were obtained only in 5 mol L −1 KOH. The material composed of TiO 2 anatase phase, which was obtained in KOH solution ranging from 10 −4 to 1 mol L −1 , showed higher photocatalytic activity than the TNTs, despite the lower surface area and lower density of hydroxyl groups on the anatase. In the heterostructure syntheses, SnO 2 NPs were identified attached to TiO 2 when 10 −4 and 10 −2 mol L −1 KOH were used, whereas at [KOH] = 1 and 5 mol L −1 , Sn remained in solution during the synthetic process and only the respective TiO 2 phase was identified. The TiO 2 :SnO 2 heterostructures were more active than the material without SnO 2 prepared at the same KOH concentrations. Highlights: ► The formation of the materials depends on the [KOH] used during syntheses. ► The heterostructures were obtained with the lower [KOH]. ► Photoactivity of the heterostructures was higher than the respective TiO 2 nanostructures. ► Titanate nanotubes showed high concentration of OH groups but low photoactivity.

  3. Saccharide-derived microporous spherical biochar prepared from hydrothermal carbonization and different pyrolysis temperatures: synthesis, characterization, and application in water treatment.

    Science.gov (United States)

    Tran, Hai Nguyen; Lee, Chung-Kung; Nguyen, Tien Vinh; Chao, Huan-Ping

    2017-08-24

    Three saccharides (glucose, sucrose, and xylose) were used as pure precursors for synthesizing spherical biochars (GB, SB, and XB), respectively. The two-stage synthesis process comprised: (1) the hydrothermal carbonization of saccharides to produce spherical hydrochar' and (2) pyrolysis of the hydrochar at different temperatures from 300°C to 1200°C. The results demonstrated that the pyrolysis temperatures insignificantly affected the spherical morphology and surface chemistry of biochar. The biochar' isoelectric point ranged from 2.64 to 3.90 (abundant oxygen-containing functionalities). The Brunauer-Emmett-Teller (BET)-specific surface areas (S BET ) and total pore volumes (V total ) of biochar increased with the increasing pyrolysis temperatures. The highest S BET and V total were obtained at a pyrolysis temperature of 900°C for GB (775 m 2 /g and 0.392 cm 3 /g), 500°C for SB (410 m 2 /g and 0.212 cm 3 /g), and 600°C for XB (426 m 2 /g and 0.225 cm 3 /g), respectively. The spherical biochar was a microporous material with approximately 71-98% micropore volume. X-ray diffraction results indicated that the biochar' structure was predominantly amorphous. The spherical biochar possessed the graphite structure when the pyrolysis temperature was higher than 600°C. The adsorption capacity of GB depended strongly on the pyrolysis temperature. The maximum Langmuir adsorption capacities ([Formula: see text]) of 900GB exhibited the following selective order: phenol (2.332 mmol/g) > Pb 2+ (1.052 mmol/g) > Cu 2+ (0.825 mmol/g) > methylene green 5 (0.426 mmol/g) > acid red 1 (0.076 mmol/g). This study provides a simple method to prepare spherical biochar - a new and potential adsorbent for adsorbing heavy metals and aromatic contaminants.

  4. Hydrothermal synthesis of Ti oxide nanostructures and TiO{sub 2}:SnO{sub 2} heterostructures applied to the photodegradation of rhodamine B

    Energy Technology Data Exchange (ETDEWEB)

    Mourao, Henrique A.J.L., E-mail: henriquepiau@yahoo.com.br [Universidade Federal de Sao Carlos, Departamento de Quimica, Rod. Washington Luiz, km 235, CEP 13565-905, Sao Carlos, SP (Brazil); EMBRAPA Instrumentacao Agropecuaria, Rua XV de Novembro, 1452, CEP 13560-970, CP 741, Sao Carlos, SP (Brazil); Junior, Waldir Avansi; Ribeiro, Caue [EMBRAPA Instrumentacao Agropecuaria, Rua XV de Novembro, 1452, CEP 13560-970, CP 741, Sao Carlos, SP (Brazil)

    2012-08-15

    The present study describes the synthesis, characterization and testing of the photocatalytic potential of TiO{sub 2} nanoparticles (NPs), TiO{sub 2}:SnO{sub 2} heterostructures and potassium titanate nanotubes (TNTs) obtained by the alkaline hydrothermal method. The materials were characterized by X-ray diffraction (XRD), energy-dispersive X-ray (EDX) spectroscopy, surface area estimated from the N{sub 2} physisorption isotherm (BET), X-ray absorption near-edge structure (XANES) spectroscopy, scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), scanning transmission electron microscopy (STEM) and Fourier transform near-infrared (FT-NIR) spectroscopy, among other methods. Photocatalytic potential was assessed by rhodamine B dye photodegradation under UVC radiation. The properties of the materials were shown to depend on the KOH concentration. Potassium TNTs with high surface area were obtained only in 5 mol L{sup -1} KOH. The material composed of TiO{sub 2} anatase phase, which was obtained in KOH solution ranging from 10{sup -4} to 1 mol L{sup -1}, showed higher photocatalytic activity than the TNTs, despite the lower surface area and lower density of hydroxyl groups on the anatase. In the heterostructure syntheses, SnO{sub 2} NPs were identified attached to TiO{sub 2} when 10{sup -4} and 10{sup -2} mol L{sup -1} KOH were used, whereas at [KOH] = 1 and 5 mol L{sup -1}, Sn remained in solution during the synthetic process and only the respective TiO{sub 2} phase was identified. The TiO{sub 2}:SnO{sub 2} heterostructures were more active than the material without SnO{sub 2} prepared at the same KOH concentrations. Highlights: Black-Right-Pointing-Pointer The formation of the materials depends on the [KOH] used during syntheses. Black-Right-Pointing-Pointer The heterostructures were obtained with the lower [KOH]. Black-Right-Pointing-Pointer Photoactivity of the heterostructures was higher than the respective TiO{sub 2

  5. Hydrothermal synthesis of layered Li[Ni1/3Co1/3Mn1/3]O2 as positive electrode material for lithium secondary battery

    International Nuclear Information System (INIS)

    Myung, Seung-Taek; Lee, Myung-Hun; Komaba, Shinichi; Kumagai, Naoaki; Sun, Yang-Kook

