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Sample records for template-free solvothermal synthesis

  1. Template-free solvothermal synthesis of 3D hierarchical nanostructured boehmite assembled by nanosheets

    Science.gov (United States)

    Li, Guangci; Guan, Lili; Liu, Yunqi; Liu, Chenguang

    2012-09-01

    In the absence of template and surfactant, hierarchical nanostructured boehmite was synthesized via a simple solvothermal route using aluminum nitrate as aluminum source and isopropanol-toluene mixture as solvent. The crystal structures, morphologies and textural properties of products were characterized by X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Scanning electron microscopy (SEM), Transmission electron microscopy (TEM) and N2 adsorption-desorption technique. The as-obtained hierarchical nanostructures consist of nanosheets keeping Brunauer-Emmett-Teller (BET) specific surface area and pore volume of ca. 264.7 m2/g and 1.2 cm3/g, respectively. The experimental results show that the longer reaction time and the lower reaction temperature are unfavorable to the formation of hierarchical nanostructures. Moreover, the properties of solvent have important influence on the morphology of product. The possible formation mechanism of boehmite hierarchical nanostructures was proposed and discussed.

  2. ROOM TEMPERATURE BULK AND TEMPLATE-FREE SYNTHESIS OF LEUCOEMARLDINE POLYANILINE NANOFIBERS

    Science.gov (United States)

    Herein, we describe a simple strategy for the bulk and template-free synthesis of reduced leucoemarldine polyaniline nanofibers size ranging from as low as 10 nm to 50 nm without the use of any reducing agents at room temperature.

  3. organic template free synthesis of zsm11 from kaolinite clay

    African Journals Online (AJOL)

    user

    Synthesis of zeolitic materials from mineral ores, encounter serious challenges due to the presence of inherent impurities with the tendencies of inhibiting formation of desired products. Structure directing agent (SDA) though helps to mitigate this effect, but impact negatively on the environment. Zeolite ZSM11 is a promising ...

  4. Hierarchically porous MgCo2O4 nanochain networks: template-free synthesis and catalytic application

    Science.gov (United States)

    Guan, Xiangfeng; Yu, Yunlong; Li, Xiaoyan; Chen, Dagui; Luo, Peihui; Zhang, Yu; Guo, Shanxin

    2018-01-01

    In this work, hierarchically porous MgCo2O4 nanochain networks were successfully synthesized by a novel template-free method realized via a facile solvothermal synthesis followed by a heat treatment. The morphologies of MgCo2O4 precursor could be adjusted from nanosheets to nanobelts and finally to interwoven nanowires, depending on the volume ratio of diethylene glycol to deionized water in the solution. After calcination, the interwoven precursor nanowires were transformed to hierarchical MgCo2O4 nanochain networks with marco-/meso-porosity, which are composed of 10-20 nm nanoparticles connected one by one. Moreover, the relative formation mechanism of the MgCo2O4 nanochain networks was discussed. More importantly, when evaluated as catalytic additive for AP thermal decomposition, the MgCo2O4 nanochain networks show excellent accelerating effect. It is benefited from the unique hierarchically porous network structure and multicomponent effect, which effectively accelerates ammonia oxidation and {{{{ClO}}}4}- species dissociation. This approach opens the way to design other hierarchically porous multicomponent metal oxides.

  5. 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.

  6. Template-free synthesis of CoMoO{sub 4} rods and their characterization

    Energy Technology Data Exchange (ETDEWEB)

    Rico, J.L., E-mail: jlrico@umich.mx [Laboratorio de Catálisis, Facultad de Ingeniería Química, Universidad Michoacana de San Nicolás de Hidalgo, Edificio V1, CU, Morelia Mich C.P. 58060 (Mexico); Ávalos-Borja, M. [Centro de Nanociencias y Nanotecnología, UNAM, Ensenada, B.C. (Mexico); Barrera, A. [Laboratorio de Nanomateriales, Universidad de Guadalajara, CUCI, Ocotlán, Jal. (Mexico); Hargreaves, J.S.J. [WestCHEM, School of Chemistry, Joseph Black Building, University of Glasgow, Glasgow G12 8QQ (United Kingdom)

    2013-11-15

    Graphical abstract: - Highlights: • Template-free synthesis of rods of CoMoO{sub 4} was achieved under hydrothermal conditions. • The width of the rods is about 100 nm and the length varies from 1 to 5 μm. • Low temperature and pressure of synthesis favour the formation of longer rods. - Abstract: The effect of pressure and temperature on the synthesis of cobalt-molybdenum oxides and their characterisation is herein reported. The synthesis was performed under hydrothermal conditions without any template. It was found that the experimental conditions affect the physical properties of the CoMoO{sub 4}. SEM images demonstrate that the synthesised powder is comprised of rods, and the width of the structures is about 100 nm but the length varies from about 5 μm to less than 1 μm. Low temperature and pressure favour the formation of longer rods.

  7. Template-free synthesis of beta-In2S3 superstructures and their photocatalytic activity.

    Science.gov (United States)

    Amutha, R; Akilandeswari, S; Ahmmad, Bashir; Muruganandham, M; Sillanpää, Mika

    2010-12-01

    In this article, we have successfully fabricated various morphological beta-Indium sulfide (In2S3) superstructures by using indium thiocyanate complex at acidic pH. All the synthesis has been performed by a template-free, hydrothermal method at 195 degrees C for 3 h. The photocatalytic activity of synthesized In2S3 have been investigated by using UV-B (lamda = 365 nm) light with Methyl Orange dye as a model pollutant. The synthesized photocatalyst was characterized by using XRD, FE-SEM, HR-TEM, DRS spectra and nitrogen adsorption analysis. The influence of indium precursors and solvents on the morphology as well as the surface properties has also been discussed. The XRD result shows that cubic phase beta-In2S3 formed under all experimental conditions. A plausible mechanism of the In2S3 microsphere formation has been discussed based on experimental observations.

  8. Facile and template-free method toward chemical synthesis of polyaniline film/nanotube structures

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Pei [Department of Electrical and Computer Engineering, Swanson School of Engineering, University of Pittsburgh, Pittsburgh Pennsylvania 15261; Zhu, Yisi [Materials Science Division, Argonne National Lab, Lemont Illinois 60439; Torres, Jorge [Department of Electrical and Computer Engineering, Swanson School of Engineering, University of Pittsburgh, Pittsburgh Pennsylvania 15261; Lee, Seung Hee [Department of BIN Fusion Technology, Chonbuk National University, Jeonju 561-786 Korea; Yun, Minhee [Department of Electrical and Computer Engineering, Swanson School of Engineering, University of Pittsburgh, Pittsburgh Pennsylvania 15261

    2017-09-05

    A facile and template-free method is reported to synthesize a new thin film structure: polyaniline (PANI) film/nanotubes (F/N) structure. The PANI F/N is a 100-nm thick PANI film embedded with PANI nanotubes. This well-controlled method requires no surfactant or organic acid as well as relatively low concentration of reagents. Synthesis condition studies reveal that aniline oligomers with certain structures are responsible for guiding the growth of the nanotubes. Electrical characterization also indicates that the PANI F/N possesses similar field-effect transistor characteristics to bare PANI film. With its 20% increased surface-area-to-volume (S/V) ratio contributed by surface embedded nanotubes and the excellent p-type semiconducting characteristic, PANI F/N shows clear superiority compared with bare PANI film. Such advantages guarantee the PANI F/N a promising future toward the development of ultra-high sensitivity and low-cost biosensors.

  9. One-step template-free synthesis of monoporous polymer microspheres with uniform sizes via microwave-mediated dispersion polymerization.

    Science.gov (United States)

    Zhu, Ming-Qiang; Chen, Gan-Chao; Li, Yun-Mei; Fan, Jun-Bing; Zhu, Ming-Feng; Tang, Zhiyong

    2011-11-01

    One-step facile synthesis of monoporous polymer microspheres via microwave-controlled dispersion polymerization is introduced. This template-free method employing the dispersion polymerization of styrene under microwave irradiation induces directly the formation of uniform monoporous polymer microspheres, with controllable morphologies and sizes, which can be tuned by simply adjusting parameters for the synthesis. A comparison to conventional heating indicates that microwave irradiation plays a vital role in the formation of this novel morphology.

  10. 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.

  11. Large-scale template-free synthesis of ordered mesoporous platinum nanocubes and their electrocatalytic properties.

    Science.gov (United States)

    Cao, Yanqin; Yang, Yong; Shan, Yufeng; Fu, Chaoli; Long, Nguyen Viet; Huang, Zhengren; Guo, Xiangxin; Nogami, Masayuki

    2015-12-14

    Here we report a facile, one-pot and template-free approach to synthesize mesoporous monocrystalline Pt nanocubes with uniform shapes and sizes, in which small Pt particles with a size of ∼5 nm are three-dimensionally and periodically built up into cubes with a size of ∼50 nm. The forming process is illustrated through a novel meso-crystal self-assembly mechanism. Very interestingly, the mesoporous structures are ordered, which are thought to be beneficial to increase their catalytic activity. Compared with nonporous Pt nanoparticles and porous Pt nanoparticles without order, the ordered mesoporous Pt nanocubes exhibit a highly improved electrocatalytic ability for methanol and formic acid oxidation, and are potentially applicable as electrocatalysts for direct methanol and formic acid fuel cells. Furthermore, this approach can be used to synthesize other Pt-series metallic mesoporous nanoparticles, such as Pd.

  12. Template-free Synthesis of One-dimensional Cobalt Nanostructures by Hydrazine Reduction Route

    Science.gov (United States)

    Zhang, Liying; Lan, Tianmin; Wang, Jian; Wei, Liangmin; Yang, Zhi; Zhang, Yafei

    2011-12-01

    One-dimensional cobalt nanostructures with large aspect ratio up to 450 have been prepared via a template-free hydrazine reduction route under external magnetic field assistance. The morphology and properties of cobalt nanostructures were characterized by scanning electron microscopy, X-ray diffractometer, and vibrating sample magnetometer. The roles of the reaction conditions such as temperature, concentration, and pH value on morphology and magnetic properties of fabricated Co nanostructures were investigated. This work presents a simple, low-cost, environment-friendly, and large-scale production approach to fabricate one-dimensional magnetic Co materials. The resulting materials may have potential applications in nanodevice, catalytic agent, and magnetic recording.

  13. Organic template free synthesis of ZSM11 from kaolinite clay | Ajayi ...

    African Journals Online (AJOL)

    Synthesis of zeolitic materials from mineral ores, encounter serious challenges due to the presence of inherent impurities with the tendencies of inhibiting formation of desired products. Structure directing agent (SDA) though helps to mitigate this effect, but impact negatively on the environment. Zeolite ZSM11 is a promising ...

  14. Template-free synthesis of sub-micrometric cobalt fibers with controlled shape and structure. Characterization and magnetic properties

    Energy Technology Data Exchange (ETDEWEB)

    Lakhdar, Allagui [Laboratoire de Physique des Matériaux Lamellaires et Nano-Matériaux Hybrides, Faculté des Sciences de Bizerte, Université de Carthage, 7021 Bizerte (Tunisia); Borges, Joao P. [i3N/CENIMAT, Department of Materials Science, Faculty of Science and Technology, Universidade NOVA de Lisboa, Campus de Caparica, 2829-516 Caparica (Portugal); Ben Haj Amara, Abdesslam [Laboratoire de Physique des Matériaux Lamellaires et Nano-Matériaux Hybrides, Faculté des Sciences de Bizerte, Université de Carthage, 7021 Bizerte (Tunisia); Dakhlaoui-Omrani, Amel, E-mail: dakhlaoui_amel@yahoo.fr [Department of Chemistry, Faculty of Sciences and Arts-Khulais, University of Jeddah, Khulais, P. O. Box 355, Postal Code 21921 (Saudi Arabia); Laboratoire de Physico-Chimie des Matériaux Minéraux et leurs Applications, Centre National des Recherches en Sciences des Matériaux, Technopôle de Bordj Cedria, BP 73, 8027 Soliman (Tunisia)

    2017-03-01

    Sub-micrometric Co fibers were prepared via a modified polyol process at 90 °C under an external magnetic field of about 550 Oe, using ethelyne glycol as solvent and hydrazine as reducing agent. The structure, the size and the morphology of the as-elaborated products were highly controlled through properly monitoring the synthesis parameters (amount of NaOH added, the amount of the reducing agent, precursor’ concentration and precursors mixing protocol). The XRD characterization confirmed the formation of pure cobalt powders with either hexagonal compact (hcp) or face-centered-cubic (fcc) structure depending on the concentration of the metal precursor and sodium hydroxide. The scanning electron microscopy observations of the powders shows sub-micrometric fibers with about 0.4–0.6 µm in diameter and a length that could reach 15 µm. Fibers prepared at high reducing ratio were constituted of flower-like spheres that coalesce in the direction of the applied magnetic field. For their high contact surface, these fibers offer new opportunities for catalysis applications. The hysteresis loop measurements show an enhancement of the Hc of the as-obtained fibers compared to their bulk counterparts and permit to confirm the relationship between the structure and the magnetic properties of the materials. - Highlights: • Template free synthesis of cobalt sub-micrometric fibers. • High control of the structure the structure, the size and the morphology of the products through properly monitoring the synthesis parameters. • cobalt sub-micrometric fibers with enhanced magnetic properties compared to bulk cobalt.

  15. Template-free synthesis of functional 3D BN architecture for removal of dyes from water.

    Science.gov (United States)

    Liu, Dan; Lei, Weiwei; Qin, Si; Chen, Ying

    2014-03-25

    Three-dimensional (3D) architectures are of interest in applications in electronics, catalysis devices, sensors and adsorption materials. However, it is still a challenge to fabricate 3D BN architectures by a simple method. Here, we report the direct synthesis of 3D BN architectures by a simple thermal treatment process. A 3D BN architecture consists of an interconnected flexible network of nanosheets. The typical nitrogen adsorption/desorption results demonstrate that the specific surface area for the as-prepared samples is up to 1156 m(2) g(-1), and the total pore volume is about 1.17 cm(3) g(-1). The 3D BN architecture displays very high adsorption rates and large capacities for organic dyes in water without any other additives due to its low densities, high resistance to oxidation, good chemical inertness and high surface area. Importantly, 88% of the starting adsorption capacity is maintained after 15 cycles. These results indicate that the 3D BN architecture is potential environmental materials for water purification and treatment.

  16. Surfactant and template free synthesis of porous ZnS nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Akhtar, Muhammad Saeed [Division of Science and Technology, University of Education, College Road Township, Lahore (Pakistan); Schools of Materials, The University of Manchester, Oxford Road, Manchester M13 9PL (United Kingdom); Riaz, Saira [Centre of Excellence in Solid State Physics, University of the Punjab, Lahore-54590 (Pakistan); Mehmood, Rana Farhat [University of Education, Lahore, D.G. Khan Campus, Kangan Road, Dera Ghazi Khan (Pakistan); Ahmad, Khuram Shahzad [Environmental Sciences Department, Fatima Jinnah Women University, The Mall, Rawalpindi (Pakistan); Alghamdi, Yousef [Department of Chemistry, Faculty of Science & Art –Rabigh, King Abdulaziz University, Jeddah (Saudi Arabia); Malik, Mohammad Azad, E-mail: Azad.malik@manchester.ac.uk [Schools of Materials, The University of Manchester, Oxford Road, Manchester M13 9PL (United Kingdom); Department of Chemistry, University of Zululand, Private Bag X1001, Kwa-Dlangezwa, 3886 (South Africa); Naseem, Shahzad [Centre of Excellence in Solid State Physics, University of the Punjab, Lahore-54590 (Pakistan)

    2017-03-01

    ZnS thin films composed of porous nanoparticles have been deposited on to glass substrates by combining three simple synthesis methodologies i.e. chemical bath deposition, co-precipitation and spin coating. The XRD results reveal the cubic phase of ZnS thin films crystallized at nano scale. The crystallite size estimated by Scherrer formula was 3.4 nm. The morphology of the samples was analyzed through scanning electron microscopy (SEM) and is evident that thin films are composed of porous nanoparticles with an average size of 150 nm and pores of 40 nm on almost every grain. Crystallinity, phase and morphology were further confirmed via transmission electron microscopy (TEM). The stoichiometry and phase purity of thin films were determined by energy dispersive X-ray (EDX) spectrum and X-ray photoelectron spectroscopy (XPS) analysis, respectively. The surface topography and homogeneity of thin films were analyzed by atomic force microscopy (AFM) and obtained root mean square roughness (4.0326 nm) reveals the morphologically homogeneous growth of ZnS on glass substrates. The UV–Vis spectroscopy and photoluminescence (PL) were carried out to estimate the band gap and observe the emission spectra in order to speculate the viability of ZnS porous nanoparticles in optoelectronic devices and sensors. - Highlights: • ZnS thin films composed of porous nanoparticles have been deposited. • Methodology is based on a combination of three techniques. • Cubic phase ZnS nanoparticles deposited onto glass substrates. • Films characterized by UV/Vis, PL, XRD, SEM, TEM, AFM and XPS.

  17. Surfactant and template free synthesis of porous ZnS nanoparticles

    International Nuclear Information System (INIS)

    Akhtar, Muhammad Saeed; Riaz, Saira; Mehmood, Rana Farhat; Ahmad, Khuram Shahzad; Alghamdi, Yousef; Malik, Mohammad Azad; Naseem, Shahzad

    2017-01-01

    ZnS thin films composed of porous nanoparticles have been deposited on to glass substrates by combining three simple synthesis methodologies i.e. chemical bath deposition, co-precipitation and spin coating. The XRD results reveal the cubic phase of ZnS thin films crystallized at nano scale. The crystallite size estimated by Scherrer formula was 3.4 nm. The morphology of the samples was analyzed through scanning electron microscopy (SEM) and is evident that thin films are composed of porous nanoparticles with an average size of 150 nm and pores of 40 nm on almost every grain. Crystallinity, phase and morphology were further confirmed via transmission electron microscopy (TEM). The stoichiometry and phase purity of thin films were determined by energy dispersive X-ray (EDX) spectrum and X-ray photoelectron spectroscopy (XPS) analysis, respectively. The surface topography and homogeneity of thin films were analyzed by atomic force microscopy (AFM) and obtained root mean square roughness (4.0326 nm) reveals the morphologically homogeneous growth of ZnS on glass substrates. The UV–Vis spectroscopy and photoluminescence (PL) were carried out to estimate the band gap and observe the emission spectra in order to speculate the viability of ZnS porous nanoparticles in optoelectronic devices and sensors. - Highlights: • ZnS thin films composed of porous nanoparticles have been deposited. • Methodology is based on a combination of three techniques. • Cubic phase ZnS nanoparticles deposited onto glass substrates. • Films characterized by UV/Vis, PL, XRD, SEM, TEM, AFM and XPS.

  18. Template-free synthesis of fully collapsed carbon nanotubes and graphene nanoribbons by chemical vapor deposition

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Yong-Xing [School of Physics and Electronic Information, Huaibei Normal University, Huaibei 235000 (China); Jia, Yong, E-mail: yjiaahedu@163.com [School of Pharmacy, Anhui University of Chinese Medicine, Hefei 230012 (China)

    2015-12-01

    Highlights: • Commercial Fe{sub 2}O{sub 3} and Al{sub 2}O{sub 3} powders were chosen to prepare Fe{sub 2}O{sub 3}/Al{sub 2}O{sub 3} catalyst. • Fully collapsed carbon nanotubes and graphene nanoribbons were synthesized through the catalytic decomposition of methane at 900 °C. • The formation mechanism of the fully collapsed carbon nanotubes was revealed. - Abstract: Fe{sub 2}O{sub 3}/Al{sub 2}O{sub 3} catalyst was prepared by simply calcining the mixture of commercial Fe{sub 2}O{sub 3} and Al{sub 2}O{sub 3} powders at 1000 °C. The obtained Fe{sub 2}O{sub 3}/Al{sub 2}O{sub 3} catalyst shows high efficiency for the synthesis of fully collapsed carbon nanotubes and graphene nanoribbons through the catalytic decomposition of methane at 900 °C. The yield of the fully collapsed carbon nanotubes and graphene nanoribbons was 19.5 wt%. Field emission scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy and thermal gravimetric analysis were used to characterize the products. A tip-growth mechanism for the fully collapsed carbon nanotubes was suggested based on the SEM and TEM images of products produced at the initial stage. The break through of the catalyst particle from graphite layers resulted in the crack and then cut open of the fully collapsed carbon nanotubes, which further resulted in the formation of the graphene nanoribbons.

  19. Lanthanide Coordination Polymer Nanosheet Aggregates: Solvothermal Synthesis and Downconversion Luminescence

    Directory of Open Access Journals (Sweden)

    Rui-Rui Su

    2016-01-01

    Full Text Available A lanthanide coordination polymers (CPs nanostructure (1 has been synthesized via a facile template-free solvothermal strategy using DMF as solvent and 2-methyl benzoic acid (2-MeBAH as ligands. The products are characterized by powder X-ray diffraction (PXRD, scanning electron microscopy (SEM, elemental analyses (EA, and downward luminescence. Product 1 built from Tb3+ and 2-MeBAH has one-dimensional structure which is connected by trinuclear second building units (SBUs. Downward luminescence shows that sample 1 exhibits characteristic transitions of the Tb3+ ion at 489, 544, 583, and 621 nm, and the strongest peak is at 544 nm ascribed to the transition of D45→F57 of Tb3+.

  20. Solvothermal synthesis of high molecular weight dithienogermole ...

    Indian Academy of Sciences (India)

    dithiadiazole alternate polymers were synthesized by the solvothermal method. Optical properties and molecular weight were investigated by UV–Vis absorption spectroscopy and Gel Permeation Chromatography. Compared with the results achieved ...

  1. Solvothermal synthesis and characterization of CZTS nanocrystals

    Science.gov (United States)

    Dumasiya, Ajay; Shah, N. M.

    2017-05-01

    Cu2ZnSnS4 (CZTS) is a promising thin film absorber material for low cost solar cell applications. CZTS nanoparticle ink synthesized using solvothermal route is an attractive option to deposit absorber layer using screen printing or spin coating method in CZTS thin film solar cell. In this study we have synthesized CZTS nanocrystals using solvothermal method from aqueous solution of Copper nitrate [Cu(NO3)2], Zinc nitrate [Zn(NO3)2], tin chloride [SnCl4] and thiourea with varying concentration of Cu(NO3)2 (viz 0.82 mmol,1.4 mmol, 1.7 mmol) keeping concentrations of rest of solutions constant. As synthesized CZTS nanocrystals are characterized using Energy Dispersive Analysis of X-rays (EDAX) to verify stoichiometry of elements. Analysis of EDAX data suggests that CZTS nanocrystals having Copper nitrate [Cu (NO3)2] concentration of 1.4 m mole is near stoichiometric. X-ray diffraction analysis study of CZTS nanocrystals having Copper nitrate [Cu (NO3)2] concentration of 1.4 m mole reveals the preferred orientation of the grains in (112), (220) and (312) direction confirming Kesterite structure of CZTS.

  2. In situ studies of solvothermal synthesis of energy materials.

    Science.gov (United States)

    Jensen, Kirsten M Ø; Tyrsted, Christoffer; Bremholm, Martin; Iversen, Bo B

    2014-06-01

    Solvothermal and hydrothermal synthesis, that is, synthesis taking place in a solvent at elevated temperature and pressure, is a powerful technique for the production of advanced energy materials as it is versatile, cheap, and environmentally friendly. However, the fundamental reaction mechanisms dictating particle formation and growth under solvothermal conditions are not well understood. In order to produce tailor-made materials with specific properties for advanced energy technologies, it is essential to obtain an improved understanding of these processes and, in this context, in situ studies are an important tool as they provide real time information on the reactions taking place. Here, we present a review of the use of powder diffraction and total scattering methods for in situ studies of synthesis taking place under solvothermal and hydrothermal conditions. The experimental setups used for in situ X-ray and neutron studies are presented, and methods of data analysis are described. Special attention is given to the methods used to extract structural information from the data, for example, Rietveld refinement, whole powder pattern modelling and pair distribution function analysis. Examples of in situ studies are presented to illustrate the types of chemical insight that can be obtained. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. 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.

  4. One-pot template-free synthesis of monodisperse zinc sulfide hollow spheres and their photocatalytic properties.

    Science.gov (United States)

    Yu, Xiaoxiao; Yu, Jiaguo; Cheng, Bei; Huang, Baibiao

    2009-07-06

    Monodisperse wurtzite ZnS hollow spheres with diameters of about 200 nm and shells composed of nanoparticles have been successfully synthesized in high yield by a one-pot template-free hydrothermal route. The reaction duration, reactant species, and reaction temperature have been shown to play important roles in the formation of ZnS hollow spheres. X-ray diffraction, scanning and transmission electron microscopy, nitrogen adsorption/desorption, UV/Vis diffuse reflectance spectroscopy, and photoluminescence were used to characterize the products. The results show that all the prepared nanospheres have hexagonal wurtzite structures and exhibit good size uniformity and regularity. A mechanism for the formation of the ZnS hollow spherical structure by localized Ostwald ripening has been proposed based on experimental observations. In addition, studies of the photocatalytic properties of the ZnS hollow spheres by exposure to UV irradiation have demonstrated that they have potential photocatalytic applications. Hydroxyl radicals (*OH) were not detected on the surface of UV-illuminated ZnS by the photoluminescence technique, which suggests that *OH is not the dominant photo-oxidant and a photogenerated hole could instead directly participate in the photocatalytic reaction. The prepared ZnS hollow spheres are also of great interest for use in flat displays, sensors, lasers, catalysis, separation technology, biomedical engineering, and nanotechnology.

  5. Synthesis of alumina powders by precipitation method and solvothermal treatment

    International Nuclear Information System (INIS)

    Politchuk, J.O.; Lima, N.B.; Lazar, D.R.R.; Ussui, V.; Yoshito, W.K.

    2012-01-01

    The improvement of alumina powders synthesis processes has been focused on the preparation of ceramic powders with well defined crystalline structure and with high specific surface area and nanometric particle size without formation of hard agglomerates. For this purpose the precipitation step should be studied and and also the temperature of alumina crystallization should be reduced. The aim of this study was to obtain alumina powders by hydroxide precipitation with ammonia in the presence of cationic surfactant, followed by solvothermal treatment and calcination. The powders were characterized by TG/DTA, X-ray diffraction, surface area measurements by gas adsorption (BET) and scanning electron microscopy. The results showed that powders produced by solvothermal treatment without surfactant have higher crystallinity. However the presence of CTAB enhances 240% the specific surface area compared with powders produced without this reagent (author)

  6. Template-free synthesis of two-dimensional titania/titanate nanosheets as electrodes for high-performance supercapacitor applications

    Science.gov (United States)

    Barai, Hasi Rani; Rahman, Md. Mahbubur; Joo, Sang Woo

    2017-12-01

    Template-free two-dimensional (2D) titania/titanate nanosheets on Ti metal foil (TiNS/Ti) is prepared by a hydrothermal method at 150 °C assisted by KOH(aq.),followed by sintering at 500 °C. A single thin layer of TiNS is grown with 2D morphology when using low concentrations of KOH(aq.) (0.25 and 0.5 M). However, the morphology is transformed to 1D when using a high concentration of KOH(aq.). The TiNS is a mixture of rutile TiO2 and K-titanate (K2Ti3O7 and K2Ti2O5) with the formation of Ti3+ interstitials. The optimized TiNS/Ti electrode exhibits quasi-rectangular cyclic voltammograms (CVs) in a wide potential range. The specific capacitance (Cs) are 6.8 × 103 and 4.7 × 103 μF/cm2 according to the CV (scan rate, 5 mV/s) and charge-discharge measurements (CD, current density, 50 μA/cm2), respectively. These values are much higher than those reported for pure 0D and 1D TiO2 nanostructures.The higher Cs for the TiNS/Ti electrode can be ascribed to the increased rate of K+ intercalation and de-intercalation during charging and discharging, as well as enhanced conductivity enable by the K in the crystal lattice (10.30%) and Ti3+ interstitials (5.2%), respectively. The TiNS/Ti electrode shows excellent stability with the Cs retention of 89% even after 5000 CD cycles.

  7. Facile one-step template-free synthesis of uniform hollow microstructures of cryptomelane-type manganese oxide K-OMS-2.

    Science.gov (United States)

    Galindo, Hugo M; Carvajal, Yadira; Njagi, Eric; Ristau, Roger A; Suib, Steven L

    2010-08-17

    Hollow microstructures of cryptomelane-type manganese oxide were produced in a template-free one-step process based on the fine-tuning of the oxidation rate of manganese species during the synthesis. The tuning of the reaction rate brought about by a mixture of the oxidants oxone and potassium nitrate becomes apparent from the gradual physical changes taking place in the reaction medium at early times of the synthesis. The successful synthesis of the hollow uniform structures could be performed in the ranges 120-160 degrees C and 8.2-10.7 for temperature and mass ratio oxone/potassium nitrate, respectively. Independent of the conditions of the synthesis, all of the complex microstructures showed the same pattern for the array of very long nanofibers in which some of these elongated around the surface confining the cavity and the other fibers grew normal to the surface created by the previous arrangement. A mechanism based on the heterogeneous nucleation of the cryptomelane phase on the surface of an amorphous precursor and the growth of the nanoscale fibers by processes such as dissolution-crystallization and lateral attachment of primary nanocrystalline fibers is proposed to explain the formation of the hollow structures.

  8. Solvothermal synthesis: a new route for preparing nitrides

    CERN Document Server

    Demazeau, G; Denis, A; Largeteau, A

    2002-01-01

    Solvothermal synthesis appears to be an interesting route for preparing nitrides such as gallium nitride and aluminium nitride, using ammonia as solvent. A nitriding additive is used to perform the reaction and, in the case of gallium nitride, is encapsulated by melt gallium. The syntheses are performed in the temperature range 400-800 deg. C and in the pressure range 100-200 MPa. The synthesized powders are characterized by x-ray diffraction and scanning electron microscopy. Finely divided gallium nitride GaN and aluminium nitride AlN, both with wurtzite-type structure, can be obtained by this route.

  9. Template-free synthesis and luminescent properties of hollow Ln:YOF (Ln = Eu or Er + Yb) microspheres

    OpenAIRE

    Martínez-Castro, Elisa; García-Sevillano, J.; Cussó, Fernando; Ocaña, Manuel

    2015-01-01

    © 2014 Elsevier B.V. All rights reserved. A method for the synthesis of hollow lanthanide doped yttrium oxyfluoride (YOF) spheres in the micrometer size range with cubic structure based on the pyrolysis at 600 °C of liquid aerosols generated from aqueous solutions containing the corresponding rare earth chlorides and trifluoroacetic acid has been developed. This procedure, which has been used for the first time for the synthesis of YFO based materials, is simpler and advantageous when compare...

  10. Synthesis of Ceria Zirconia Oxides using Solvothermal Treatment

    Directory of Open Access Journals (Sweden)

    Machmudah Siti

    2018-01-01

    Full Text Available Ceria oxide (CeO2 is widely used as catalyst with high oxygen storage capacity at low temperature. The addition of zirconia oxide (ZrO2 to CeO2 can enhance oxygen storage capacity as well as thermal stability. In this work, ceria zirconia oxides has been synthesized via a low temperature solvothermal treatment in order to produce ceria zirconia oxides composite with high oxygen storage capacity as electrolyte of solid oxide fuel cells (SOFC. Under solvothermal conditions, solvent may control the direction of crystal growth, morphology, particle size and size distribution, because of the controllability of thermodynamics and transport properties by pressure and temperature. Water, mixed of water and ethanol (70/30 vol/vol, and mixed of water and ethylene glycol (70/30 vol/vol were used as solvent, while Ce(NO33 and ZrO(NO32 with 0.06 M concentration were used as precursor. The experiments were conducted at temperature of 150 °C and pressure for 2 h in a Teflon-lined autoclave of 100 mL volume. The synthesized products were dried at 60 °C for 6 and 12 h and then calcined at 900 °C for 6 h. The particle products were characterized using SEM, XRD, TG/DTA, and Potentiostat. The results showed that the morphology of particles formed were affected by the solvent. Solid plate shaped particles were produced in water, and tend to be pore with the addition of ethylene glycol. The addition of ethanol decreased the size of particles with sphere shaped. The XRD pattern indicated that ceria-zirconia oxides particles are uniformly distributed in the structure to form a homogeneous solid solution. Based on the electrochemical analysis, ceria zirconia oxides produced via solvothermal synthesis had high conductivity ion of 0.5594 S/cm, which is higher than minimum conductivity ion requirement of 0.01 S/cm for SOFC electrolyte. It indicated that ceria zirconia oxides produced via solvothermal synthesis is suitable for SOFC electrolyte.

  11. Template Free Synthesis of Hollow Ball-Like Nano-Fe2O3 and Its Application to the Detection of Dimethyl Methylphosphonate at Room Temperature

    Directory of Open Access Journals (Sweden)

    Guang Li

    2012-04-01

    Full Text Available This paper is focused on the template-free synthesis of nanosized ferric oxide (nano-Fe2O3 and its application in quartz crystal microbalance (QCM resonators to detect dimethyl methylphosphonate (DMMP, a simulant of Sarin. The X-ray diffraction (XRD patterns confirm that the synthesized samples are made of Fe2O3 and the scanning electron microscopy (SEM pictures show that the samples have ball-like shapes. The DMMP sensors with a sensing film of hollow ball-like and solid ball-like Fe2O3 are fabricated and their sensing characteristics are compared. The sensitivity of the hollow ball-like Fe2O3 sensor is more than 500% higher than the one of the solid ball-like Fe2O3 sensor. The hollow ball-like nano-Fe2O3 can be synthesized by a novel low temperature hydrothermal method. The sensors with the hollow ball-like Fe2O3 film perform well in a range of 1 to 6 ppm, with a sensitivity of 29 Hz/ppm at room temperature, while the appropriate recoverability and selectivity are maintained. In addition, the performance of different thicknesses of the sensing film of the hollow ball-like nano-Fe2O3 is investigated and the optimized relative film thickness of the hollow ball-like nano-Fe2O3 is found to be 20 μg/mm2.

  12. Shape-controlled solvothermal synthesis of bismuth subcarbonate nanomaterials

    International Nuclear Information System (INIS)

    Cheng Gang; Yang Hanmin; Rong Kaifeng; Lu Zhong; Yu Xianglin; Chen Rong

    2010-01-01

    Much effort has been devoted to the synthesis of novel nanostructured materials because of their unique properties and potential applications. Bismuth subcarbonate ((BiO) 2 CO 3 ) is one of commonly used antibacterial agents against Helicobacter pylori (H. pylori). Different (BiO) 2 CO 3 nanostructures such as cube-like nanoparticles, nanobars and nanoplates, were fabricated from bismuth nitrate via a simple solvothermal method. The nanostructures were characterized by powder X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). It was found that the solvents and precursors have an influence on the morphologies of (BiO) 2 CO 3 nanostructures. The possible formation mechanism of different (BiO) 2 CO 3 nanostructures fabricated under different conditions was also discussed. - Graphical abstract: Different bismuth subcarbonate ((BiO) 2 CO 3 ) nanostructures were successfully synthesized by a simple solvothermal method. It was found that the solvents and precursors have an influence on the morphologies of (BiO) 2 CO 3 nanostructures.

  13. Simple template-free synthesis of high surface area mesoporous ceria and its new use as a potential adsorbent for carbon dioxide capture.

    Science.gov (United States)

    Kamimura, Yoshihiro; Shimomura, Marie; Endo, Akira

    2014-12-15

    The development of an efficient technique for carbon dioxide (CO2) capture from a variety of large stationary sources is in important global issue. If we are to achieve an energy-efficient and effectively higher CO2 capture process based on an adsorption approach, we need new adsorbent materials realistic enough to provide higher CO2 loading on a volumetric basis. For this reason we have focused on the practical use of high surface area mesoporous ceria as a new application in the field of CO2 capture. In this regard, we demonstrate the simple and inexpensive template-free synthesis of mesoporous ceria with a high surface area up to 200 m(2) g(-1), and characterize it as an effective CO2 adsorbent for the first time. The mesoporous ceria is prepared based on sol-gel chemistry, where the product is simply precipitated by the self-assembly of ceria nanoparticles within a short reaction period at room temperature under highly alkaline conditions with optimized chemical compositions. The results of CO2 adsorption-desorption measurement at 298 K show that the obtained ceria with an enhanced surface area exhibits a noticeably higher CO2 adsorption capacity per volume than commercially available non-porous ceria, activated carbon and zeolite 13X over a wide pressure range with robust stability as well as regenerability. This work enables us to prepare promising new materials for the CO2 capture process based on an easy-to-handle synthesis system, and this effective material will have a broad applicability to the efficient CO2 separation from variety of industrial emission sources. The features of the obtained mesoporous ceria are reported and discussed. Copyright © 2014 Elsevier Inc. All rights reserved.