    2005-01-01

    In attempts to prepare layered Li[Ni 1/3 Co 1/3 Mn 1/3 ]O 2 , hydrothermal method was employed. The hydrothermal precursor, [Ni 1/3 Co 1/3 Mn 1/3 ](OH) 2 , was synthesized via a coprecipitation route. The sphere-shaped powder precursor was hydrothermally reacted with LiOH aqueous solution at 170 deg. C for 4 days in autoclave. From X-ray diffraction and scanning electron microscopic studies, it was found that the as-hydrothermally prepared powders were crystallized to layered α-NaFeO 2 structure and the particles had spherical shape. The as-prepared Li[Ni 1/3 Co 1/3 Mn 1/3 ]O 2 delivered an initial discharge of about 110 mA h g -1 due to lower crystallinity. Heat treatment of the hydrothermal product at 800 deg. C was significantly effective to improve the structural integrity, which consequently affected the increase in the discharge capacity to 157 (4.3 V cut-off) and 182 mA h g -1 (4.6 V cut-off) at 25 deg. C with good reversibility

  6. One-step synthesis of single phase micro-sized BaFe12O19 hexaplates via a modified hydrothermal approach

    International Nuclear Information System (INIS)

    Cao, Liangliang; Zeng, Yanwei; Ding, Chuan; Li, Rongjie; Li, Chuanming; Zhang, Chengzhe

    2016-01-01

    Single phase BaFe 12 O 19 ferrite identified by X-ray diffraction and Raman spectroscopy has been successfully synthesized using Fe(NO 3 ) 3 ·9H 2 O and Ba(NO 3 ) 2 as starting materials and NaOH as a precipitant via a modified one-step hydrothermal approach which involves the elimination of carbonate radicals from reaction system based on the stoichiometric ratio of [Ba 2+ ]/[Fe 3+ ]. Hydrothermal products under various synthetic conditions were studied, including different addition amounts of Ba(NO 3 ) 2 in the modified operation, reaction temperatures and times, and hydroxyl concentrations. The BaFe 12 O 19 particles featuring an excellent hexagonal plates shape can be hydrothermally synthesized with the aid of polyethylene glycol. It has been found that the presence of α-Fe 2 O 3 in a traditional hydrothermal process is motivated by the deviation from the desired [Ba 2+ ]/[Fe 3+ ] ratio caused by the negligent precipitation of Ba 2+ ions to BaCO 3 . An investigation on the preferred hydrothermal product through thermodynamic calculation shows that the reduction in Gibbs free energy for the exclusive formation of BaFe 12 O 19 with 1 mol of Fe 3+ ions at 220 °C is approximately 32 kJ higher than that for the complete transformation to α-Fe 2 O 3 with an equal consumption quantity of Fe 3+ ions. - Highlights: • Pure BaFe 12 O 19 was hydrothermally synthesized based on the stoichiometric ratio. • A modified operation was employed to eliminate self-invited carbonate ions. • BaFe 12 O 19 particles feature an excellent micro-sized hexaplates shape. • BaFe 12 O 19 was thermodynamically confirmed to be preferred result instead of α-Fe 2 O 3 .

  7. Hydrothermal synthesis, characterization and luminescent ...

    Indian Academy of Sciences (India)

    ical transformations under the influence of surfactant. It is known that citric acid can be adsorbed strongly on metal and mineral surfaces and significantly alters the surface proper- ties and mineral growth behaviour [30]. Here, citric acid may play a crucial role in the formation of undoped and doped- submicron rods. First, the ...

  8. Hydrothermal synthesis, characterization and luminescent ...

    Indian Academy of Sciences (India)

    (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), energy-dispersive X-ray spectra (EDS), particle size by dynamic light scattering (DLS), Fourier transform infrared (FTIR) spectrum and photoluminescence (PL) techniques. Nanoparticles consist of well-crystallized hexagonal phase ...

  9. Hydrothermal synthesis of polycrystalline carbonates

    Science.gov (United States)

    Tareen, J. A. K.; Basavalingu, B.; Kutty, T. R. N.

    1981-11-01

    Polycrystals of orthorhobic carbonates RCO 3 (R = Sr, Ba and Pb) were synthesised for the first time using formic acid as mineraliser. The unit cell parameters of this synthetic pure carbonates are: BaCO 3: a=5.309, b=8.889, c=6.401; SrCO 3: a=5.108, b=8.420, c=6.040; PbCO 3: a=5.176, b=8.511, c=6.137.

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

    Science.gov (United States)

    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. © 2015 Wiley Periodicals, Inc.

  11. Synthesis of cobalt ferrite with enhanced magnetostriction properties by the sol−gel−hydrothermal route using spent Li-ion battery

    International Nuclear Information System (INIS)

    Yao, Lu; Xi, Yuebin; Xi, Guoxi; Feng, Yong

    2016-01-01

    The combination of a sol–gel method and a hydrothermal method was successfully used for synthesizing the nano-crystalline cobalt ferrite powders with a spinel structure using spent Li-ion batteries as the raw materials. The phase composition, microstructure, magnetic properties and magnetostriction coefficient of cobalt ferrite were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), magnetometer and magnetostrictive measurement instrument. The microstructure of the products exhibited hedgehog-like microspheres with particle size of approximately 5 μm. The different crystalline sizes and the microstructure of cobalt ferrites precursor were controlled by varying the hydrothermal time, which significantly affected the super-exchange and the deflection direction of the magnetic domain, and led to the change of the magnetic properties of sintered cylindrical samples. The saturation magnetization and maximum magnetostriction coefficient were 81.7 emu/g and −158.5 ppm, respectively, which was larger than that of products prepared by the sol-gel sintered method alone. - Graphical abstract: The magnetostriction of cobalt ferrites with a spinel structure was successfully prepared using the sol–gel–hydrothermal route using spent Li-ion batteries. On the basis of the aforementioned SEM observation, the formation of a hedgehog-like microsphere structure might involve two important steps: Ostwald ripening and self-assembly. - Highlights: • The cobalt ferrites were prepared by the sol–gel–hydrothermal route. • The cobalt ferrites show hedgehog-like microsphere particles in shape. • The microspheres size increased with increasing hydrothermal time. • The magnetostriction properties of the cobalt ferrite were enhanced.