  14. Template-free synthesis of three-dimensional nanoporous N-doped graphene for high performance fuel cell oxygen reduction reaction in alkaline media

    International Nuclear Information System (INIS)

    Tang, Sheng; Zhou, Xuejun; Xu, Nengneng; Bai, Zhengyu; Qiao, Jinli; Zhang, Jiujun

    2016-01-01

    Highlights: • 3-D porous N-doped graphene was prepared using one-step silica template-free method. • High specific surface area of 920 m 2 g −1 was achieved for 3-D porous N-doped graphene. • Much higher ORR activity was observed for N-doped graphene than S-doped one in 0.1 M KOH. • The as-prepared catalyst gave a peak power density of 275 mW cm −2 as zinc–air battery cathode. - Abstract: Three-dimensional nanoporous nitrogen-doped graphene (3D-PNG) has been synthesized through a facial one-step synthesis method without additional silica template. The as-prepared 3D-PNGwas used as an electrocatalyst for the oxygen reduction reaction (ORR), which shows excellent electrochemistry performance, demonstrated by half-cell electrochemical evaluation in 0.1 M KOH including prominent ORR activity, four electron-selectivity and remarkable methanol poisoning stability compared to commercial 20%Pt/C catalyst. The physical and surface properties of 3D-PNG catalyst were characterized by scanning electron microscopy (SEM), high-resolution transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and BET surface area analysis. The experiments show that 3D-PNG catalyst possesses super-large specific surface area reaching 920 m 2 g −1 , which is superior to our most recently reported 3D-PNG synthesized by silica template (670 m 2 g −1 ) and other doped graphene catalysts in literature. When used for constructing a zinc–air battery cathode, such an 3D-PNG catalyst can give a discharge peak power density of 275 mW cm −2 . All the results announce a unique procedure to product high-efficiency graphene-based non-noble metal catalyst materials for electrochemical energy devices including both fuel cells and metal–air batteries.

  15. Synthesis of metal nanoparticles by microwave-assisted solvothermal technique

    Science.gov (United States)

    Li, Dongsheng

    Metal nanoparticles of Ag, Ni, Pd, and Pt were synthesized in this research work by microwave-assisted solvothermal technique. The microwave-assisted solvothermol technique was found to be faster than the conventional solvothermal process in the synthesis of all the metal nanoparticles investigated here. Ethylene glycol, methanol, and ethanol were used as both reducing agents and solvents. The particle size and morphology were observed using a transmission electron miroscope (TEM). Particle size and size distribution were calculated by Image J(TM) software. Optical properties of synthesized metal nanoparticles were characterized by UV-Visible (UV-Vis) Spectrophotometer. Silver nanoparticles of about 10 to 50 nm were synthesized with ethylene glycol as reducing agent. The morphology and particle size of Ag nanoparticle were controlled by varying the concentration of Ag metal source (AgNO 3), polyvinyl pyrrolidone (PVP) molecular weight, and the type of ligands. Furthermore, the growth rate was increased by adding NaOH in the system. Well-dispersed Ni nanoparticles were synthesized with ethylene glycol as reducing agent in a binary protecting agent system of PVP and dodecylamine (DDA) with or without Pt seeding. By neutralizing the H+ formed from the reductive reaction and coordinating with Ni particles, DDA added in the reaction system contributed to the morphology and size control and also led to the formation of Ni nanoparticles without Pt seeding. Palladium and platinum nanoparticles were synthesized with methanol and ethanol as reducing agents. The morphology and particle size were controlled by the concentration of metal precursors, the PVP to metal ions ratio, and the type of reducing agents.

  16. Deep eutectic-solvothermal synthesis of nanostructured ceria

    Science.gov (United States)

    Hammond, Oliver S.; Edler, Karen J.; Bowron, Daniel T.; Torrente-Murciano, Laura

    2017-01-01

    Ceria is a technologically important material with applications in catalysis, emissions control and solid-oxide fuel cells. Nanostructured ceria becomes profoundly more active due to its enhanced surface area to volume ratio, reactive surface oxygen vacancy concentration and superior oxygen storage capacity. Here we report the synthesis of nanostructured ceria using the green Deep Eutectic Solvent reline, which allows morphology and porosity control in one of the less energy-intensive routes reported to date. Using wide Q-range liquid-phase neutron diffraction, we elucidate the mechanism of reaction at a molecular scale at considerably milder conditions than the conventional hydrothermal synthetic routes. The reline solvent plays the role of a latent supramolecular catalyst where the increase in reaction rate from solvent-driven pre-organization of the reactants is most significant. This fundamental understanding of deep eutectic-solvothermal methodology will enable future developments in low-temperature synthesis of nanostructured ceria, facilitating its large-scale manufacturing using green, economic, non-toxic solvents.

  17. CdS nanobubbles and Cd-DMS nanosheets: solvothermal synthesis and formation mechanism.

    Science.gov (United States)

    Feng, Miao; Zhan, Hongbing

    2013-02-01

    CdS nanobubbles and Cd-DMS nanosheets have been prepared by a solvothermal method from a solution of Cd2+ in dimethyl sulfoxide in the absence of elemental S. A formation mechanism for the nanobubble morphology arising during the CdS nanocrystal growth has been proposed, based on the results of transmission electron microscopy and photoluminescence spectrophotometry. The correlation of the morphology with reaction time was also suggested, and may be applicable to the solvothermal synthesis of other nanomaterials.

  18. Template-Free Synthesis of Hollow-Structured Co 3 O 4 Nanoparticles as High-Performance Anodes for Lithium-Ion Batteries

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Deli; Yu, Yingchao; He, Huan; Wang, Jie; Zhou, Weidong; Abruña, Hector D.

    2015-02-24

    We have developed a template-free procedure to synthesize Co3O4 hollow-structured nanoparticles on a Vulcan XC-72 carbon support. The material was synthesized via an impregnation–reduction method followed by air oxidation. In contrast to spherical particles, the hollow-structured Co3O4 nanoparticles exhibited excellent lithium storage capacity, rate capability, and cycling stability when used as the anode material in lithium-ion batteries. Electrochemical testing showed that the hollow-structured Co3O4 particles delivered a stable reversible capacity of about 880 mAh/g (near the theoretical capacity of 890 mAh/g) at a current density of 50 mA/g after 50 cycles. The superior electrochemical performance is attributed to its unique hollow structure, which combines nano- and microscale properties that facilitate electron transfer and enhance structural robustness.

  19. Template-free hydrothermal synthesis of MgO-TiO2 microcubes toward high potential removal of toxic water pollutants

    Science.gov (United States)

    Chowdhury, Ipsita Hazra; Kundu, Sukanya; Naskar, Milan Kanti

    2018-01-01

    MgO-TiO2 microcubes were synthesized by a facile template-free hydrothermal method followed by calcination. Different analytical tools such as XRD, DTA/TG, FTIR, N2 adsorption-desorption study, FESEM, TEM and UV-DRS were used to characterize the sample. The FESEM images exhibited cube shaped particles of size 2-4 μm. The MgO-TiO2 microcubes exhibit a high potential removal of toxic Pb (II) ions and photocatalytic degradation of organic dye methyl orange from water. The absorption capacity was determined by changing different experimental conditions. The spontaneity of the reaction was confirmed by thermodynamic study. The prepared MgO-TiO2 microcubes showed superior adsorption capacity up to 2900 mg g-1 for Pb (II) ions, and about 95% of photodegradation of methyl orange (MO), the water pollutants.

  20. Large pyramid shaped single crystals of BiFeO{sub 3} by solvothermal synthesis method

    Energy Technology Data Exchange (ETDEWEB)

    Sornadurai, D.; Ravindran, T. R.; Paul, V. Thomas; Sastry, V. Sankara [Condensed Matter Physics Division, Materials Science Group, Physical Metallurgy Division, Metallurgy and Materials Group, Indira Gandhi Centre for Atomic Research, Kalpakkam, Tamil Nadu (India); Condensed Matter Physics Division, Materials Science Group (India)

    2012-06-05

    Synthesis parameters are optimized in order to grow single crystals of multiferroic BiFeO{sub 3}. 2 to 3 mm size pyramid (tetrahedron) shaped single crystals were successfully obtained by solvothermal method. Scanning electron microscopy with EDAX confirmed the phase formation. Raman scattering spectra of bulk BiFeO3 single crystals have been measured which match well with reported spectra.

  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. Template-free synthesis of hierarchical yolk-shell Co and N codoped porous carbon microspheres with enhanced performance for oxygen reduction reaction

    Science.gov (United States)

    Chao, Shujun; Cui, Qian; Wang, Kui; Bai, Zhengyu; Yang, Lin; Qiao, Jinli

    2015-08-01

    The structures and compositions of materials have important influences on their performance. Herein, hierarchically structured yolk-shell Co and N codoped porous carbon microspheres (YS-Co/N-PCMs) have been successfully synthesized by using low-cost melamine, formaldehyde and cobalt acetate as raw materials via a facile template-free hydrothermal method and a subsequent pyrolysis. The formation process of the yolk-shell precursor is systematically investigated, involving a morphological evolution process from solid microspheres, ultrathin and wrinkled shells wrap, to yolk-shell structure formation. More importantly, the unique structure combines the favorable features towards oxygen reduction reaction (ORR), such as high surface area, sufficient Co-Nx and graphitic N active sites and suitable pore structures. As a result, the YS-Co/N-PCMs catalyst shows high catalytic activity for ORR in alkaline media for fuel cells, which not only outperforms commercial Pt-based catalysts in terms of resistance to methanol crossover and long-time stability, but is also better than many non-precious metal doped carbon-based catalysts reported previously. In addition, the YS-Co/N-PCMs catalyst also has high catalytic activity toward oxygen evolution reaction (OER). Therefore, the YS-Co/N-PCMs catalyst may serve as a promising alternative to Pt/C catalyst for ORR and OER in alkaline media.

  3. Solvothermal synthesis of cobalt ferrite hollow spheres with chitosan.

    Science.gov (United States)

    Briceño, Sarah; Suarez, Jorge; Gonzalez, Gema

    2017-09-01

    Cobalt ferrite hollow spheres with chitosan (CoFe 2 O 4 /CS) were synthesized by two different approaches using the solvothermal method. The first approach involves in-situ incorporation of FeCl 3 :6H 2 O and CoNO 3 :6H 2 O in the solvothermal reaction (M1) and in second approach already prepared CoFe 2 O 4 nanoparticles (NPs) using the thermal decomposition method was placed in the solvothermal reaction to form the hollow spheres (M2). Structural identification of the samples were characterized by Fourier transform infrared spectra (FTIR), powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermogravimetric analyses (DSC-TGA) and energy dispersive X-ray spectroscopy (EDX). The magnetic properties were evaluated using a vibrating sample magnetometer (VSM). The presence of chitosan on the hollow sphere was confirmed by FTIR. The XRD analyses proved that the synthesized samples were cobalt ferrite with spinel structure. The structure of the surface and the average particle size of the spheres were observed by SEM and TEM showing the nano scale of the CoFe 2 O 4 component. Structural characterization demonstrating that chitosan does not affect the crystallinity, chemical composition, and magnetic properties of the CoFe 2 O 4 /CS. This work demonstrates that the CoFe 2 O 4 /CS prepared using the as synthesized CoFe 2 O 4 NPs have better structural and magnetic properties. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Accessing magnetic chalcogenides with solvothermal synthesis: KFeS2 and KFe2S3

    Science.gov (United States)

    Han, Insung; Jiang, Zhelong; dela Cruz, Clarina; Zhang, Hong; Sheng, Huaping; Bhutani, Ankita; Miller, Dean J.; Shoemaker, Daniel P.

    2018-04-01

    Semiconducting binary sulfides are often produced with controlled size and shape by solvothermal synthesis using amine solvents. The versatility of this method, however, has not been extended to dense ternary sulfides that include alkali and transition metal ions, which are renowned for their complex magnetic and electronic properties. We report the solvothermal synthesis of the alkali-transition metal sulfides KFeS2 and KFe2S3. The latter compound is not accessible by direct solid-state synthesis. Magnetic susceptibility measurements indicate antiferromagnetic ordering of KFeS2 and KFe2S3, which contain single and double chains of FeS4 tetrahedra, respectively. Given the ability to access KFe2S3 here, further development of this method may lead to isolation of new functional compounds.

  5. The formation mechanism of bimetallic PtRu alloy nanoparticles in solvothermal synthesis

    Science.gov (United States)

    Mi, Jian-Li; Nørby, Peter; Bremholm, Martin; Becker, Jacob; Iversen, Bo B.

    2015-10-01

    An understanding of the nucleation and growth mechanism of bimetallic nanoparticles in solvothermal synthesis is important for further development of nanoparticles with tailored nanostructures and properties. Here the formation of PtRu alloy nanoparticles in a solvothermal synthesis using metal acetylacetonate salts as precursors and ethanol as both the solvent and reducing agent has been studied by in situ synchrotron radiation powder X-ray diffraction (SR-PXRD). Unlike the classical mechanism for the synthesis of monodisperse sols, the nucleation and growth processes of bimetallic PtRu nanoparticles occur simultaneously under solvothermal conditions. In the literature co-reduction of Pt and Ru is often assumed to be required to form PtRu bimetallic nanocrystals, but it is shown that monometallic Pt nanocrystals nucleate first and rapidly grow to an average size of 5 nm. Subsequently, the PtRu bimetallic alloy is formed in the second nucleation stage through a surface nucleation mechanism related to the reduction of Ru. The calculated average crystallite size of the resulting PtRu nanocrystals is smaller than that of the primary Pt nanocrystals due to the large disorder in the PtRu alloyed structure.An understanding of the nucleation and growth mechanism of bimetallic nanoparticles in solvothermal synthesis is important for further development of nanoparticles with tailored nanostructures and properties. Here the formation of PtRu alloy nanoparticles in a solvothermal synthesis using metal acetylacetonate salts as precursors and ethanol as both the solvent and reducing agent has been studied by in situ synchrotron radiation powder X-ray diffraction (SR-PXRD). Unlike the classical mechanism for the synthesis of monodisperse sols, the nucleation and growth processes of bimetallic PtRu nanoparticles occur simultaneously under solvothermal conditions. In the literature co-reduction of Pt and Ru is often assumed to be required to form PtRu bimetallic nanocrystals, but

  6. Microwave solvothermal synthesis and characterization of manganese-doped ZnO nanoparticles

    OpenAIRE

    Jacek Wojnarowicz; Roman Mukhovskyi; Elzbieta Pietrzykowska; Sylwia Kusnieruk; Jan Mizeracki; Witold Lojkowski

    2016-01-01

    Mn-doped zinc oxide nanoparticles were prepared by using the microwave solvothermal synthesis (MSS) technique. The nanoparticles were produced from a solution of zinc acetate dihydrate and manganese(II) acetate tetrahydrate using ethylene glycol as solvent. The content of Mn2+ in Zn1−xMnxO ranged from 1 to 25 mol %. The following properties of the nanostructures were investigated: skeleton density, specific surface area (SSA), phase purity (XRD), lattice parameters, dopant content, average pa...

  7. Solvothermal synthesis of tetravalent uranium with isophthalate or pyromellitate ligands

    Energy Technology Data Exchange (ETDEWEB)

    Falaise, Clement; Delille, Jason; Volkringer, Christophe; Loiseau, Thierry [Contribution from Unite de Catalyse et Chimie du Solide (UCCS) - UMR CNRS 8181, Universite de Lille, USTL-ENSCL, Villeneuve d' Ascq (France)

    2015-06-15

    Three new coordination polymers bearing tetravalent uranium have been isolated with the O-donor ligands such as isophthalate (1,3-bdc) or pyromellitate (btec). The compounds 1 and 3 have been solvothermally synthesized in N,N-dimethylformamide (DMF). The crystal structure of U(1,3-bdc){sub 2}(DMF) (1) is built up from discrete tricapped trigonal-primastic UO{sub 9} units, for which one carbonyl oxygen atom from DMF is bound to uranium. The connection of the UO{sub 9} units with the isophthalate linkers occurs in a chelating and bidentate fashion and gives rise to the formation of a 3D framework, delimiting narrow channels running along the [101] direction. Upon heating, the DMF molecules are removed, generating the second phase U(1,3-bdc){sub 2} (2) compound, closely related to 1. Indeed, the coordination environment of uranium is reduced to eight with a distorted square-antiprismatic geometry. This transition induces the relative shrinkage of the network (ΔV = 23 %). The structure of the compound U(btec)(DMF){sub 2} (3) also exhibits a 3D framework composed of an isolated bicapped square-antiprismatic UO{sub 10} unit, for which two carbonyl oxygen atoms from DMF are bonded to uranium. Pyromellitate ensures the connection of the UO{sub 10} units through the carboxylate arms in a chelating mode. This results in the formation of a network with diamond-shaped channels, developed along the c axis and encapsulating the DMF molecules. In contrast to 1, no stable phase is observed upon removing the DMF species by heating. (Copyright copyright 2015 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  8. A Facile Solvothermal Synthesis of Octahedral Fe3O4 Nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Ooi, Frances; DuChene, Joseph S.; Qiu, Jianqing; Graham, Jeremy O.; Engelhard, Mark H.; Cao, Guixin; Gai, Zheng; Wei, Wei

    2015-06-01

    Magnetic nanoparticles are of great technological interest because they promise numerous potential opportunities in biomedicine and data storage. Although intriguing, these applications require exquisite control over nanostructure morphology in order to appropriately harness their magnetic properties. Most synthesis strategies reported to date are unable to routinely produce anisotropic Fe3O4 nanostructures with appropriate sizes to enable integration into biological systems. Here, we report a simple solvothermal synthesis for obtaining octahedral Fe3O4 nanoparticles with suitable sizes for cellular internalization. Furthermore, these ferromagnetic Fe3O4 octahedrons exhibit substantial saturation magnetization with minimal remanence, suggesting their potential applicability for a host of biomedical applications.

  9. Synthesis of sub-micron silver and silver sulfide particles via solvothermal silver azide decomposition

    International Nuclear Information System (INIS)

    Grocholl, Luke; Wang Jianjun; Gillan, Edward G.

    2003-01-01

    Many transition-metal azides are thermodynamically unstable with respect to the elements and thus, may serve as energetic precursor sources in nanoscale metal particle synthesis. This report describes the use of silver azide (AgN 3 ) in nonaqueous, solvothermal decomposition reactions to produce crystalline sub-micron silver particles and interconnected structures. The thermal decomposition of AgN 3 directly produces silver and N 2 and no secondary chemical reducing agent is required. This solvothermal conversion was examined in toluene, tetrahydrofuran (THF), and trioctylamine below 250 deg. C. The coordinating solvents produced the smallest particles (150-500 nm), while the toluene reaction products were near 1 μm in size. The addition of soluble elemental sulfur to the THF reaction results in the growth of silver sulfide particles near 1 μm in size. The silver and Ag 2 S products are crystalline by X-ray diffraction and show some faceting by scanning electron microscopy

  10. Solvothermal synthesis of Sm3+-doped Fe3O4 nanoparticles.

    Science.gov (United States)

    Lastovina, T A; Budnyk, A P; Kudryavtsev, E A; Nikolsky, A V; Kozakov, A T; Chumakov, N K; Emelyanov, A V; Soldatov, A V

    2017-11-01

    Magnetic iron oxide nanoparticles doped with samarium were prepared by solvothermal polyol method. An introduction of 2,2'-bipyridine during the synthesis reduces the particle diameter to about 9nm in average. The difference in physical and magnetic properties of the samples prepared with and without capping agent was outlined on the basis of complex characterization by a number of experimental techniques. The characteristics of resulted product make it suitable for biomedical applications, for instance, as a contrast agent for MRI. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. 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.

  12. An in situ study of resin-assisted solvothermal metal-organic framework synthesis

    International Nuclear Information System (INIS)

    Moorhouse, Saul J.; Wu, Yue; O’Hare, Dermot

    2016-01-01

    A newly developed in situ monochromatic high-energy X-ray diffraction setup was used to investigate the synthesis of MOFs using cation-impregnated polymer resin beads as a ion source. The Co–NDC–DMF (NDC=2,6-naphthalenedicarboxylate; DMF=dimethylformamide) system was investigated, a system which is known to produce at least three distinct frameworks. It was found that the resin-assisted synthesis results in the preferential formation of a topology previously impossible to synthesise in bulk, while the comparable nitrate-salt synthesis appeared to form an alternative phases. It was also found that the resin-assisted synthesis is highly diffusion-controlled. - Graphical abstract: In situ monochromatic high-energy X-ray diffraction study of a MOF synthesis. - Highlights: • Resin-assisted solvothermal MOF synthesis was studied using in situ diffraction. • Full kinetics of reaction can be obtained from in situ data. • Kinetics show that this resin-assisted synthesis is diffusion controlled. • Resin-assisted synthesis enables the production of an alternative bulk phase.

  13. A simple template-free synthesis of nanoporous ZnS-In2S3-Ag2S solid solutions for highly efficient photocatalytic H2 evolution under visible light.

    Science.gov (United States)

    Li, Yingxuan; Chen, Gang; Zhou, Chao; Sun, Jingxue

    2009-04-21

    Nanoporous ZnS-In(2)S(3)-Ag(2)S solid solutions synthesized by a facile template-free method showed relatively high activities for photocatalytic H(2) evolution under visible-light irradiation (lambda >400 nm) even in the absence of co-catalysts.

  14. Low-temperature solvothermal synthesis of EuS hollow microspheres

    Energy Technology Data Exchange (ETDEWEB)

    Peng, Yong; Wang, Hong; Li, Peng; Fu, Yao, E-mail: fuyaozn@126.com; Xing, Mingming; Jiang, Tao; Luo, Xixian, E-mail: luoxixiandl@126.com

    2014-09-15

    Graphical abstract: Synthesis of EuS hollow microspheres at low-temperature via solvothermal method for the first time. - Highlights: • We adopt an improved method to synthesise the (Phen)Eu(Et{sub 2}CNS{sub 2}){sub 3} in deionized water. • We have successfully synthesised the EuS hollow microsphere at 230 °C in acetonitrile. • The price of acetonitrile is more inexpensive, so the price of preparation was reduced. - Abstract: EuS crystals are synthesized by low-temperature solvothermal decomposition of the single source precursor complex (Phen)Eu(Et{sub 2}CNS{sub 2}){sub 3} in acetonitrile. X-ray powder diffraction, scanning electron microscopy, granulocyte diameter statistical analysis, surface energy-dispersive X-ray spectroscopy analysis, and UV–vis absorption spectroscopy are used to characterize the structure and properties of the obtained EuS crystals. The results show that the formed EuS crystals are uniform hollow microspheres with a typical cubic phase structure of rock salt and the average particle size of 2.01 μm. The mechanisms for the thermal decomposition of the precursor complex and the formation of the EuS hollow microspheres are postulated based on the experimental observations and previous reports.

  15. Lyotropic liquid crystal based on zinc oxide nanoparticles obtained by microwave solvothermal synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Omelchenko, M.M., E-mail: momelchenko@chem.uw.edu.pl [Department of Chemistry, Warsaw University, Al. Zwirki i Wigury 101, 02-089, Warsaw (Poland); Wojnarowicz, J. [Institute of High Pressure Physics, Polish Academy of Sciences, Sokolowska 29/37, Warsaw, 01-142 (Poland); Salamonczyk, M. [Department of Chemistry, Warsaw University, Al. Zwirki i Wigury 101, 02-089, Warsaw (Poland); Lojkowski, W. [Institute of High Pressure Physics, Polish Academy of Sciences, Sokolowska 29/37, Warsaw, 01-142 (Poland)

    2017-05-01

    Abstract: The ZnO nanoparticles, obtained by microwave solvothermal synthesis, were used for the liquid crystal phase preparation. The structure of the material was investigated by X-ray diffraction (XRD), helium pycnometry, specific surface area (SSA), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM). The stability of aqueous suspensions was monitored by Multiple Light Scattering (MLS) technique and the average agglomerate size in suspensions was obtained by dynamic light scattering (DLS) technique. The lyotropic columnar hexagonal phase was formed by doping ZnO nanoparticles into the cetylpiridinium chloride/water/hexanol system. The structure of this phase was confirmed by x-ray diffraction. The luminescent properties of the LC phase were compared with properties of ZnO nanoparticles isolated in solution and analogues lyotropic system without nanoparticles.

  16. Solvothermal Synthesis of Sphere-Like ZnS Microparticles and Its Visible-Light Catalytic Properties.

    Science.gov (United States)

    Li, Jian; Yan, Long; Wang, Yufei; Kang, Yuhong; Ma, Wei; Liang, Lei

    2018-02-01

    The cauliflower-like ZnS microspheres consisting of the nanospheres were prepared via one step template-free approach employing a solvothermal process using Zn(NO3)2·6H2O and CH4N2S as precursors in the mixture solution. The morphology, structure characterization, and crystal structure of the as-prepared ZnS were performed by X-ray diffraction, scanning electron microscopy, UV-visible absorption, and X-ray photoelectron spectroscopy. The results showed that cauliflowerlike ZnS microspheres were prepared under this condition and the size of the particles were about 3~5 μm. In addition, the excellent photocatalytic activity and degradation mechanism of ZnS microspheres have been investigated and discussed in detail. The degradation of Rhodamine B (RhB) aqueous solution was carried out to investigate the visible-light catalytic activity under metal halide lamp. The results indicated that different size of ZnS had photocatalytic activity to RhB under visible light, and sphere-like ZnS displayed high photodegradation efficiency with degradation rate of 98% within 140 min.

  17. Size control mechanism of ZnO nanoparticles obtained in microwave solvothermal synthesis

    Science.gov (United States)

    Wojnarowicz, Jacek; Chudoba, Tadeusz; Koltsov, Iwona; Gierlotka, Stanislaw; Dworakowska, Sylwia; Lojkowski, Witold

    2018-02-01

    The aim of the paper is to explain the mechanism of zinc oxide (ZnO) nanoparticle (NP) size control, which enables the size control of ZnO NPs obtained in microwave solvothermal synthesis (MSS) within the size range between circa 20 and 120 nm through the control of water content in the solution of zinc acetate in ethylene glycol. Heavy water was used in the tests. The mechanism of ZnO NPs size control was explained, discussed and experimentally verified. The discovery and investigation of this mechanism was possible by tracking the fate of water molecules during the whole synthesis process. All the synthesis products were identified. It was indicated that the MSS of ZnO NPs proceeded through the formation and conversion of intermediates such as Zn5(OH)8(CH3COO)2 · xH2O. Esters and H2O were the by-products of the MSS reaction of ZnO NPs. We justified that the esterification reaction is the decisive stage that is a prerequisite of the formation of ZnO NPs. The following parameters of the obtained ZnO NPs and of the intermediate were determined: pycnometric density, specific surface area, phase purity, average particles size, particles size distribution and chemical composition. The ZnO NPs morphology and structure were determined using scanning electron microscopy.

  18. Solvothermal synthesis and characterization of ceria-zirconia mixed oxides for catalytic applications

    Science.gov (United States)

    Devaraju, M. K.; Liu, Xiangwen; Yusuke, Kikuchi; Yin, S.; Sato, T.

    2009-10-01

    Solvothermal synthesis under supercritical conditions (400 °C) and high autogenous pressure (about 40 MPa), has been carried out for the direct preparation of nanocrystalline powders of CeO2, Ce0.85Zr0.15O2, Ce0.75Zr0.25O2, Ce0.65Zr0.35O2 and Ce0.5Zr0.5O2 which are characterized for applications as catalysts for oxygen storage in automotive catalysis. The synthesis was carried out in the presence of polyethylene glycol and water. For the characterization, x-ray diffraction (XRD), transmission electron microscopy (TEM), dynamic light scattering (DLS) and the Brunauer-Emmet-Teller (BET) technique were employed. The oxygen storage capacity (OSC) of as-prepared and calcined samples without loading of noble metals was measured using thermogravimetric-differential thermal analysis (TG-DTA) at 600 °C with a continuous flow of CO-N2 gas and air alternately. Ce0.5Zr0.5O2 nanoparticles with a BET surface area of 102 m2 g-1 exhibited the highest OSC of 0.073 50 mol-O2/mol-CeO2. The OSC values obtained increased with increasing the amount of ZrO2 doping in the samples.

  19. The microwave-assisted solvothermal synthesis of a crystalline two-dimensional covalent organic framework with high CO2 capacity.

    Science.gov (United States)

    Wei, Hao; Chai, Shuangzhi; Hu, Nantao; Yang, Zhi; Wei, Liangming; Wang, Lin

    2015-08-07

    We report the synthesis of a two-dimensional enamine-linked covalent organic framework (COF) using a rapid microwave-assisted solvothermal method in significantly less time and high yield under a relatively low temperature. This COF was found to have a high crystallinity, high stability, high BET surface area, and a high CO2 capacity and adsorption selectivity of CO2/N2.

  20. A Simple and High Yield Solvothermal Synthesis of Uniform Silver Nanowires with Controllable Diameters

    Directory of Open Access Journals (Sweden)

    M. Khademalrasool

    2015-10-01

    Full Text Available Silver nanowires were synthesized by solvothermal method through reducing silver nitrate (AgNO3 with ethylene glycol (EG in the presence of polyvinylpyrrolidone (PVP. In order to prevent the agglomeration of Ag+ in the initial Ag seeds formation, sodium chloride (NaCl was added into the solution to form AgCl colloids. By dissolving AgCl in the late stages, Ag+ ions were released into the solution. So the diameters of silver nanowires could be controlled by modifying the PVP concentration. The effect of reaction time, reaction temperature, and for first time purity of EG over the shape of resulted silver nanowires were investigated. The wire, sphere and tree-like nanostructures were formed with changing these parameters. The structural and optical properties of the silver nanostructures were studied by X-ray diffraction (XRD, scanning electron microscopy (SEM, field emission scanning electron microscopy (FESEM, Fourier transform infrared spectroscopy (FTIR, and UV–visible absorption spectrophotometer. In order to synthesis silver nanowires with smaller diameters and longer lengths, the optimum molar ratio of PVP/AgNO3, reaction time, reaction temperature, and EG purity were found to be 1.5, 2.5 h, 160 °C, and 99.5%, respectively.

  1. Enhanced microbial electrosynthesis with three-dimensional graphene functionalized cathodes fabricated via solvothermal synthesis

    International Nuclear Information System (INIS)

    Aryal, Nabin; Halder, Arnab; Tremblay, Pier-Luc; Chi, Qijin; Zhang, Tian

    2016-01-01

    Highlights: • A 3D-graphene/carbon felt cathode was fabricated via solvothermal synthesis. • Specific surface area of this novel electrode was increased 2 fold. • The composite electrode was tested in a microbial electrosynthesis reactor. • Microbial electrosynthesis of acetate from CO 2 was 6.8 fold faster. • Higher current consumption and biofilm density were also observed. - Abstract: The biological reduction of CO 2 into multicarbon chemicals can be driven by electrons derived from the cathode of a bioelectrochemical reactor via microbial electrosynthesis (MES). To increase MES productivity, conditions for optimal electron transfer between the cathode and the microbial catalyst must be implemented. Here, we report the development of a 3D-graphene functionalized carbon felt composite cathode enabling faster electron transfer to the microbial catalyst Sporomusa ovata in a MES reactor. Modification with 3D-graphene network increased the electrosynthesis rate of acetate from CO 2 by 6.8 fold. It also significantly improved biofilm density and current consumption. A 2-fold increase in specific surface area of the 3D-graphene/carbon felt composite cathode explained in part the formation of more substantial biofilms compared to untreated control. Furthermore, in cyclic voltammetry analysis, 3D-graphene/carbon felt composite cathode exhibited higher current response. The results indicate that the development of a 3D-network cathode is an effective approach to improve microbe-electrode interactions leading to productive MES systems.

  2. Microwave solvothermal synthesis and characterization of manganese-doped ZnO nanoparticles.

    Science.gov (United States)

    Wojnarowicz, Jacek; Mukhovskyi, Roman; Pietrzykowska, Elzbieta; Kusnieruk, Sylwia; Mizeracki, Jan; Lojkowski, Witold

    2016-01-01

    Mn-doped zinc oxide nanoparticles were prepared by using the microwave solvothermal synthesis (MSS) technique. The nanoparticles were produced from a solution of zinc acetate dihydrate and manganese(II) acetate tetrahydrate using ethylene glycol as solvent. The content of Mn(2+) in Zn1- x Mn x O ranged from 1 to 25 mol %. The following properties of the nanostructures were investigated: skeleton density, specific surface area (SSA), phase purity (XRD), lattice parameters, dopant content, average particle size, crystallite size distribution, morphology. The average particle size of Zn1- x Mn x O was determined using Scherrer's formula, the Nanopowder XRD Processor Demo web application and by converting the specific surface area results. X-ray diffraction of synthesized samples shows a single-phase wurtzite crystal structure of ZnO without any indication of additional phases. Spherical Zn1- x Mn x O particles were obtained with monocrystalline structure and average particle sizes from 17 to 30 nm depending on the content of dopant. SEM images showed an impact of the dopant concentration on the morphology of the nanoparticles.

  3. A Facile Solvothermal Method for Synthesis of CuInS2 Nanostructures

    Directory of Open Access Journals (Sweden)

    M. Mousavi-Kamazani

    2012-09-01

    Full Text Available CuInS2 nanostructures were  synthesized  via  a  simple  surfactant-free solvothermal  route.  In  this  synthesis,  thiosemicarbazide  and thioglycolic acid were used as sulfur sources. The effects of different parameters such as type of precursor and time on the morphology and particle  size  of  the  samples  have  been  investigated.  The nanostructures  were  characterized  by  means  of  X-ray  diffraction (XRD,  scanning  electron microscopy  (SEM,  energy-dispersive X- ray  analysis  (EDX,  Fourier  transform  infrared  (FT-IR  and photoluminescence  (PL  spectroscopy.  The  fill  factor  (FF,  open circuit voltage  (Voc, and  short circuit current  (Isc were obtained by I–V characterization.

  4. Microwave solvothermal synthesis and characterization of manganese-doped ZnO nanoparticles

    Directory of Open Access Journals (Sweden)

    Jacek Wojnarowicz

    2016-05-01

    Full Text Available Mn-doped zinc oxide nanoparticles were prepared by using the microwave solvothermal synthesis (MSS technique. The nanoparticles were produced from a solution of zinc acetate dihydrate and manganese(II acetate tetrahydrate using ethylene glycol as solvent. The content of Mn2+ in Zn1−xMnxO ranged from 1 to 25 mol %. The following properties of the nanostructures were investigated: skeleton density, specific surface area (SSA, phase purity (XRD, lattice parameters, dopant content, average particle size, crystallite size distribution, morphology. The average particle size of Zn1−xMnxO was determined using Scherrer’s formula, the Nanopowder XRD Processor Demo web application and by converting the specific surface area results. X-ray diffraction of synthesized samples shows a single-phase wurtzite crystal structure of ZnO without any indication of additional phases. Spherical Zn1−xMnxO particles were obtained with monocrystalline structure and average particle sizes from 17 to 30 nm depending on the content of dopant. SEM images showed an impact of the dopant concentration on the morphology of the nanoparticles.

  5. The role anions on the synthesis of AlOOH nanoparticles using simple solvothermal method

    Directory of Open Access Journals (Sweden)

    Mozaffar Abdollahifar

    2018-03-01

    Full Text Available Effect of aluminium salts on the synthesis of AlOOH nanostructures has been successfully investigated in detail using solvothermal method, when ethanol and NaOH are solvent and pH adjusting agent, respectively. Fourier transform infrared spectroscopy (FTIR, X-ray powder diffraction (XRD, and field emission scanning electron microscopy (FESEM, were used to characterize the synthesized samples. The specific surface area, pore size distribution and pore structure of the different AlOOH structures were also discussed by the N2 adsorption/desorption test. According to our experimental results, the structure characterization revealed that for synthesized AlOOH nanostructures no obvious XRD peaks arising from other phases of alumina are found indicating pure AlOOH phase of products. Furthermore, the nitrogen adsorption and desorption measurements indicated that the obtained AlOOH nanoparticles from aluminium chloride at basic condition possess a high BET surface area of approximately 90 m2/g. Resumen: El efecto de las sales de aluminio sobre la síntesis de las nanoestructuras de AlOOH ha sido analizado en detalle satisfactoriamente usando el método solvotérmico, cuando el etanol y el NaOH son el disolvente y el agente de regulación del pH, respectivamente. Para clasificar las muestras sintetizadas se utilizaron la espectroscopia infrarroja por transformada de Fourier (FTIR, difracción de rayos X por polvo (XRD y microscopia electrónica de barrido de emisión de campo (FESEM. El área superficial específica, la distribución del tamaño del poro y la estructura de poros de las diferentes estructuras de AlOOH también se debatieron mediante la prueba de adsorción/desorción de N2. De acuerdo con nuestros resultados experimentales, la clasificación de la estructura reveló que en las nanoestructuras de AlOOH sintetizadas no se observan picos XRD evidentes derivados de otras fases de la alúmina que indican la fase pura de AlOOH de los productos

  6. Synthesis of Framework Isomer MOFs Containing Zinc and 4-Tetrazolyl Benzenecarboxylic Acid via a Structure Directing Solvothermal Approach

    Directory of Open Access Journals (Sweden)

    Carlos Ordonez

    2015-04-01

    Full Text Available The solvothermal synthesis of framework isomers was carried out using the hybrid carboxylate and tetrazolate functional ligand, 4-tetrazolyl benzenecarboxylic acid (H2TBC, TBC = 4-tetrazolyl benzenecarboxylate and zinc. H2TBC was also synthesized with the solvothermal approach, and is referred herein as structure 1. Using single-crystal X-ray diffraction, we found that the tetrazolate groups of TBC show an unusual “opposite-on” coordination mode with zinc. Three previously characterized metal-organic frameworks (MOFs were obtained by systematically changing the solvents of the H2TBC-Zn reaction, (1 ZnTBC, 2, which has a non-porous structure; (2 Zn2(TBC2(H2O, 3, which has an amphiphilic pore structure and (3 Zn2(TBC2{guest}, 4, which is porous and has channels containing uncoordinated N heteroatoms. Fluorescence spectra of 4 reveal a strong blue emission mainly from the TBC ligands.

  7. Solvothermal synthesis of tin sulfide (SnS) nanorods and investigation of its field emission properties

    Science.gov (United States)

    Bhorde, Ajinkya; Pawbake, Amit; Sharma, Priyanka; Nair, Shruthi; Funde, Adinath; Bankar, Prashant; More, Mahendra; Jadkar, Sandesh

    2018-02-01

    In the present study, we report synthesis of tin sulfide (SnS) nano-rods using a simple solvothermal method at different reaction time period. The formation of single phase SnS has been confirmed by X-ray diffraction (XRD) and Raman analysis. The XRD analysis revealed that the predominant phase in all prepared samples is orthorhombic SnS. The formation of nano-rods of SnS was confirmed by scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HR-TEM) analysis. To investigate the optical properties of SnS nano-rods UV-visible spectroscopy analysis was carried out. We observed that the band gap of SnS nano-rods decreases with increase in reaction time and can be attributed to the quantum confinement effect. Finally, field emission investigations on the SnS nano-rods at the base pressure of 1 × 10- 8 mbar were carried out and found to be superior to the other chalcogenide nanostructures. As-synthesized SnS nano-rods emitter exhibits excellent field emission properties such as low turn-on field ( 2.5 V/µm for 10 µA/ cm2), high emission current density ( 647 µA/cm2 at 3.9 V/µm) and superior current stability ( 5 h for 1 µA). Thus, the facile one-step synthesis approach and robust nature of SnS nano-rods emitter can provide prospects for the future development of large-area emitter applications such as flat-panel-display devices.

  8. One-pot solvothermal synthesis of dual-phase titanate/titania Nanoparticles and their adsorption and photocatalytic Performances

    International Nuclear Information System (INIS)

    Cheng, Yu Hua; Gong, Dangguo; Tang, Yuxin; Ho, Jeffery Weng Chye; Tay, Yee Yan; Lau, Wei Siew; Wijaya, Olivia; Lim, Jiexiang; Chen, Zhong

    2014-01-01

    Dual phase titanate/titania nanoparticles undergo phase transformation gradually with the increase of solvothermal synthesis temperature from 100 °C to 200 °C, and eventually are fully transformed into anatase TiO 2 . The crystal structure change results in the changes of optical absorption, sensitizer/dopant formation and surface area of the materials which finally affect the overall dye removal ability. Reactions under dark and light have been conducted to distinguish the contributions of surface adsorption from photocatalytic degradation. The sample synthesized at 160 °C (S160) shows the best performances for both adsorption under dark and photocatalytic degradation of methylene blue (MB) under visible light irradiation. The adsorption mechanism for S160 is determined as monolayer adsorption based on the adsorption isotherm test under dark condition, and an impressive adsorption capacity of 162.19 mg/g is achieved. For the photocatalytic application, this sample at 0.1 g/L loading is also able to degrade 20 ppm MB within 6 hours under the visible light (>420 nm) condition. - Graphical abstract: The effect of solvothermal synthesis temperature on the formation and dye removal performance of dual phase titanate/titania nanoparticles was unveiled and optimized. - Highlights: • Low temperature one-pot solvothermal synthesis of dual-phase photocatalysts. • Correlation of the synthesis temperature is made with the phase composition. • Adsorption isotherm, kinetics, photocatalytic degradation were studied. • Synthesis at 160 °C yields the best material for adsorption of MB in dark. • The same sample also shows the best visible light degradation of MB

  9. One-pot solvothermal synthesis of dual-phase titanate/titania Nanoparticles and their adsorption and photocatalytic Performances

    Energy Technology Data Exchange (ETDEWEB)

    Cheng, Yu Hua; Gong, Dangguo; Tang, Yuxin; Ho, Jeffery Weng Chye; Tay, Yee Yan; Lau, Wei Siew; Wijaya, Olivia; Lim, Jiexiang; Chen, Zhong, E-mail: aszchen@ntu.edu.sg

    2014-06-01

    Dual phase titanate/titania nanoparticles undergo phase transformation gradually with the increase of solvothermal synthesis temperature from 100 °C to 200 °C, and eventually are fully transformed into anatase TiO{sub 2}. The crystal structure change results in the changes of optical absorption, sensitizer/dopant formation and surface area of the materials which finally affect the overall dye removal ability. Reactions under dark and light have been conducted to distinguish the contributions of surface adsorption from photocatalytic degradation. The sample synthesized at 160 °C (S160) shows the best performances for both adsorption under dark and photocatalytic degradation of methylene blue (MB) under visible light irradiation. The adsorption mechanism for S160 is determined as monolayer adsorption based on the adsorption isotherm test under dark condition, and an impressive adsorption capacity of 162.19 mg/g is achieved. For the photocatalytic application, this sample at 0.1 g/L loading is also able to degrade 20 ppm MB within 6 hours under the visible light (>420 nm) condition. - Graphical abstract: The effect of solvothermal synthesis temperature on the formation and dye removal performance of dual phase titanate/titania nanoparticles was unveiled and optimized. - Highlights: • Low temperature one-pot solvothermal synthesis of dual-phase photocatalysts. • Correlation of the synthesis temperature is made with the phase composition. • Adsorption isotherm, kinetics, photocatalytic degradation were studied. • Synthesis at 160 °C yields the best material for adsorption of MB in dark. • The same sample also shows the best visible light degradation of MB.

  10. Paramagnetism of cobalt-doped ZnO nanoparticles obtained by microwave solvothermal synthesis

    Directory of Open Access Journals (Sweden)

    Jacek Wojnarowicz

    2015-09-01

    Full Text Available Zinc oxide nanopowders doped with 1–15 mol % cobalt were produced by the microwave solvothermal synthesis (MSS technique. The obtained nanoparticles were annealed at 800 °C in nitrogen (99.999% and in synthetic air. The material nanostructure was investigated by means of the following techniques: X-ray diffraction (XRD, helium pycnometry density, specific surface area (SSA, inductively coupled plasma optical emission spectrometry (ICP-OES, extended X-ray absorption fine structure (EXAFS spectroscopy, scanning electron microscopy (SEM, energy dispersive X-ray spectroscopy (EDS and with magnetometry using superconducting quantum interference device (SQUID. Irrespective of the Co content, nanoparticles in their initial state present a similar morphology. They are composed of loosely agglomerated spherical particles with wurtzite-type crystal structure with crystallites of a mean size of 30 nm. Annealing to temperatures of up to 800 °C induced the growth of crystallites up to a maximum of 2 μm in diameter. For samples annealed in high purity nitrogen, the precipitation of metallic α-Co was detected for a Co content of 5 mol % or more. For samples annealed in synthetic air, no change of phase structure was detected, except for precipitation of Co3O4 for a Co content of 15 mol %. The results of the magentometry investigation indicated that all as-synthesized samples displayed paramagnetic properties with a contribution of anti-ferromagnetic coupling of Co–Co pairs. After annealing in synthetic air, the samples remained paramagnetic and samples annealed under nitrogen flow showed a magnetic response under the influences of a magnetic field, likely related to the precipitation of metallic Co in nanoparticles.

  11. Solvothermal synthesis and characterization of acicular α-Fe2O3 ...

    Indian Academy of Sciences (India)

    Nanometer-sized -Fe2O3 particles have been prepared by a simple solvothermal method using ferric acetylacetonate as a precursor. The products were characterized by X-ray diffraction (XRD), energy dispersive X-ray microanalysis (EDAX), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), ...

  12. Solvothermal synthesis of hierarchical TiO2 nanostructures with tunable morphology and enhanced photocatalytic activity

    Science.gov (United States)

    Fan, Zhenghua; Meng, Fanming; Zhang, Miao; Wu, Zhenyu; Sun, Zhaoqi; Li, Aixia

    2016-01-01

    This paper presents controllable growth and photocatalytic activity of TiO2 hierarchical nanostructures by solvothermal method at different temperatures. It is revealed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) that the morphology of TiO2 can be effectively controlled as rose-like, chrysanthemum-like and sea-urchin-like only changing solvothermal temperature. BET surface area analysis confirms the presence of a mesoporous network in all the nanostructures, and shows high surface area at relatively high temperature. The photocatalytic activities of the photocatalysts are evaluated by the photodegradation of RhB under UV light irradiation. The TiO2 samples exhibit high activity on the photodegradation of RhB, which is higher than that of the commercial P25. The enhancement in photocatalytic performance can be attributed to the synergetic effect of the surface area, crystallinity, band gap and crystalline size.

  13. Solvothermal Synthesis of Well-Disperse ZnS Nanorods with Efficient Photocatalytic Properties

    OpenAIRE

    Chen, Yun; Yin, Rong-hui; Wu, Qing-sheng

    2012-01-01

    Well-disperse short-range-ordered ZnS nanorods with efficient photocatalytic property for photodegradation of Rhodamin B have been successfully synthesized through a solvothermal method. Solvent used can be recovered and reused, which makes the route environment-friendly. Dodecylamine was found effective in organizing nanorods to ordered monolayer. Characterization showed that these nanorods were uniform with the diameter of about 3 nm and length of nearly 30 nm. And it is expected that these...

  14. Solvothermal Synthesis of Well-Disperse ZnS Nanorods with Efficient Photocatalytic Properties

    Directory of Open Access Journals (Sweden)

    Yun Chen

    2012-01-01

    Full Text Available Well-disperse short-range-ordered ZnS nanorods with efficient photocatalytic property for photodegradation of Rhodamin B have been successfully synthesized through a solvothermal method. Solvent used can be recovered and reused, which makes the route environment-friendly. Dodecylamine was found effective in organizing nanorods to ordered monolayer. Characterization showed that these nanorods were uniform with the diameter of about 3 nm and length of nearly 30 nm. And it is expected that these monodisperse ZnS nanorods have potential applications in electroluminescence materials.

  15. Simple synthesis of ultra-long Ag2Te nanowires through solvothermal co-reduction method

    International Nuclear Information System (INIS)

    Xiao Feng; Chen Gang; Wang Qun; Wang Lin; Pei Jian; Zhou Nan

    2010-01-01

    Ultra-long single crystal β-Ag 2 Te nanowires with the diameter of about 300 nm were fabricated through a solvothermal route in ethylene glycol (EG) system without any template. The long single crystal wires were curves, with high purity, well-crystallized, and dislocation-free and characterized by using X-ray powder diffraction (XRD), Differential scanning calorimetry (DSC) analysis, X-ray photoelectron spectroscope (XPS), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and high-resolution transmission microscopy (HRTEM). The detailed topotactic transformation process from particles into single crystal wires was studied. Furthermore, the electrical conductivity and Seebeck coefficient have been systematically studied between 300 and 600 K. - Graphical abstract: Ultra-long single crystal β-Ag 2 Te nanowires with the diameter of about 300 nm were fabricated by the solvothermal route in ethylene glycol (EG) system without any template. The diagram displays the variation of the phases and morphologies of products with different reaction time.

  16. Solvothermal synthesis and electrochemical performance of Li2MnSiO4/C cathode materials for lithium ion batteries

    International Nuclear Information System (INIS)

    Wang, Yan-Chao; Zhao, Shi-Xi; Zhai, Peng-Yuan; Li, Fang; Nan, Ce-Wen

    2014-01-01

    Highlights: • Li 2 MnSiO 4 /C nanocomposite has been synthesized by the solvothermal method. • The particles of Li 2 MnSiO 4 /C are much smaller and more uniform. • The presence of Ni improves discharge capacity of Li 2 MnSiO 4 /C cathode material. • The initial discharge capacity of Ni-modified Li 2 MnSiO 4 /C is 274.5 mAh g −1 at 25 °C. - Abstract: Orthorhombic structure Li 2 MnSiO 4 /C with Pmn2 1 space group is synthesized by the solvothermal method. Carbon coating and Ni 2+ doping are used to improve the electronic conductivity and the cycling performance of Li 2 MnSiO 4 cathode material, respectively. The particles of Li 2 MnSiO 4 /C are much smaller and more uniform than those of Li 2 MnSiO 4 due to the carbon coating. It is shown that Ni 2+ has been reduced into metal Ni during the synthesis process. The synthesized Ni-modified Li 2 MnSiO 4 /C (denoted as (LMS@Ni)/C) cathode material exhibits better electrochemical performance in comparison with Li 2 MnSiO 4 /C, attributing to higher lithium ion diffusion coefficient as well as electronic conductivity. The initial discharge capacity of (LMS@Ni)/C is 274.5 mA h g −1 and the reversible capacity after 20 cycles is 119.8 mA h g −1 at 25 °C

  17. Solvothermal synthesis of 3D photonic crystals based on ZnS/opal system

    International Nuclear Information System (INIS)

    Chang Xin; Cao Jieming; Ji Hongmei; Fang Baoqing; Feng Jie; Pan Lijia; Zhang Fang; Wang, Haiyan

    2005-01-01

    We made photonic crystals composed of artificial opals infiltrated with ZnS semiconductor nanocrystals by using self-assembly and solvothermal methods. SEM images show that the silica spheres exhibit a well-ordered arrangement and the ZnS nanocrystals infiltrate within the opal templates by heterogeneous nucleation and growth processing, and the as-synthesized ZnS nanocrystals reveal a cubic phase from X-ray diffraction pattern. Furthermore, the optical properties of the infiltrated opals with different ZnS filling ratio are also studied by transmission spectroscopy, respectively. It is proposed that the position of the stop band can be easily designed by controlling the infiltration ratio of ZnS. These results demonstrate an easy-to-handle and efficient route to obtain high performance photonic crystal structures

  18. Solvothermal synthesis and electrical conductivity model for the zinc oxide-insulated oil nanofluid

    International Nuclear Information System (INIS)

    Shen, L.P.; Wang, H.; Dong, M.; Ma, Z.C.; Wang, H.B.

    2012-01-01

    A new kind of nanofluid, ZnO-insulated oil nanofluid was prepared from ZnO nanoparticles synthesized by solvothermal method. Electrical property measurement shows that the electrical conductivity increases by 973 times after adding 0.75% volumetric fraction of ZnO nanoparticles into the insulated oil. A linear dependence of the electrical conductivity on the volumetric fraction has been observed, while the temperature dependence of the electrical conductivity reveals a nonlinear relationship. An electrical conductivity model is established for the nanofluid by considering both the Brownian motion and electrophoresis of the ZnO nanoparticles. -- Highlights: ► Stable ZnO-insulated oil nanofluid was successfully prepared. ► The electrical conductivity of the ZnO nanofluid is investigated. ► A new model is established to explain the electrical properties of the nanofluid.

  19. Solvothermal synthesis of vanadium phosphates in the form of xerogels, aerogels and mesostructures

    Energy Technology Data Exchange (ETDEWEB)

    Sydorchuk, V.; Zazhigalov, V. [Institute of Sorption and Endoecology, National Academy of Sciences of Ukraine, 13 General Naumov Str., Kyiv 03164 (Ukraine); Khalameida, S., E-mail: svkhal@ukr.net [Institute of Sorption and Endoecology, National Academy of Sciences of Ukraine, 13 General Naumov Str., Kyiv 03164 (Ukraine); Diyuk, E. [Institute of Sorption and Endoecology, National Academy of Sciences of Ukraine, 13 General Naumov Str., Kyiv 03164 (Ukraine); Skubiszewska-Zieba, J.; Leboda, R. [Faculty of Chemistry, Maria Curie-Sklodowska University, Maria Curie-Sklodowska Sq. 3, 20-031 Lublin (Poland); Kuznetsova, L. [Institute of Sorption and Endoecology, National Academy of Sciences of Ukraine, 13 General Naumov Str., Kyiv 03164 (Ukraine)

    2010-09-15

    Regularities and peculiarities of physicochemical changes, first of all phase transformations, during solvothermal treatment (with conventional and microwave heating) of the vanadium pentoxide and orthophosphoric acid mixture in organic solvents in the presence of reducing agents have been studied. Hemihydrate of vanadium hydrophosphate - the precursor of vanadium pyrophosphate, the active phase for n-butane to maleic anhydride oxidation, and ion exchanger with variable physicochemical characteristics, i.e. crystal structure, specific surface area, crystallite size and acidic properties - has been synthesized in the temperature range 170-200 {sup o}C. The obtained phases were examined using XRD, DTA-TG, SEM, FTIR spectroscopy, nitrogen adsorption as well as gas chromatographic determination of acidity through organic bases adsorption. The catalytic activity of prepared samples for n-butane oxidation has been investigated.

  20. Mixed-solvothermal synthesis of CdS micro/nanostructures and their optical properties

    International Nuclear Information System (INIS)

    Zhong Shengliang; Zhang Linfei; Huang Zhenzhong; Wang Shangping

    2011-01-01

    Several novel cadmium sulfide (CdS) micro/nanostructures, including cauliflower-like microspheres, football-like microspheres, tower-like microrods, and dendrites were controllably prepared via an oxalic acid-assisted solvothermal route using ethylene glycol (EG) and H 2 O as pure and mixed solvents with different S sources. The as-prepared products were characterized by X-ray powder diffraction (XRD), scanning electronic microscope (SEM) and UV-vis spectrophotometer (UV). It was found that CdS micro/nanostructures can be selectively obtained by varying the composition of solvent, concentration of oxalic acid, and sulfur sources. UV-vis absorption spectra reveal that their absorption properties are shape-dependent. The possible formation process of the CdS micro/nanostructures was briefly discussed. This route provides a facile way to tune the morphologies of CdS over a wide range.

  1. A facile solvothermal synthesis of large-grain iron cubes and cuboids with enhanced performances

    International Nuclear Information System (INIS)

    Yang, Bai; Yang, Xueying; Li, Xiaopan; Cao, Ying; Yu, Ronghai

    2016-01-01

    The cubic and cuboid pure iron particles with particle size ranging from 500 nm to 2 μm have been fabricated using a solvothermal method in ethanol solution. The controlled morphology and size distribution can be easily tuned by adjusting the reaction temperatures. The morphologies of the as-synthesized iron particles can be transformed from cubes to cuboids with the reaction temperature increasing from 100 to 150 °C. Uniform particles with narrow size distribution and good dispersion can be obtained under 120 °C. These chemically synthesized Fe particles exhibit good air stability and very slight surface oxidation. High saturation magnetization of 208–211 A m 2 /kg and very low coercivity of 19–26 Oe can be achieved in these micron-level iron particles due to their high purity and small shape anisotropy. The relatively simple preparation process with low cost, good air stability and high saturation magnetization for these large-grain pure iron particles promise their great potential applications in complicated shape and miniaturized Fe-based composite magnetic components. - Highlights: • The micron-level cubic and cuboid pure iron particles have been prepared. • The morphologies of the large-grain iron particles can be tuned. • These iron particles show slight surface oxidation and good air stability. • These iron particles exhibit high saturation magnetization of 208–211 A m 2 kg −1 .

  2. Facile solvothermal synthesis of a graphene nanosheet-bismuth oxide composite and its electrochemical characteristics

    Energy Technology Data Exchange (ETDEWEB)

    Wang Huanwen [Key Laboratory of Eco-Environment-Related Polymer Materials of Ministry of Education, Key Laboratory of Polymer Materials of Gansu Province, College of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou 730070 (China); Hu Zhongai, E-mail: zhongai@nwnu.edu.c [Key Laboratory of Eco-Environment-Related Polymer Materials of Ministry of Education, Key Laboratory of Polymer Materials of Gansu Province, College of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou 730070 (China); Chang Yanqin; Chen Yanli; Lei Ziqiang; Zhang Ziyu; Yang Yuying [Key Laboratory of Eco-Environment-Related Polymer Materials of Ministry of Education, Key Laboratory of Polymer Materials of Gansu Province, College of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou 730070 (China)

    2010-12-01

    This work demonstrates a novel and facile route for preparing graphene-based composites comprising of metal oxide nanoparticles and graphene. A graphene nanosheet-bismuth oxide composite as electrode materials of supercapacitors was firstly synthesized by thermally treating the graphene-bismuth composite, which was obtained through simultaneous solvothermal reduction of the colloidal dispersions of negatively charged graphene oxide sheets in N,N-dimethyl formamide (DMF) solution of bismuth cations at 180 {sup o}C. The morphology, composition, and microstructure of the composites together with pure graphite oxide, and graphene were characterized using powder X-ray diffraction (XRD), FT-IR, field emission scanning electron microscopy (FESEM), transmission electron microscope (TEM), thermogravimetry and differential thermogravimetry (TG-DTG). The electrochemical behaviors were measured by cyclic voltammogram (CV), galvanostatic charge-discharge and electrochemical impedance spectroscopy (EIS). The specific capacitance of 255 F g{sup -1} (based on composite) is obtained at a specific current of 1 A g{sup -1} as compared with 71 F g{sup -1} for pure graphene. The loaded-bismuth oxide achieves a specific capacitance as high as 757 F g{sup -1} even at 10 A g{sup -1}. In addition, the graphene nanosheet-bismuth oxide composite electrode exhibits the excellent rate capability and well reversibility.

  3. Solvothermal synthesis, characterization and photoluminescence studies of ZnS:Eu nanocrystals

    Science.gov (United States)

    Ashwini, K.; Yashaswini; Pandurangappa, C.

    2014-11-01

    Europium doped zinc sulfide nanocrystals (ZnS:Eu) are prepared by solvothermal method. Crystallite size and lattice constant of the prepared samples are calculated from the X-ray diffraction patterns. The as-prepared samples are found to be a mixture of complex chemical groups. Heat treatment of the samples at 300 °C resulted in ZnS:Eu state. The crystal structure is not affected by the increase in the concentration of Eu from 1 mol% to 5 mol%. Fourier Transform Infrared Spectroscopy (FTIR) studies showed that characteristic absorption bands of hydroxyl groups and the acetate bands increased with increase in Eu concentration. The morphological results studied using Scanning Electron Microscopy (SEM) indicate agglomeration of nanoparticles and a marginal increase in the particle size. Photoluminescence (PL) spectra of the samples showed a prominent emission band peaked at ∼400 nm besides three weak ones at ∼422, 485 and 530 nm. The PL intensity increased with increase in Eu concentration.

  4. Solvothermal synthesis of V2O5/graphene nanocomposites for high performance lithium ion batteries

    International Nuclear Information System (INIS)

    Chen, Da; Yi, Ran; Chen, Shuru; Xu, Terrence; Gordin, Mikhail L.; Lv, Dongping; Wang, Donghai

    2014-01-01

    Highlights: • A homogeneous V 2 O 5 /graphene nanocomposite is successfully synthesized. • V 2 O 5 nanoparticles are highly encapsulated in the 2D graphene matrix. • V 2 O 5 /graphene nanocomposite shows much better performance than bare V 2 O 5 . - Abstract: In this work, V 2 O 5 /graphene nanocomposites have been synthesized by a facile solvothermal approach. The V 2 O 5 nanoparticles, around 20–40 nm in size, were encapsulated in the 2D graphene matrix. The reversible Li-cycling properties of V 2 O 5 /graphene have been evaluated by galvanostatic discharge–charge cycling, cyclic voltammetry, and impedance spectroscopy. Compared with the bare V 2 O 5 nanoparticles, the V 2 O 5 /graphene nanocomposites exhibited enhanced electrochemical performance with higher reversible capacity and improved cycling stability and rate capability. The graphene nanosheets act not only as an electronically conductive matrix to improve the electronic and ionic conductivity of the composite electrode, but also as a flexible buffer matrix to maintain the structural integrity of the composite electrodes by preventing particle agglomeration, thus leading to the improvement of the electrochemical performance of V 2 O 5

  5. Solvothermal synthesis of mesoporous magnetite nanoparticles for Cr(IV) ions uptake and microwave absorption

    KAUST Repository

    Shen, Peng

    2016-05-12

    Abstract: Colloidal mesoporous magnetite nanoparticles with tunable porosity were realized by a simple and scalable solvothermal route with the aid of AOT as ligands. AOT was used to induce the anisotropic crystal growth of smaller nanocrystals and restrain their tight aggregation so as to form more mesoscale pores. Morphologies and microstructures investigation by SEM and TEM revealed that the bigger nanoparticles were composed of smaller nanocrystals with an average size of 18 nm. A possible formation mechanism was proposed for the mesoporous nanoparticles. Study of nitrogen adsorption–desorption isotherm revealed that the Brunauer–Emmett–Teller (BET) specific surface area of mesoporous nanoparticles is up to 209 m2/g, resulting from the slit-shaped pores created by the aggregation of polyhedral nanocrystals. Magnetic properties study indicated that the as-prepared nanoparticles are superparamagnetic at room temperature. Optimized mesoporous magnetite nanoparticles exhibit a maximum Cr(VI) ion sorption capacity of 12.9 mmol/g, and its absorption behavior followed a Freundlich model. Microwave absorption study indicated that porous nanoparticles own higher permeability values than that of solid nanoparticles, leading to a higher dielectric loss in the frequency range of 2–18 GHz. Graphical Abstract: [Figure not available: see fulltext.] © 2016, Springer Science+Business Media Dordrecht.

  6. Ionic liquid-assisted complex-solvothermal synthesis of ZnSe hollow microspheres

    International Nuclear Information System (INIS)

    Liu Xiaodi; Ma Jianmin; Peng Peng; Zheng Wenjun

    2008-01-01

    Dispersible ZnSe hollow microspheres with an average diameter of about 1.0 μm have been successfully prepared by the ionic liquid-assisted complex-solvothermal method. The structure and morphology of the as-prepared ZnSe hollow microspheres were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), and transmission electron microscope (TEM). The results indicated that the ZnSe hollow microspheres had the zinc blende structure and were composed of ZnSe nanoparticles of about 18.8 nm. Additionally, results from photoluminescence (PL) showed that the obtained product had two strong emission peaks centered at 425 and 440 nm. The application of the ionic liquid 1-butyl-3-methylimidazolium bromide ([Bmim]Br), which has high ionic conductivity and low surface tension, affected the morphologies of the products and allowed the reactions to be carried out under mild conditions. The growth mechanism of ZnSe hollow microspheres has been discussed

  7. Solvothermal synthesis of mesoporous magnetite nanoparticles for Cr(IV) ions uptake and microwave absorption

    Science.gov (United States)

    Shen, Peng; Zhang, Haitao; Zhang, Suojiang; Yuan, Pei; Yang, Yang; Zhang, Qiang; Zhang, Xixiang

    2016-05-01

    Colloidal mesoporous magnetite nanoparticles with tunable porosity were realized by a simple and scalable solvothermal route with the aid of AOT as ligands. AOT was used to induce the anisotropic crystal growth of smaller nanocrystals and restrain their tight aggregation so as to form more mesoscale pores. Morphologies and microstructures investigation by SEM and TEM revealed that the bigger nanoparticles were composed of smaller nanocrystals with an average size of 18 nm. A possible formation mechanism was proposed for the mesoporous nanoparticles. Study of nitrogen adsorption-desorption isotherm revealed that the Brunauer-Emmett-Teller (BET) specific surface area of mesoporous nanoparticles is up to 209 m2/g, resulting from the slit-shaped pores created by the aggregation of polyhedral nanocrystals. Magnetic properties study indicated that the as-prepared nanoparticles are superparamagnetic at room temperature. Optimized mesoporous magnetite nanoparticles exhibit a maximum Cr(VI) ion sorption capacity of 12.9 mmol/g, and its absorption behavior followed a Freundlich model. Microwave absorption study indicated that porous nanoparticles own higher permeability values than that of solid nanoparticles, leading to a higher dielectric loss in the frequency range of 2-18 GHz.

  8. Solvothermal Synthesis of TiO2 Photocatalysts in Ketone Solvents with Low Boiling Points

    Directory of Open Access Journals (Sweden)

    Chau Thanh Nam

    2013-01-01

    Full Text Available The titanium dioxide (TiO2 photocatalysts were synthesized by a solvothermal process in highly alkaline 70 : 30 water : ketone solutions with a TiO2-P25 precursor and calcined at different temperatures. The ketone solvents, such as acetone and methyl ethyl ketone (MEK, had low boiling points (<100°C. The as-prepared samples were characterized by XRD, TEM, FTIR, UV-vis and Raman spectroscopy. The effects of the different solvents on the nanostructure, the morphology, and the photocatalytic performance of the TiO2 products were investigated. Nanotubes formed in water and water-MEK, while nanoparticle/nanowires formed in water-acetone and water-acetone-MEK. The ketone solvents played an important role in the improving nanostructure properties of these products, which affected their photocatalytic reactions. The results indicated that samples synthesized in solvents such as water and MEK had high adsorption and photocatalytic behaviors. The photocatalytic reactivity was the greatest for the TiO2 prepared in MEK and calcined at 100°C, which was even more reactive than the sample prepared in water and TiO2-P25 powder.

  9. Solvothermal synthesis of a polyaniline nanocomposite – a prospective biosensor electrode material

    Directory of Open Access Journals (Sweden)

    R. K. Agrawalla

    2016-09-01

    Full Text Available Polyaniline (PANI is the most important conducting polymer with excellent electrochemical properties. So PANIbased biosensors may find wide applications in medical diagnostics. We report here a ternary nanocomposite of gold nanoparticle-decorated single- walled carbon nanotubes (SWCNTs embedded in sulfonated polyaniline matrix, prepared using a simple solvothermal chemical route. The structural and morphological characteristics have been determined by electron microscopy, X-ray diffraction and Raman spectroscopy. Optical characteristics of the nanocomposite have been determined by ultraviolet (UV-visible absorption spectroscopy and photoluminescence spectroscopy. The direct current (DC-conductivity measurement of the material shows a significant increase in electrical conductivity at 353 K from 7.80·10–2 S/m for pure SPANI to 10.91 S/m for the 3-phase nanocomposite as synthesized in the present investigations. Thus the incorporation of SWCNT/Au nanohybrid fibers in the PANI matrix enhanced its electrical properties. Sulfonation increased the processability of the material, as the samples have now been found to be soluble in water and common organic solvents like DMSO. Such a functional nanocomposite will make an excellent biosensor electrode material.

  10. One-step solvothermal synthesis of carnation flower-like SnS2 as superior electrodes for supercapacitor applications

    Science.gov (United States)

    Mishra, Rajneesh Kumar; Baek, Geun Woo; Kim, Kyuwon; Kwon, Hyuck-In; Jin, Sung Hun

    2017-12-01

    We report the synthesis of carnation flower-like SnS2 (CF-SnS2) via a one-step solvothermal method for potential application as supercapacitor electrodes in energy storage devices. The structural and morphological properties of CF-SnS2 were characterized by X-ray diffraction, Raman analysis, and field-emission scanning and transmission electron microscopies. X-ray photoelectron spectroscopy and scanning tunneling electron microscopy with color mapping verified the distribution of Sn and S, and depicted the successful formation of SnS2. Electrochemical studies were performed to explore the supercapacitive nature of CF-SnS2. Supercapacitors with CF-SnS2 electrodes delivered excellent cyclic voltammetry performances, superior gravimetric specific capacitances, and high power densities. The evaluated specific capacitance and power density reached ∼524.5 F/g and 12.3 W/kg, respectively, at a current density of 0.08 A/g, and ∼215.9 F/g and 61.4 W/kg, respectively, at a current density of 0.38 A/g. These values are at least two times higher than those previously reported. The long-term cyclic stability was also tested to demonstrate the endurance of the CF-SnS2-based supercapacitor, with a 66% rate retention and galvanostatic charge/discharge reversibility. These electrochemical findings indicate that CF-SnS2 is a promising candidate for electrode materials in supercapacitor applications.

  11. 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 ...

  12. 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 ( ...

  13. Synthesis of hexagonal wurtzite Cu{sub 2}ZnSnS{sub 4} prisms by an ultrasound-assisted microwave solvothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Long, Fei, E-mail: long.drf@gmail.com [Key Laboratory of New Processing Technology for Nonferrous Metals and Materials of Ministry of Education, Guilin University of Technology, Guilin 541004 (China); Chi, Shangsen [Key Laboratory of New Processing Technology for Nonferrous Metals and Materials of Ministry of Education, Guilin University of Technology, Guilin 541004 (China); Institute of Advanced Materials and Technology, University of Science and Technology Beijing, Beijing 100083 (China); He, Jinyun; Wang, Jilin; Wu, Xiaoli; Mo, Shuyi; Zou, Zhengguang [Key Laboratory of New Processing Technology for Nonferrous Metals and Materials of Ministry of Education, Guilin University of Technology, Guilin 541004 (China)

    2015-09-15

    Wurtzite Cu{sub 2}ZnSnS{sub 4} (CZTS) hexagonal prisms were synthesized by a simple ultrasound-microwave solvothermal method. The product was characterized by XRD, FESEM, EDS, TEM, Raman and UV–vis spectrometer. The hexagonal prisms were 0.5–2 μm wide and 5–12 μm long. The PVP played an important role in the formation of the CZTS hexagonal prisms. In addition, the ultrasound-assisted microwave process was helpful for synthesis of wurtzite rather than kesterite phase CZTS. A nucleation–dissolution–recrystallization mechanism was also proposed to explain the growth of the CZTS hexagonal prisms. - Graphical abstract: Wurtzite Cu{sub 2}ZnSnS{sub 4} hexagonal prisms were synthesized by ultrasound-microwave solvothermal method. The ultrasound-assisted microwave process and PVP were useful to the growth of CZTS. A nucleation–dissolution–recrystallization growth mechanism was also proposed. - Highlights: • Wurtzite Cu{sub 2}ZnSnS{sub 4} was prepared by ultrasound-assisted microwave solvothermal method. • The wurtzite CZTS hexagonal prisms are demonstrated a band gap of 1.49 eV. • Synergistic effect of ultrasound and microwave is helpful to prepare Wurtzite CZTS. • PVP plays an important role in the formation of the CZTS hexagonal prisms. • Nucleation–dissolution–recrystallization growth mechanism of the CZTS was proposed.

  14. One-pot solvothermal synthesis of ordered intermetallic Pt{sub 2}In{sub 3} as stable and efficient electrocatalyst towards direct alcohol fuel cell application

    Energy Technology Data Exchange (ETDEWEB)

    Jana, Rajkumar; Peter, Sebastian C., E-mail: sebastiancp@jncasr.ac.in

    2016-10-15

    Ordered intermetallic Pt{sub 2}In{sub 3} nanoparticles have been synthesized by superhydride reduction of K{sub 2}PtCl{sub 4} and InCl{sub 3}.xH{sub 2}O precursors using facile, one-pot solvothermal method. We report surfactant free solvothermal synthesis of a novel ordered Pt{sub 2}In{sub 3} intermetallic nanoparticles for the first time. The structure and morphology of the catalyst has been confirmed by powder X-ray diffraction, transmission electron microscopy, field emission scanning electron microscopy, energy-dispersive spectrometry and X-ray photoelectron spectroscopy. The electrocatalytic properties of the catalysts have been investigated by cyclic voltammetry and chronoamperometry. The as prepared Pt{sub 2}In{sub 3} catalyst exhibit far superior electrocatalytic activity and stability towards alcohol oxidation over commercial Pt/C. The specific activity of as synthesized catalyst was found to be ~3.2 and ~2.3 times higher than commercial Pt/C for methanol and ethanol oxidation, respectively. This improved activity and durability of the Pt{sub 2}In{sub 3} nanoparticles can make the catalyst an ideal catalyst candidate for direct alcohol fuel cell. - Graphical abstract: The ordered structure of Pt{sub 2}In{sub 3} nanoparticles synthesized by solvothermal method has confirmed through XRD and TEM. Cyclic voltametry and chronoamperometry showed improved catalytic activity and stability compared to commercial Pt/C. - Highlights: • Ordered Pt{sub 2}In{sub 3} nanoparticles were synthesized by solvothermal method. • Electrooxidation of alcohols on Pt{sub 2}In{sub 3} catalyst was investigated in acidic medium. • Pt{sub 2}In{sub 3} catalyst has superior catalytic activity compared to commercial Pt/C. • Pt{sub 2}In{sub 3} catalyst exhibited much higher stability than commercial Pt/C.

  15. One-pot solvothermal synthesis of highly water-dispersible size-tunable functionalized magnetite nanocrystal clusters for lipase immobilization.