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

    International Nuclear Information System (INIS)

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

    2014-01-01

    Rutile TiO 2 nanorod arrays (TNRs) were achieved by hydrothermal process on TiCl 4 pretreated Ti foil. Subsequently, TNRs were hydrothermally etched in HCl solution to form hollow TiO 2 nanorod arrays (H-TNRs). The TiCl 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 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 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 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 2 nanorod array photoanode obtained from original TiO 2 nanorod array photoanode by hydrothermal etching demonstrates enhanced photoelectric efficiency of DSSC. - Highlights: • TiO 2 nanorods are prepared via hydrothermal process on TiCl 4 -pretreated Ti foil. • Hollow TiO 2 nanorods are obtained by hydrothermal etching of TiO 2 nanorods. • TiCl 4 pretreatment plays a key role in protecting Ti foil from chemical corrosion. • Hollow TiO 2 nanorods photoanode shows enhanced photoelectric efficiency for DSSC

  13. Synthesis of cobalt ferrite with enhanced magnetostriction properties by the sol−gel−hydrothermal route using spent Li-ion battery

    Energy Technology Data Exchange (ETDEWEB)

    Yao, Lu, E-mail: yaolu1020@126.com [Key Laboratory for Yellow River and Huai River Water Environment and Pollution Control, Ministry of Education, College of Environment, Henan Normal University, Xinxiang 453007 (China); College of Chemistry and Chemical Engineering, Xinxiang University, Xinxiang Henan 453003 (China); Xi, Yuebin [Key Laboratory for Yellow River and Huai River Water Environment and Pollution Control, Ministry of Education, College of Environment, Henan Normal University, Xinxiang 453007 (China); Xi, Guoxi, E-mail: yaolu001@163.com [Key Laboratory for Yellow River and Huai River Water Environment and Pollution Control, Ministry of Education, College of Environment, Henan Normal University, Xinxiang 453007 (China); Feng, Yong [Key Laboratory for Yellow River and Huai River Water Environment and Pollution Control, Ministry of Education, College of Environment, Henan Normal University, Xinxiang 453007 (China)

    2016-09-25

    The combination of a sol–gel method and a hydrothermal method was successfully used for synthesizing the nano-crystalline cobalt ferrite powders with a spinel structure using spent Li-ion batteries as the raw materials. The phase composition, microstructure, magnetic properties and magnetostriction coefficient of cobalt ferrite were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), magnetometer and magnetostrictive measurement instrument. The microstructure of the products exhibited hedgehog-like microspheres with particle size of approximately 5 μm. The different crystalline sizes and the microstructure of cobalt ferrites precursor were controlled by varying the hydrothermal time, which significantly affected the super-exchange and the deflection direction of the magnetic domain, and led to the change of the magnetic properties of sintered cylindrical samples. The saturation magnetization and maximum magnetostriction coefficient were 81.7 emu/g and −158.5 ppm, respectively, which was larger than that of products prepared by the sol-gel sintered method alone. - Graphical abstract: The magnetostriction of cobalt ferrites with a spinel structure was successfully prepared using the sol–gel–hydrothermal route using spent Li-ion batteries. On the basis of the aforementioned SEM observation, the formation of a hedgehog-like microsphere structure might involve two important steps: Ostwald ripening and self-assembly. - Highlights: • The cobalt ferrites were prepared by the sol–gel–hydrothermal route. • The cobalt ferrites show hedgehog-like microsphere particles in shape. • The microspheres size increased with increasing hydrothermal time. • The magnetostriction properties of the cobalt ferrite were enhanced.

  14. Vapor–liquid equilibria of triglycerides–methanol mixtures and their influence on the biodiesel synthesis under supercritical conditions of methanol

    Directory of Open Access Journals (Sweden)

    ALEKSANDAR ORLOVIC

    2007-01-01

    Full Text Available The non-catalytic synthesis of biodiesel (fatty acids methyl esters from triglycerides and methanol proceeds at elevated pressures above 100 bar and temperatures above 523 K. Kinetic investigations of the system revealed an unusual behavior of the reaction rate constant with increasing temperature and pressure. In order to explain this phenomenon, the phase behavior of the triglycerides–methanol mixture was investigated. The phase equilibria of the binary system sunflower oil–methanol were measured at different temperatures between 473 and 503 K, and a range of pressures between 10 and 56 bar. The experimental data were correlated using the Peng–Robinson, Soave–Redlich–Kwong and Redlich–Kwong–Aspen equations of state and different mixing rules. The best results were obtained with the RK–ASPEN equation of state and the Van derWaals mixing rule (VdW, which were then used to calculate the distribution of the phases at pressures and temperatures usual for the non-catalytic synthesis of biodiesel under high pressures. The obtained data indicated a strong influence of the phase equilibria on the reaction kinetics.

  15. Synthesis and characterization on titanium dioxide prepared by precipitation and hydrothermal treatment; Sintese e caracterizacao de dioxido de titanio preparado por precipitacao e tratamento hidrotermico

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Andre V.P. dos; Yoshito, Walter K.; Lazar, Dolores R.R.; Ussui, Valter, E-mail: vussui@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2012-07-01

    Surface properties of titanium dioxide (titania) are outstanding among ceramic materials and enables uses as catalysts, photoelectrochemical devices, solar cells and others. In many of these applications, it is necessary to keep the anatase phase, that is stable only in low temperatures (<400 deg C). In the present work, the influence of hydrothermal treatment on physical characteristics and crystal structure of titania powders synthesized by precipitation was investigated. Characterizations of obtained powders were carried out by X-ray diffraction, surface area analysis by N2 gas sorption (BET) and microstructure of powders and ceramics were analyzed by scanning electron microscopy. As prepared powders were formed as cylindrical pellets by uniaxial pressing and sintered at 1500 deg C for 01 hour. Results showed that anatase phase without formation of rutile phase can be formed in hydrothermally treated samples . Rutile phase is predominant in calcined and/or sintered samples (author)

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

    International Nuclear Information System (INIS)

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

    2012-01-01

    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 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: ► Aqueous iron oxide ferrofluids were synthesized by hydrothermal-reduction route. ► Citric acid acted as reducing agent and surfactant in the route. ► This is a facile, low energy and environmental friendly route. ► The aqueous iron oxide ferrofluids were monodispersed and stable at pH of 7. ► The calculated intrinsic loss power of the synthesized ferrofluids was very high.