    Science.gov (United States)

    Zhu, Hao; Hou, Chen; Li, Yijing; Zhao, Guanghui; Liu, Xiao; Hou, Ke; Li, Yanfeng

    2013-07-01

    A facile one-pot synthesis of highly water-dispersible size-tunable magnetite (Fe3O4) nanocrystal clusters (MNCs) end-functionalized with amino or carboxyl groups by a modified solvothermal reduction reaction has been developed. Dopamine and 3,4-dihydroxyhydroxycinnamic acid were used for the first time as both a surfactant and interparticle linker in a polylol process for economical and environment-friendly purposes. Morphology, chemical composition, and magnetic properties of the prepared particles were investigated by several methods, including FESEM, TEM, XRD, XPS, Raman, FTIR, TGA, zeta potential, and VSM. The sizes of the particles could be easily tuned over a wide range from 175 to 500 nm by varying the surfactant concentration. Moreover, ethylene glycol/diethylene glycol (EG/DEG) solvent mixtures with different ratios could be used as reductants to obtain the particles with smaller sizes. The XRD data demonstrated that the surfactants restrained the crystal growth of the grains. The nanoparticles showed superior magnetic properties and high colloidal stability in water. The cytotoxicity results indicated the feasibility of using the synthesized nanocrystals in biology-related fields. To estimate the applicability of the obtained MNCs in biotechnology, Candida rugosa lipase was selected for the enzyme immobilization process. The immobilized lipase exhibited excellent thermal stability and reusability in comparison with the free enzyme. This novel strategy would simplify the reaction protocol and improve the efficiency of materials functionalization, thus offering new potential applications in biotechnology and organocatalysis. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Surfactant-controlled composition and crystal structure of manganese(II sulfide nanocrystals prepared by solvothermal synthesis

    Directory of Open Access Journals (Sweden)

    Elena Capetti

    2015-12-01

    Full Text Available We investigated how the outcome of the solvothermal synthesis of manganese(II sulfide (MnS nanocrystals (NCs is affected by the type and amount of long chain surfactant present in the reaction mixture. Prompted by a previous observation that a larger than stoichiometric amount of sulfur is required [Puglisi, A.; Mondini, S.; Cenedese, S.; Ferretti, A. M.; Santo, N.; Ponti A. Chem. Mater. 2010, 22, 2804–2813], we carried out a wide set of reactions using Mn(II carboxylates and Mn2(CO10 as precursors with varying amounts of sulfur and carboxylic acid. MnS NCs were obtained provided that the S/Mn ratio was larger than the L/Mn ratio, otherwise MnO NCs were produced. Since MnS can crystallize in three distinct phases (rock salt α-MnS, zincblende β-MnS, and wurtzite γ-MnS, we also investigated whether the surfactant affected the NC polymorphism. We found that MnS polymorphism can be controlled by appropriate selection of the surfactant. γ-MnS nanocrystals formed when a 1:2 mixture of long chain carboxylic acid and amine was used, irrespective of the presence of carboxylic acid as a free surfactant or ligand in the metal precursor. When we used a single surfactant (carboxylic acid, alcohol, thiol, amine, α-MnS nanocrystals were obtained. The peculiar role of the amine seems to be related to its basicity. The nanocrystals were characterized by TEM and electron diffraction; ATR-FTIR spectroscopy provided information about the surfactants adsorbed on the NCs.

  17. Solvothermal synthesis of nanocrystalline KTaO.sub.3./sub. : Effect of solvent dielectric constant

    Czech Academy of Sciences Publication Activity Database

    Makarova, Marina; Bykov, Pavlo; Drahokoupil, Jan; Čerňanský, Marian; Dlabáček, Zdeněk; Dejneka, Alexandr; Jastrabík, Lubomír; Trepakov, Vladimír

    2012-01-01

    Roč. 47, č. 7 (2012), s. 1798-1773 ISSN 0025-5408 R&D Projects: GA AV ČR KAN301370701; GA ČR GAP108/12/1941 Institutional research plan: CEZ:AV0Z10100522; CEZ:AV0Z10100520 Keywords : nanostructures * chemical synthesis * Raman spectroscopy * X-ray diffraction Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.913, year: 2012

  18. Low-temperature solvothermal approach to the synthesis of La4Ni3O8 by topotactic oxygen deintercalation.

    Science.gov (United States)

    Blakely, Colin K; Bruno, Shaun R; Poltavets, Viktor V

    2011-07-18

    A chimie douce solvothermal reduction method is proposed for topotactic oxygen deintercalation of complex metal oxides. Four different reduction techniques were employed to qualitatively identify the relative reduction activity of each including reduction with H(2) and NaH, solution-based reduction using metal hydrides at ambient pressure, and reduction under solvothermal conditions. The reduction of the Ruddlesden-Popper nickelate La(4)Ni(3)O(10) was used as a test case to prove the validity of the method. The completely reduced phase La(4)Ni(3)O(8) was produced via the solvothermal technique at 150 °C--a lower temperature than by other more conventional solid state oxygen deintercalation methods.

  19. The growth of high density network of MOF nano-crystals across macroporous metal substrates - Solvothermal synthesis versus rapid thermal deposition

    Science.gov (United States)

    Maina, James W.; Gonzalo, Cristina Pozo; Merenda, Andrea; Kong, Lingxue; Schütz, Jürg A.; Dumée, Ludovic F.

    2018-01-01

    Fabrication of metal organic framework (MOF) films and membranes across macro-porous metal substrates is extremely challenging, due to the large pore sizes across the substrates, poor wettability, and the lack of sufficient reactive functional groups on the surface, which prevent high density nucleation of MOF crystals. Herein, macroporous stainless steel substrates (pore size 44 × 40 μm) are functionalized with amine functional groups, and the growth of ZIF-8 crystals investigated through both solvothermal synthesis and rapid thermal deposition (RTD), to assess the role of synthesis routes in the resultant membranes microstructure, and subsequently their performance. Although a high density of well interconnected MOF crystals was observed across the modified substrates following both techniques, RTD was found to be a much more efficient route, yielding high quality membranes under 1 h, as opposed to the 24 h required for solvothermal synthesis. The RTD membranes also exhibited high gas permeance, with He permeance of up to 2.954 ± 0.119 × 10-6 mol m-2 s-1 Pa-1, and Knudsen selectivities for He/N2, Ar/N2 and CO2/N2, suggesting the membranes were almost defect free. This work opens up route for efficient fabrication of MOF films and membranes across macro-porous metal supports, with potential application in electrically mediated separation applications.

  20. Diamond network: template-free fabrication and properties.

    Science.gov (United States)

    Zhuang, Hao; Yang, Nianjun; Fu, Haiyuan; Zhang, Lei; Wang, Chun; Huang, Nan; Jiang, Xin

    2015-03-11

    A porous diamond network with three-dimensionally interconnected pores is of technical importance but difficult to be produced. In this contribution, we demonstrate a simple, controllable, and "template-free" approach to fabricate diamond networks. It combines the deposition of diamond/β-SiC nanocomposite film with a wet-chemical selective etching of the β-SiC phase. The porosity of these networks was tuned from 15 to 68%, determined by the ratio of the β-SiC phase in the composite films. The electrochemical working potential and the reactivity of redox probes on the diamond networks are similar to those of a flat nanocrystalline diamond film, while their surface areas are hundreds of times larger than that of a flat diamond film (e.g., 490-fold enhancement for a 3 μm thick diamond network). The marriage of the unprecedented physical/chemical features of diamond with inherent advantages of the porous structure makes the diamond network a potential candidate for various applications such as water treatment, energy conversion (batteries or fuel cells), and storage (capacitors), as well as electrochemical and biochemical sensing.

  1. Controllable 5-sulfosalicylic acid assisted solvothermal synthesis of monodispersed superparamagnetic Fe{sub 3}O{sub 4} nanoclusters with tunable size

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Wentao [State Key Laboratory of Fine Chemicals, Dalian University of Technology, Dalian 116024 (China); Tang, Bingtao, E-mail: tangbt@dlut.edu.cn [State Key Laboratory of Fine Chemicals, Dalian University of Technology, Dalian 116024 (China); Wu, Suli; Gao, Zhanming; Ju, Benzhi [State Key Laboratory of Fine Chemicals, Dalian University of Technology, Dalian 116024 (China); Teng, Xiaoxu [School of Chemistry and Chemical Engineering, Yangtze Normal University, Chongqing 408100 (China); Zhang, Shufen [State Key Laboratory of Fine Chemicals, Dalian University of Technology, Dalian 116024 (China)

    2017-02-01

    Monodispersed Fe{sub 3}O{sub 4} nanoclusters were synthesized in a one-pot solvothermal route with 5-sulfosalicylic acid (SSA) as the functional ligand in a mixed-solvent system of diethylene glycol/ethylene glycol (DEG/EG). Nucleation and aggregation growth model was responsible for the formation of secondary structure of the clusters. In the process, the size of the clusters can be effectively controlled by varying the amounts of SSA and the volume ratio of DEG/EG. The nanoclusters exhibited superparamagnetic properties with high saturation magnetization value of about 68.7 emu g{sup −1} at room temperature. The water-soluble small-molecule SSA grafted on the surface of Fe{sub 3}O{sub 4} nanocrystals rendered the superparamagnetic clusters dispersible in water, which is crucial for potential applications in biomedical fields. - Graphical abstract: 5-sulfosalicylic acid assisted solvothermal synthesis of monodispersed superparamagnetic Fe{sub 3}O{sub 4} nanoclusters with tunable size by a mixed-solvent system of DEG/EG. - Highlights: • Monodispersed Fe{sub 3}O{sub 4} nanoclusters were synthesized in a one-pot 5-sulfosalicylic acid assisted solvothermal route. • The size of the clusters are tunable by varying the amounts of 5-sulfosalicylic acid and the volume ratio of DEG/EG. • The nanoclusters exhibited superparamagnetic properties with high saturation magnetization value. • The 5-sulfosalicylic acid grafted Fe{sub 3}O{sub 4} nanoclusters can be dispersed in water.

  2. Template-free and filamentary growth of silver nanowires: application to anisotropic conductive transparent flexible electrodes

    Science.gov (United States)

    Park, Sun Hwa; Shin, Ho Sun; Kim, Young Heon; Park, Hyun Min; Song, Jae Yong

    2013-02-01

    Silver nanowires (NWs) are currently fabricated via template-free or template-assisted methods. The former is based on a medium-mediated anisotropic synthesis, which enables precursor atoms to be selectively adsorbed onto specific crystallographic planes, and the latter is performed via directional growth guided by preformed templates. These methods are costly and complicated. We outline a facile and low-cost approach for the electrochemical synthesis of silver NWs in a manner that is template- and surfactant-free and that provides control over the NW diameter in the range of 80 to 800 nm by the repetition of nucleation and dissolution. The nanowires vertically grow with the help of the interface anisotropy driven by a field enhancement at the tips of the islands nucleated on the substrate in ultra-dilute electrolytes (ca. 10-5 M), which is similar to a lightning-rod effect. The silver nanowires of vertical configuration are utilized for fabrication of anisotropic conducting, transparent, and flexible films.Silver nanowires (NWs) are currently fabricated via template-free or template-assisted methods. The former is based on a medium-mediated anisotropic synthesis, which enables precursor atoms to be selectively adsorbed onto specific crystallographic planes, and the latter is performed via directional growth guided by preformed templates. These methods are costly and complicated. We outline a facile and low-cost approach for the electrochemical synthesis of silver NWs in a manner that is template- and surfactant-free and that provides control over the NW diameter in the range of 80 to 800 nm by the repetition of nucleation and dissolution. The nanowires vertically grow with the help of the interface anisotropy driven by a field enhancement at the tips of the islands nucleated on the substrate in ultra-dilute electrolytes (ca. 10-5 M), which is similar to a lightning-rod effect. The silver nanowires of vertical configuration are utilized for fabrication of

  3. Walnut-like In2S3 microspheres: ionic liquid-assisted solvothermal synthesis, characterization and formation mechanism.

    Science.gov (United States)

    Chai, Bo; Zeng, Peng; Zhang, Xiaohu; Mao, Jin; Zan, Ling; Peng, Tianyou

    2012-04-07

    Walnut-like In(2)S(3) microspheres were synthesized through an ionic liquid-assisted solvothermal method for the first time. The crystal structure and morphology of the as-synthesized products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), energy-dispersive X-ray (EDX) spectroscopy, X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectra (DRS) and nitrogen adsorption-desorption measurement. It was found that the additional amount of ionic liquid, solvothermal temperature and time played crucial roles in controlling the structure and morphology of the In(2)S(3) microspheres. A possible formation mechanism of the walnut-like In(2)S(3) microsphere was proposed on the basis of the experimental results. This journal is © The Royal Society of Chemistry 2012

  4. Solvothermal synthesis of hierarchical TiO{sub 2} nanostructures with tunable morphology and enhanced photocatalytic activity

    Energy Technology Data Exchange (ETDEWEB)

    Fan, Zhenghua [School of Physics and Materials Science, Anhui University, Hefei 230601 (China); 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, Miao [School of Physics and Materials Science, Anhui University, Hefei 230601 (China); Wu, Zhenyu [College of Chemistry & Chemical Engineering, Anhui University, Hefei 230601 (China); Sun, Zhaoqi; Li, Aixia [School of Physics and Materials Science, Anhui University, Hefei 230601 (China)

    2016-01-01

    Graphical abstract: - Highlights: • Hierarchical anatase TiO{sub 2} nanostructures with enhanced photocatalytic activity are synthesized by solvothermal method. • A mechanism for enhanced photocatalytic activity of chrysanthemum-like hierarchical TiO{sub 2} nanostructures is proposed. • A possible formation mechanism is suggested to explain the transformation from rose-like to chrysanthemum-like, and to sea-urchin-like. - Abstract: This paper presents controllable growth and photocatalytic activity of TiO{sub 2} hierarchical nanostructures by solvothermal method at different temperatures. It is revealed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) that the morphology of TiO{sub 2} can be effectively controlled as rose-like, chrysanthemum-like and sea-urchin-like only changing solvothermal temperature. BET surface area analysis confirms the presence of a mesoporous network in all the nanostructures, and shows high surface area at relatively high temperature. The photocatalytic activities of the photocatalysts are evaluated by the photodegradation of RhB under UV light irradiation. The TiO{sub 2} samples exhibit high activity on the photodegradation of RhB, which is higher than that of the commercial P25. The enhancement in photocatalytic performance can be attributed to the synergetic effect of the surface area, crystallinity, band gap and crystalline size.

  5. Novel microwave-assisted solvothermal synthesis of NaYF4:Yb,Er upconversion nanoparticles and their application in cancer cell imaging.

    Science.gov (United States)

    Mi, Congcong; Tian, Zhenhuang; Cao, Can; Wang, Zhijia; Mao, Chuanbin; Xu, Shukun

    2011-12-06

    This work reports the novel microwave-assisted solvothermal synthesis and structural, topographic, spectroscopic characterization of NaYF(4):Yb,Er upconversion nanoparticles (UCNPs) as well as their application in the labeling of HeLa cells. The nanoparticles were prepared in ethylene glycol, with rare earth acetates as precursor and NH(4)F and NaCl as the fluorine and sodium sources. X-ray diffraction, transmission electron microscopy, and luminescence spectroscopy were applied to characterize the nanoparticles. Experimental results showed that the microwave-assisted solvothermal method is an effective approach to create highly crystalline, strongly luminescent UCNPs at a lower temperature (160 °C) and within a significantly shortened reaction time (only 1 h) compared to the traditional methods. The effect of fluorine source on the optical properties of UCNPs was investigated by using NH(4)F, NH(4)HF(2), NaF, and 1-butyl-3-methylimidazolium tetrafluoroborate (BmimBF(4)) as different fluorine sources; NH(4)F proved to be the best one, making the luminescent intensity increase at least 2 orders of magnitude. The UCNPs with four different colors (green, yellow, orange, and cyan) were successfully obtained. After being modified with amino groups and coupled with CEA-8 antibody, the obtained nanoparticles were successfully applied in the specific fluorescent immunolabeling and imaging of HeLa cells to further verify their function as a marker in immunolabeling. © 2011 American Chemical Society

  6. One-pot solvothermal synthesis of ordered intermetallic Pt2In3 as stable and efficient electrocatalyst towards direct alcohol fuel cell application

    Science.gov (United States)

    Jana, Rajkumar; Peter, Sebastian C.

    2016-10-01

    Ordered intermetallic Pt2In3 nanoparticles have been synthesized by superhydride reduction of K2PtCl4 and InCl3.xH2O precursors using facile, one-pot solvothermal method. We report surfactant free solvothermal synthesis of a novel ordered Pt2In3 intermetallic nanoparticles for the first time. The structure and morphology of the catalyst has been confirmed by powder X-ray diffraction, transmission electron microscopy, field emission scanning electron microscopy, energy-dispersive spectrometry and X-ray photoelectron spectroscopy. The electrocatalytic properties of the catalysts have been investigated by cyclic voltammetry and chronoamperometry. The as prepared Pt2In3 catalyst exhibit far superior electrocatalytic activity and stability towards alcohol oxidation over commercial Pt/C. The specific activity of as synthesized catalyst was found to be 3.2 and 2.3 times higher than commercial Pt/C for methanol and ethanol oxidation, respectively. This improved activity and durability of the Pt2In3 nanoparticles can make the catalyst an ideal catalyst candidate for direct alcohol fuel cell.

  7. Solvothermal synthesis of uniform hexagonal-phase ZnS nanorods using a single-source molecular precursor

    International Nuclear Information System (INIS)

    Zhang Yongcai; Wang Guiyun; Hu Xiaoya; Chen Weiwei

    2006-01-01

    Pure and uniform hexagonal-phase ZnS nanorods with quantum confinement effect were synthesized by solvothermal decomposition of an air-stable, easily obtained single-source molecular precursor (zinc diethyldithiocarbamate, Zn-(DDTC) 2 ) in hydrazine hydrate aqueous solutions at 150-200 deg. C, and characterized by powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED) and UV-vis absorption spectra. The possible formation mechanism of one-dimensional ZnS nanostructure in the present system was also briefly discussed

  8. Solvothermal synthesis and high optical performance of three-dimensional sea-urchin-like TiO{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Yi, E-mail: zhouyihn@163.com; Wang, Yutang; Li, Mengyao; Li, Xuzhi; Yi, Qin; Deng, Pan; Wu, Hongyan

    2015-06-15

    Graphical abstract: I–V characteristics of different TiO{sub 2} microspheres based DSSCs (a) 3D sphere-like, (b) 3D flower-like, (c) 3D sea-urchin-like. - Highlights: • 3D sea-urchin-like TiO{sub 2} was synthesized by solvothermal method. • The effects of preparation parameters on the microstructure of the microspheres were investigated. • The photoelectric properties of 3D sea-urchin-like TiO{sub 2} were studied upon DSSCs. • The PCE of the 3D sea-urchin-like TiO{sub 2} was higher than that of other morphologies. - Abstract: Three-dimensional (3D) sea-urchin-like TiO{sub 2} microspheres were successfully synthesised by solvothermal method. The effects of preparation parameters including reaction temperature, concentration and mass fraction of precursor, and solvent volume on the microstructure of the microspheres were investigated. Results of scanning electron microscopy showed that the preparation parameters played a critical role in the morphology of 3D sea-urchin-like TiO{sub 2}. In addition, when the sea-urchin-like TiO{sub 2} nanostructures were used as the dye-sensitized solar cells (DSSCs) anode, the power-conversion efficiency was higher than that of other morphologies, which was due to the special 3D hierarchical nanostructure, large specific surface area, and enhanced absorption of UV–vis of the TiO{sub 2} nanostructures.

  9. Solvothermal synthesis of octahedral NiFe{sub 2}O{sub 4} nanocrystals and catalytic properties for the reduction of some aromatic nitrocompounds

    Energy Technology Data Exchange (ETDEWEB)

    Zheng, Hangsong [College of Chemistry and Materials Science, Key Laboratory of Functional Molecular Solids of Ministry of Education, Anhui Laboratory of Molecule-Based Materials, Anhui Key Laboratory of Functional Molecular Solids, Anhui Normal University, 1 Beijing Eastern Road, Wuhu 241000 (China); Ni, Yonghong, E-mail: niyh@mail.ahnu.edu.cn [College of Chemistry and Materials Science, Key Laboratory of Functional Molecular Solids of Ministry of Education, Anhui Laboratory of Molecule-Based Materials, Anhui Key Laboratory of Functional Molecular Solids, Anhui Normal University, 1 Beijing Eastern Road, Wuhu 241000 (China); Xiang, Nannan [College of Chemistry and Materials Science, Key Laboratory of Functional Molecular Solids of Ministry of Education, Anhui Laboratory of Molecule-Based Materials, Anhui Key Laboratory of Functional Molecular Solids, Anhui Normal University, 1 Beijing Eastern Road, Wuhu 241000 (China); Ma, Xiang [Center of Modern Analyses, Nanjing University, Nanjing 210093 (China); Wan, Fengying [Library of Anhui Normal University, 1 Beijing Eastern Road, Wuhu 241000 (China)

    2015-05-05

    In this paper, we report the successful synthesis of octahedral NiFe{sub 2}O{sub 4} nanocrystals with room-temperature ferrimagnetism via a mixed solvothermal process at 170 °C for 15 h, using Fe(NO{sub 3}){sub 3} and NiCl{sub 2} as starting reactants. The phase and morphology of the as-prepared product is characterized by means of powder X-ray diffraction, energy dispersive spectrometry, selected area electron diffraction (SAED), (high resolution) transmission electron microscopy, and scanning electron microscopy. Experiments showed that the as-prepared octahedral NiFe{sub 2}O{sub 4} nanocrystals owned strong catalytic activity for the reduction of some aromatic nitro-compounds such as 4-nitrophenol, 2-nitroaniline, 4-nitroaniline, and 2,4-dinitrophenol. Under the presence of 9 mg NiFe{sub 2}O{sub 4} nanocrystals, the rate constants of the reductive reactions were in turn 3.16 × 10{sup −2} min{sup −1} for 4-nitrophenol, 4.28 × 10{sup −2} min{sup −1} for 2-nitroaniline, 6.79 × 10{sup −2} min{sup −1} for 4-nitroaniline, and 3.26 × 10{sup −2} min{sup −1} for 2,4-dinitrophenol. Moreover, the present catalyst could be conveniently recycled due to its magnetism. After ten cycles, its catalytic efficiency did not obviously decrease. - Highlights: • Octahedral NiFe{sub 2}O{sub 4} nanocrystals were successfully prepared by an emulsion-solvothermal route. • NiFe{sub 2}O{sub 4} nanocrystals with the room-temperature magnetism could be used as a recyclable catalyst. • NiFe{sub 2}O{sub 4} nanocrystals showed strong catalytic activity for the reduction of 4-NP in NaBH{sub 4} solution.

  10. Solvothermal synthesis of octahedral NiFe2O4 nanocrystals and catalytic properties for the reduction of some aromatic nitrocompounds

    International Nuclear Information System (INIS)

    Zheng, Hangsong; Ni, Yonghong; Xiang, Nannan; Ma, Xiang; Wan, Fengying

    2015-01-01

    In this paper, we report the successful synthesis of octahedral NiFe 2 O 4 nanocrystals with room-temperature ferrimagnetism via a mixed solvothermal process at 170 °C for 15 h, using Fe(NO 3 ) 3 and NiCl 2 as starting reactants. The phase and morphology of the as-prepared product is characterized by means of powder X-ray diffraction, energy dispersive spectrometry, selected area electron diffraction (SAED), (high resolution) transmission electron microscopy, and scanning electron microscopy. Experiments showed that the as-prepared octahedral NiFe 2 O 4 nanocrystals owned strong catalytic activity for the reduction of some aromatic nitro-compounds such as 4-nitrophenol, 2-nitroaniline, 4-nitroaniline, and 2,4-dinitrophenol. Under the presence of 9 mg NiFe 2 O 4 nanocrystals, the rate constants of the reductive reactions were in turn 3.16 × 10 −2 min −1 for 4-nitrophenol, 4.28 × 10 −2 min −1 for 2-nitroaniline, 6.79 × 10 −2 min −1 for 4-nitroaniline, and 3.26 × 10 −2 min −1 for 2,4-dinitrophenol. Moreover, the present catalyst could be conveniently recycled due to its magnetism. After ten cycles, its catalytic efficiency did not obviously decrease. - Highlights: • Octahedral NiFe 2 O 4 nanocrystals were successfully prepared by an emulsion-solvothermal route. • NiFe 2 O 4 nanocrystals with the room-temperature magnetism could be used as a recyclable catalyst. • NiFe 2 O 4 nanocrystals showed strong catalytic activity for the reduction of 4-NP in NaBH 4 solution

  11. One-step solvothermal synthesis, a worm-shaped morphology and luminescence properties of green-emitting Y2O2S:Tb3+ nanophosphors

    Science.gov (United States)

    Liu, Fan; Lian, Jingbao; Wu, Nianchu; He, Jiao; Zhang, Xue; Liu, Feng

    2018-02-01

    The worm-shaped Y2O2S:Tb3+ nanophosphors have been successfully prepared via one-step solvothermal synthesis, using ethanediamine as the main solvent and sublimed sulfur powder as the source of sulfur without adding additional structure-directing reagents. XRD, FT-IR, FESEM, PL and CIE chromaticity diagram were used to characterize the obtained products. XRD results demonstrate that all diffraction peaks of the sample can be well indexed to pure hexagonal phase of Y2O2S with optimal condition, i.e. the molar ration of S/Y3+m = 10, solvothermal temperature T = 220 °C and synthetic time t = 24 h. When t varies from 2 h to 24 h, the morphology of Y2O2S transforms from cauliflower-like structure to worm-shaped nanoparticles with the length of ∼80 nm. The formation mechanism depending on t has also been proposed. Upon 250 nm ultraviolet (UV) light excitation, the worm-shaped Y2O2S:Tb3+ nanophosphors exhibit green emissions, corresponding to the 5D4 → 7FJ (J = 6, 5, 4, 3) transitions of Tb3+ions. The quenching concentration is 7% and its corresponding lifetime is 1216 μs. The CIE chromaticity coordinates show the tuneable emission shifting from yellow green to yellowish green with increasing concentration of Tb3+ions from 1% to 7%. Those results suggest that the worm-shaped Y2O2S:Tb3+ nanophosphors may have potential applications in X-ray intensifying screens, fluorescence and biomedical fields.

  12. A Novel and Facile One-Pot Solvothermal Synthesis of PEDOT-PSS/Ni-Mn-Co-O Hybrid as an Advanced Supercapacitor Electrode Material.

    Science.gov (United States)

    Yin, Chengjie; Yang, Chunming; Jiang, Min; Deng, Cuifen; Yang, Lishan; Li, Junhua; Qian, Dong

    2016-02-03

    In this work, a novel and facile one-pot method has been developed for the synthesis of a hybrid consisting of Ni-Mn-Co ternary oxide and poly(3,4-ethylenedioxythiophene)-polystyrenesulfonate (PEDOT-PSS/NMCO) with a hierarchical three-dimensional net structure via a solvothermal-coprecipitation coupled with oxidative polymerization route. Apart from the achievement of polymerization, coprecipitation, and solvothermal in one pot, the hydroxyl (OH(-)) ions generated from the oxidative polymerization of organic monomer by neutral KMnO4 solution were skillfully employed as precipitants for metal ions. As compared with the PEDOT-PSS/Ni-Mn binary oxide, PEDOT-PSS/Co-Mn binary oxide, and PEDOT-PSS/MnO2, PEDOT-PSS1.5/NMCO exhibits overwhelmingly superior supercapacitive performance, more specifically, a high specific capacitance of 1234.5 F g(-1) at a current density of 1 A g(-1), a good capacitance retention of 83.7% at a high current density of 5 A g(-1) after 1000 cycles, an energy density of 51.9 W h kg(-1) at a power density of 275 W kg(-1), and an energy density of 21.4 W h kg(-1) at an extremely elevated power density of 5500 W kg(-1). Noticeably, the energy density and power density of PEDOT-PSS/NMCO are by far higher than those of the existing analogues recently reported. The exceptional performance of PEDOT-PSS/NMCO benefits from its unique mesoporous architecture, which could provide a larger reaction surface area, faster ion and electron transfer ability, and good structural stability. The desirable integrated performance enables the multicomponent composite to be a promising electrode material for energy storage applications.

  13. Microwave-assisted solvothermal synthesis and characterization of metastable LiFe(1-x)(VO)(x)PO4 cathodes.

    Science.gov (United States)

    Harrison, Katharine L; Manthiram, Arumugam

    2011-04-18

    Vanadyl ion substituted LiFePO(4) cathodes of the form LiFe(1-x)(VO)(x)PO(4) for 0 ≤ x ≤ 0.25 have been synthesized by a rapid microwave-solvothermal process at neutrality, results in a decrease in the unit cell volume with increasing x despite the substitution of larger (VO)(2+) for Fe(2+). Charge-discharge data of the vanadyl ion substituted samples suggest suppression of the two-phase plateau behavior that is characteristic of LiFePO(4). Electrochemical data collected without any carbon coating reveal that the capacity and rate capability decreases, but the capacity retention improves with (VO)(2+) substitution.

  14. Controlled synthesis of multi-morphology Te crystals by a convenient Lewis acid/base-assisted solvothermal method

    Science.gov (United States)

    Wu, XiaoPing; Yuan, Lin; Zhou, ShaoMin; Lou, ShiYun; Wang, YongQiang; Gao, Tao; Liu, YuBiao; Shi, XiaoJing

    2012-08-01

    This paper reports on the controlled growth of multi-morphology Te crystals by a convenient Lewis acid/base-assisted solvothermal method for the first time. The morphological transformation from one-dimension (1D) nanostructures to 2D hierarchical flowerlike microarchitecture has been observed. The nanorods and nanowires with a well-defined crystallographical structure and the hierarchical flowers microarchitecture were obtained by changing the Lewis acids/bases. Lewis acids/bases were found to be crucial for the formation of the products by not only acting as the pH regulator but also as the shape controller, owing to their hydrolysis in the solvent to in situ form H+/OH- and hydrates. The results suggest that this should be an effective approach to the control the growth of t-Te crystals with interesting multiple morphologies, which are of interest for both theoretical investigations and practical applications.

  15. Controlled synthesis of multi-morphology Te crystals by a convenient Lewis acid/base-assisted solvothermal method

    International Nuclear Information System (INIS)

    Wu Xiaoping; Yuan Lin; Zhou Shaomin; Lou Shiyun; Wang Yongqiang; Gao Tao; Liu YuBiao; Shi Xiaojing

    2012-01-01

    This paper reports on the controlled growth of multi-morphology Te crystals by a convenient Lewis acid/base-assisted solvothermal method for the first time. The morphological transformation from one-dimension (1D) nanostructures to 2D hierarchical flowerlike microarchitecture has been observed. The nanorods and nanowires with a well-defined crystallographical structure and the hierarchical flowers microarchitecture were obtained by changing the Lewis acids/bases. Lewis acids/bases were found to be crucial for the formation of the products by not only acting as the pH regulator but also as the shape controller, owing to their hydrolysis in the solvent to in situ form H + /OH − and hydrates. The results suggest that this should be an effective approach to the control the growth of t-Te crystals with interesting multiple morphologies, which are of interest for both theoretical investigations and practical applications.

  16. Solvothermal Synthesis of Caesium Tungsten Bronze in the Presence of Various Organic Acids and Its NIR Absorption Properties

    Energy Technology Data Exchange (ETDEWEB)

    Guo, Chongshen; Yin, Shu; Sato, Tsugio [Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai (Japan); Adachi, Kenji; Chonan, Takeshi, E-mail: bigguop@mail.tagen.tohoku.ac.jp [Ichikawa Research Laboratory, Sumitomo Metal Mining Co., Ltd (Japan)

    2011-10-29

    Nanoparticles of caesium tungsten bronze were successfully synthesized by solvothermal reactions in ethanol with the introduction of different organic fatty acids with various carbon numbers of 1 to 5. Compared to the sample prepared in pure ethanol, the samples obtained by mixed solvent of ethanol and fatty acids showed higher production yield, smaller particle size, more uniform particles size distribution and higher Cs/W atomic ratio. In addition, all of samples obtained using acids-ethanol mixed solvent exhibited higher visible light transmittance and greater NIR absorption performance, indicating the potential application for smart window and heat-ray shielding materials. The addition of acetic acid showed the best performance to facilitate the formation of well dispersed Cs{sub x}WO{sub 3} regular nanorods, leading to its excellent optical properties.

  17. Low temperature solvothermal synthesis of nanosized NiSb as a Li-ion battery anode material

    International Nuclear Information System (INIS)

    Xie, J.; Zhao, X.B.; Yu, H.M.; Qi, H.; Cao, G.S.; Tu, J.P.

    2007-01-01

    Nanosized intermetallic compound NiSb was successfully synthesized by a solvothermal route and studied as a promising anode material for secondary lithium-ion batteries. The as-prepared NiSb powder was characterized by X-ray diffraction (XRD), transmission electron microscope (TEM) and field emission scanning electron microscope (FESEM). The electrochemical performance of the nanosized NiSb electrode was investigated by constant current charge and discharge cycling and electrochemical impedance spectroscopy (EIS). It was found that the nanosized NiSb shows a higher initial capacity compared to microsized one prepared by a levitation-melting/ball-milling route due to larger specific surface area of the nanomaterial. The nanosized NiSb shows a rapid capacity fade due to the pulverization and exfoliation of active material caused by severe electrochemical grinding upon long-term cycling

  18. Facile and efficient one-pot solvothermal and microwave-assisted synthesis of stable colloidal solutions of MFe{sub 2}O{sub 4} spinel magnetic nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Solano, Eduardo; Perez-Mirabet, Leonardo [Universitat Autonoma de Barcelona, Departament de Quimica (Spain); Martinez-Julian, Fernando; Guzman, Roger; Arbiol, Jordi; Puig, Teresa; Obradors, Xavier [Institut de Ciencia de Materials de Barcelona, ICMAB-CSIC (Spain); Yanez, Ramon [Universitat Autonoma de Barcelona, Departament de Quimica (Spain); Pomar, Alberto; Ricart, Susagna, E-mail: ricart@icmab.es [Institut de Ciencia de Materials de Barcelona, ICMAB-CSIC (Spain); Ros, Josep [Universitat Autonoma de Barcelona, Departament de Quimica (Spain)

    2012-08-15

    Well-defined synthesis conditions of high quality MFe{sub 2}O{sub 4} (M = Mn, Fe, Co, Ni, Zn, and Cu) spinel ferrite magnetic nanoparticles, with diameters below 10 nm, have been described based on facile and efficient one-pot solvothermal or microwave-assisted heating procedures. Both methods are reproducible and scalable and allow forming concentrated stable colloidal solutions in polar solvents, but microwave-assisted heating allows reducing 15 times the required annealing time and leads to an enhanced monodispersity of the nanoparticles. Non-agglomerated nanoparticles dispersions have been achieved using a simple one-pot approach where a single compound, triethyleneglycol, behaves at the same time as solvent and capping ligand. A narrow nanoparticle size distribution and high quality crystallinity have been achieved through selected nucleation and growth conditions. High resolution transmission electron microscopy images and electron energy loss spectroscopy analysis confirm the expected structure and composition and show that similar crystal faceting has been formed in both synthetic approaches. The spinel nanoparticles behave as ferrimagnets with a high saturation magnetization and are superparamagnetic at room temperature. The influence of synthesis route on phase purity and unconventional magnetic properties is discussed in some particular cases such as CuFe{sub 2}O{sub 4}, CoFe{sub 2}O{sub 4}, and ZnFe{sub 2}O{sub 4}.

  19. Facile and efficient one-pot solvothermal and microwave-assisted synthesis of stable colloidal solutions of MFe2O4 spinel magnetic nanoparticles

    International Nuclear Information System (INIS)

    Solano, Eduardo; Perez-Mirabet, Leonardo; Martinez-Julian, Fernando; Guzmán, Roger; Arbiol, Jordi; Puig, Teresa; Obradors, Xavier; Yañez, Ramón; Pomar, Alberto; Ricart, Susagna; Ros, Josep

    2012-01-01

    Well-defined synthesis conditions of high quality MFe 2 O 4 (M = Mn, Fe, Co, Ni, Zn, and Cu) spinel ferrite magnetic nanoparticles, with diameters below 10 nm, have been described based on facile and efficient one-pot solvothermal or microwave-assisted heating procedures. Both methods are reproducible and scalable and allow forming concentrated stable colloidal solutions in polar solvents, but microwave-assisted heating allows reducing 15 times the required annealing time and leads to an enhanced monodispersity of the nanoparticles. Non-agglomerated nanoparticles dispersions have been achieved using a simple one-pot approach where a single compound, triethyleneglycol, behaves at the same time as solvent and capping ligand. A narrow nanoparticle size distribution and high quality crystallinity have been achieved through selected nucleation and growth conditions. High resolution transmission electron microscopy images and electron energy loss spectroscopy analysis confirm the expected structure and composition and show that similar crystal faceting has been formed in both synthetic approaches. The spinel nanoparticles behave as ferrimagnets with a high saturation magnetization and are superparamagnetic at room temperature. The influence of synthesis route on phase purity and unconventional magnetic properties is discussed in some particular cases such as CuFe 2 O 4 , CoFe 2 O 4 , and ZnFe 2 O 4 .

  20. Impact of concentration and Si doping on the properties and phase transformation behavior of nanocrystalline alumina prepared via solvothermal synthesis

    International Nuclear Information System (INIS)

    Mekasuwandumrong, Okorn; Tantichuwet, Panutin; Chaisuk, Choowong; Praserthdam, Piyasan

    2008-01-01

    Solvothermal reaction of 20 g aluminum isopropoxide (AIP) in mineral oil at 300 deg. C for 2 h gave χ-alumina showing high thermal stability while the reaction with higher amounts of starting AIP (30 and 40 g) contributed contamination of pseudoboehmite. The χ-alumina thus obtained directly transformed into α-alumina completely at approximately 1400 deg. C bypassing the other transition alumina phases whereas some part of the contaminated product transformed to γ-alumina through θ-alumina and finally α-alumina. When silicon was doped in the alumina matrix (5, 10, 20 and 50 at.%) using tetraethylorthosilicate as the silicon (Si) precursor, χ-alumina was still observed without any contaminations at low concentration doping (5-20 at.%). Amorphous structure was obtained by doping 50 at.% Si. The phase transformation temperature was shifted to the high temperature after loading the Si. The α-phase transformation did not go to completion even after calcinations at 1500 deg. C. This could be due to the incorporation of Si atom in alumina lattice forming SiO 2 -Al 2 O 3 solid solution

  1. Solvothermal synthesis and photoluminescence properties of ZnS:Mn2+/ZnO core-shell nanocrystals.

    Science.gov (United States)

    Wang, Yuhua; Li, Chengyan; Peng, Lingling

    2010-03-01

    High-quality ZnS:Mn2+ and ZnS:Mn2+/ZnO core-shell nanocrystals (NCs) were synthesized via a solvothermal method, and characterized by X-ray diffraction (XRD), Transmission electron microscopy (TEM), ultraviolet-visible (UV-vis) and photoluminescence (PL) spectra. Compared with the bare ZnS:Mn2+ NCs (10 nm), the obtained ZnS:Mn2+/ZnO core-shell NCs have a smaller size (4 nm) and better dispersion, which could be attributed to the added ammonia that adsorbed on the surface of ZnS nuclei and hindered their further growth. From the PL spectrum of ZnS:Mn2+NCs, orange luminescence at about 595 nm is observed, which is attributed to the 4T1-6A1 transition of the Mn2+. Meanwhile, the PL intensity of the ZnS:Mn2+/ZnO core-shell NCs is enhanced, and the emission peak is shifted from 595 to 581 nm. The enhancement of the PL intensity is due to the elimination of the surface defects after the growth of the ZnO shell on ZnS:Mn2+ NCs, while the peak blue shift is mainly ascribed to the stress from the mismatch of lattice constants between ZnS and ZnO NCs.

  2. Solvothermal synthesis, electromagnetic and electrochemical properties of jellylike cylinder graphene-Mn3O4 composite with highly coupled effect

    Science.gov (United States)

    Long, Yuting; Xie, Junliang; Li, Hong; Liu, Zirui; Xie, Yahong

    2017-12-01

    Jellylike cylinder graphene-Mn3O4 composite with highly coupled effect was successfully synthesized by a simple solvothermal process. Without using toxic reducing agent and expensive equipment, this method is environmental compatible and suitable for low cost mass production. High capacitance Mn3O4 nanoparticles are homogeneously anchored on excellent conductivity graphene framework and a growth mechanism is hypothesized. Excellent electron conductivity and unique structure of Mn3O4-graphene composite give rise to various applications such as microwave absorber and electrode material. As a microwave absorber, the composite exhibits lowest reflection loss of -14.2 dB in the frequency range of 2-18 GHz. Good microwave absorption performance is due to the structure of the composite where conductive channels form between nano sized Mn3O4 and high conductivity graphene with defects and dangling bonds. As for electrochemical property, Mn3O4-graphene composite with coupled effect shows excellent performance with highest specific capacitance of 246.7 F g-1 in saturated K2SO4 at a scan rate of 5 mV s-1. Good electrochemical property is also attributed to the structure with high utilization of Mn3O4, fast charge carrier transmission, and excellent electronic conductivity. This composite shows a promising application in absorbing materials and electrodes.

  3. Solvothermal synthesis of CdIn2S4 photocatalyst for selective photosynthesis of organic aromatic compounds under visible light.

    Science.gov (United States)

    Ling, Cancan; Ye, Xiangju; Zhang, Jinghu; Zhang, Jinfeng; Zhang, Sujuan; Meng, Sugang; Fu, Xianliang; Chen, Shifu

    2017-02-09

    Ternary chalcogenide semiconductor, cadmium indium sulfide (CdIn 2 S 4 ), was prepared by a simple solvothermal method using ethylene glycol as a solvent, as well as indium chloride tetrahydrate (InCl 3 . 4H 2 O), cadmium nitrate tetrahydrate [Cd(NO 3 ) 2 . 4H 2 O], and thiacetamide (TAA) as precursors. The resulted sample was subject to a series of characterizations. It is the first time to use CdIn 2 S 4 sample as a visible light-driven photocatalyst for simultaneous selective redox transformation of organic aromatic compounds. The results indicate that the as-synthesized CdIn 2 S 4 photocatalyst not only has excellent photocatalytic performance compared with pure In 2 S 3 and CdS for the selective oxidation of aromatic alcohols in an oxygen environment, but also shows high photocatalytic redox activities under nitrogen atmosphere. A possible mechanism for the photocatalytic redox reaction in the coupled system was proposed. It is hoped that our current work could extend the applications of CdIn 2 S 4 photocatalyst and provide new insights for selective transformations of organic compounds.

  4. Solvothermal synthesis and good microwave absorbing properties for magnetic porous-Fe3O4/graphene nanocomposites

    Directory of Open Access Journals (Sweden)

    Xiaojun Zeng

    2017-05-01

    Full Text Available The magnetic porous-Fe3O4/graphene nanocomposites have been fabricated by a facile solvothermal method. The porous Fe3O4 nanospheres are embedded uniformly in the graphene oxide (GO sheets to form a 3D Fe3O4/GO nanocomposite network. The dielectric properties for the Fe3O4/GO composites can be greatly improved by the 7 wt% GO additions. Good impedance matching can be also obtained in these Fe3O4/GO composites, which is proved to dominate their excellent microwave absorbing properties including the minimum reflection loss (RL value of -43.7 dB at 6.8 GHz with a sample thickness of 5 mm and a broad absorption bandwidth of 5.92 GHz (below -10 dB. These porous-Fe3O4/GO composites also exhibit the good structural stability and low density, which shows their great potential application in high-performance electromagnetic microwave-absorbing materials.

  5. Synthesis of Cu-Poor Copper-Indium-Gallium-Diselenide Nanoparticles by Solvothermal Route for Solar Cell Applications

    Directory of Open Access Journals (Sweden)

    Chung Ping Liu

    2014-01-01

    Full Text Available Copper-indium-gallium-diselenide (CIGS thin films were fabricated using precursor nanoparticle ink and sintering technology. The precursor was a Cu-poor quaternary compound with constituent ratios of Cu/(In+Ga=0.603, Ga/(In+Ga=0.674, and Se/(Cu+In+Ga=1.036. Cu-poor CIGS nanoparticles of chalcopyrite for solar cells were successfully synthesized using a relatively simple and convenient elemental solvothermal route. After a fixed reaction time of 36 h at 180°C, CIGS nanocrystals with diameters in the range of 20–70 nm were observed. The nanoparticle ink was fabricated by mixing CIGS nanoparticles, a solvent, and an organic polymer. Analytical results reveal that the Cu-poor CIGS absorption layer prepared from a nanoparticle-ink polymer by sintering has a chalcopyrite structure and a favorable composition. For this kind of sample, its mole ratio of Cu : In : Ga : Se is equal to 0.617 : 0.410 : 0.510 : 2.464 and related ratios of Ga/(In+Ga and Cu/(In+Ga are 0.554 and 0.671, respectively. Under the condition of standard air mass 1.5 global illumination, the conversion efficiency of the solar cell fabricated by this kind of sample is 4.05%.

  6. Photocatalytic degradation of methyl orange over nitrogen-fluorine codoped TiO2 nanobelts prepared by solvothermal synthesis.

    Science.gov (United States)

    He, Zuoli; Que, Wenxiu; Chen, Jing; Yin, Xingtian; He, Yucheng; Ren, Jiangbo

    2012-12-01

    Anatase type nitrogen-fluorine (N-F) codoped TiO(2) nanobelts were prepared by a solvothermal method in which amorphous titania microspheres were used as the precursors. The as-prepared TiO(2) nanobelts are composed of thin narrow nanobelts and it is noted that there are large amount of wormhole-like mesopores on these narrow nanobelts. Photocatalytic activity of the N-F codoped TiO(2) nanobelts was measured by the reaction of photocatalytic degradation of methyl orange. Results indicate that the photocatalytic activity of the N-F codoped TiO(2) nanobelts is higher than that of P25, which is mainly ascribed to wormhole-like mesopores like prison, larger surface area, and enhanced absorption of light due to N-F codoping. Interestingly, it is also found that the photocatalytic activity can be further enhanced when tested in a new testing method because more photons can be captured by the nanobelts to stimulate the formation of the hole-electron pair.

  7. Tailored super magnetic nanoparticles synthesized via template free hydrothermal technique

    Science.gov (United States)

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

    2016-01-01

    Magnetite nanoparticles of controlled shape and dimensions were synthesized using a modified hydrothermal technique. The influence of different synthesis conditions on the shape, size (length and diameter), structure and magnetic properties of the prepared nanoparticles is presented. The mineral phases, the morphologies, size distribution of the resulting magnetic nanoparticles and their magnetic properties were characterized using different characterization methods. We designed magnetite nanoparticles with different morphologies (nanospheres, nanorods, nanocubes and hexagons) and with improved saturation magnetization reaching 90 emu/g.

  8. Hierarchical assembly of inorganic nanostructure building blocks to octahedral superstructures-a true template-free self-assembly

    International Nuclear Information System (INIS)

    Kuchibhatla, Satyanarayana V N T; Karakoti, Ajay S; Seal, Sudipta

    2007-01-01

    A room temperature, template-free, wet chemical synthesis of ceria nanoparticles and their long term ageing characteristics are reported. High resolution transmission electron microscopy and UV-visible spectroscopy techniques are used to observe the variation in size, structure and oxidation state, respectively as a function of time. The morphology variation and the hierarchical assembly (octahedral superstructure) of nanostructures are imputed to the inherent structural aspects of cerium oxide. It is hypothesized that the 3-5 nm individual building blocks will undergo an intra-agglomerate re-orientation to attain the low energy configuration. This communication also emphasizes the need for long term ageing studies of nanomaterials in various solvents for multiple functionalities

  9. Solvothermal synthesis of TiO{sub 2} nanocrystals with {001} facets using titanic acid nanobelts for superior photocatalytic activity

    Energy Technology Data Exchange (ETDEWEB)

    Cao, Yuhui; Zong, Lanlan [National & Local Joint Engineering Research Center for Applied Technology of Hybrid Nanomaterials, Henan University, Kaifeng, 475004 (China); Li, Qiuye, E-mail: qiuyeli@henu.edu.cn [National & Local Joint Engineering Research Center for Applied Technology of Hybrid Nanomaterials, Henan University, Kaifeng, 475004 (China); Collaborative Innovation Center of Nano Functional Materials and Applications of Henan Province, Henan University, Kaifeng, 475004 (China); Li, Chen; Li, Junli [National & Local Joint Engineering Research Center for Applied Technology of Hybrid Nanomaterials, Henan University, Kaifeng, 475004 (China); Yang, Jianjun, E-mail: yangjianjun@henu.edu.cn [National & Local Joint Engineering Research Center for Applied Technology of Hybrid Nanomaterials, Henan University, Kaifeng, 475004 (China); Collaborative Innovation Center of Nano Functional Materials and Applications of Henan Province, Henan University, Kaifeng, 475004 (China)

    2017-01-01

    Highlights: • TiO{sub 2} exposed with {001} facets were firstly prepared using TAN as Ti source. • The mineralization rate of MO on sample with 77% {001} facets was as high as 96%. • The superior photocatalytic activity was greatly due to {001} facets exposing. - Abstract: Anatase TiO{sub 2} nanocrystals exposed with {001} facets were fabricated by solvothermal strategy in HF-C{sub 4}H{sub 9}OH mixed solution, using titanic acid nanobelts (TAN) as a precursor. The shape of TAN is a long flat plane with a high aspect ratio, and F{sup −} is easily adsorbed on the surface of the nanobelts, inducing a higher exposure of {001} facet of TiO{sub 2} nanoparticles during the structure reorganization. The exposed percentage of {001} facets could vary from 40 to 77% by adjusting the amount of HF. The as-prepared samples were characterized by transmission electron microscopy, N{sub 2} adsorption-desorption isotherms, X-ray diffraction, Raman spectroscopy, and X-ray photoelectron spectroscope. The photocatalytic measurement showed that TiO{sub 2} nanocrystals with 77% {001} facets exhibited much superior photocatalytic activity for photodegradation of methyl orange, methylene blue, and rhodamine B. And what’s more, the mineralization rate of methyl orange was as high as 96% within 60 min. The photocatalytic enhancement is due to a large amount of the high energetic {001} facets exposing, the special truncated octahedral morphology and a stronger ability for dyes adsorption.

  10. One-step solvothermal synthesis of TiO2-reduced graphene oxide nanocomposites with enhanced visible light photoreduction of Cr(VI)

    Science.gov (United States)

    Shaikh, Aasiya; Mishra, Shailendra Prasad; Mohapatra, Priyabrata; Parida, Smrutiranjan

    2017-06-01

    Hexavalent chromium, Cr(VI), is a mutagenic and carcinogenic heavy metal environmental pollutant. Photoreduction is one of the remediation methods of the hexavalent chromium Cr(VI), which necessitates design of an efficient catalyst for visible light performance. Here, we report a one-step solvothermal synthesis of TiO2-reduced graphene oxide (TiO2- xRGO) composite catalysts using a mild reducing agent, dimethylformamide (DMF). Nanoscale TiO2 particles in the size range of 4-9 nm were formed on the reduced graphene sheets. The formation of the composite catalysts was accompanied by the appearance of a large fluorescence quenching, which indicates an efficient separation of photogenerated electrons and holes. The composites displayed excellent photoreduction of Cr(VI) in the visible light, which was found to be a function of the weight percentage of RGO in the composite. At the optimum composition of TiO2- xRGO, a maximum removal rate of 96% was recorded, which was higher than that of the pristine TiO2, which showed no appreciable catalytic activity under the same condition. The performance degraded with increasing RGO content in the composite, which can be attributed to the higher electron-hole recombination on the RGO surface. The Cr(VI) photoreduction also exhibited a pH dependence. The highest removal rate was observed in the acidic medium.

  11. Green synthesis of CuInS2/ZnS core-shell quantum dots by facile solvothermal route with enhanced optical properties

    Science.gov (United States)

    Jindal, Shikha; Giripunje, Sushama M.; Kondawar, Subhash B.; Koinkar, Pankaj

    2018-03-01

    We report an eco-friendly green synthesis of highly luminescent CuInS2/ZnS core-shell quantum dots (QDs) with average particle size ∼ 3.9 nm via solvothermal process. The present study embodies the intensification of CuInS2/ZnS QDs properties by the shell growth on the CuInS2 QDs. The as-prepared CuInS2 core and CuInS2/ZnS core-shell QDs have been characterized using a range of optical and structural techniques. By adopting a low temperature growth of CuInS2 core and high temperature growth of CuInS2/ZnS core-shell growth, the tuning of absorption and photoluminescence emission spectra were observed. Optical absorption and photoluminescence spectroscopy probe the effect of ZnS passivation on the electronic structure of the CuInS2 dots. In addition, QDs have been scrutinized using ultra violet photoelectron spectroscopy (UPS) to explore their electronic band structure. The band level positions of CuInS2 and CuInS2/ZnS QDs suffices the demand of non-toxic acceptor material for electronic devices. The variation in electronic energy levels of CuInS2 core with the coating of wide band gap ZnS shell influence the removal of trap assisted recombination on the surface of the core. QDs exhibited tunable emission from red to orange region. These studies reveal the feasibility of QDs in photovoltaic and light emitting diodes.

  12. Microwave-assisted solvothermal synthesis of flower-like Ag/AgBr/BiOBr microspheres and their high efficient photocatalytic degradation for p-nitrophenol

    International Nuclear Information System (INIS)

    Li, Tingting; Luo, Shenglian; Yang, Lixia

    2013-01-01

    Flower-like Ag/AgBr/BiOBr microspheres were successfully fabricated by the approach of microwave-assisted solvothermal and in situ photo-assisted reduction. A reactive ionic liquid 1-hexadecyl-3-methylimidazolium bromide ([C 16 mim]Br) was employed as Br source in the presence of surfactant polyvinylpyrrolidone (PVP). The photocatalytic activity of Ag/AgBr/BiOBr towards the decomposition of p-nitrophenol under visible light irradiation was evaluated. The results indicated that Ag/AgBr/BiOBr showed enhanced photocatalytic activity towards p-nitrophenol, comparing with P25, BiOBr and Ag/AgBr. More than 96% of p-nitrophenol was decomposed in 3.5 h under visible-light irradation. The excellent photocatalytic activity of flower-like Ag/AgBr/BiOBr microspheres can be attributed to the large specific surface area, strong visible-light absorption, suitable energy band structure and surface plasmon resonance effect of Ag nanoparticles. The possible photocatalytic mechanism was proposed based on the active species test and band gap structure analysis. - Graphical abstract: The photocatalytic reaction mechanisms of the as-prepared Ag/AgBr/BiOBr. Display Omitted - Highlights: • Successful synthesis of flower-like Ag/AgBr/BiOBr microspheres. • The Ag/AgBr/BiOBr showed much higher photocatalytic activity towards p-nitrophenol as compared to BiOBr and Ag/AgBr. • The reasons for the excellent photocatalytic activity are the large specific surface area, strong visible-light absorption and surface plasmon resonance effect of Ag nanoparticles. • The O 2 · − , Br 0 and photogenerated h + play key roles in the photocatalytic degradation process

  13. Facile solvothermal synthesis of mesoporous manganese ferrite (MnFe2O4) microspheres as anode materials for lithium-ion batteries.

    Science.gov (United States)

    Zhang, Zailei; Wang, Yanhong; Tan, Qiangqiang; Zhong, Ziyi; Su, Fabing

    2013-05-15

    We report the synthesis and characterization of the mesoporous manganese ferrite (MnFe2O4) microspheres as anode materials for Li-ion batteries. MnFe2O4 microspheres were synthesized by a facile solvothermal method using Mn(CH3COO)2 and FeCl3 as metal precursors in the presence of CH3COOK, CH3COOC2H5, and HOCH2CH2OH. The samples were characterized by X-ray diffraction, transmission electron microscopy, scanning electron microscopy, nitrogen adsorption, thermal gravimetric, X-ray photoelectron spectroscopy, temperature programmed reduction, and temperature programmed oxidation. The synthesized mesoporous MnFe2O4 microspheres composed of nanoparticles (10-30 nm) were 100-500 nm in diameter and had surface areas between 60.2 and 86.8 m(2) g(-1), depending on the CH3COOK amounts added in the preparation. After calcined at 600°C, MnFe2O4 was decomposed to Mn2O3 and Fe2O3 mixture. The mesoporous MnFe2O4 microspheres calcined at 400°C showed a capacity of 712.2 mA h g(-1) at 0.2C and 552.2 mA h g(-1) at 0.8C after 50 cycles, and an average capacity fading rate of around 0.28%/cycle and 0.48%/cycle, much better than those of the samples without calcination and calcined at 600°C. The work would be helpful in the fabrication of binary metal oxide anode materials for Li-ion batteries. Copyright © 2013 Elsevier Inc. All rights reserved.

  14. Particle size-controllable microwave-assisted solvothermal synthesis of the high-voltage cathode material LiCoPO4 using water/ethylene glycol solvent blends

    Science.gov (United States)

    Ludwig, Jennifer; Haering, Dominik; Doeff, Marca M.; Nilges, Tom

    2017-03-01

    Particle size-tuned platelets of the high-voltage cathode material LiCoPO4 for Li-ion batteries have been synthesized by a simple one-step microwave-assisted solvothermal process using an array of water/ethylene glycol (EG) solvent mixtures. Particle size control was achieved by altering the concentration of the EG co-solvent in the mixture between 0 and 100 vol%, with amounts of 0-80 vol% EG producing single phase, olivine-type LiCoPO4. The particle sizes of the olivine materials were significantly reduced from about 1.2 μm × 1.2 μm × 500 nm (0 vol% EG) to 200 nm × 100 nm × 50 nm (80 vol% EG) with increasing EG content, while specific surface areas increased from 2 to 13 m2 g-1. The particle size reduction could mainly be attributed to the modified viscosities of the solvent blends. Owing to the soft template effect of EG, the crystals exhibited the smallest dimensions along the [010] direction of the Li diffusion pathways in the olivine crystal structure, resulting in enhanced lithium diffusion properties. The relationship between the synthesis, crystal properties and electrochemical performance was further elucidated, indicating that the electrochemical performances of the as-prepared materials mainly depend on the solvent composition and the respective particle size range. LiCoPO4 products obtained from reaction media with low and high EG contents exhibited good electrochemical performances (initial discharge capacities of 87-124 mAh g-1 at 0.1 C), whereas materials made from medium EG concentrations (40-60 vol% EG) showed the highest capacities and gravimetric energy densities (up to 137 mAh g-1 and 658 Wh kg-1 at 0.1 C), excellent rate capabilities, and cycle life.

  15. Conformational Sampling in Template-Free Protein Loop Structure Modeling: An Overview

    Directory of Open Access Journals (Sweden)

    Yaohang Li

    2013-02-01

    Full Text Available Accurately modeling protein loops is an important step to predict three-dimensional structures as well as to understand functions of many proteins. Because of their high flexibility, modeling the three-dimensional structures of loops is difficult and is usually treated as a “mini protein folding problem” under geometric constraints. In the past decade, there has been remarkable progress in template-free loop structure modeling due to advances of computational methods as well as stably increasing number of known structures available in PDB. This mini review provides an overview on the recent computational approaches for loop structure modeling. In particular, we focus on the approaches of sampling loop conformation space, which is a critical step to obtain high resolution models in template-free methods. We review the potential energy functions for loop modeling, loop buildup mechanisms to satisfy geometric constraints, and loop conformation sampling algorithms. The recent loop modeling results are also summarized.

  16. CONFORMATIONAL SAMPLING IN TEMPLATE-FREE PROTEIN LOOP STRUCTURE MODELING: AN OVERVIEW

    Directory of Open Access Journals (Sweden)

    Yaohang Li

    2013-02-01

    Full Text Available Accurately modeling protein loops is an important step to predict three-dimensional structures as well as to understand functions of many proteins. Because of their high flexibility, modeling the three-dimensional structures of loops is difficult and is usually treated as a “mini protein folding problem” under geometric constraints. In the past decade, there has been remarkable progress in template-free loop structure modeling due to advances of computational methods as well as stably increasing number of known structures available in PDB. This mini review provides an overview on the recent computational approaches for loop structure modeling. In particular, we focus on the approaches of sampling loop conformation space, which is a critical step to obtain high resolution models in template-free methods. We review the potential energy functions for loop modeling, loop buildup mechanisms to satisfy geometric constraints, and loop conformation sampling algorithms. The recent loop modeling results are also summarized.

  17. Conformational sampling in template-free protein loop structure modeling: an overview.

    Science.gov (United States)

    Li, Yaohang

    2013-01-01

    Accurately modeling protein loops is an important step to predict three-dimensional structures as well as to understand functions of many proteins. Because of their high flexibility, modeling the three-dimensional structures of loops is difficult and is usually treated as a "mini protein folding problem" under geometric constraints. In the past decade, there has been remarkable progress in template-free loop structure modeling due to advances of computational methods as well as stably increasing number of known structures available in PDB. This mini review provides an overview on the recent computational approaches for loop structure modeling. In particular, we focus on the approaches of sampling loop conformation space, which is a critical step to obtain high resolution models in template-free methods. We review the potential energy functions for loop modeling, loop buildup mechanisms to satisfy geometric constraints, and loop conformation sampling algorithms. The recent loop modeling results are also summarized.

  18. Solvothermal growth of single-crystal CdS nanowires

    Indian Academy of Sciences (India)

    Cadmium sulfide (CdS) nanowires (NWs) were prepared by the solvothermal method using ethylenedi- amine as a solvent. Two sets of ... discovery of new physical and chemical properties (Wang et al 2011). One-dimensional ... mal synthesis is widely used to prepare semiconductor NWs, particularly CdS. This synthesis ...

  19. Effects of hydrazine on the solvothermal synthesis of Cu2ZnSnSe4 and Cu2CdSnSe4 nanocrystals for particle-based deposition of films

    International Nuclear Information System (INIS)

    Chiang, Ming-Hung; Fu, Yaw-Shyan; Shih, Cheng-Hung; Kuo, Chun-Cheng; Guo, Tzung-Fang; Lin, Wen-Tai

    2013-01-01

    The effects of hydrazine on the synthesis of Cu 2 ZnSnSe 4 (CZTSe) and Cu 2 CdSnSe 4 (CCTSe) nanocrystals in an autoclave as a function of temperature and time were explored. On heating at 190 °C for 24-72 h, pure CZTSe and CCTSe nanocrystals could readily grow in the hydrazine-added solution, while in the hydrazine-free solution the intermediate phases such as ZnSe, Cu 2 Se, and Cu 2 SnSe 3 , and Cu 2 SnSe 3 and CdSe associated with the CZTSe and CCTSe nanocrystals grew, respectively. This result reveals that hydrazine can speed up the synthesis of pure CZTSe and CCTSe nanocrystals via a solvothermal process. The mechanisms for the hydrazine-enhanced growth of CZTSe and CCTSe nanocrystals were discussed. The pure CZTSe and CCTSe nanocrystals were subsequently fabricated to the smooth films by spin coating without further annealing in selenium atmosphere. This processing may be beneficial to the fabrication of the absorber layer for solar cells and thermoelectric devices. - Highlights: • Hydrazine enhances the growth of pure Cu 2 ZnSnSe 4 and Cu 2 CdSnSe 4 nanocrystals. • The nanocrystals can be fabricated to films by spin coating without annealing. • This solvothermal processing is promising for the fabrication of thin film devices

  20. Effects of hydrazine on the solvothermal synthesis of Cu{sub 2}ZnSnSe{sub 4} and Cu{sub 2}CdSnSe{sub 4} nanocrystals for particle-based deposition of films

    Energy Technology Data Exchange (ETDEWEB)

    Chiang, Ming-Hung [Department of Materials Science and Engineering, National Cheng Kung University, Tainan, Taiwan 701 (China); Fu, Yaw-Shyan, E-mail: ysfu@mail.nutn.edu.tw [Department of Greenergy, National University of Tainan, Tainan, Taiwan 700 (China); Shih, Cheng-Hung; Kuo, Chun-Cheng [Department of Materials Science and Engineering, National Cheng Kung University, Tainan, Taiwan 701 (China); Guo, Tzung-Fang [Department of Photonics, Advanced Optoelectronic Technology Center, National Cheng Kung University, Tainan, Taiwan 701 (China); Lin, Wen-Tai, E-mail: wtlin@mail.ncku.edu.tw [Department of Materials Science and Engineering, National Cheng Kung University, Tainan, Taiwan 701 (China)

    2013-10-01

    The effects of hydrazine on the synthesis of Cu{sub 2}ZnSnSe{sub 4} (CZTSe) and Cu{sub 2}CdSnSe{sub 4} (CCTSe) nanocrystals in an autoclave as a function of temperature and time were explored. On heating at 190 °C for 24-72 h, pure CZTSe and CCTSe nanocrystals could readily grow in the hydrazine-added solution, while in the hydrazine-free solution the intermediate phases such as ZnSe, Cu{sub 2}Se, and Cu{sub 2}SnSe{sub 3}, and Cu{sub 2}SnSe{sub 3} and CdSe associated with the CZTSe and CCTSe nanocrystals grew, respectively. This result reveals that hydrazine can speed up the synthesis of pure CZTSe and CCTSe nanocrystals via a solvothermal process. The mechanisms for the hydrazine-enhanced growth of CZTSe and CCTSe nanocrystals were discussed. The pure CZTSe and CCTSe nanocrystals were subsequently fabricated to the smooth films by spin coating without further annealing in selenium atmosphere. This processing may be beneficial to the fabrication of the absorber layer for solar cells and thermoelectric devices. - Highlights: • Hydrazine enhances the growth of pure Cu{sub 2}ZnSnSe{sub 4} and Cu{sub 2}CdSnSe{sub 4} nanocrystals. • The nanocrystals can be fabricated to films by spin coating without annealing. • This solvothermal processing is promising for the fabrication of thin film devices.

  1. Durability of template-free Fe-N-C foams for electrochemical oxygen reduction in alkaline solution

    Science.gov (United States)

    Mufundirwa, Albert; Harrington, George F.; Smid, Břetislav; Cunning, Benjamin V.; Sasaki, Kazunari; Lyth, Stephen M.

    2018-01-01

    Due to the high cost and limited availability of platinum, the development of non-platinum-group metals (non-PGM) catalysts is of paramount importance. A promising alternative to Pt are Fe-N-C-based materials. Here we present the synthesis, characterization and electrochemistry of a template-free nitrogen-doped carbon foam, impregnated with iron. This low-cost and gram-scale method results in materials with micron-scale pore size and large surface area (1600 m2g-1). When applied as an oxygen reduction reaction (ORR) electrocatalyst in alkaline solution, the Fe-N-C foams display extremely high initial activity, slightly out-performing commercially available non-PGM catalysts (NCP-2000, Pajarito Powder). The load-cycle durability in alkaline solution is investigated, and the performance steadily degrades over 60,000 potential cycles, whilst the commercial catalyst is remarkably stable. The post-operation catalyst microstructure is elucidated by transmission electron microscopy (TEM), to provide insight into the degradation processes. The resulting images suggest that potential cycling leads to leaching of atomically dispersed Fe-N2/4 sites in all the catalysts, whereas encapsulated iron nanoparticles are protected.

  2. Key insights on the structural characterization of textured Er{sub 2}O{sub 3}-ZrO{sub 2} nano-oxides prepared by a surfactant-free solvothermal route

    Energy Technology Data Exchange (ETDEWEB)

    Julian-Lopez, Beatriz, E-mail: julian@qio.uji.es [Departamento de Quimica Inorganica y Organica, Universitat Jaume I, Avda. Vicente Sos Baynat s/n, 12071 Castellon (Spain); Luz, Veronica de la; Gonell, Francisco; Cordoncillo, Eloisa [Departamento de Quimica Inorganica y Organica, Universitat Jaume I, Avda. Vicente Sos Baynat s/n, 12071 Castellon (Spain); Lopez-Haro, Miguel; Calvino, Jose J. [Departamento de Ciencia de los Materiales e Ingenieria Metalurgica y Quimica Inorganica, Facultad de Ciencias, Universidad de Cadiz, Campus Rio San Pedro, Puerto Real, 11510 Cadiz (Spain); Escribano, Purificacion [Departamento de Quimica Inorganica y Organica, Universitat Jaume I, Avda. Vicente Sos Baynat s/n, 12071 Castellon (Spain)

    2012-04-05

    Highlights: Black-Right-Pointing-Pointer Structural resolution of fluorite vs. pyrochlore in small nanocrystals. Black-Right-Pointing-Pointer Simple template-free solvothermal synthesis of Er{sub 2}O{sub 3}-ZrO{sub 2} nanooxides. Black-Right-Pointing-Pointer Good control over size, morphology and surface properties (280 m{sup 2} g{sup -1}). - Abstract: Zirconia-mixed oxides can exhibit cubic fluorite and pyrochlore structure. Their discrimination is not easy in nanooxides with a crystal size close to that of a few unit cells. In this work, high resolution transmission electron microscopy (HRTEM) has been employed to provide key insights on the structural characterization of a nanometric and porous mixed Er{sub 2}O{sub 3}-ZrO{sub 2} oxide. The material was prepared by a simple template-free solvothermal route that provided nanocrystalline powders at low temperature (170 Degree-Sign C) with spherical morphology, and high surface area ({approx}280 m{sup 2} g{sup -1}). The porosity was mainly originated from the assembling of organic complexing agents used in the synthesis to limit the crystal growth and to control hydrolysis and condensation reaction rates. The samples were characterized by thermal analysis, X-ray diffraction, scanning electron microscopy and N{sub 2} adsorption measurements. A detailed study by HRTEM was conducted on microtomed samples. It was observed that the material was made of nanocrystals packed into spherical agglomerates. HRTEM simulations indicated that it is not possible to identify the pyrochlore phase in nanoparticles with diameter below 2 nm. In our samples, the analysis of the HRTEM lattice images by means of fast Fourier transform (FFT) techniques revealed well defined spots that can be assigned to different planes of a cubic fluorite-type phase, even in the raw material. Raman spectroscopy was also a powerful technique to elucidate the crystalline phase of the materials with the smallest nanoparticles. HREM and Raman results evidenced

  3. Synthesis of solvothermal derived TiO2 nanocrystals supported on ground nano egg shell waste and its utilization for the photocatalytic dye degradation

    Science.gov (United States)

    Singh, Rohini; Kumari, Pooja; Chavan, Prakash Dhondiram; Datta, Sudipta; Dutta, Suman

    2017-11-01

    TiO2 nanoparticles with excellent crystallinity were synthesized via solvothermal method and supported on the ground nano-sized egg shell waste at different loading concentrations. The photocatalytic degradation of the mixture of Methylene blue (MB) and Rhodamine 6G (Rh 6G) in aqueous solution utilizing prepared TiO2 nano composite under visible light irradiation was analysed. Different characterizations including UV-Visible (UV-Vis) spectroscopy, Field emission scanning electron microscopic (FE-SEM), energy dispersive studies (EDS), Transmission electron microscopy (TEM) were performed to investigate the physicochemical properties of the prepared catalyst. In addition, FE-SEM and EDS analysis of the prepared egg shell support were carried out to confirm the morphology, particle size distribution, and composition. The solvothermal derived TiO2 nanocrystals supported on ground nano-sized egg shell waste exhibited enhanced photocatalytic activity as compared to the as-prepared TiO2 nanoparticles. The synergistic effect of TiO2 nanoparticles and nano egg shell support is attributed to the effective dispersion of TiO2 that offers high specific surface area.

  4. Solvothermal synthesis of MnFe{sub 2}O{sub 4} nanoparticles: The role of polymer coating on morphology and magnetic properties

    Energy Technology Data Exchange (ETDEWEB)

    Aslibeiki, B., E-mail: b.aslibeiki@tabrizu.ac.ir [Department of Physics, University of Tabriz, Tabriz 51666-16471 (Iran, Islamic Republic of); Kameli, P. [Department of Physics, Isfahan University of Technology, Isfahan 84156-83111 (Iran, Islamic Republic of); Ehsani, M.H. [Department of Physics, Semnan University, Semnan 35195-363 (Iran, Islamic Republic of); Salamati, H. [Department of Physics, Isfahan University of Technology, Isfahan 84156-83111 (Iran, Islamic Republic of); Muscas, G.; Agostinelli, E.; Foglietti, V. [Istituto di Struttura della Materia, CNR, Area Roma1, via Salaria km 29.300, 00015 Monterotondo Scalo, (RM) Italy (Italy); Casciardi, S. [Department of Occupational and Environmental Medicine, Epidemiology and Hygiene, National Institution for Insurance Against Accidents at Work (INAIL Research), Monte Porzio Catone, 00040 Rome (Italy); Peddis, D. [Istituto di Struttura della Materia, CNR, Area Roma1, via Salaria km 29.300, 00015 Monterotondo Scalo, (RM) Italy (Italy)

    2016-02-01

    Manganese spinel ferrite nanoparticles were synthesized by a solvothermal route based on high temperature decomposition of metal nitrates in the presence of different contents of Triethylene glycol. This simple and low cost method can be applied to prepare large quantities of nanoparticles (tens of grams). Powder X-ray diffraction (PXRD) and Transmission Electron Microscopy (TEM) confirmed that nanoparticles with a good crystalline quality were obtained. A good agreement between the average particle size calculated by PXRD and TEM was observed. Fourier-transform infrared spectra showed that polymer molecules have the tendency to form bonds with the surface of ferrite nanoparticles reducing the surface spin disorder, and then enhancing the saturation magnetization (M{sub S}). Therefore, much higher M{sub S} value (up to ∼91 emu/g at 5 K) was observed compared with that of bare nanoparticles without surfactant. The blocking temperature showed a remarkable shift to lower values with increasing the polymer starting amount. In addition, by increasing the polymer initial content, a more homogeneous size distribution was obtained and the initial strongly interacting superspin glass behavior changed to a weakly interacting superparamagnetic state. - Highlights: • Ferrite nanoparticles were synthesized by a simple solvothermal method. • Large scale and high quality of nanoparticles can be obtained with this method. • Strongly interacting superspin glass state changed to superparamagnetism behaviore. • Polymer coating improved the magnetization of nanoparticles.