  17. Synthesis and Characterization of Pyrochlore Bi2Sn2O7 Doping with Praseodymium by Hydrothermal Method and Its Photocatalytic Activity Study

    OpenAIRE

    Xu, Weicheng; Zhou, Guangyin; Fang, Jianzhang; Liu, Zhang; Chen, YunFang; Cen, Chaoping

    2013-01-01

    Praseodymium doped Bi2Sn2O7 (BSO), as a visible-light responsive photocatalyst, was prepared by a hydrothermal method with different dopant contents. The as-prepared photocatalysts were investigated by X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), N2 adsorption-desorption isotherm, X-ray photoelectron spectroscopy analysis (XPS), and UV-Vis diffuse reflectance spectroscopy (DRS). The photocatalytic activity of prepared catalysts was evalu...

  18. CTAB-Assisted Hydrothermal Synthesis of Bi2Sn2O7 Photocatalyst and Its Highly Efficient Degradation of Organic Dye under Visible-Light Irradiation

    OpenAIRE

    Xu, Weicheng; Liu, Zhang; Fang, Jianzhang; Zhou, Guangyin; Hong, Xiaoting; Wu, Shuxing; Zhu, Ximiao; Chen, YunFang; Cen, Chaoping

    2013-01-01

    Pyrochlore-type Bi2Sn2O7 (BSO) nanoparticles have been prepared by a hydrothermal method assisted with a cationic surfactant cetyltrimethylammonium bromide (CTAB). These BSO products were characterized by powder X-ray diffraction (XRD), infrared spectroscopy (IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Brunauer-Emmett-Teller (BET), and UV-visible diffuse reflectance spectroscopy (DRS). The results indicated that CTAB alters the surface parameters and the m...

  19. Microwave-assisted hydrothermal synthesis of highly luminescent ZnSe-based quantum dots with a quantum yield higher than 90%

    Science.gov (United States)

    Lee, Yong-Shin; Nakano, Kaoru; Bu, Hang-Beom; Gwi Kim, Dae

    2017-06-01

    Highly luminescent ZnSe-based quantum dots (QDs) were synthesized by a microwave-assisted hydrothermal method. The characteristics of the ZnSe precursor solution strongly influenced the photoluminescence (PL) quantum yields (QYs) of the QDs. The PL QY of ZnSe-core QDs synthesized under the optimum conditions reached 60%. Furthermore, the PL QY further increased to higher than 90% when a ZnS shell was applied to prepare ZnSe/ZnS-core/shell QDs.

  20. Gel-hydrothermal synthesis of carbon and boron co-doped TiO{sub 2} and evaluating its photocatalytic activity

    Energy Technology Data Exchange (ETDEWEB)

    Wu Yongmei; Xing Mingyang [Key Lab for Advanced Materials and Institute of Fine Chemicals, East China University of Science and Technology, 130 Meilong Road, Shanghai 200237 (China); Zhang Jinlong, E-mail: jlzhang@ecust.edu.cn [Key Lab for Advanced Materials and Institute of Fine Chemicals, East China University of Science and Technology, 130 Meilong Road, Shanghai 200237 (China)

    2011-08-15

    Graphical abstract: Carbon and boron co-doped TiO{sub 2} photocatalysts were prepared firstly by the gel-hydrothermal method, which presented excellent visible light photocatalytic activities, resulting from the coke carbon photosensitization and B-N synergistic effect. Display Omitted Highlights: {yields} Carbon and boron co-doped TiO{sub 2} photocatalysts with larger surface area were prepared firstly by the gel-hydrothermal method. {yields} Surface coke carbon photosensitization effect is responsible for its high photocatalytic activity in the visible light irradiation. {yields} B-C synergistic effects play the major role in its effective photo-degradation of 2,4-DCP under the visible light. - Abstract: Carbon and boron co-doped TiO{sub 2} photocatalysts were prepared firstly by the gel-hydrothermal method, that is, synthesized through sol-gel process followed by hydrothermal in the glucose solution. The prepared photocatalysts were characterized by XRD, Raman spectra, TEM, N{sub 2} physical adsorption, XPS, and UV-vis absorption spectra. It was found that the co-doped TiO{sub 2} has a larger BET surface areas and a narrower band gap than undoped TiO{sub 2}. The experimental results show that the coke carbon generated on the carbon doped TiO{sub 2} surface act as a photosensitizer and has the photosensitization effect under the visible light. Except for carbon sensitization effect, the boron and carbon co-doped TiO{sub 2} has synergistic effect which is responsible for effective photo-degradation of 2,4-dichlorophenol in the visible light irradiation.

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

    Energy Technology Data Exchange (ETDEWEB)

    Hojamberdiev, Mirabbos, E-mail: mirabbos_uz@yahoo.com [Shaanxi Key Laboratory of Nano-materials and Technology, Xi' an University of Architecture and Technology, Xi' an 710055 (China); Zhu, Gangqiang [School of Physics and Information Technology, Shaanxi Normal University, Xi' an 710062 (China); Xu, Yunhua [Shaanxi Key Laboratory of Nano-materials and Technology, Xi' an University of Architecture and Technology, Xi' an 710055 (China)

    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.

  2. Influence of synthesis condition on product formation: hydrothermal auto-oxidated synthesis of five copper halides with ratio of Cu(I)/Cu(II) in 1:1, 2:1, 3:1, 4:1 and 1:0

    Science.gov (United States)

    Zhang, Shuai; Cao, Yanning; Zhang, Hanhui; Chai, Xiaochuan; Chen, Yiping; Sun, Ruiqing

    2008-12-01

    The hydrothermal synthesis and structural characterization of five copper iodides derived from chelated ligands, 1, 10-phenanthroline (phen), ethylenediamine (en) and 1, 3-propanediamine, are reported. Except monovalent copper compound 1 ((phen)Cu 3I 31), other four compounds ([Cu(phen) 2I][CuI 2] 2, [Cu(phen) 2I][Cu 3I 4] 3, [Cu(en) 2][Cu 4(phen) 2I 6] 4 and [Cu(1, 3-propanediamine) 2][CuI 2] 25) are mixed-valent Cu(I)-Cu(II) compounds by partially auto-oxidated from Cu(I). Supramolecular frameworks of these compounds can be assembled by C/N-H⋯I hydrogen bonds, Cu(I)-Cu(I) interaction, weak Cu-I semicoordinate interaction, C-H⋯ π and π- π stacking interactions. It's noteworthy that we find hydrothermal synthesis under higher pH value, higher synthesis temperature and longer reaction time can obtain higher ratio of Cu(I)/Cu(II) copper iodides and organic ligand with lower steric hinderance is prone to coordinated with divalent copper to form cation unit. Finally, the fluorescent study shows 1 exhibits intense orange-red luminescence with long lifetime at 293 K and more intense emission and longer lifetime at 77 K. Moreover, the room temperature EPR spectra of above five compounds not only show the valence of copper but demonstrate the coordination environment of Cu(II) centre.

  3. Ideas and perspectives: hydrothermally driven redistribution and sequestration of early Archaean biomass - the "hydrothermal pump hypothesis"

    Science.gov (United States)

    Duda, Jan-Peter; Thiel, Volker; Bauersachs, Thorsten; Mißbach, Helge; Reinhardt, Manuel; Schäfer, Nadine; Van Kranendonk, Martin J.; Reitner, Joachim

    2018-03-01

    Archaean hydrothermal chert veins commonly contain abundant organic carbon of uncertain origin (abiotic vs. biotic). In this study, we analysed kerogen contained in a hydrothermal chert vein from the ca. 3.5 Ga Dresser Formation (Pilbara Craton, Western Australia). Catalytic hydropyrolysis (HyPy) of this kerogen yielded n-alkanes up to n-C22, with a sharp decrease in abundance beyond n-C18. This distribution ( ≤ n-C18) is very similar to that observed in HyPy products of recent bacterial biomass, which was used as reference material, whereas it differs markedly from the unimodal distribution of abiotic compounds experimentally formed via Fischer-Tropsch-type synthesis. We therefore propose that the organic matter in the Archaean chert veins has a primarily microbial origin. The microbially derived organic matter accumulated in anoxic aquatic (surface and/or subsurface) environments and was then assimilated, redistributed and sequestered by the hydrothermal fluids (hydrothermal pump hypothesis).

  4. Recent progress in biocatalysis using supercritical carbon dioxide.

    Science.gov (United States)

    Matsuda, Tomoko

    2013-03-01

    The latest advances in biocatalysis using supercritical carbon dioxide (scCO(2)) are reviewed. Stability and stabilization methodologies of enzymes in scCO(2) as well as reactions for organic synthesis are described. Especially, varieties of examples for lipase-catalyzed synthesis of chiral compounds using scCO(2) are given. Furthermore, asymmetric reduction by alcohol dehydrogenase in scCO(2) and carboxylation by decarboxylase in scCO(2) are also introduced. Copyright © 2012 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.

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

    Energy Technology Data Exchange (ETDEWEB)

    Lara-García, Hugo A.; Romero-Ibarra, Issis C.; Pfeiffer, Heriberto, E-mail: pfeiffer@iim.unam.mx

    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.

  6. Facile one-step hydrothermal synthesis toward strongly coupled TiO2/graphene quantum dots photocatalysts for efficient hydrogen evolution

    International Nuclear Information System (INIS)

    Min, Shixiong; Hou, Jianhua; Lei, Yonggang; Ma, Xiaohua; Lu, Gongxuan

    2017-01-01

    Highlights: • TiO 2 /GQDs composites were prepared by a facile one-step hydrothermal method. • GQDs were strongly coupled onto the surface of TiO 2 nanoparticles by this method. • The TiO 2 /GQDs showed enhanced light absorption and charge separation efficiency. • The TiO 2 /GQDs exhibited higher photocatalytic H 2 evolution activity than pure TiO 2 . • GQDs play synergistic roles by acting as both photosensitizer and electron acceptor. - Abstract: The coupling of semiconductor photocatalysts with graphene quantum dots (GQDs) has been proven to be an effective strategy to enhance the photocatalytic and photoelectrical conversion performances of the resulted composites; however, the preparation of semiconductor/GQDs composites usually involves several time-inefficient and tedious post-treatment steps. Herein, we present a facile one-step hydrothermal route for the preparation of GQDs coupled TiO 2 (TiO 2 /GQDs) photocatalysts using 1,3,6-trinitropyrene (TNP) as the sole precursor of GQDs. During the hydrothermal process, TNP molecules undergo an intramolecular fusion to form GQDs, which simultaneously decorate on the surface of TiO 2 nanoparticles, leading to a strong surface interaction between the two components. The effective coupling of GQDs on TiO 2 can effectively extend the light absorption of the TiO 2 to visible region and enhance the charge separation efficiency of TiO 2 /GQDs composites as a result of GQDs acting as a photosensitizer and an excellent electron acceptor. These key advances make the TiO 2 /GQDs photocatalyst highly active towards the H 2 evolution reaction, resulting in 7 and 3 times higher H 2 evolution rate and photocurrent response at optimal GQDs content than TiO 2 alone, respectively. This study provides a new methodology for the development of high-performance GQDs modified semiconductor photocatalysts for energy conversion applications.

  7. Ionic liquid-assisted hydrothermal synthesis and excitation wavelength-dependent luminescence of YBO3:Eu3+ nano-/micro-crystals

    International Nuclear Information System (INIS)

    Tian, Yue; Tian, Bining; Chen, Baojiu; Cui, Cai’e; Huang, Ping; Wang, Lei; Hua, Ruinian

    2014-01-01

    Graphical abstract: Three dimensional (3D) architectures YBO 3 :Eu 3+ phosphors were prepared via ionic liquid assisted hydrothermal process. The pH values and ionic liquid play an important role on the morphology of products. Excitation wavelength-dependent luminescent behavior was found in the as-prepared tyre-like YBO 3 :Eu 3+ microspheres. Highlights: • YBO 3 :Eu 3+ phosphors were prepared via ionic liquid assisted hydrothermal process. • pH values and ionic liquid play an important role on the morphology of products. • Excitation wavelength-dependent luminescent behavior was found. -- Abstract: Three dimensional (3D) architectures YBO 3 :Eu 3+ phosphors were prepared via ionic liquid-assisted hydrothermal process and characterized by X-ray diffraction (XRD), field emission scanning electron microscope (FE-SEM) and photoluminescence (PL). The pH value and ionic liquid play an important role in the control of morphology of products. By comparing with the corresponding bulk, the tyre-like YBO 3 :5 mol%Eu 3+ microspheres demonstrate a red shift of the charge transfer band (CTB), appearance of a long excitation tail at the long wavelength side of the CTB and high improved chromaticity. Two Eu 3+ environments in the tyre-like sample, namely interior and outside Eu 3+ , were found by selective excitation under the different wavelength light. Finally, fluorescent decays and Judd–Ofelt (J–O) theory were utilized to analyze the local crystal environments around Eu 3+ ions in the tyre-like and bulk phosphors