  5. Solvothermal synthesis of V{sub 4}O{sub 9} flake-like morphology and its photocatalytic application in the degradation of methylene blue

    Energy Technology Data Exchange (ETDEWEB)

    Chine, M.K. [Laboratoire de Chimie de la Matière Condensée, IPEITunis, 2 rue Jawaher Lel Nehru 1008, B.P. 229 Montfleury, Tunis (Tunisia); Sediri, F., E-mail: faouzi.sediri@ipeit.rnu.tn [Laboratoire de Chimie de la Matière Condensée, IPEITunis, 2 rue Jawaher Lel Nehru 1008, B.P. 229 Montfleury, Tunis (Tunisia); Faculté des Sciences de Tunis, Université, Tunis-Elmanar, 2092 Elmanar, Tunis (Tunisia); Gharbi, N. [Laboratoire de Chimie de la Matière Condensée, IPEITunis, 2 rue Jawaher Lel Nehru 1008, B.P. 229 Montfleury, Tunis (Tunisia)

    2012-11-15

    Highlights: ► Flake-like nanocrystalline V{sub 4}O{sub 9} was synthesized by a solvothermal route. ► Photocatalytic activity has been evaluated by the degradation of methylene blue under visible light irradiation. ► V{sub 4}O{sub 9} nanoflakes exhibited much higher photocatalytic activity two times higher than the bulk V{sub 2}O{sub 5}. -- Abstract: Flake-like nanocrystalline V{sub 4}O{sub 9} has been successfully synthesized by solvothermal process using V{sub 2}O{sub 5} as vanadium source and phenolphthalein as a reducing agent and a structure-directing template. Techniques X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy and ultraviolet–visible (UV–vis) spectroscopy have been used to characterize the structure, the morphology and the composition of the material. The photocatalytic activity of the material has been evaluated by the degradation of methylene blue under visible light irradiation. As a result, after the lapse of 150 min, around 93.54% bleaching was observed, with V{sub 4}O{sub 9} nanoflakes yielding more photodegradation compared to that of bulk V{sub 2}O{sub 5}. This presents a degradation percentage of about 44.67%.

  6. The synthesis of porous Co{sub 3}O{sub 4} micro cuboid structures by solvothermal approach and investigation of its gas sensing properties and catalytic activity

    Energy Technology Data Exchange (ETDEWEB)

    Jamil, Saba, E-mail: saba_hrb@yahoo.com [Key Laboratory of Superlight Material and Surface Technology, Ministry of Education, Harbin Engineering University, 150001 (China); Jing, Xiaoyan [Key Laboratory of Superlight Material and Surface Technology, Ministry of Education, Harbin Engineering University, 150001 (China); Institute of Advanced Marine Materials, Harbin Engineering University, 150001 (China); Wang, Jun, E-mail: zhqw1888@sohu.com [Key Laboratory of Superlight Material and Surface Technology, Ministry of Education, Harbin Engineering University, 150001 (China); Li, Songnan; Liu, Jingyuan [Key Laboratory of Superlight Material and Surface Technology, Ministry of Education, Harbin Engineering University, 150001 (China); Zhang, Milin [Key Laboratory of Superlight Material and Surface Technology, Ministry of Education, Harbin Engineering University, 150001 (China); Institute of Advanced Marine Materials, Harbin Engineering University, 150001 (China)

    2013-11-15

    Graphical abstract: - Highlights: • Micro cuboid Co{sub 3}O{sub 4} particle prepared by solvothermal method. • Study of morphology of synthesized cuboids before and after calcinations. • Investigation of formation mechanism of porous Co{sub 3}O{sub 4} from cuboid CoCO{sub 3}. • Investigation of gas sensing properties of porous Co{sub 3}O{sub 4}. • Study of catalytic activity of product. - Abstract: The cobalt carbonate cuboids are prepared by adopting a simple solvothermal approach by using diethylene glycol and water in specific ratio as solvent. The prepared cobalt carbonate is subjected to different instrumentation to investigate its morphology and other properties. It is clear from the scanning electron microscopy (SEM) and transmission electron microscopy (TEM) that the product is distinct cuboid in shape with a size of approximately 3 μm from each face of the cube. Each particle of cuboid cobalt carbonate seems to comprise of layer by layer assembly of unit cells that consequently leads to a cuboid geometry. The cuboid cobalt carbonate was calcined at 700 °C in a furnace under argon atmosphere that decompose cobalt carbonate into porous Co{sub 3}O{sub 4} with the loosely packed arrangement of nano architectures. The gas sensing properties and catalytic activity of porous cuboids Co{sub 3}O{sub 4} are also investigated.

  7. The synthesis of porous Co3O4 micro cuboid structures by solvothermal approach and investigation of its gas sensing properties and catalytic activity

    International Nuclear Information System (INIS)

    Jamil, Saba; Jing, Xiaoyan; Wang, Jun; Li, Songnan; Liu, Jingyuan; Zhang, Milin

    2013-01-01

    Graphical abstract: - Highlights: • Micro cuboid Co 3 O 4 particle prepared by solvothermal method. • Study of morphology of synthesized cuboids before and after calcinations. • Investigation of formation mechanism of porous Co 3 O 4 from cuboid CoCO 3 . • Investigation of gas sensing properties of porous Co 3 O 4 . • Study of catalytic activity of product. - Abstract: The cobalt carbonate cuboids are prepared by adopting a simple solvothermal approach by using diethylene glycol and water in specific ratio as solvent. The prepared cobalt carbonate is subjected to different instrumentation to investigate its morphology and other properties. It is clear from the scanning electron microscopy (SEM) and transmission electron microscopy (TEM) that the product is distinct cuboid in shape with a size of approximately 3 μm from each face of the cube. Each particle of cuboid cobalt carbonate seems to comprise of layer by layer assembly of unit cells that consequently leads to a cuboid geometry. The cuboid cobalt carbonate was calcined at 700 °C in a furnace under argon atmosphere that decompose cobalt carbonate into porous Co 3 O 4 with the loosely packed arrangement of nano architectures. The gas sensing properties and catalytic activity of porous cuboids Co 3 O 4 are also investigated

  8. Zigzag-shaped nickel nanowires via organometallic template-free route

    Energy Technology Data Exchange (ETDEWEB)

    Shviro, Meital; Paszternak, Andras [Bar Ilan Institute of Nanotechnology and Advanced Materials (BINA), Bar Ilan University, Department of Chemistry (Israel); Chelly, Avraham [Bar Ilan Institute of Nanotechnology and Advanced Materials (BINA), Bar Ilan University, Department of Engineering (Israel); Zitoun, David, E-mail: david.zitoun@biu.ac.il [Bar Ilan Institute of Nanotechnology and Advanced Materials (BINA), Bar Ilan University, Department of Chemistry (Israel)

    2013-08-15

    In this manuscript, the formation of nickel nanowires of 10-20 nm in diameter (average size: several tens to hundreds of {mu}m long and 1.0-1.5 {mu}m wide) at low temperature is found to be driven by dewetting of liquid organometallic precursors during spin-coating process and by self-assembly of Ni clusters. Elaboration of metallic thin films by low-temperature deposition technique makes the preparation process compatible with most of the substrates. The use of iron and cobalt precursor shows that the process could be extended to other metallic systems. In this work, AFM and SEM are used to follow the assembly of Ni clusters into straight or zigzag lines. The formation of zigzag structure is specific to the Ni precursor at appropriate preparation parameters. This template-free process allows a control of anisotropic structures with homogeneous sizes and angles on the standard Si/SiO{sub 2} surface.

  9. Self-assembled mesoporous Co and Ni-ferrite spherical clusters consisting of spinel nanocrystals prepared using a template-free approach.

    Science.gov (United States)

    Yu, Byong Yong; Kwak, Seung-Yeop

    2011-10-21

    Based on a self-assembly strategy, spherical mesoporous cobalt and nickel ferrite nanocrystal clusters with a large surface area and narrow size distribution were successfully synthesized for the first time via a template-free solvothermal process in ethylene glycol and subsequent heat treatment. In this work, the mesopores in the ferrite clusters were derived mainly from interior voids between aggregated primary nanoparticles (with crystallite size of less than 7 nm) and disordered particle packing domains. The concentration of sodium acetate is shown herein to play a crucial role in the formation of mesoporous ferrite spherical clusters. These ferrite clusters were characterized in detail using wide-angle X-ray diffraction, thermogravimetric-differential thermal analysis, (57)Fe Mössbauer spectroscopy, X-ray photoelectron spectroscopy, field-emission scanning electron microscopy, standard and high-resolution transmission electron microscopy, and other techniques. The results confirmed the formation of both pure-phase ferrite clusters with highly crystalline spinel structure, uniform size (about 160 nm) and spherical morphology, and worm-like mesopore structures. The BET specific surface areas and mean pore sizes of the mesoporous Co and Ni-ferrite clusters were as high as 160 m(2) g(-1) and 182 m(2) g(-1), and 7.91 nm and 6.87 nm, respectively. A model for the formation of the spherical clusters in our system is proposed on the basis of the results. The magnetic properties of both samples were investigated at 300 K, and it was found that these materials are superparamagnetic. This journal is © The Royal Society of Chemistry 2011

  10. Solvothermal synthesis and structure of coordination polymers of Nd(III) and Dy(III) with rigid isophthalic acid derivatives and flexible adipic acid

    Science.gov (United States)

    Kariem, Mukaddus; Kumar, Manesh; Yawer, Mohd; Sheikh, Haq Nawaz

    2017-12-01

    Two new coordination polymers (CPs) with the formula [Nd(hip)(adip) 0.5(H2O)2]n.nH2O (1) and [Dy(aip)(adip)0.5(H2O)2]n.nH2O (2) were synthesized by self-assembly of lanthanide salts with rigid [5-hydroxyisophthalic acid (H2hip)], [5-aminoisophthalic acid (H2aip)] and flexible [adipic acid (H2adip)] linkers under solvothermal conditions. The CPs 1 &2 crystallize in monoclinic C2/c space group. Both the CPs have 1D linear ladder shaped extension with the linkages having the backbone of hip2-, aip2- and adip2- ligands. The 1D linear ladder chains generate three dimensional (3D) supramolecular frameworks via significant π-π and hydrogen bonding interactions. The CP 2 (Dy) emit strong ligand sensitized characteristic f-f luminescence emission. The CP 2 also exhibit weak ferromagnetic interactions at low temperatures.

  11. Trisodium citrate-assisted synthesis of highly water-dispersible and superparamagnetic mesoporous Fe{sub 3}O{sub 4} hollow microspheres via solvothermal process

    Energy Technology Data Exchange (ETDEWEB)

    Jiang, Xi; Wang, Fumin; Cai, Wangfeng; Zhang, Xubin, E-mail: tjzxb@tju.edu.cn

    2015-07-05

    Highlights: • Mesoporous Fe{sub 3}O{sub 4} hollow microspheres were prepared by a facile trisodium citrate-assisted solvothermal method. • The product exhibits high water-dispersibility and superparamagnetism at room temperature. • Ostwald ripening process was responsible for the formation of hollow structures. • The Fe{sub 3}O{sub 4} hollow microspheres are ideal candidates for various biomedical applications. - Abstract: Highly water-dispersible and superparamagnetic mesoporous Fe{sub 3}O{sub 4} hollow microspheres were prepared by a facile trisodium citrate-assisted solvothermal method. The composition, morphology and structure of the product were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier-transform infrared (FT-IR) spectroscopy, thermogravimetric (TG) analysis, Brunauer–Emmett–Teller (BET) and vibrating sample magnetometer (VSM). The results showed that the obtained Fe{sub 3}O{sub 4} hollow microspheres were composed of nanoparticles about 21 nm in diameter and exhibited superparamagnetic properties with relatively high saturation magnetization at room temperature. Trisodium citrate played a crucial role as an electrostatic stabilizer in the formation of Fe{sub 3}O{sub 4} hollow microspheres and Ostwald ripening process was responsible for the formation of hollow structures. The Fe{sub 3}O{sub 4} hollow microspheres were mesoporous and highly water-dispersible, indicating that the Fe{sub 3}O{sub 4} hollow microspheres are ideal candidates for various biomedical applications.

  12. Large scale solvothermal synthesis and a strategy to obtain stable Langmuir–Blodgett film of CoFe2O4 nanoparticles

    International Nuclear Information System (INIS)

    Thampi, Arya; Babu, Keerthi; Verma, Seema

    2013-01-01

    Highlights: • Large scale, monodisperse CoFe 2 O 4 nanoparticles by solvothermal route. • LB technique to obtain stable film of CoFe 2 O 4 nanoparticles over a large area. • Hydrophobicity of substrate was enhanced utilizing LB films of cadmium arachidate. • P–A isotherm and AFM cross sectional height profile analysis confirms stability. • Large scale organization of nanoparticles for surface pressure higher than 15 mN/m. -- Abstract: Nearly monodisperse oleic acid coated cobalt ferrite nanoparticles were synthesized in large scale by a simple solvothermal method utilizing N-methyl 2-Pyrrolidone (NMP) as a high boiling solvent. The magnetic oxide was further investigated by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM) and vibrating sample magnetometer (VSM). Langmuir–Blodgett (LB) technique is discussed to obtain a 2D assembly of oleic acid coated CoFe 2 O 4 nanoparticles over a large area. We describe a method to obtain stable, condensed three layers of cadmium arachidate on a piranha treated glass substrate. The hydrophobic surface thus obtained was subsequently used for forming a stable monolayer of oleic acid stabilized cobalt ferrite nanoparticles at the air–water interface. The stability of the LB films at the air–water interface was studied by pressure–area isotherm curves and atomic force microscopy (AFM) cross sectional height profile analysis. 2D organization of the magnetic nanoparticles at different surface pressures was studied by TEM. Preparation of large area LB films of CoFe 2 O 4 nanoparticles is reported for a surface pressure more than 15 mN/m

  13. Solvothermal synthesis of Zn{sub 2}GeO{sub 4}:Mn{sup 2+} nanophosphor in water/diethylene glycol system

    Energy Technology Data Exchange (ETDEWEB)

    Takeshita, Satoru; Honda, Joji [Department of Applied Chemistry, Faculty of Science and Technology, Keio University, 3-14-1 Hiyoshi, Kohoku-ku, Yokohama 223-8522 (Japan); Isobe, Tetsuhiko, E-mail: isobe@applc.keio.ac.jp [Department of Applied Chemistry, Faculty of Science and Technology, Keio University, 3-14-1 Hiyoshi, Kohoku-ku, Yokohama 223-8522 (Japan); Sawayama, Tomohiro; Niikura, Seiji [SINLOIHI Company, Limited, 2-19-12 Dai, Kamakura 247-8550 (Japan)

    2012-05-15

    The influence of aging of the suspension containing the amorphous precusors on structural, compositional and photoluminescent properties is studied to understand the mechanism on the formation of Zn{sub 2}GeO{sub 4}:Mn{sup 2+} nanoparticles during the solvothermal reaction in the water/diethylene glycol mixed solvent. Aging at 200 Degree-Sign C for 20 min forms the crystalline Zn{sub 2}GeO{sub 4} nanorods and then they grow up to {approx} 50 nm in mean length after aging for 240 min. Their interplanar spacing of (410) increases with increasing the aging time. The photoluminescence intensity corresponding to the d-d transition of Mn{sup 2+} increases with increasing the aging time up to 120 min, and then decreases after aging for 240 min. The photoluminescence lifetime decreases with increasing the aging time, indicating the locally concentrated Mn{sup 2+} ions. These results reveal that Mn{sup 2+} ions gradually replace Zn{sup 2+} ions near surface through repeating dissolusion and precipitation processes during prolonged aging after the complete crystallization of Zn{sub 2}GeO{sub 4}. - Graphical abstract: TEM images of Zn{sub 2}GeO{sub 4}:Mn{sup 2+} nanoparticles aged at 200 Degree-Sign C for different aging times in the mixed solvent of water and diethylene glycol. Highlights: Black-Right-Pointing-Pointer Mechanism on formation of Zn{sub 2}GeO{sub 4}:Mn{sup 2+} nanophosphor under solvothermal condition. Black-Right-Pointing-Pointer Zn{sub 2}GeO{sub 4} nanorods crystallize via amorphous precursors. Black-Right-Pointing-Pointer Gradual substitution of Mn{sup 2+} during prolonged aging. Black-Right-Pointing-Pointer Such an inhomogeneous Mn{sup 2+} doping process results in concentration quenching.

  14. Erbium and nitrogen co-doped SrTiO3 with highly visible light photocatalytic activity and stability by solvothermal synthesis

    International Nuclear Information System (INIS)

    Xu, Jing; Wei, Yuelin; Huang, Yunfang; Wang, Jing; Zheng, Xuanqing; Sun, Zhixian; Wu, Ying; Tao, Xinling; Fan, Leqing; Wu, Jihuai

    2015-01-01

    Highlights: • Er/N co-doped SrTiO 3 was prepared by a solvothermal process at low temperature. • The co-doping induces the band gap narrowing and prominent absorbance in visible light region. • The samples show excellent catalytic activity and stability under visible light irradiation. - Abstract: Erbium–nitrogen co-doped SrTiO 3 photocatalysts have been synthesized by a facile solvothermal method. The resulting samples were analyzed by FE-SEM, XRD, BET-surface area and UV–vis. The UV–vis absorption spectra of these powders indicated that erbium–nitrogen co-doped SrTiO 3 possessed stronger absorption bands in the visible light region in comparison with that of pure SrTiO 3 . The occurrence of the erbium–nitrogen co-doped cubic SrTiO 3 induced the higher photocatalytic activities for the degradation of methyl orange (MO) under irradiation by ultraviolet light and visible light, respectively, being superior to that of pure SrTiO 3 and commercial TiO 2 (P-25) powders. In addition, the Er–N co-doped SrTiO 3 (initial molar ratios of Sr/Er/N = 1:0.015:0.1, designated as S5) sample showed the best photocatalytic activity with the degradation rate as high as 98% after 30 min under the visible light irradiation. After five cycles, the photocatalytic activity of the S5 catalyst showed no significant decrease, which indicated that the photocatalysts were stable under visible light irradiation

  15. Facile solvothermal synthesis of monodisperse Pt2.6Co1 nanoflowers with enhanced electrocatalytic activity towards oxygen reduction and hydrogen evolution reactions

    International Nuclear Information System (INIS)

    Jiang, Liu-Ying; Lin, Xiao-Xiao; Wang, Ai-Jun; Yuan, Junhua; Feng, Jiu-Ju; Li, Xin-Sheng

    2017-01-01

    Highlights: • Uniform Pt 2.6 Co 1 nanoflowers were prepared by a simple solvothermal method. • Glucose and CTAC were used as the green reductant and structure director, respectively. • The architectures had the enlarged ECSA. • The architectures exhibited excellent catalytic performances for HER in acid and alkaline media. • The architectures showed highly catalytic performances for ORR in acid media. - Abstract: Herein, uniform Pt 2.6 Co 1 nanoflowers (NFs) were synthesized in oleylamine by a one-pot solvothermal method, using cetyltrimethylammonium chloride (CTAC) and glucose as the capping agent and green reducing agent. The samples were mainly characterized by transmission electron microscopy (TEM), high angle annular dark-field scanning TEM (HAADF-STEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). The architectures had larger electrochemically active surface area (ECSA) of 23.84 m 2 g −1 Pt than Pt 1.2 Co 1 nanocrystals (NCs, 14.96 m 2 g −1 Pt ), Pt 3.7 Co 1 NCs (16.96 m 2 g −1 Pt ) and commercial Pt black (20.35 m 2 g −1 Pt ). And the as-obtained Pt 2.6 Co 1 catalyst displayed superior catalytic performance and better durability for hydrogen evolution reaction (HER) as compared to Pt 1.2 Co 1 NCs, Pt 3.7 Co 1 NCs, commercial 50% Pt/C and Pt black catalysts in acid and alkaline media. Meanwhile, the electrocatalytic performance of Pt 2.6 Co 1 NFs for oxygen reduction reaction (ORR) is better in acid media as compared with that in alkaline media. It indicates the great potential applications of the as-prepared catalyst in fuel cells.

  16. Solvothermal synthesis of MnFe{sub 2}O{sub 4}-graphene composite—Investigation of its adsorption and antimicrobial properties

    Energy Technology Data Exchange (ETDEWEB)

    Chella, Santhosh [Centre for Nanotechnology Research, VIT University, Vellore 632014 (India); Kollu, Pratap, E-mail: pk419@cam.ac.uk [Thin Film Magnetism Group, Cavendish Laboratory, Department of Physics, University of Cambridge, Cambridge CB3 0HE (United Kingdom); Komarala, Eswara Vara P R; Doshi, Sejal [Department of Metallurgical Engineering and Materials Science, Indian Institute of Technology Bombay, Mumbai (India); Saranya, Murugan; Felix, Sathiyanathan; Ramachandran, Rajendran [Centre for Nanotechnology Research, VIT University, Vellore 632014 (India); Saravanan, Padmanapan [Defence Metallurgical Research Laboratory, Hyderabad 5000058 (India); Koneru, Vijaya Lakshmi [Development Alternatives, Qutub Institutional Area, New Delhi 110016 (India); Venugopal, Velmurugan [Centre for Nanotechnology Research, VIT University, Vellore 632014 (India); Jeong, Soon Kwan [Climate Change Technology Research Division, Korea Institute of Energy Research, Yuseong-gu, Daejeon 305-343 (Korea, Republic of); Nirmala Grace, Andrews, E-mail: anirmalagrace@vit.ac.in [Centre for Nanotechnology Research, VIT University, Vellore 632014 (India)

    2015-02-01

    Graphical abstract: - Highlights: • Graphene manganese ferrite composite was synthesized by a solvothermal process. • Adsorption of Pb and Cd metal ions were tested with MnFe{sub 2}O{sub 4}-G material. • The MnFe{sub 2}O{sub 4}-G material showed good adsorption capacity for metal ions. • MnFe{sub 2}O{sub 4}-G showed the higher antibacterial activity of 82%, than graphene. - Abstract: Graphene manganese ferrite (MnFe{sub 2}O{sub 4}-G) composite was prepared by a solvothermal process. The as-prepared graphene manganese ferrite composite was tested for the adsorption of lead (Pb(II)) and cadmium (Cd(II)) ions by analytical methods under diverse experimental parameters. With respect to contact time measurements, the adsorption of Pb and Cd ions increased and reached equilibrium within 120 and 180 min at 37 °C with a maximum adsorption at pH 5 and 7 respectively. The Langmuir model correlates to the experimental data showing an adsorption capacity of 100 for Pb(II) and 76.90 mg g{sup −1} for Cd(II) ions. Thermodynamic studies revealed that the adsorption of Pb and Cd ions onto MnFe{sub 2}O{sub 4}-G was spontaneous, exothermic and feasible in the range of 27–47 °C. Cytotoxicity behavior of graphene against bacterial cell membrane is well known. To better understand its antimicrobial mechanism, the antibacterial activity of graphene and MnFe{sub 2}O{sub 4}-G nanocomposite was compared. Under similar concentration and incubation conditions, nanocomposite MnFe{sub 2}O{sub 4}-G dispersion showed the highest antibacterial activity of 82%, as compared to graphene showing 37% cell loss. Results showed that the prepared composite possess good adsorption efficiency and thus could be considered as an excellent material for removal of toxic heavy metal ions as explained by adsorption isotherm. Hence MnFe{sub 2}O{sub 4}-G can be used as an adsorbent as well as an antimicrobial agent.

  17. The structure and properties of PEDOT synthesized by template-free solution method.

    Science.gov (United States)

    Zhao, Qin; Jamal, Ruxangul; Zhang, Li; Wang, Minchao; Abdiryim, Tursun

    2014-01-01

    In this study, a simple one-step template-free solution method was developed for the preparation of poly(3,4-ethylenedioxythiophene) (PEDOTs) with different morphologies by adjusting various ratios of oxidant (FeCl3·6H2O) to monomer (3,4-ethylenedioxythiophene (EDOT)). The results from structural analysis showed that the structure of PEDOT was strongly affected by the oxidant/monomer ratio, and the polymerization degree, conjugation length, doping level, and crystallinity of PEDOT decreased with increasing of the oxidant/monomer ratio. The morphological analysis showed that PEDOT prepared from an oxidant/monomer ratio of 3:1 displayed a special coral-like morphology, and the branches of 'coral' would adjoin or grow together with increasing content of oxidant in the reaction medium; consequently, the morphology of PEDOT changed from coral to sheets (at an oxidant/monomer ratio of 9:1). The electrochemical analysis proved that the PEDOT prepared from an oxidant/monomer ratio of 3:1 had the lowest resistance and the highest specific capacitances (174 F/g) at a current density of 1 A/g with a capacity retention rate of 74% over 1,500 cycles, which indicated that the PEDOT with a coral-like morphology could be applied as a promising electrode material for supercapacitors.

  18. Ultrasonically assisted solvothermal synthesis of novel Ni/Al layered double hydroxide for capturing of Cd(II) from contaminated water

    Science.gov (United States)

    Rahmanian, Omid; Maleki, Mohammad Hassan; Dinari, Mohammad

    2017-11-01

    A novel adsorbent of nickel aluminum layered double hydroxide (Ni/Al-LDH) was prepared through the precipitation of metal nitrates by ultrasonically assisted solvothermal method. The surface morphology, chemical structure and thermal properties of this compound were examined by X-ray diffraction (XRD), Fourier Transform Infrared (FT-IR), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and thermogravimetric analysis (TGA) techniques. The XRD, TEM and FE-SEM results established that the synthesized LDH have a well-ordered layer structure with good crystalline nature. Then it was applied to remove excessive Cd(II) ions from water and the effects of contact time, pH and adsorbent dose were examined at initial Cd(II) concentration of 10 mg/L. Results show that the time required to reach equilibrium was fast (40 min) and working pH solution was neutral (pH 7). Langmuir and Freundlich model of adsorption isotherms were explored; the results show that the Freundlich model was better fitted than that Langmuir model. This results predicting a multilayer adsorption of Cd(II) on LDH. The equilibrium kinetic adsorption data were fixed to the pseudo-second order kinetic equation.

  19. Synthesis of gadolinium carbonate-conjugated-poly(ethylene)glycol (Gd{sub 2}(CO{sub 3}){sub 3}@PEG) particles via a modified solvothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Nasution, Erika L. Y.; Ahab, Atika [Physics of Electronic Materials Research Division Departement of Physics, Institut Teknologi Bandung, Bandung 40132 Indonesia (Indonesia); Nuryadin, Bebeh W. [Departement of Physics, Faculty of Science and Technology UIN Sunan Gunung Djati Bandung, Bandung 40614 (Indonesia); Haryanto, Freddy; Arif, Idam [Nuclear Physics and Biophysics Research Division, Departement of Physics, Institut Teknologi Bandung, Bandung 40132 Indonesia (Indonesia); Iskandar, Ferry, E-mail: ferry@fi.itb.ac.id [Physics of Electronic Materials Research Division Departement of Physics, Institut Teknologi Bandung, Bandung 40132 Indonesia (Indonesia); Research Center for Nanoscience and Nanotechnology Institut Teknologi Bandung, Bandung 40132 Indonesia (Indonesia)

    2016-02-08

    PEGylated gadolinium carbonate ((Gd{sub 2}(CO{sub 3}){sub 3})@PEG) powder was successfully synthesized by a modified solvothermal method. The synthesized products were characterized by means of X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM), and Energy Dispersive X-ray Spectroscopy (EDS). A systematic change in the chemical surface composition, crystallinity and size properties of the Gd{sub 2}(CO{sub 3}){sub 3}@PEG particles was observed by increasing the reaction time at 5 hours, 7 hours, and 8 hours. The corresponding XRD patterns showed that the Gd{sub 2}(CO{sub 3}){sub 3} particles had hexagonal symmetry (JCPDS No. 37-0559) with a crystallite size of 3.5, 2.9, and 4.6 nm. FTIR spectra showed that the Gd{sub 2}(CO{sub 3}){sub 3})@PEG particles were formed with the PEG as carbonyl and hydroxyl group attached to the surface. SEM analysis showed that the Gd{sub 2}(CO{sub 3}){sub 3})@PEG particles had a flake-like morphology of homogeneous sized particles and agglomerates. EDS analysis confirmed the presence of constituent Gd{sub 2}(CO{sub 3}){sub 3} elements.

  20. One-pot synthesis of uniform hollow cuprous oxide spheres fabricated by single-crystalline particles via a simple solvothermal route

    International Nuclear Information System (INIS)

    Li Shikuo; Li Chuanhao; Huang Fangzhi; Wang Yang; Shen Yuhua; Xie Anjian; Wu Qiong

    2011-01-01

    Uniform Cu 2 O hollow spheres fabricated by single-crystalline particles (smaller than 20 nm) are facile synthesized in ethylene glycol (EG) solution by a simple solvothermal route without using pre-fabricated templates and reductive agents. EG in this protocol is not only used as a solvent, complexing agent, and reducing agent, but also served as a structure-directing agent for the formation of hollow structure. By control of reaction conditions, such as reaction time, temperature, and the anions, the morphology and structure of the hollow spheres can be tuned. A coordination adsorption and oriented attachment and Ostwald ripening mechanism is proposed for explaining the formation process of hollow Cu 2 O spheres in EG solution; and importantly, the hollow Cu 2 O spheres exhibit an excellent property for the electro-catalytic oxidization of ascorbic acid in acetic acid buffer solution. Moreover, the hollow spherical Cu 2 O particles could be potentially applied in catalysis, sensor, and as model for fundamental research.

  1. Modified solvothermal synthesis of cobalt ferrite (CoFe2O4) magnetic nanoparticles photocatalysts for degradation of methylene blue with H2O2/visible light

    Science.gov (United States)

    Kalam, Abul; Al-Sehemi, Abdullah G.; Assiri, Mohammed; Du, Gaohui; Ahmad, Tokeer; Ahmad, Irfan; Pannipara, M.

    2018-03-01

    Different grads of magnetic nano-scaled cobalt ferrites (CoFe2O4) photocatalysts were synthesized by modified Solvothermal (MST) process with and without polysaccharide. The indigenously synthesized photocatalysts were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), thermo gravimetric analysis (TGA), Fourier transform infrared (FT-IR), UV-visible (UV-vis) spectroscopy and N2 adsorption-desorption isotherm method. The Fourier transform infrared spectroscopy study showed the Fe-O stretching vibration 590-619 cm-1, confirming the formation of metal oxide. The crystallite size of the synthesized photocatalysts was found in the range between 20.0 and 30.0 nm. The surface area of obtained magnetic nanoparticles is found to be reasonably high in the range of 63.0-76.0 m2/g. The results shown that only MST-2 is the most active catalyst for photo-Fenton like scheme for fast photodegradation action of methylene blue dye, this is possible due to optical band gap estimated of 2.65 eV. Captivatingly the percentage of degradation efficiency increases up to 80% after 140 min by using MST-2 photocatalyst. Photocatalytic degradation of methylene blue (MB) dye under visible light irradiation with cobalt ferrite magnetic nanoparticles followed first order kinetic constant and rate constant of MST-2 is almost 2.0 times greater than MST-1 photocatalyst.

  2. Solvothermal Synthesis of Hierarchical TiO2Microstructures with High Crystallinity and Superior Light Scattering for High-Performance Dye-Sensitized Solar Cells.

    Science.gov (United States)

    Li, Zhao-Qian; Mo, Li-E; Chen, Wang-Chao; Shi, Xiao-Qiang; Wang, Ning; Hu, Lin-Hua; Hayat, Tasawar; Alsaedi, Ahmed; Dai, Song-Yuan

    2017-09-20

    In this article, hierarchical TiO 2 microstructures (HM-TiO 2 ) were synthesized by a simple solvothermal method adopting tetra-n-butyl titanate as the titanium source in a mixed solvent composed of N,N-dimethylformamide and acetic acid. Due to the high crystallinity and superior light-scattering ability, the resultant HM-TiO 2 are advantageous as photoanodes for dye-sensitized solar cells. When assembled to the entire photovoltaic device with C101 dye as a sensitizer, the pure HM-TiO 2 -based solar cells showed an ultrahigh photovoltage up to 0.853 V. Finally, by employing the as-obtained HM-TiO 2 as the scattering layer and optimizing the architecture of dye-sensitized solar cells, both higher photovoltage and incident photon-to-electron conversion efficiency value were harvested with respect to TiO 2 nanoparticles-based dye-sensitized solar cells, resulting in a high power conversion efficiency of 9.79%. This work provides a promising strategy to develop photoanode materials with outstanding photoelectric conversion performance.

  3. Solvothermal Synthesis of a Hollow Micro-Sphere LiFePO₄/C Composite with a Porous Interior Structure as a Cathode Material for Lithium Ion Batteries.

    Science.gov (United States)

    Liu, Yang; Zhang, Jieyu; Li, Ying; Hu, Yemin; Li, Wenxian; Zhu, Mingyuan; Hu, Pengfei; Chou, Shulei; Wang, Guoxiu

    2017-11-03

    To overcome the low lithium ion diffusion and slow electron transfer, a hollow micro sphere LiFePO₄/C cathode material with a porous interior structure was synthesized via a solvothermal method by using ethylene glycol (EG) as the solvent medium and cetyltrimethylammonium bromide (CTAB) as the surfactant. In this strategy, the EG solvent inhibits the growth of the crystals and the CTAB surfactant boots the self-assembly of the primary nanoparticles to form hollow spheres. The resultant carbon-coat LiFePO₄/C hollow micro-spheres have a ~300 nm thick shell/wall consisting of aggregated nanoparticles and a porous interior. When used as materials for lithium-ion batteries, the hollow micro spherical LiFePO₄/C composite exhibits superior discharge capacity (163 mAh g -1 at 0.1 C), good high-rate discharge capacity (118 mAh g -1 at 10 C), and fine cycling stability (99.2% after 200 cycles at 0.1 C). The good electrochemical performances are attributed to a high rate of ionic/electronic conduction and the high structural stability arising from the nanosized primary particles and the micro-sized hollow spherical structure.

  4. Facile synthesis of zinc oxide nanoparticles decorated graphene oxide composite via simple solvothermal route and their photocatalytic activity on methylene blue degradation.

    Science.gov (United States)

    Atchudan, Raji; Edison, Thomas Nesakumar Jebakumar Immanuel; Perumal, Suguna; Karthikeyan, Dhanapalan; Lee, Yong Rok

    2016-09-01

    Zinc oxide nanoparticles decorated graphene oxide (ZnO@GO) composite was synthesized by simple solvothermal method where zinc oxide (ZnO) nanoparticles and graphene oxide (GO) were synthesized via simple thermal oxidation and Hummers method, respectively. The obtained materials were thoroughly characterized by various physico-chemical techniques such as X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, field emission scanning electron microscopy (FESEM), high resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), and Raman spectroscopy. Raman spectrum shows the intensity of D to G value was close to one which confirms the obtained GO and ZnO@GO composite possesses moderate graphitization. TEM images shows the ZnO nanoparticles mean size of 15±5nm were dispersed over the wrinkled graphene layers. The photocatalytic performance of ZnO@GO composite on degradation of methylene blue (MB) is investigated and the results show that the GO plays an important role in the enhancement of photocatalytic performance. The synthesized ZnO@GO composite achieves a maximum degradation efficiency of 98.5% in a neutral solution under UV-light irradiation for 15min as compared with pure ZnO (degradation efficiency is 49% after 60min of irradiation) due to the increased light absorption, the reduced charge recombination with the introduction of GO. Moreover, the resulting ZnO@GO composite possesses excellent degradation efficiency as compared to ZnO nanoparticles alone on MB. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. From Extraction of Local Structures of Protein Energy Landscapes to Improved Decoy Selection in Template-Free Protein Structure Prediction

    Directory of Open Access Journals (Sweden)

    Nasrin Akhter

    2018-01-01

    Full Text Available Due to the essential role that the three-dimensional conformation of a protein plays in regulating interactions with molecular partners, wet and dry laboratories seek biologically-active conformations of a protein to decode its function. Computational approaches are gaining prominence due to the labor and cost demands of wet laboratory investigations. Template-free methods can now compute thousands of conformations known as decoys, but selecting native conformations from the generated decoys remains challenging. Repeatedly, research has shown that the protein energy functions whose minima are sought in the generation of decoys are unreliable indicators of nativeness. The prevalent approach ignores energy altogether and clusters decoys by conformational similarity. Complementary recent efforts design protein-specific scoring functions or train machine learning models on labeled decoys. In this paper, we show that an informative consideration of energy can be carried out under the energy landscape view. Specifically, we leverage local structures known as basins in the energy landscape probed by a template-free method. We propose and compare various strategies of basin-based decoy selection that we demonstrate are superior to clustering-based strategies. The presented results point to further directions of research for improving decoy selection, including the ability to properly consider the multiplicity of native conformations of proteins.