  8. Hydrothermal synthesis of one-dimensional assemblies of Pt nanoparticles and their sensor application for simultaneous determination of dopamine and ascorbic acid

    Energy Technology Data Exchange (ETDEWEB)

    Wang Wei [Qingdao University of Science and Technology, Key Laboratory of Nanostructured Materials (China); Wang Qingxiang [Zhangzhou Normal University (China); Zhang Zhikun, E-mail: zhangzk@qust.edu.c [Qingdao University of Science and Technology, Key Laboratory of Nanostructured Materials (China)

    2008-12-15

    One-dimensional assemblies of Pt nanoparticles (NPs) with the size range of 10-20 nm have been synthesized via a simple hydrothermal route using soluble starch as both template and reducing agent. The formation mechanism of the product was studied in details. The electrochemical behavior of dopamine (DA) and ascorbic acid (AA) on the prepared one-dimensionally assembled Pt NPs modified glassy carbon electrode were studied by cyclic voltammetry (CV) and differential pulse voltammetry (DPV) techniques and showed satisfactory results for the simultaneous determination of DA and AA by resolving the overlapping voltammetric responses of DA and AA into two voltammetric peaks.

  9. Technology with Supercritical Fluid. Part 2. Applications

    International Nuclear Information System (INIS)

    Marongiu, B.; De Giorgi, M. R.; Porcedda, S.; Cadoni, E.

    1998-01-01

    The present article is based on a bibliographical analysis of the main applications of the supercritical fluid in various fields, as: extraction from solid matrices, division of liquid charges, chromatography HPLC with supercritical eluent, chemical and biochemical reactions in supercritical solvents etc [it

  10. ZnS/Ni{sub 2}P core/shell composites: Simple hydrothermal synthesis, characterization and its photocatalytic degradation of pyronine B

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Shuling, E-mail: shulingliu@aliyun.com [Key Laboratory of Auxiliary Chemistry & Technology for Chemical Industry, Ministry of Education, Shaanxi University of Science & Technology, Xi’an, Shaanxi 710021 (China); College of Chemistry & Chemical Engineering, Shaanxi University of Science & Technology, Xi’an, Shaanxi 710021 (China); Ma, Lanbing; Zhang, Hongzhe; Ma, Chenlu [Key Laboratory of Auxiliary Chemistry & Technology for Chemical Industry, Ministry of Education, Shaanxi University of Science & Technology, Xi’an, Shaanxi 710021 (China); College of Chemistry & Chemical Engineering, Shaanxi University of Science & Technology, Xi’an, Shaanxi 710021 (China)

    2016-05-15

    Highlights: • ZnS/Ni{sub 2}P composites have been firstly synthesized via a gentle hydrothermal route. • The composites have been characterized by XRD, SEM and TEM. • ZnS/Ni{sub 2}P showed enhanced photocatalytic degradation activity for pyronine B. • The reason for the enhanced photocatalytic activity has been discussed. - Abstract: ZnS/Ni{sub 2}P core/shell composites were successfully synthesized using a hydrothermal method. The composites have been characterized by XRD, SEM, TEM and the corresponding results showed that the composites were composed of the cubic ZnS microspheres, which were made up of ZnS nanoparticles, and Ni{sub 2}P nanoparticles coated on the surfaces of ZnS microspheres. Compared with ZnS microspheres, ZnS/Ni{sub 2}P core/shell composites showed enhanced photocatalytic degradation activity for pyronine B under UV irradiation. This may be related to the effective separation of photogenerated electron–hole pairs in ZnS/Ni{sub 2}P composites which can greatly reduce the chance of their recombination. Furthermore, superoxide ions and hydroxyl radical can be more easily produced through ZnS/Ni{sub 2}P composites, which is also beneficial for the degradation of pyronine B.

  11. Hydrothermal synthesis of NiCo{sub 2}O{sub 4} nanowires/nitrogen-doped graphene for high-performance supercapacitor

    Energy Technology Data Exchange (ETDEWEB)

    Yu, Mei, E-mail: yumei@buaa.edu.cn; Chen, Jianpeng; Ma, Yuxiao; Zhang, Jingdan; Liu, Jianhua; Li, Songmei; An, Junwei

    2014-09-30

    Highlights: • NCO/NG composites were synthesized in a water–glycerol mixed solvent via hydrothermal treatment and subsequent calcination. • NiCo{sub 2}O{sub 4} nanowires are dispersed on NG nanosheets and the composite has porous structure. • The NCO/NG composite exhibits a high specific capacitance and long cycling performance. - Abstract: NiCo{sub 2}O{sub 4} nanowires/nitrogen-doped graphene (NCO/NG) composite materials were synthesized by hydrothermal treatment in a water–glycerol mixed solvent and subsequent thermal transformation. The obtained materials were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy and Raman spectroscopy. The electrochemical performance of the composites was evaluated by cyclic voltammetry, galvanostatic charge/discharge and electrochemical impedance spectrum techniques. NiCo{sub 2}O{sub 4} nanowires are densely coated by nitrogen-doped graphene and the composite displays good electrochemical performance. The maximum specific capacitance of NCO/NG is 1273.13 F g{sup −1} at 0.5 A g{sup −1} in 6 M KOH aqueous solution, and it exhibits good capacity retention without noticeable degradation after 3000 cycles at 4 A g{sup −1}.

  12. Ultrasonic-assisted hydrothermal synthesis and catalytic behavior of a novel SAPO-34/Clinoptilolite nanocomposite catalyst for high propylene demand in MTO process

    Science.gov (United States)

    Moradiyan, Eshagh; Halladj, Rouein; Askari, Sima; Moghimpour Bijani, Parisa

    2017-08-01

    SAPO-34 as a catalyst has high selectivity and hydrothermal stability, but it is rapidly deactivated by the formation of coke in its micropores. Evaluating the natural Clinoptilolite capability as a binder in nanocomposite catalysts is of interest because of its low cost, and accelerating the reaction. The SAPO-34/Clinoptilolite (S/C) nanocomposite catalysts were synthesized via ultrasonic-assisted hydrothermal method using Clinoptilolite as a binder. Subsequent performance of the catalyst was investigated in the methanol to olefins (MTO) reaction. The structures of synthesized nanocomposite were characterized with several methods such as XRD, XRF, FESEM, TEM, NH3-TPD, FT-IR, and nitrogen adsorption techniques. The modified Clinoptilolite was attained using nitric acid treatment. Although the physicochemical analysis indicated that HNO3-treatment decreases the crystallinity of the Clinoptilolite, the specific surface area of natural zeolite enhances considerably from 20.07 to 187.8 m2/g. The nanocomposite catalysts showed high selectivity toward light olefins with 100% conversion and 90% selectivity to light olefins as desired products at 450 °C. Nanocomposite with the additional diffusion paths for mass transfer provided by binder-filled space ascend to higher catalytic lifetimes in compare with free SAPO-34 catalyst.