  6. From Extraction of Local Structures of Protein Energy Landscapes to Improved Decoy Selection in Template-Free Protein Structure Prediction.

    Science.gov (United States)

    Akhter, Nasrin; Shehu, Amarda

    2018-01-19

    Due to the essential role that the three-dimensional conformation of a protein plays in regulating interactions with molecular partners, wet and dry laboratories seek biologically-active conformations of a protein to decode its function. Computational approaches are gaining prominence due to the labor and cost demands of wet laboratory investigations. Template-free methods can now compute thousands of conformations known as decoys, but selecting native conformations from the generated decoys remains challenging. Repeatedly, research has shown that the protein energy functions whose minima are sought in the generation of decoys are unreliable indicators of nativeness. The prevalent approach ignores energy altogether and clusters decoys by conformational similarity. Complementary recent efforts design protein-specific scoring functions or train machine learning models on labeled decoys. In this paper, we show that an informative consideration of energy can be carried out under the energy landscape view. Specifically, we leverage local structures known as basins in the energy landscape probed by a template-free method. We propose and compare various strategies of basin-based decoy selection that we demonstrate are superior to clustering-based strategies. The presented results point to further directions of research for improving decoy selection, including the ability to properly consider the multiplicity of native conformations of proteins.

  7. Stem-Loop RNA Hairpins in Giant Viruses: Invading rRNA-Like Repeats and a Template Free RNA

    Directory of Open Access Journals (Sweden)

    Hervé Seligmann

    2018-02-01

    Full Text Available We examine the hypothesis that de novo template-free RNAs still form spontaneously, as they did at the origins of life, invade modern genomes, contribute new genetic material. Previously, analyses of RNA secondary structures suggested that some RNAs resembling ancestral (tRNAs formed recently de novo, other parasitic sequences cluster with rRNAs. Here positive control analyses of additional RNA secondary structures confirm ancestral and de novo statuses of RNA grouped according to secondary structure. Viroids with branched stems resemble de novo RNAs, rod-shaped viroids resemble rRNA secondary structures, independently of GC contents. 5′ UTR leading regions of West Nile and Dengue flavivirid viruses resemble de novo and rRNA structures, respectively. An RNA homologous with Megavirus, Dengue and West Nile genomes, copperhead snake microsatellites and levant cotton repeats, not templated by Mimivirus' genome, persists throughout Mimivirus' infection. Its secondary structure clusters with candidate de novo RNAs. The saltatory phyletic distribution and secondary structure of Mimivirus' peculiar RNA suggest occasional template-free polymerization of this sequence, rather than noncanonical transcriptions (swinger polymerization, posttranscriptional editing.

  8. Oxidation of aniline in dopant-free template-free dilute reaction media

    Czech Academy of Sciences Publication Activity Database

    Rakić, A.; Bajuk-Bogdanovic, D.; Mojovic, M.; Ciric-Marjanovic, G.; Milojević-Rakić, M.; Mentus, S.; Marjanovic, B.; Trchová, Miroslava; Stejskal, Jaroslav

    2011-01-01

    Roč. 127, č. 3 (2011), s. 501-510 ISSN 0254-0584 R&D Projects: GA ČR GA203/08/0686 Institutional research plan: CEZ:AV0Z40500505 Keywords : polyaniline * nanostructures * chemical synthesis Subject RIV: CD - Macromolecular Chemistry Impact factor: 2.234, year: 2011

  9. High Efficiency Gene Correction in Hematopoietic Cells by Donor-Template-Free CRISPR/Cas9 Genome Editing

    Directory of Open Access Journals (Sweden)

    Duran Sürün

    2018-03-01

    Full Text Available The CRISPR/Cas9 prokaryotic adaptive immune system and its swift repurposing for genome editing enables modification of any prespecified genomic sequence with unprecedented accuracy and efficiency, including targeted gene repair. We used the CRISPR/Cas9 system for targeted repair of patient-specific point mutations in the Cytochrome b-245 heavy chain gene (CYBB, whose inactivation causes chronic granulomatous disease (XCGD—a life-threatening immunodeficiency disorder characterized by the inability of neutrophils and macrophages to produce microbicidal reactive oxygen species (ROS. We show that frameshift mutations can be effectively repaired in hematopoietic cells by non-integrating lentiviral vectors carrying RNA-guided Cas9 endonucleases (RGNs. Because about 25% of most inherited blood disorders are caused by frameshift mutations, our results suggest that up to a quarter of all patients suffering from monogenic blood disorders could benefit from gene therapy employing personalized, donor template-free RGNs.

  10. Template-Free Supracolloidal Self-Assembly of Atomically Precise Gold Nanoclusters: From 2D Colloidal Crystals to Spherical Capsids.

    Science.gov (United States)

    Nonappa; Lahtinen, Tanja; Haataja, Johannes S; Tero, Tiia-Riikka; Häkkinen, Hannu; Ikkala, Olli

    2016-12-23

    We report supracolloidal self-assembly of atomically precise and strictly monodisperse gold nanoclusters involving p-mercaptobenzoic acid ligands (Au 102 -pMBA 44 ) under aqueous conditions into hexagonally packed monolayer-thick two-dimensional facetted colloidal crystals (thickness 2.7 nm) and their bending to closed shells leading to spherical capsids (d ca. 200 nm), as controlled by solvent conditions. The 2D colloidal assembly is driven in template-free manner by the spontaneous patchiness of the pMBA ligands around the Au 102 -pMBA 44 nanoclusters preferably towards equatorial plane, thus promoting inter-nanocluster hydrogen bonds and high packing to planar sheets. More generally, the findings encourage to explore atomically precise nanoclusters towards highly controlled colloidal self-assemblies. © 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Solvothermal synthesis of high molecular weight dithienogermole ...

    Indian Academy of Sciences (India)

    cation of the resulting organic products by the Soxhlet extraction gave the target polymers with high molecular weight and low polydispersity index (PDI). The higher molecular weight of pDTG-PH may be ascribed to high solubility of the polymers than those of pDTG-BTA. The long branched alkyl chain in acceptor part may.

  12. Solvothermal synthesis of high molecular weight dithienogermole ...

    Indian Academy of Sciences (India)

    The onset oxidation potentials of the films were very similar to those reported for pDTS-PH23 and. pDTG-BTA.21,24. 3.4 Thermal stability of polymers. Thermal stability of the polymers was investigated by thermogravimetric analysis (TGA) in nitrogen and 5% weight loss temperatures (T 5 d ) were noted as listed in table 1.

  13. Supported Zeolite Beta Layers via an Organic Template-Free Preparation Route

    Directory of Open Access Journals (Sweden)

    Stephanie Reuss

    2018-01-01

    Full Text Available Layers of high silica zeolites, synthesized with an organic structure directing agent (OSDA and grown onto porous support structures, frequently suffer from the thermal stress during the removal of OSDA via the calcination process. The different thermal expansion coefficients of the zeolite and the support material, especially when stainless steel is used as a support, causes enormous tension resulting in defect formation in the zeolite layer. However, the calcination is an easy procedure to decompose the OSDA in the pore system of the zeolite. Recently, methods to synthesize zeolite beta without the use of an organic structure directing agent have been described. In the present study, a seed-directed synthesis is used to prepare OSDA-free zeolite beta layers on stainless steel supports via an in situ preparation route. For the application as membrane, a porous stainless steel support has been chosen. The beta/stainless steel composites are characterized by X-ray diffraction (XRD and scanning electron microscopy (SEM. To prove its possible application as a membrane, the beta/stainless steel composites were also tested by single gas permeances of H2, He, CO2, N2, and CH4.

  14. Supported Zeolite Beta Layers via an Organic Template-Free Preparation Route.

    Science.gov (United States)

    Reuss, Stephanie; Sanwald, Dirk; Schülein, Marion; Schwieger, Wilhelm; Al-Thabaiti, Shaeel A; Mokhtar, Mohamed; Basahel, Sulaiman N

    2018-01-21

    Layers of high silica zeolites, synthesized with an organic structure directing agent (OSDA) and grown onto porous support structures, frequently suffer from the thermal stress during the removal of OSDA via the calcination process. The different thermal expansion coefficients of the zeolite and the support material, especially when stainless steel is used as a support, causes enormous tension resulting in defect formation in the zeolite layer. However, the calcination is an easy procedure to decompose the OSDA in the pore system of the zeolite. Recently, methods to synthesize zeolite beta without the use of an organic structure directing agent have been described. In the present study, a seed-directed synthesis is used to prepare OSDA-free zeolite beta layers on stainless steel supports via an in situ preparation route. For the application as membrane, a porous stainless steel support has been chosen. The beta/stainless steel composites are characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). To prove its possible application as a membrane, the beta/stainless steel composites were also tested by single gas permeances of H₂, He, CO₂, N₂, and CH₄.

  15. Phase controlled solvothermal synthesis of Cu{sub 2}ZnSnS{sub 4}, Cu{sub 2}ZnSn(S,Se){sub 4} and Cu{sub 2}ZnSnSe{sub 4} Nanocrystals: The effect of Se and S sources on phase purity

    Energy Technology Data Exchange (ETDEWEB)

    Pal, Mou [Instituto de Energías Renovables, Universidad Nacional Autónoma de México, 62580 Temixco, Morelos (Mexico); Instituto de Física, BUAP, Av. San Claudio y Blvd. 18 Sur Col. San Manuel, Ciudad Universitaria, C.P. 72570, Puebla (Mexico); Mathews, N.R. [Instituto de Energías Renovables, Universidad Nacional Autónoma de México, 62580 Temixco, Morelos (Mexico); Paraguay-Delgado, F. [Departamento de Materiales Nanoestructurados, Centro de Investigación en Materiales Avanzados (CIMAV), Chihuahua (Mexico); Mathew, X., E-mail: xm@ier.unam.mx [Instituto de Energías Renovables, Universidad Nacional Autónoma de México, 62580 Temixco, Morelos (Mexico)

    2015-09-15

    In this study, we have reported the synthesis of Cu{sub 2}ZnSnSe{sub 4} (CZTSe), Cu{sub 2}ZnSnS{sub 4} (CZTS) and Cu{sub 2}ZnSn(S,Se){sub 4} (CZTSSe) nanocrystals with tunable band gap and composition obtained by solvothermal method. The crystalline structure, composition, morphology and optical properties of the nanoparticles were characterized by X-ray diffraction (XRD), Raman scattering, energy dispersive X-ray spectroscopy, transmission electron microscopy and diffuse reflectance (DR) spectroscopy. While the XRD patterns of CZTS and CZTSe nanoparticles prepared with elemental S/Se powder revealed the presence of phase pure nanoparticles, the CZTSSe nanoparticles obtained using a mixture of S and Se, were found to contain many secondary phases under the same synthesis protocol. Formation of impurity phases in CZTSSe sample, can be avoided by using a mixture of 1-dodecanethiol (DT; CH{sub 3}(CH{sub 2}){sub 11}SH)/oleylamine (OLA) instead of S powder and following the same experimental procedure. The incorporation of S in CZTSe nanocrystals prepared in presence of DDT/OLA mixture was confirmed through structural and optical characterizations. The optical properties of the quaternary chalcogenide nanocrystals were found to vary with the chemical composition of the material. - Highlights: • Solvothermal synthesis of CZTS, CZTSSe and CZTSe nanocrystals and discussion on possible formation mechanism. • Use of dodecanethiol/oleylamine mixture to synthesize phase-pure CZTSSe nanocrystals. • Formation of impurity phases can be controlled with proper S and Se sources.

  16. Template-free formation of vertically oriented TiO2 nanorods with uniform distribution for organics-sensing application

    International Nuclear Information System (INIS)

    Mu Qinghui; Li Yaogang; Zhang Qinghong; Wang Hongzhi

    2011-01-01

    Graphical abstract: - Abstract: High-density arrays of vertically oriented TiO 2 nanorods with uniform distribution on Ti foil have been formed through template-free oxidation of Ti in hydrogen peroxide solutions. Subsequent thermal treatment was applied for growing mixed crystal structures to pursue higher performance. Morphology characterization using field emission scanning electron microscopy (FESEM) shows a nanorod diameter in the range of 20-50 nm with a length of 1.5 μm. X-ray diffraction (XRD) measurement demonstrates the crystallization of the TiO 2 nanorods prior to thermal treatment and the formation of anatase and rutile mixed phase after thermal treatment. The mixed crystal TiO 2 nanorods show a much higher performance than pure anatase in photoelectrochemical experiments. Steady-state photocurrent resulted from photocatalytic oxidation of organic compounds by TiO 2 nanorods is employed as response signal in determination of the organics to yield a linear range of 0-1.1 mM for glucose. For other organics, an excellent linear relationship between the net steady-state photocurrent and the concentration of electrons transferred in exhaustive oxidation for these organics is obtained, which empowers the mixed crystal TiO 2 nanorods to serve as versatile material in organics-sensing application.

  17. A template-free sol-gel technique for controlled growth of ZnO nanorod arrays

    International Nuclear Information System (INIS)

    Huang, N.; Zhu, M.W.; Gao, L.J.; Gong, J.; Sun, C.; Jiang, X.

    2011-01-01

    The growth of ZnO nanorod arrays via a template-free sol-gel process was investigated. The nanorod is single-crystalline wurtzite structure with [0 0 0 1] growth direction determined by the transmission electron microscope. The aligned ZnO arrays were obtained directly on the glass substrates by adjusting the temperatures and the withdrawal speeds, without seed-layer or template assistant. A thicker oriented ZnO nanorod arrays was obtained at proper experimental conditions by adding dip-coating layers. Room temperature photoluminescence spectrum exhibits an intensive UV emission with a weak broad green emission as well as a blue double-peak emission located at 451 and 468 nm, respectively. Further investigation results show that the difference in the alignment of nanorods ascribes to the different orientations of the nanoparticles-packed film formed prior to nanorods on the substrate. Well ordered ZnO nanorods are formed from this film with good c-axis orientation. Our study is expected to pave a way for direct growth of oriented nanorods by low-cost solution approaches.

  18. Facile surfactant- and template-free synthesis and electrochemical properties of SnO{sub 2}/graphene composites

    Energy Technology Data Exchange (ETDEWEB)

    Li, Jing, E-mail: xy13787103391@126.com [School of Materials Science and Engineering, Southwest University of Science and Technology, Mianyang 621010 (China); State Key Laboratory Cultivation Base for Nonmetal Composites and Functional Materials, Southwest University of Science and Technology, Mianyang 621010 (China); Zhang, Xia, E-mail: zyx02090229@163.com [School of Materials Science and Engineering, Southwest University of Science and Technology, Mianyang 621010 (China); State Key Laboratory Cultivation Base for Nonmetal Composites and Functional Materials, Southwest University of Science and Technology, Mianyang 621010 (China); Guo, Jianqiang; Peng, Rufang [School of Materials Science and Engineering, Southwest University of Science and Technology, Mianyang 621010 (China); State Key Laboratory Cultivation Base for Nonmetal Composites and Functional Materials, Southwest University of Science and Technology, Mianyang 621010 (China); Xie, Ruishi [Analytical and Testing Center, Southwest University of Science and Technology, Mianyang 621010 (China); Huang, Yeju; Qi, Yongcheng [School of Materials Science and Engineering, Southwest University of Science and Technology, Mianyang 621010 (China); State Key Laboratory Cultivation Base for Nonmetal Composites and Functional Materials, Southwest University of Science and Technology, Mianyang 621010 (China)

    2016-07-25

    In this work, we demonstrate a facile and green hydrothermal process without using any surfactant or template to synthesize SnO{sub 2} nanoflowers (NFs)/graphene nanosheets (GNSs) composites as a high-performance electrode material for electric double layer capacitors (EDLCs). The crystal structure and morphology of the products were characterized by X-ray diffraction, scanning electron microscopy, and transition electron microscopy. The electrochemical properties were investigated by galvanostatic charge/discharge cycling and cycling voltammetry in a voltage range of −0.2–0.8 V. The results exhibit that the addition of GNSs did not change the tetragonal crystal structure of SnO{sub 2}, and the GNSs were successfully coated on the flower-like surface of SnO{sub 2}. The grain morphology of SnO{sub 2}@GNSs composites has a flower-like appearance suggesting excellent electrochemical properties which were confirmed by electrochemical techniques. Compared with the GNSs, the SnO{sub 2}@GNSs composites exhibit a high specific discharge capacitance of 126 F g{sup −1} at 0.2 A g{sup −1} and remains 98.2% after 2000 charge–discharge cycles. The combination of GNSs and SnO{sub 2} could significantly improve the electrical conductivity, enhance the interactions between GNSs and SnO{sub 2} NFs and provide more reaction sites, thereby resulting in improved electrochemical properties for the SnO{sub 2}@GNSs composites in contrast with the pristine GNSs sample. The high specific capacity and long stability make the SnO{sub 2}@GNSs nanocomposite as a electrode material for high-performance supercapacitors. - Highlights: • SnO{sub 2} nanoflowers (NFs)/Graphene nanosheets(GNSs) composites were prepared by a simple and rapid hydrothermal process. • The results show that the GNSs were homogeneously and tightly attached on the surface of SnO{sub 2} NFs. • The SnO{sub 2} NFs/GNSs composites electrode exhibited the enhanced capacitive performances than those of pure GNSs.

  19. Template-free synthesis of vertically aligned CdS nanorods and its application in hybrid solar cells

    Energy Technology Data Exchange (ETDEWEB)

    Jiang, Xiaoxia; Chen, Fei; Qiu, Weiming; Shi, Minmin; Wang, Mang [Key Laboratory of Macromolecule Synthesis and Functionalization of Ministry of Education, State Key Lab of Silicon Materials, and Department of Polymer Science and Engineering, Zhejiang University, Hangzhou 310027 (China); Xu, Hao; Yang, Ligong [Zhejiang-California International Nanosystems Institute, Zhejiang University, Hangzhou 310027 (China); Chen, Hongzheng [Key Laboratory of Macromolecule Synthesis and Functionalization of Ministry of Education, State Key Lab of Silicon Materials, and Department of Polymer Science and Engineering, Zhejiang University, Hangzhou 310027 (China); Zhejiang-California International Nanosystems Institute, Zhejiang University, Hangzhou 310027 (China)

    2010-02-15

    We have fabricated and investigated hybrid solar cells based on one-step fabricated vertically aligned CdS nanorod arrays and poly(2-methoxy-5-(2'-ethylhexyloxy)-1,4-phenylenevinylene) (MEH-PPV). The vertically aligned CdS nanorods provide the minimal electron transport path to reduce the charge carrier recombination at the heterojunction interface. The photoactive layers were prepared by two deposition methods, dip- and spin-coating of MEH-PPV on CdS nanorods. Scanning electron microscope (SEM) showed that the extent of infiltration of the soft MEH-PPV phase into the rigid CdS nanorods arrays can be controlled by different deposition methods, which strongly influence the PV device performance. The influence of annealing treatment on the device performance is also studied; the power conversion efficiency is quadrupled for dip-coating and doubled for spin-coating after the annealing treatment. (author)

  20. Template free synthesis of silver-gold alloy nanoparticles and cellular uptake of gold nanoparticles in Chinese Hamster Ovary cell

    International Nuclear Information System (INIS)

    Pal, Angshuman; Shah, Sunil; Kulkarni, Vijay; Murthy, R.S.R.; Devi, Surekha

    2009-01-01

    Gold-silver alloy nanoparticles were synthesized by simultaneous reduction of varying mole fractions of HAuCl 4 and AgNO 3 by sodium citrate in aqueous solution without using stabilizing agents such as surfactant or polymer. Appearance of single absorption peak in visible spectrum indicated formation of homogeneous gold-silver alloy nanoparticles. Transmission electron micrographs also support formation of alloy nanoparticles rather than core-shell particles. The plasmon absorption bands for Au-Ag nanoparticles show linear bathochromic shift with increasing Au content. No significant change in surface plasmon band was observed on storage of samples at 25 ± 2 deg. C for 6 months, indicating stability of the particles. Particle size distribution, zeta-potential and conduction of these colloidal suspensions were measured by dynamic light scattering along with Zetasizer. Gold and Au-Ag alloy nanoparticles exhibited fluorescence at 600 nm and in between 600 and 486 nm respectively depending on alloy composition. Gold nanoparticles were used for cell line study using liposome as a carrier. This liposome entrapped gold nanoparticles showed enhanced uptake by Chinese Hamster Ovary (CHO) cells compared to gold nanoparticles

  1. Template-free synthesis of ordered ZnO@ZnS core-shell arrays for high performance supercapacitors.

    Science.gov (United States)

    Yan, Hailong; Li, Tong; Lu, Yang; Cheng, Jinbing; Peng, Tao; Xu, Jinyou; Yang, Linying; Hua, Xiangqiang; Liu, Yunxin; Luo, Yongsong

    2016-11-28

    In this article, ordered ZnO@ZnS core-shell structures have been produced on a stainless mesh by a two-step approach without using a template. ZnO nanorods fabricated by a chemical vapor method are transferred into a 50 ml autoclave for a second stage ion-exchange reaction followed by heating at 120 °C for 4-16 h. The ZnO core is prepared as the conducting channel and ZnS as the active material. Such unique architecture exhibits remarkable electrochemical performance with high capacitance and desirable cycle life. When evaluating as the electrode for supercapacitors, the ZnO@ZnS core-shell structure delivers a high specific capacitance of 603.8 F g -1 at a current density of 2 A g -1 , with 9.4% capacitance loss after cycling 3000 times. The fabrication strategy presented here is simple and cost-effective, which can open new avenues for large-scale applications of the novel materials in energy storage.

  2. Template-free synthesis of porous graphitic carbon nitride/carbon composite spheres for electrocatalytic oxygen reduction reaction.

    Science.gov (United States)

    Fu, Xiaorui; Hu, Xiaofei; Yan, Zhenhua; Lei, Kaixiang; Li, Fujun; Cheng, Fangyi; Chen, Jun

    2016-01-28

    Porous graphitic carbon nitride/carbon composite spheres were synthesized using melamine and cyanuric acid, and glucose as the carbon nitride and carbon precursor, respectively. The 3D hierarchical composites efficiently catalyzed the oxygen reduction reaction with an onset potential of 0.90 V and a kinetic current density of 23.92 mA cm(-2). These merit their promising applications in fuel cells and metal-air batteries.

  3. GREEN APPROACH TO BULK AND TEMPLATE-FREE SYNTHESIS OF THERMALLY STABLE REDUCED POLYANILINE NANOFIBERS FOR CAPACITOR APPLICATIONS

    Science.gov (United States)

    An extremely simple green approach is described that generates bulk quantities of nanofibers of the electronic polymer polyaniline in fully reduced state (leucoemeraldine form) in one step without using any reducing agent, surfactants, and/or large amounts of insoluble templates....

  4. Template-free synthesis of porous ZnO/Ag microspheres as recyclable and ultra-sensitive SERS substrates

    Science.gov (United States)

    Liu, Yanjun; Xu, Chunxiang; Lu, Junfeng; Zhu, Zhu; Zhu, Qiuxiang; Manohari, A. Gowri; Shi, Zengliang

    2018-01-01

    The porous structured zinc oxide (ZnO) microspheres decorated with silver nanoparticles (Ag NPs) have been fabricated as surface-enhanced Raman scattering (SERS) substrate for ultra-sensitive, highly reproducible and stable biological/chemical sensing of various organic molecules. The ZnO microspheres were hydrothermally synthesized without any template, and the Ag NPs decorated on microspheres via photochemical reaction in situ, which provided stable Ag/ZnO contact to achieve a sensitive SERS response. It demonstrates a higher enhancement factor (EF) of 2.44 × 1011 and a lower detection limit of 10-11 M-10-12 M. This porous SERS substrate could also be self-cleaned through a photocatalytic process and then further recycled for the detection of same or different molecules, such as phenol red (PhR), dopamine (DA) and glucose (GLU) with ultra-low concentration and it possessed a sensitive response. The excellent performances are attributed to morphology of porous microspheres, hybrid structure of semiconductor/metal and corresponding localized field enhancement of surface plasmons. Therefore, it is expected to design the recyclable ultra-sensitive SERS sensors for the detection of biological molecules and organic pollutant monitoring.

  5. Solvothermal preparation of micro/nanostructured TiO{sub 2} with enhanced lithium storage capability

    Energy Technology Data Exchange (ETDEWEB)

    Li, Jie [School of Physics and Mechanical & Electronical Engineering, Hubei University of Education, Wuhan, 430205 (China); Wang, Chao [Department of Architecture and Material Engineering, Hubei University of Education, Wuhan, 430205 (China); Zheng, Ping; Zhang, Lei; Chen, Gongxuan [College of Chemistry and Life Science, Hubei University of Education, Wuhan, 430205 (China); Tang, Chengchun [School of Materials Science and Engineering, Hebei University of Technology, Tianjin 300130 (China); Wu, Tian, E-mail: twu@whu.edu.cn [School of Physics and Mechanical & Electronical Engineering, Hubei University of Education, Wuhan, 430205 (China); College of Chemistry and Life Science, Hubei University of Education, Wuhan, 430205 (China); Department of Architecture and Material Engineering, Hubei University of Education, Wuhan, 430205 (China)

    2017-04-01

    Facile and controllable preparation of TiO{sub 2} is of prime importance to elaborately tailor and then fully exploit its intriguing functionalities in energy storage, catalysis and environmental remediation. Herein, a solvothermal method combined with post annealing is conducted, in which the hydrolysis of tetrabutyl titanate is controlled by the in-situ generated water during solvothermal treatment. By controlling synthetic conditions (i.e. reactant ratio, solvothermal temperature and reaction time), we manage to tailor the morphologies of TiO{sub 2}. Specially, three typical structures (nanoparticle, nanoneedle and nanorod) are studied to reveal the growth mechanism and the effects of the synthesis conditions. Nanoneedle-structured TiO{sub 2} shows higher specific capacity and enhanced cycle stability as anode material for lithium ion batteries. - Highlights: • Controllable preparation of nano-TiO{sub 2} is achieved by a solvothermal method. • TiO{sub 2} morphology is tailored by tuning reactant ratio, temperature and duration. • Needle structured TiO{sub 2} shows enhanced lithium storage capability.

  6. Solvothermal synthesis, crystal structure, and second-order nonlinear optical properties of a new noncentrosymmetric gallium-organic framework material, [N(C3H7)4]3Ga3[C6H3(CO2)3]4

    Science.gov (United States)

    Lee, Dong Woo; Jo, Vinna; Ok, Kang Min

    2012-10-01

    A novel noncentrosymmetric (NCS) gallium-organic framework material, [N(C3H7)4]3Ga3[C6H3(CO2)3]4 (CAUMOF-11) has been synthesized by a solvothermal reaction using Ga(NO3)3·xH2O, 1,3,5-C6H3(CO2H)3, N(C3H7)4Cl, HNO3, and HCON(CH3)2 at 180 °C. The structure of the reported material has been determined by single-crystal X-ray diffraction. CAUMOF-11 has an anionic three-dimensional framework with aligned four-coordinate GaO4 tetrahedra and 1,3,5-benzenetricarboxylate groups. Tetrapropylammonim cations reside within the channel and maintain the charge balance. Detailed structural analyses with full characterization including infrared spectroscopy, thermogravimetric analysis, elemental analysis, ion-exchange reactions, topotactic decomposition, and gas adsorption experiments are reported. Powder second-harmonic generating (SHG) measurements on CAUMOF-11, using 1064 nm radiation, exhibit SHG efficiency of 15 times that of α-SiO2 and the material is phase-matchable (type-1).

  7. Regulation of deprotonation of 3,3-di(1H-tetrazol-5-yl)pentanedioic acid: Solvothermal synthesis of La(III) and heterometallic La(III)/Cu(II) compounds for ablation of A549 cells

    Science.gov (United States)

    Guo, Meng Yue; Zhang, Xin; Zhao, Liang; Li, Yue Kang; Chen, Dian Yu; Yang, Gao Wen; Li, Qiao Yun

    2018-03-01

    3,3-di(1H-tetrazol-5-yl)pentanedioic acid (H4dtzpda) can display tunable valence when reacted with different metal ions because it has four acidic hydrogen atoms of both tetrazole rings and carboxylate groups. Solvothermal reactions of H4dtzpda with La(NO3)2·6H2O or La(NO3)3·6H2O/Cu(NO3)2·6H2O afforded a one dimensional [La(Hdtzpda)(H2O)4]·4H2O (1) and a three dimensional [La2Cu(dtzpda)2(H2O)10]·4H2O (2), respectively, where only three acidic hydrogen atoms of H4dtzpda are deprotonated in compound 1 while all the four acidic ones are deprotonated in compound 2. In compound 1, Hdtzpda3- is a penta-dentate ligand to bridge La(III) centers via only oxygen atoms of the carboxylate group while in compound 2, dtzpda4- is a hepta-dentate one via not only the oxygen atoms of the carboxylate group but also the nitrogen atoms of the tetrazole rings. PEG-5000 (poly(ethyleneglycol-5000)) coated compound 1 or 2 nanoparticles (NPs) have good dispersity in water. Cytotoxicity study on A549 cells (human caucasian lung carcinoma) shows that compound 2 (half-maximal inhibitory concentration, IC50~18 μg/mL) is superior to compound 1 (IC50~38 μg/mL). Furthermore, both NPs of the two compounds are able to inhibit the migration of A549 cells, indicating their potential to inhibit the transfer of tumors in vivo.

  8. Unprecedented propane–SCR-NOx activity over template-free synthesized Al-rich Co-BEA* zeolite

    Czech Academy of Sciences Publication Activity Database

    Sazama, Petr; Mokrzycki, Lukasz; Wichterlová, Blanka; Vondrová, Alena; Pilař, Radim; Dědeček, Jiří; Sklenák, Štěpán; Tabor, Edyta

    2015-01-01

    Roč. 332, DEC 2015 (2015), s. 201-211 ISSN 0021-9517 R&D Projects: GA TA ČR(CZ) TH01021259; GA ČR GA15-13876S Institutional support: RVO:61388955 Keywords : beta zeolite * Al-rich BEA* * OSDA-free synthesis Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 7.354, year: 2015

  9. RNA 3D Structure Modeling by Combination of Template-Based Method ModeRNA, Template-Free Folding with SimRNA, and Refinement with QRNAS.

    Science.gov (United States)

    Piatkowski, Pawel; Kasprzak, Joanna M; Kumar, Deepak; Magnus, Marcin; Chojnowski, Grzegorz; Bujnicki, Janusz M

    2016-01-01

    RNA encompasses an essential part of all known forms of life. The functions of many RNA molecules are dependent on their ability to form complex three-dimensional (3D) structures. However, experimental determination of RNA 3D structures is laborious and challenging, and therefore, the majority of known RNAs remain structurally uncharacterized. To address this problem, computational structure prediction methods were developed that either utilize information derived from known structures of other RNA molecules (by way of template-based modeling) or attempt to simulate the physical process of RNA structure formation (by way of template-free modeling). All computational methods suffer from various limitations that make theoretical models less reliable than high-resolution experimentally determined structures. This chapter provides a protocol for computational modeling of RNA 3D structure that overcomes major limitations by combining two complementary approaches: template-based modeling that is capable of predicting global architectures based on similarity to other molecules but often fails to predict local unique features, and template-free modeling that can predict the local folding, but is limited to modeling the structure of relatively small molecules. Here, we combine the use of a template-based method ModeRNA with a template-free method SimRNA. ModeRNA requires a sequence alignment of the target RNA sequence to be modeled with a template of the known structure; it generates a model that predicts the structure of a conserved core and provides a starting point for modeling of variable regions. SimRNA can be used to fold small RNAs (models for larger RNAs that have a correctly modeled core. ModeRNA can be either downloaded, compiled and run locally or run through a web interface at http://genesilico.pl/modernaserver/ . SimRNA is currently available to download for local use as a precompiled software package at http://genesilico.pl/software/stand-alone/simrna and as a

  10. Visible light photocatalytic activities of template free porous graphitic carbon nitride-BiOBr composite catalysts towards the mineralization of reactive dyes

    Science.gov (United States)

    Kanagaraj, Thamaraiselvi; Thiripuranthagan, Sivakumar; Paskalis, Sahaya Murphin Kumar; Abe, Hideki

    2017-12-01

    Template free porous g-C3N4 (pGCN) and flower like bismuth oxybromide catalysts were synthesized by poly condensation and precipitation methods respectively. Various weight percentages of porous GCN-BiOBr composite catalysts (x% pGCN-BiOBr where x = 5, 10, 30, 50 & 70 wt% of pGCN) were synthesized by impregnation method. All the synthesized catalysts were characterized by X-Ray diffractometer, Fourier transform infrared spectrophotometer, BET surface area analyzer, UV Visible diffuse reflectance spectrophotometer, X-Ray photoelectron spectrophotometer, SEM with Energy dispersive X-ray analyzer (SEM/EDAX) and elemental mapping, Transmission electron microscope, Photoluminescence spectrophotometer and Electrochemical impedance. Photocatalytic degradation of all the synthesized catalysts were tested towards the harmful reactive dyes such as reactive blue 198 (RB 198), reactive black 5 (RB 5) and reactive yellow 145 (RY 145) in presence of visible irradiation. Among the catalysts 30% pGCN-BiOBr resulted in the highest photocatalytic activity towards the degradation of all the three dyes in presence of UV, visible and solar irradiations. Kinetics studies on the photocatalytic mineralization of dyes indicated that it followed pseudo first order. HPLC, TOC and COD studies confirm that the dyes are mineralized into CO2, water and mineral salts.

  11. Template-free fabrication of hierarchical macro/mesoporpous SnS2/TiO2 composite with enhanced photocatalytic degradation of Methyl Orange (MO)

    Science.gov (United States)

    Dai, Gaopeng; Qin, Haiquan; Zhou, Huan; Wang, Wanqiang; Luo, Tianxiong

    2018-02-01

    Ordered macro/mesoporous SnS2/TiO2 composite was successfully prepared via a template-free aqueous technique using tetrabutyl titanate as the titanium precursor and SnCl4•5H2O as the tin precursor. The photocatalytic activity of SnS2/TiO2 composite was tested by the degradation of Methyl Orange (MO) aqueous solution under irradiation of the simulated sunlight. It was found that SnS2/TiO2 composite displayed an enhanced photocatalytic activity with a 0.055 min-1 apparent rate constant (degradation efficiency of 90.9% within 50 min). The ordered macro/mesoporous structure and SnS2/TiO2 heterostructure were considered to play synergistic effects in its enhanced photocatalytic performance, because the ordered porous structure can improve mass transfer and light capture, and heterostructure between SnS2 and TiO2 can reduce the recombination rate of photogenerated electrons and holes.

  12. TiO2 synthesized by microwave assisted solvothermal method: Experimental and theoretical evaluation

    International Nuclear Information System (INIS)

    Moura, K.F.; Maul, J.; Albuquerque, A.R.; Casali, G.P.; Longo, E.; Keyson, D.; Souza, A.G.; Sambrano, J.R.; Santos, I.M.G.

    2014-01-01

    In this study, a microwave assisted solvothermal method was used to synthesize TiO 2 with anatase structure. The synthesis was done using Ti (IV) isopropoxide and ethanol without templates or alkalinizing agents. Changes in structural features were observed with increasing time of synthesis and evaluated using periodic quantum chemical calculations. The anatase phase was obtained after only 1 min of reaction besides a small amount of brookite phase. Experimental Raman spectra are in accordance with the theoretical one. Micrometric spheres constituted by nanometric particles were obtained for synthesis from 1 to 30 min, while spheres and sticks were observed after 60 min. - Graphical abstract: FE-SEM images of anatase obtained with different periods of synthesis associated with the order–disorder degree. Display Omitted - Highlights: • Anatase microspheres were obtained by the microwave assisted hydrothermal method. • Only ethanol and titanium isopropoxide were used as precursors during the synthesis. • Raman spectra and XRD patterns were compared with quantum chemical calculations. • Time of synthesis increased the short-range disorder in one direction and decreased in another

  13. Template-Free Synthesis of Sb2S3 Hollow Microspheres as Anode Materials for Lithium-Ion and Sodium-Ion Batteries

    Science.gov (United States)

    Xie, Jianjun; Liu, Li; Xia, Jing; Zhang, Yue; Li, Min; Ouyang, Yan; Nie, Su; Wang, Xianyou

    2018-03-01

    Hierarchical Sb2S3 hollow microspheres assembled by nanowires have been successfully synthesized by a simple and practical hydrothermal reaction. The possible formation process of this architecture was investigated by X-ray diffraction, focused-ion beam-scanning electron microscopy dual-beam system, and transmission electron microscopy. When used as the anode material for lithium-ion batteries, Sb2S3 hollow microspheres manifest excellent rate property and enhanced lithium-storage capability and can deliver a discharge capacity of 674 mAh g-1 at a current density of 200 mA g-1 after 50 cycles. Even at a high current density of 5000 mA g-1, a discharge capacity of 541 mAh g-1 is achieved. Sb2S3 hollow microspheres also display a prominent sodium-storage capacity and maintain a reversible discharge capacity of 384 mAh g-1 at a current density of 200 mA g-1 after 50 cycles. The remarkable lithium/sodium-storage property may be attributed to the synergetic effect of its nanometer size and three-dimensional hierarchical architecture, and the outstanding stability property is attributed to the sufficient interior void space, which can buffer the volume expansion. [Figure not available: see fulltext.