  13. Facile Br{sup -} assisted hydrothermal synthesis of Bi{sub 2}MoO{sub 6} nanoplates with enhanced visible-light photocatalytic activity

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Peng [Yangtze Normal University, Chongqing Key Laboratory of Inorganic Special Functional Materials, Chongqing (China); Yangtze Normal University, College of Chemistry and Chemical Engineering, Chongqing (China); Teng, Xiaoxu; Liu, Dongsheng; Fu, Liang; Xie, Hualin [Yangtze Normal University, College of Chemistry and Chemical Engineering, Chongqing (China); Zhang, Guoqing [Yangtze Normal University, Chongqing Key Laboratory of Inorganic Special Functional Materials, Chongqing (China); Ding, Shimin [Yangtze Normal University, Collaborative Innovation Center for Green Development in Wuling Mountain Areas, Chongqing (China)

    2017-10-15

    Bi{sub 2}MoO{sub 6} nanoplates have been controllably synthesized via a facile hydrothermal process with the assistance of Br{sup -} containing surfactant cetyltrimethylammonium bromide (CTAB) or KBr. A remarkable enhancement in the visible-light-driven photocatalytic degradation of Rhodamine B was observed. It was found that reaction temperature and surfactant play crucial roles in the formation and properties of the Bi{sub 2}MoO{sub 6} nanoplates. The best results as photocatalyst were obtained with the sample hydrothermally synthesized at 150 C with the assistance of CTAB. The improved photocatalytic performance could be ascribed to the {001}-oriented nanostructure of the Bi{sub 2}MoO{sub 6} nanoplates. KBr-templated Bi{sub 2}MoO{sub 6} nanoplates also showed better photocatalytic efficiency compared with that of flower-like Bi{sub 2}MoO{sub 6} but inferior to that of CTAB-templated Bi{sub 2}MoO{sub 6} nanoplates. (orig.)

  14. Mn{sup 4+}-activated BaSiF{sub 6} red phosphor: Hydrothermal synthesis and dependence of its luminescent properties on reaction conditions

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Qiang; Zhou, Yayun [Key Laboratory of Comprehensive Utilization of Mineral Resources in Ethnic Regions, Joint Research Centre for International Cross-border Ethnic Regions Biomass Clean Utilization in Yunnan, School of Chemistry & Environment, Yunnan Minzu University, Kunming, 650500 (China); Lu, Fengqi [MOE Key Laboratory of New Processing Technology for Nonferrous Metals and Materials, College of Materials Science and Engineering, Guilin University of Technology, Guilin, 541004 (China); Liu, Yong [Key Laboratory of Comprehensive Utilization of Mineral Resources in Ethnic Regions, Joint Research Centre for International Cross-border Ethnic Regions Biomass Clean Utilization in Yunnan, School of Chemistry & Environment, Yunnan Minzu University, Kunming, 650500 (China); Wang, Qin [College of Chemistry and Chemical Engineering, Yunnan Normal University, Kunming, Yunnan, 650500 (China); Luo, Lijun [Key Laboratory of Comprehensive Utilization of Mineral Resources in Ethnic Regions, Joint Research Centre for International Cross-border Ethnic Regions Biomass Clean Utilization in Yunnan, School of Chemistry & Environment, Yunnan Minzu University, Kunming, 650500 (China); Wang, Zhengliang, E-mail: wangzhengliang@foxmail.com [Key Laboratory of Comprehensive Utilization of Mineral Resources in Ethnic Regions, Joint Research Centre for International Cross-border Ethnic Regions Biomass Clean Utilization in Yunnan, School of Chemistry & Environment, Yunnan Minzu University, Kunming, 650500 (China)

    2016-02-15

    In this work, a series of BaSiF{sub 6}:Mn{sup 4+} red phosphors were synthesized through a hydrothermal route. The crystal structure and morphology were characterized by powder X-ray diffraction (XRD) with Rietveld refinement, scanning electron microscopy (SEM), and energy dispersive spectrometer (EDS) in detail. The influence of reaction conditions, including the concentration of KMnO{sub 4} and HF, reaction temperature and time, on the photoluminescence properties were investigated systematically. It can emit intense red light (∼636 nm) under blue light (∼458 nm) illumination. The white LED device based on YAG:Ce–BaSiF{sub 6}:Mn{sup 4+} mixture shows warm white light with low color temperature and high correlated color index, which reveals its potential application in WLED. - Highlights: • The crystal structure of BaSiF{sub 6}:Mn{sup 4+} has been verified using Rietveld refinement. • The optimum hydrothermal reaction condition for BaSiF{sub 6}:Mn{sup 4+} has been confirmed. • The white LED based on YAG:Ce–BaSiF{sub 6}:Mn{sup 4+} mixture presents warmer white light than that only with YAG:Ce.

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

    Directory of Open Access Journals (Sweden)

    Ivan Velasco-Davalos

    2016-06-01

    Full Text Available 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 (SrO34− 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(NO33 and Fe(NO33 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.

  16. Hydrothermal synthesis and properties of NiFe2O4@BaTiO3 composites with well-matched interface

    Science.gov (United States)

    Zhou, Jian-Ping; Lv, Li; Liu, Qian; Zhang, Yu-Xiang; Liu, Peng

    2012-08-01

    NiFe2O4@BaTiO3 multiferroic composite particles were produced by a simple hydrothermal method in two steps: preparing NiFe2O4 nanoparticles and then synthesizing core-shell nanocomposites. Multiferroic composite ceramics were sintered from these powders. X-ray diffraction, Raman scattering and energy dispersive x-ray analyses indicated that the core-shell composites with a NiFe2O4 core and BaTiO3 shell were formed in the hydrothermal environment. Different types of sharp interfaces were self-assembled owing to the minimization of direct elastic energy. The saturation magnetization of the composites linearly increased with the NiFe2O4 content while the dielectric constant decreased. A dielectric peak appeared at around 460 °C because of the oxygen vacancies in the BaTiO3 ceramics. It resulted in an enhancement of magnetic permeability in the composites, indicating magnetoelectric coupling that was also observed by direct magnetoelectric measurements.

  17. Controllable synthesis of Bi2WO6 nanoplate self-assembled hierarchical erythrocyte microspheres via a one-pot hydrothermal reaction with enhanced visible light photocatalytic activity

    Science.gov (United States)

    Yang, Zhenya; Huang, Lin; Xie, Yanyu; Lin, Zheguan; Fan, Yunyan; Liu, Dan; Chen, Lu; Zhang, Zizhong; Wang, Xuxu

    2017-05-01

    This work provides a simple approach of the F--assisted one-pot hydrothermal reaction to successfully synthesize Bi2WO6 hierarchical erythrocyte microspheres. The importance role of F- was systematically investigated by comparing different type of halogen ions, hydrothermal temperature and time. The possible growth mechanism of Bi2WO6 hierarchical structures was proposed. The hierarchical erythrocytes were formed through the well-ordered and oriented self-assembly of thin Bi2WO6 nanoplate primary subunits. F- ions were absorbed on Bi2WO6 nanoplate surface to suppress the nanoplate stack but to induce a self-assembly through the edge interaction of Bi2WO6 nanoplates into erythrocyte-like hierarchical microspheres superstructures. This erythrocyte structure narrowed the band gap energy and enhanced the visible-light photocatalytic activity of Bi2WO6. Moreover, superoxide radical anions and h+ were revealed as the main active species responding for the RhB degradation on Bi2WO6 under visible light irradiation.

  18. Supercritical Fluid Reactions for Coal Processing

    Energy Technology Data Exchange (ETDEWEB)

    Charles A. Eckert

    1997-11-01

    Exciting opportunities exist for the application of supercritical fluid (SCF) reactions for the pre-treatment of coal. Utilizing reactants which resemble the organic nitrogen containing components of coal, we developed a method to tailor chemical reactions in supercritical fluid solvents for the specific application of coal denitrogenation. The tautomeric equilibrium of a Schiff base was chosen as one model system and was investigated in supercritical ethane and cosolvent modified supercritical ethane. The Diels-Alder reaction of anthracene and 4-phenyl-1,2,4-triazoline-3,5-dione (PTAD) was selected as a second model system, and it was investigated in supercritical carbon dioxide.

  19. Facile one-step hydrothermal synthesis toward strongly coupled TiO{sub 2}/graphene quantum dots photocatalysts for efficient hydrogen evolution

    Energy Technology Data Exchange (ETDEWEB)

    Min, Shixiong, E-mail: sxmin@nun.edu.cn [School of Chemistry and Chemical Engineering, Beifang University of Nationalities, Yinchuan, 750021, Ningxia Province (China); Hou, Jianhua; Lei, Yonggang; Ma, Xiaohua [School of Chemistry and Chemical Engineering, Beifang University of Nationalities, Yinchuan, 750021, Ningxia Province (China); Lu, Gongxuan [State Key Laboratory for Oxo Synthesis and Selective Oxidation, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou, 730000 (China)

    2017-02-28

    Highlights: • TiO{sub 2}/GQDs composites were prepared by a facile one-step hydrothermal method. • GQDs were strongly coupled onto the surface of TiO{sub 2} nanoparticles by this method. • The TiO{sub 2}/GQDs showed enhanced light absorption and charge separation efficiency. • The TiO{sub 2}/GQDs exhibited higher photocatalytic H{sub 2} evolution activity than pure TiO{sub 2}. • GQDs play synergistic roles by acting as both photosensitizer and electron acceptor. - Abstract: The coupling of semiconductor photocatalysts with graphene quantum dots (GQDs) has been proven to be an effective strategy to enhance the photocatalytic and photoelectrical conversion performances of the resulted composites; however, the preparation of semiconductor/GQDs composites usually involves several time-inefficient and tedious post-treatment steps. Herein, we present a facile one-step hydrothermal route for the preparation of GQDs coupled TiO{sub 2} (TiO{sub 2}/GQDs) photocatalysts using 1,3,6-trinitropyrene (TNP) as the sole precursor of GQDs. During the hydrothermal process, TNP molecules undergo an intramolecular fusion to form GQDs, which simultaneously decorate on the surface of TiO{sub 2} nanoparticles, leading to a strong surface interaction between the two components. The effective coupling of GQDs on TiO{sub 2} can effectively extend the light absorption of the TiO{sub 2} to visible region and enhance the charge separation efficiency of TiO{sub 2}/GQDs composites as a result of GQDs acting as a photosensitizer and an excellent electron acceptor. These key advances make the TiO{sub 2}/GQDs photocatalyst highly active towards the H{sub 2} evolution reaction, resulting in 7 and 3 times higher H{sub 2} evolution rate and photocurrent response at optimal GQDs content than TiO{sub 2} alone, respectively. This study provides a new methodology for the development of high-performance GQDs modified semiconductor photocatalysts for energy conversion applications.

  20. Studies on hydrothermal synthesis of photolumniscent rare earth (Eu3+ & Tb3+) doped NG@FeMoO4 for enhanced visible light photodegradation of methylene blue dye

    Science.gov (United States)

    Singh, R.; Kumar, M.; Khajuria, H.; Sharma, S.; Sheikh, H. Nawaz

    2018-02-01

    FeMoO4 nanorods and their rare earth (Eu3+ and Tb3+) doped composites with nitrogen doped graphene (NG) were synthesized by facile hydrothermal method in aqueous medium. X-ray diffraction (XRD) analysis of the as-synthesized samples was done to study the phase purity and crystalline nature. FTIR and Raman Spectroscopy have been studied for investigating the bonding in nanostructures. The surface morphology of the samples was investigated with field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The photolumniscent nature of the samples was investigated by the using the fluorescence spectrophotometer. The photocatalytic degradation efficiency of the prepared pure FeMoO4 and its rare earth doped composites with nitrogen doped graphene was evaluated as function of visible light irradiation versus concentration of methylene blue (MB dye). The prepared nanocomposites show enhanced photocatalytic efficiency as compared to the bare FeMoO4 nanorods.