  14. Green Template-Free Synthesis of Hierarchical Shuttle-Shaped Mesoporous ZnFe2 O4 Microrods with Enhanced Lithium Storage for Advanced Li-Ion Batteries.

    Science.gov (United States)

    Hou, Linrui; Hua, Hui; Lian, Lin; Cao, Hui; Zhu, Siqi; Yuan, Changzhou

    2015-09-07

    Invited for the cover of this issue is Changzhou Yuan and co-workers at the Anhui University of Technology. The image depicts hierarchical shuttle-shaped mesoporous ZnFe2 O4 micro-rods, as a low-cost yet high-performance anode, for advanced next-generation Li-ion batteries. Read the full text of the article at 10.1002/chem.201501876. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Solvothermal synthesis and theoretical study of a polypyridium ...

    Indian Academy of Sciences (India)

    . 4 -(4-Pyridyl)-2,2 :6 ,2 -terpyridine (pytpy)1–5 is a de- rivative from pyridyl-donor ligands, such as pyrazine6 and 4,4 -bipyridine.7 The 2,2 :6 ,2 -terpyridine (terpy) substituent presents interesting electronic, photonic and magnetic properties ...

  16. Effect of temperature and time on solvothermal synthesis of ...

    Indian Academy of Sciences (India)

    lier literature (Buessem et al 1966; Bell et al 1984; Arlt et al. 1985; Arlt 1987; Kanata et al 1987; Dutta and Gregg 1992) reported that to stabilize tetragonal BaTiO3, it is important that crystal size should exceed 1 μm to accommodate the strains caused by the transformation from cubic to tetragonal structure. Few successful ...

  17. Effect of temperature and time on solvothermal synthesis of ...

    Indian Academy of Sciences (India)

    days) size XRD (nm) SEM (nm) c/a. EtOH-1. 185. 6. 66. 120. 1·008. EtOH-2. 185. 3. 64. 90 ... C after 6 days is around 120 nm, whereas its value is around 80–90 nm at .... lier literature (Buessem et al 1966; Bell et al 1984; Arlt et al. 1985; Arlt 1987 ...

  18. Solvothermal synthesis and theoretical study of a polypyridium ...

    Indian Academy of Sciences (India)

    and magnetic properties when coordinating to tran- sition metal.8,9 Substituted pyridines including 4 -(4- pyridyl)-2,2 :6 ,2 -terpyridine are prominent building blocks in both organic and inorganic supramolecular chemistry because of their π-stacking ability, direc- tional H-bonding and coordination properties.10 Pytpy.

  19. Solvothermally Synthesized Sb2Te3 Platelets Show Unexpected Optical Contrasts in Mid-Infrared Near-Field Scanning Microscopy.

    Science.gov (United States)

    Hauer, Benedikt; Saltzmann, Tobias; Simon, Ulrich; Taubner, Thomas

    2015-05-13

    We report nanoscale-resolved optical investigations on the local material properties of Sb2Te3 hexagonal platelets grown by solvothermal synthesis. Using mid-infrared near-field microscopy, we find a highly symmetric pattern, which is correlated to a growth spiral and which extends over the entire platelet. As the origin of the optical contrast, we identify domains with different densities of charge carriers. On Sb2Te3 samples grown by other means, we did not find a comparable domain structure.

  20. Morphological evolution of Bi2Se3 nanocrystalline materials synthesized by microwave assisted solvothermal method

    Science.gov (United States)

    Bera, Sumit; Behera, P.; Mishra, A. K.; Krishnan, M.; Patidar, M. M.; Singh, D.; Gangrade, M.; Venkatesh, R.; Deshpande, U. P.; Phase, D. M.; Ganesan, V.

    2018-04-01

    Structural, morphological and spectroscopic properties of Bi2Se3 nanoparticles synthesized by microwave assisted solvothermal method were investigated systematically. A controlled synthesis of different morphologies by a small variation in synthesis procedure is demonstrated. Powder X-ray diffraction (XRD) confirmed the formation of single phase. Crystallite and particle size reductions were studied with XRD and AFM (Atomic Force Microscopy). Different morphologies such as hexagonal nanoflakes with cross section of around˜6µm, nanoflower and octahedral agglomerated crystals of nearly ˜60 nm size have been observed in scanning electron microscope while varying the microwave assisted synthesis procedures. A significant blue shift observed in diffuse reflectance spectroscopy evidences the energy gap tuning as a result of morphological evolution. The difference in morphology observed in this three fast, facile and scalable synthesis is advantageous for tuning the thermoelectric figure of merit and for probing the surface states of these topological insulators. Low temperature resistivity remains similar for all three variants depicting a 2D character as evidenced by a -lnT term of localization.

  1. Self-templating synthesis of hollow spheres of zeolite ZSM-5 from spray-dried aluminosilicate precursor

    Czech Academy of Sciences Publication Activity Database

    Pashková, Veronika; Tokarová, V.; Brabec, Libor; Dědeček, Jiří

    2016-01-01

    Roč. 228, JUL 2016 (2016), s. 59-63 ISSN 1387-1811 R&D Projects: GA ČR GA15-13876S; GA MŠk LM2015073 Institutional support: RVO:61388955 Keywords : MFI * zeolite shells * template free synthesis Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 3.615, year: 2016

  2. Solvothermal synthesis, crystal structure, and second-order nonlinear optical properties of a new noncentrosymmetric gallium-organic framework material, [N(C{sub 3}H{sub 7}){sub 4}]{sub 3}Ga{sub 3}[C{sub 6}H{sub 3}(CO{sub 2}){sub 3}]{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Dong Woo; Jo, Vinna [Department of Chemistry, Chung-Ang University, Seoul, 156-756 (Korea, Republic of); Ok, Kang Min, E-mail: kmok@cau.ac.kr [Department of Chemistry, Chung-Ang University, Seoul, 156-756 (Korea, Republic of)

    2012-10-15

    A novel noncentrosymmetric (NCS) gallium-organic framework material, [N(C{sub 3}H{sub 7}){sub 4}]{sub 3}Ga{sub 3}[C{sub 6}H{sub 3}(CO{sub 2}){sub 3}]{sub 4} (CAUMOF-11) has been synthesized by a solvothermal reaction using Ga(NO{sub 3}){sub 3}{center_dot}xH{sub 2}O, 1,3,5-C{sub 6}H{sub 3}(CO{sub 2}H){sub 3}, N(C{sub 3}H{sub 7}){sub 4}Cl, HNO{sub 3}, and HCON(CH{sub 3}){sub 2} at 180 Degree-Sign C. The structure of the reported material has been determined by single-crystal X-ray diffraction. CAUMOF-11 has an anionic three-dimensional framework with aligned four-coordinate GaO{sub 4} tetrahedra and 1,3,5-benzenetricarboxylate groups. Tetrapropylammonim cations reside within the channel and maintain the charge balance. Detailed structural analyses with full characterization including infrared spectroscopy, thermogravimetric analysis, elemental analysis, ion-exchange reactions, topotactic decomposition, and gas adsorption experiments are reported. Powder second-harmonic generating (SHG) measurements on CAUMOF-11, using 1064 nm radiation, exhibit SHG efficiency of 15 times that of {alpha}-SiO{sub 2} and the material is phase-matchable (type-1). - Graphical Abstract: Second-order nonlinear optical measurements on CAUMOF-11 reveal that the material is phase-matchable (type-1) with SHG efficiency of 15 times that of {alpha}-SiO{sub 2}. Highlights: Black-Right-Pointing-Pointer A new NCS Ga-organic framework was solvothermally synthesized. Black-Right-Pointing-Pointer CAUMOF-11 exhibits SHG efficiency of 15 times that of {alpha}-SiO{sub 2}. Black-Right-Pointing-Pointer Thermal decomposition of CAUMOF-11 crystal maintains the original morphology.

  3. The effect of precursor on the optical properties of carbon quantum dots synthesized by hydrothermal/solvothermal method

    Science.gov (United States)

    Mozdbar, Afsaneh; Nouralishahi, Amideddin; Fatemi, Shohreh; Mirakhori, Ghazaleh

    2018-01-01

    In the recent decade, Carbon Quantum Dots (CQDs) have attracted lots of attention due to their excellent properties such as tunable photoluminescence, high chemical stability, low toxicity, and biocompatibility. Among all synthesis methods, the hydrothermal/solvothermal rout has been considered as one of the most common and simplest method. The type of precursors can affect the size of CQDs and determine their surface functional groups, the essential properties that deeply influence the optical specifications. In this work, the effect of different precursors on the final properties of carbon quantum dots is investigated. The carbon quantum dots were synthesized by hydrothermal/solvothermal rout using citric acid, thiourea, ethylamine and monoethanolamine as precursors in almost the same conditions of time and temperature. Resultant CQDs were characterized by using FTIR, UV-Visible Spectroscopy and Photoluminescence (PL) analysis. The results of UV-Vis spectroscopy showed that quantum dots synthesized from monoethanolamine have wider absorption band rather than the CQDs from other precursors and the absorption edge shifted from about 270 nm for ethylamine to about 470 nm in monoethanolamine. Furthermore, the results demonstrate that using citric acid and monoethanolamine as precursor improved production efficiency and emission quantum yield of the carbon dots.

  4. Structural and optical characterization of CdS nanorods synthesized by a PVA-assisted solvothermal method

    International Nuclear Information System (INIS)

    Wang Hongmei; Fang Pengfei; Chen Zhe; Wang Shaojie

    2008-01-01

    Cadmium sulphide (CdS) 1D nanocrystals were prepared using a simple poly(vinyl-alcohol) (PVA)-assisted solvothermal method which employed ethylenediamine (en) as solvent. The obtained nanorods were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), ultraviolet-visible (UV-vis) absorption, and photoluminescence (PL) spectra. XRD results show that the nanorods are hexagonal phase. The TEM results indicate that the synthesized CdS nanorods with PVA-assisted showed larger aspect ratio and uniform faces compared with the sample prepared in the absence of PVA. The results of the photoluminescence and UV-vis spectroscopy measurements reveal that the as-prepared CdS nanorods show a quantum confinement effect. It is also found that the dosage of PVA is a vital factor in the morphology and optical properties of CdS nanorods. Moreover, when the best dosage of 3 g PVA/70 ml en was used, CdS nanorods with regular morphology and longer length were obtained. The probable mechanism for PVA-assisted solvothermal synthesis of CdS nanorods was also discussed

  5. Copper-indium-gallium-diselenide nanoparticles synthesized by a solvothermal method for solar cell application

    Directory of Open Access Journals (Sweden)

    Chiou Chuan-Sheng

    2017-01-01

    Full Text Available Chalcopyrite copper-indium-gallium-diselenide (CIGS nanoparticles are useful for photovoltaic applications. In this study, the synthesis of CIGS powder was examined, and the powder was successfully synthesized using a relatively simple and convenient elemental solvothermal route. From the reactions of elemental Cu, In, Se and Ga(NO33 powders in an autoclave with ethylenediamine as a solvent, spherical CIGS nanoparticles, with diameters ranging from 20-40 nm, were obtained using a temperature of 200°C for 36h. The structure, morphology, chemical composition and optical properties of the as-synthesized CIGS were characterized using X-ray diffraction, transmission electron microscopy, selected area electron diffraction, scanning electron microscopy, inductively coupled plasma-mass spectrometry. In this sample, the mole ratio of Cu:In:Ga:Se was equal to 0.89:0.71:0.29:2.01, and the optical band gap was found to be 1.18 eV. The solar cell obtained a power conversion efficiency of 5.62% under standard air mass 1.5 global illumination.

  6. Fabrication of white light-emitting diodes based on solvothermally synthesized copper indium sulfide quantum dots as color converters

    Science.gov (United States)

    Song, Woo-Seuk; Yang, Heesun

    2012-04-01

    A facile, large-scalable solvothermal synthesis of copper indium sulfide (CIS) quantum dots (QDs) and their application to the fabrication of QD-based white light-emitting diodes (LEDs) are reported. Depending on CIS QD growth time of 2 versus 5 h, the core/shell structured QDs of CIS/ZnS exhibit tunable emissions of yellow-orange with excellent quantum yields of 55%-91%. A white QD-LED is realized by applying CIS (2 h)/ZnS QD as a blue-to-yellow color converter. Furthermore, a white QD-LED having a blend of yellow and orange QDs is fabricated to improve a color rendering property through spectral extension, and its electroluminescent properties are evaluated.

  7. Antifungal activity of gold nanoparticles prepared by solvothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Ahmad, Tokeer, E-mail: tahmad3@jmi.ac.in [Nanochemistry Laboratory, Department of Chemistry, Jamia Millia Islamia, New Delhi 110025 (India); Wani, Irshad A.; Lone, Irfan H.; Ganguly, Aparna [Nanochemistry Laboratory, Department of Chemistry, Jamia Millia Islamia, New Delhi 110025 (India); Manzoor, Nikhat; Ahmad, Aijaz [Department of Biosciences, Jamia Millia Islamia, New Delhi 110025 (India); Ahmed, Jahangeer [Department of Chemistry, Michigan State University, East Lansing, MI 48824 (United States); Al-Shihri, Ayed S. [Department of Chemistry, Faculty of Science, King Khalid University, Abha 61413, P.O. Box 9004 (Saudi Arabia)

    2013-01-15

    Graphical abstract: Gold nanoparticles (7 and 15 nm) of very high surface area (329 and 269 m{sup 2}/g) have been successfully synthesized through solvothermal method by using tin chloride and sodium borohydride as reducing agents. As-prepared gold nanoparticles shows very excellent antifungal activity against Candida isolates and activity increases with decrease in the particle size. Display Omitted Highlights: ► Effect of reducing agents on the morphology of gold nanoparticles. ► Highly uniform and monodisperse gold nanoparticles (7 nm). ► Highest surface area of gold nanoparticles (329 m{sup 2/}g). ► Excellent antifungal activity of gold nanoparticles against Candida strains. -- Abstract: Gold nanoparticles have been successfully synthesized by solvothermal method using SnCl{sub 2} and NaBH{sub 4} as reducing agents. X-ray diffraction studies show highly crystalline and monophasic nature of the gold nanoparticles with face centred cubic structure. The transmission electron microscopic studies show the formation of nearly spherical gold nanoparticles of average size of 15 nm using SnCl{sub 2}, however, NaBH{sub 4} produced highly uniform, monodispersed and spherical gold nanoparticles of average grain size of 7 nm. A high surface area of 329 m{sup 2}/g for 7 nm and 269 m{sup 2}/g for 15 nm gold nanoparticles was observed. UV–vis studies assert the excitations over the visible region due to transverse and longitudinal surface plasmon modes. The gold nanoparticles exhibit excellent size dependant antifungal activity and greater biocidal action against Candida isolates for 7 nm sized gold nanoparticles restricting the transmembrane H{sup +} efflux of the Candida species than 15 nm sized gold nanoparticles.

  8. Antifungal activity of gold nanoparticles prepared by solvothermal method

    International Nuclear Information System (INIS)

    Ahmad, Tokeer; Wani, Irshad A.; Lone, Irfan H.; Ganguly, Aparna; Manzoor, Nikhat; Ahmad, Aijaz; Ahmed, Jahangeer; Al-Shihri, Ayed S.

    2013-01-01

    Graphical abstract: Gold nanoparticles (7 and 15 nm) of very high surface area (329 and 269 m 2 /g) have been successfully synthesized through solvothermal method by using tin chloride and sodium borohydride as reducing agents. As-prepared gold nanoparticles shows very excellent antifungal activity against Candida isolates and activity increases with decrease in the particle size. Display Omitted Highlights: ► Effect of reducing agents on the morphology of gold nanoparticles. ► Highly uniform and monodisperse gold nanoparticles (7 nm). ► Highest surface area of gold nanoparticles (329 m 2/ g). ► Excellent antifungal activity of gold nanoparticles against Candida strains. -- Abstract: Gold nanoparticles have been successfully synthesized by solvothermal method using SnCl 2 and NaBH 4 as reducing agents. X-ray diffraction studies show highly crystalline and monophasic nature of the gold nanoparticles with face centred cubic structure. The transmission electron microscopic studies show the formation of nearly spherical gold nanoparticles of average size of 15 nm using SnCl 2 , however, NaBH 4 produced highly uniform, monodispersed and spherical gold nanoparticles of average grain size of 7 nm. A high surface area of 329 m 2 /g for 7 nm and 269 m 2 /g for 15 nm gold nanoparticles was observed. UV–vis studies assert the excitations over the visible region due to transverse and longitudinal surface plasmon modes. The gold nanoparticles exhibit excellent size dependant antifungal activity and greater biocidal action against Candida isolates for 7 nm sized gold nanoparticles restricting the transmembrane H + efflux of the Candida species than 15 nm sized gold nanoparticles.

  9. Preparation of Hierarchical BiOBr Microspheres for Visible Light-Induced Photocatalytic Detoxification and Disinfection

    Directory of Open Access Journals (Sweden)

    Ayla Ahmad

    2016-01-01

    Full Text Available Photocatalytic degradation is a promising alternative to traditional wastewater treatment methods. Recently developed visible light-responsive photocatalyst, BiOBr, has attracted extensive attentions. Hereby, a detailed investigation of application of BiOBr to bacterial inactivation and organic pollutants degradation is reported. Hydrothermal catalyst was prepared using template-free method. While, for solvothermal synthesis, CTAB was used as a template. Results indicate a higher photocatalytic activity by the solvothermally prepared catalyst. Solvothermally prepared BiOBr exhibited high photocatalytic activities in both water detoxification and disinfection.

  10. Fabrication of 2D sheet-like BiOCl/carbon quantum dot hybrids via a template-free coprecipitation method and their tunable visible-light photocatalytic activities derived from different size distributions of carbon quantum dots.

    Science.gov (United States)

    Deng, Fang; Lu, Xiaoying; Zhong, Fei; Pei, Xule; Luo, Xubiao; Luo, Shenglian; Dionysiou, Dionysios D; Au, Chaktong

    2016-02-12

    A series of two-dimensional (2D) interlaced BiOCl/carbon quantum dot composites (denoted as BiOCl/CQD composites) were synthesized by a template-free coprecipitation method at room temperature, and the influence of different particle size distributions of the CQDs on the physiochemical properties and photocatalytic activities of the BiOCl/CQD composites was studied. CQDs can change the morphology and increase the specific surface area of the BiOCl/CQD composites. Moreover, the particle size distribution of the CQDs (CQD loading amount) has some effect on the light absorption, separation of photogenerated charge carriers, and photocatalytic performance of  the BiOCl/CQD composites. The optimized size distribution of the CQDs is 50-150 nm. BiOCl/CQD (50-150 nm) composites showed the best improvement of light absorption and the highest photocurrent density of 0.44 μA cm(-2), and exhibited the highest photocatalytic activity with almost 100% 2-nitrophenol removal under visible-light irradiation. The high efficacy of BiOCl/CQD (50-150 nm) composites could be attributed to their excellent light absorption and highly effective separation of photogenerated charge carriers.

  11. Structural and Morphological Tuning of LiCoPO4 Materials Synthesized by Solvo-Thermal Methods for Li-Cell Applications

    Directory of Open Access Journals (Sweden)

    Jessica Manzi

    2015-12-01

    Full Text Available Olivine-type lithium metal phosphates (LiMPO4 are promising cathode materials for lithium-ion batteries. LiFePO4 (LFP is commonly used in commercial Li-ion cells but the Fe3+/Fe2+ couple can be usefully substituted with Mn3+/Mn2+, Co3+/Co2+, or Ni3+/Ni2+, in order to obtain higher redox potentials. In this communication we report a systematic analysis of the synthesis condition of LiCoPO4 (LCP using a solvo-thermal route at low temperature, the latter being a valuable candidate to overcome the theoretical performances of LFP. In fact, LCP shows higher working potential (4.8 V vs. 3.6 V compared to LFP and similar theoretical capacity (167 mAh·g−1. Our goal is to show the effect of the synthesis condition of the ability of LCP to reversibly cycle lithium in electrochemical cells. LCP samples have been prepared through a solvo-thermal method in aqueous-non aqueous solvent blends. Different Co2+ salts have been used to study the effect of the anion on the crystal growth as well as the effect of solution acidity, temperature and reaction time. Materials properties have been characterized by Fast-Fourier transform infrared spectroscopy, X-ray diffraction and scanning electron microscopies. The correlation between structure/morphology and electrochemical performances has been investigated by galvanostatic charge-discharge cycles.

  12. Effect of solvent medium on the structural, morphological and optical properties of ZnS nanoparticles synthesized by solvothermal route

    Energy Technology Data Exchange (ETDEWEB)

    Mendil, R., E-mail: radia.mendil@yahoo.fr [Laboratoire de Physique des Matériaux et des Nanomatériaux appliquée à l' Environnement, Université de Gabès, Faculté des Sciences de Gabès, Cité Erriadh Manara Zrig, 6072 Gabès (Tunisia); Ben Ayadi, Z. [Laboratoire de Physique des Matériaux et des Nanomatériaux appliquée à l' Environnement, Université de Gabès, Faculté des Sciences de Gabès, Cité Erriadh Manara Zrig, 6072 Gabès (Tunisia); Djessas, K. [Laboratoire Procédés, Matériaux et Energie Solaire (PROMES-CNRS), TECNOSUD, Rambla de la thermodynamique, 66100 Perpignan (France); Université de Perpignan Via Domitia, 52 avenue Paul Alduy, 68860, Perpignan Cedex9 (France)

    2016-09-05

    Different morphologies of ZnS have been synthesized by a facile solvothermal approach in a mixed solvent made of Ethylenediamine (EN) and distilled water. The effect of solvent medium on the structural, morphological and optical properties of ZnS nanoparticles were investigated. The formation mechanism of different morphologies was proposed based on the experiment results. The as-prepared samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), energy dispersive spectrometer (EDS), Raman spectroscopy and UV-Vis-IR spectrophotometer. The results show that phase transformation is easily induced and there is a strong correlation between morphology and structure of the ZnS nanocrystals by changing the solvent. The results also show that we have successfully produced hexagonal phase ZnS nanorods with mixed solvent. The grain sizes in the range of 17–22 nm were obtained according to elaboration conditions. Raman spectra show the intense peak at 346 cm{sup −1}, which is a typical Raman peak of bulk ZnS crystal, no signature of secondary phases. The band gap of ZnS increased from 3.49 to 3.74 eV with an increase in the EN composition in the solvent, implying that the optical properties of these materials are clearly affected by the synthesis medium. - Highlights: • ZnS was prepared at low temperature using solvothermal method. • The phase transformation and shape evolution processes were studied. • The role of solvent (EN/W) has been discussed for formation of ZnS nanostructures with different morphology. • The properties and growth mechanism of ZnS nanoparticles were investigated. • Optical band gap of ZnS powder were investigated using UV vis spectroscopy.

  13. Solvothermal preparation of nano-β-HgS from a precursor, bis(dibenzyldithiocarbamato)mercury(II)

    Science.gov (United States)

    Marimuthu, G.; Ramalingam, K.; Rizzoli, C.; Arivanandhan, M.

    2012-02-01

    A simple solvothermal method for the selective synthesis of β-HgS (meta cinnabar) nanoparticles in aqueous solutions is reported with bis(dibenzyldithiocarbamato)mercury(II) as the precursor. Crystal structure, size, morphology and composition of the products are characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX) analysis, high-resolution transmission electron microscopy (HRTEM), SAED and X-ray photoelectron spectroscopy (XPS). PXRD shows (111), (220), (200), (311), (222), (400), (331), (420) reflections characteristic of β-HgS. SEM micrographs display the spherical nature of the nano-β-HgS. EDX analysis showed the presence of Hg and S. HRTEM images indicate the spherical nature of the nanoparticles with their size in the range of 10-15 nm and the FFT pattern shows the crystalline nature of the spherical particles. The results are in agreement with those estimated from the XRD pattern. XPS signals observed at 162.6 and 162.8 eV are due to S2 p 3/2 and S2 p 1/2 electrons and the S2 s was observed at 222.3 eV. The band gap of nano-β-HgS has been found to be 3.6 eV from the UV-visible spectral measurement. The blue-shifted band gap compared to the bulk HgS is a consequence of "size quantization" effect. A comprehensive characterization of the precursor by IR and single crystal X-ray crystallography shows the presence of HgS4 coordination environment, with a distinct Hg-S bond asymmetry.

  14. A novel solvothermal route for obtaining strontium titanate nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Marquez-Herrera, A., E-mail: alfredo.marquez@uaslp.mx [Universidad Autonoma de San Luis Potosi, Departamento de Ingenieria Mecanica Administrativa, Coordinacion Academica Region Altiplano (COARA) (Mexico); Ovando-Medina, Victor M.; Corona-Rivera, Miguel A. [Universidad Autonoma de San Luis Potosi, Departamento de Ingenieria Quimica, Coordinacion Academica Region Altiplano (COARA) (Mexico); Hernandez-Rodriguez, E.; Zapata-Torres, M. [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, Unidad Legaria IPN (Mexico); Campos-Gonzalez, E.; Guillen-Cervantes, A.; Zelaya-Angel, O.; Melendez-Lira, M. [CINVESTAV-IPN, Departamento de Fisica (Mexico)

    2013-04-15

    Strontium titanate (SrTiO{sub 3}) has attracted a lot of attention because of its possible applications in new microelectronic devices. It is a material with a high dielectric constant, low leakage current, and some of its properties can be changed by adding or modifying the concentration of a dopant, which can be used for a wide range of functional purposes, from simple capacitors to complicated microwave devices. Therefore, in this work, we report the development of a new route to synthesize SrTiO{sub 3} nanoparticles based on the solvothermal method by employing two precursor solutions: strontium chloride and titanium(IV) butoxide. Our route allows the production of cubic SrTiO{sub 3} nanoparticles with a narrow size distribution. The particle sizes range between 8 and 24 nm, forming agglomerates of SrTiO{sub 3} in the range of 128-229 nm. It was demonstrated that the Ti/Sr molar ratio employed into the precursor solution has an important effect onto the chemical composition of the resulting SrTiO{sub 3} nanoparticles: when using Ti/Sr < 1, the formation and incorporation of the SrCO{sub 3} compound into the nanoparticles was observed while with Ti/Sr {>=} 1 nanoparticles are free of contaminants. The as-prepared nanoparticles were characterized by energy-dispersive X-ray spectroscopy, X-ray diffraction, transmission electron microscopy, high-resolution TEM, selected area electron diffraction, scanning electron microscopy, and dynamic light scattering.

  15. Iron (III) oxyhydroxide in isopropyl alcohol preparation, characterization and solvothermal treatment

    International Nuclear Information System (INIS)

    Carvalho, E.L.C.N.; Jafelicci Junior, M.

    1989-01-01

    Iron (III) nitrate hydrolysis was carried out in isopropyl alcohol solution by an aqueous amonia gas stream resulting in iron (III) oxyhydroxide sol. It has been investigated in this work the solvothermal treatment of this colloidal system at 120 0 C and 24 hours. Iron (III) oxyhydroxide freshly obtained and solvothermally treated. Samples were dryed by lyophilization. Products obtained were characterized by the following techniques: spectrophotometric iron analysis by 1,10-orthophenantroline complexation method, powder X-ray diffraction, vibrational infrared spectra and differential thermal analysis. After solvothermal treatment resulting product was crystallized into hematite, while freshly iron (III) oxyhydroxide was non crystalline. Both of them are very active powder, showing high water adsorption [pt

  16. Facile preparation of porous carbon from coffee bean waste using low temperature solvothermal method

    Science.gov (United States)

    Baroroh, L. A. Al; Fitria, D.; Amal, M. I.; Wismogroho, A. S.; Widayatno, W. B.

    2018-03-01

    In this study, porous carbon made from coffee bean waste (CBW) was carbonized at 500 °C, 600 °C, and 700 °C to find effective temperature. It is verified from the IR spectrum that carbonization process at certain temperature can effectively break cellulose bonding and make aromatics functional group while preserving its carbon structure. The TG-DTA curve shows four stages of decomposition process and confirms most effective carbonization temperature. Activation process of as-carbonized CBW was carried out using solvothermal method in KOH and NH4OH steam environment at 200 °C with variation of 30%, 40%, and 50% solvothermal volume. Scanning electron micrographs reveals significant increase of porosity on the carbon surface and differences of structural pores between the variations. The results show the possible potential of utilizing low temperature-solvothermal method for nanoporous carbon material.

  17. Characterization of crystalline silica nanorods synthesized via a solvothermal route using polyvinylbutyral as a template

    International Nuclear Information System (INIS)

    Chen, Lin-Jer; Liao, Jiunn-Der; Chuang, Yu-Ju; Fu, Yaw-Shyan

    2011-01-01

    The preparation of crystalline silica nanorods is presented. Crystalline silica nanorods were synthesized via a simple solvothermal route using polyvinylbutyral (PVB) as a template in an autoclave with ethylenediamine as a solvent at 180 °C for 25 h. Silica nanorods with diameters in the range of 50–80 nm were obtained. The solvothermal route with a PVB template played affected the crystallization process and the growth of the silica nanorods. The as-synthesized products were characterized using X-ray diffraction, energy dispersive spectrometry, scanning electron microscopy, and transmission electron microscopy.

  18. Flowerlike vanadium sesquioxide: solvothermal preparation and electrochemical properties.

    Science.gov (United States)

    Liu, Haimei; Wang, Yonggang; Li, Huiqiao; Yang, Wensheng; Zhou, Haoshen

    2010-10-25

    A novel 3D hierarchical flowerlike vanadium sesquioxide (V(2)O(3)) nano/microarchitecture consisting of numerous nanoflakes is prepared via a solvothermal approach followed by an appropriate heating treatment. The as-obtained nanostructured V(2)O(3) flower is characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Brunauer-Emmett-Teller (BET) analysis, and transmission electron microscopy (TEM) (or/and high-resolution TEM, HRTEM), and it is found that the V(2)O(3) flower is constructed by single-crystalline nanoflakes. Furthermore, it is demonstrated that the surface of the flowerlike V(2)O(3) material is composed of nanostructured pores, which derive from the adsorption/desorption of nitrogen, and that the pore-size distribution depends on the unique three-dimensional interconnection between nanoflakes and on their intrinsic properties. The electrochemical behavior of the V(2)O(3) flower for lithium-ion insertion/extraction in non-aqueous solution as well as the faradaic capacitance for pesudocapacitors in a neutral aqueous solution are also investigated. A reversible discharge capacity as high as 325 mA h g(-1) is obtained at a current density of 0.02 A g(-1) from a LiClO(4)/EC:DEC electrolyte solution (i.e. LiClO(4) in ethyl carbonate and diethyl carbonate). When used as the cathode material of pesudocapacitors in Li(2)SO(4), the flowerlike oxide displayed a very high initial capacitance of 218 F g(-1) at a current density of 0.05 A g(-1). We believe that the good performance of the flowerlike V(2)O(3) electrode is most probably due to its unique 3D hierarchical nano/microarchitecture, which shows that the electrochemical properties of a cathodic material do not only depend on the oxidation state of that material but also-to a large extent-on its crystalline structure and morphology. The aforementioned properties suggest that the present V(2)O(3) flower materials may have a great potential to be employed as electrode materials in

  19. Improved electrochemical performance of Li4Ti5O12 with a variable amount of graphene as a conductive agent for rechargeable lithium-ion batteries by solvothermal method

    International Nuclear Information System (INIS)

    Rai, Alok Kumar; Gim, Jihyeon; Kang, Sung-Won; Mathew, Vinod; Anh, Ly Tuan; Kang, Jungwon; Song, Jinju; Paul, Baboo Joseph; Kim, Jaekook

    2012-01-01

    We report on the solvothermal preparation of pure Li 4 Ti 5 O 12 and Li 4 Ti 5 O 12 /graphene (15 wt% and 30 wt%) nanocomposites anode for high-performance lithium-ion batteries. Structure and morphology studies of the nanocomposites by X-ray diffraction, field-emission scanning electron microscopy and field-emission transmission electron microscopy reveal Li 4 Ti 5 O 12 nanoparticles embedded onto the graphene nanosheets. On comparison to pure spinel Li 4 Ti 5 O 12 , the electrochemical performances of the Li 4 Ti 5 O 12 /graphene nanocomposites indicate higher capacities and enhanced cycle performances within the voltage domain of 1.0–2.5 V, under current rates as high as 10.4 C. The production of phase pure Li 4 Ti 5 O 12 nanoparticles ensures the short ion-diffusion paths while the presence of graphene facilitates improved structural network and hence enhanced electronic transport in the prepared nanocomposites. These factors eventually amount to impressive electrochemical properties. Highlights: ► A simple polyol-based approach to obtain the graphene nanosheets. ► Li 4 Ti 5 O 12 /graphene nanocomposites synthesis by polyol-based solvothermal process. ► Low temperature solvothermal strategy is one-step process to control nanoparticle sizes. ► The nanoparticles are well anchored onto the graphene nanosheets in the nanocomposites. ► Li 4 Ti 5 O 12 /graphene nanocomposites exhibit impressive electrochemical performances.

  20. From dihydrated iron(III) phosphate to monohydrated ammonium-iron(II) phosphate: Solvothermal reaction mediated by acetone-urea mixtures

    Energy Technology Data Exchange (ETDEWEB)

    Alfonso, Belen F., E-mail: mbafernandez@uniovi.es [Departamento de Fisica, Universidad de Oviedo, Calvo Sotelo, s/n 33007 Oviedo (Spain); Trobajo, Camino [Departamento de Quimica Organica e Inorganica, Universidad de Oviedo-CINN, Julian Claveria 8, 33006 Oviedo (Spain); Pique, Carmen [Departamento de Fisica, Universidad de Oviedo, Calvo Sotelo, s/n 33007 Oviedo (Spain); Garcia, Jose R. [Departamento de Quimica Organica e Inorganica, Universidad de Oviedo-CINN, Julian Claveria 8, 33006 Oviedo (Spain); Blanco, Jesus A. [Departamento de Fisica, Universidad de Oviedo, Calvo Sotelo, s/n 33007 Oviedo (Spain)

    2012-12-15

    By reaction between synthetic phosphosiderite FePO{sub 4}{center_dot}2H{sub 2}O, urea (NH{sub 2}){sub 2}CO, and acetone (CH{sub 3}){sub 2}CO, we report a novel solvothermal synthesis of polycrystalline NH{sub 4}FePO{sub 4}{center_dot}H{sub 2}O. The preparation of other two individual phases, NH{sub 4}Fe{sub 2}(OH)(PO{sub 4}){sub 2}{center_dot}2H{sub 2}O and NH{sub 4}Fe{sub 2}(PO{sub 4}){sub 2}, is also described. The obtained product is a function of the reaction time and the N/P molar ratio in the reagent mixture, and the existence of structural memory in the dissolution-precipitation processes is discussed. Below 25 K, NH{sub 4}FePO{sub 4}{center_dot}H{sub 2}O behaves magnetically in a complex way, because both ferromagnetic and antiferromagnetic signals are superimposed, suggesting the existence of a canting of iron(II) magnetic moments. - Graphical abstract: Solvothermal synthesis of polycrystalline NH{sub 4}FePO{sub 4}{center_dot}H{sub 2}O is presented. The preparation of other two individual phases, NH{sub 4}Fe{sub 2}(OH)(PO{sub 4}){sub 2}{center_dot}2H{sub 2}O and NH{sub 4}Fe{sub 2}(PO{sub 4}){sub 2} as a function of the N/P molar ratio in the reagent mixture and the reaction time, is also described. Highlights: Black-Right-Pointing-Pointer Solvothermal synthesis of NH{sub 4}FePO{sub 4}{center_dot}H{sub 2}O from an Fe(III) phosphate: reduction process. Black-Right-Pointing-Pointer Formation of two intermediate metastable phases: phase diagram. Black-Right-Pointing-Pointer Thermal decomposition in two steps: mass loss of both water and ammonia. Black-Right-Pointing-Pointer Magnetic behaviour: AF+constant spontaneous magnetization.

  1. Hydro- and solvothermally-prepared ZnO and its catalytic effect on photodegradation of reactive orange 16 dye

    Directory of Open Access Journals (Sweden)

    Simović Bojana

    2014-01-01

    Full Text Available In this work, zinc oxide powders were obtained by two different techniques: hydro- and solvothermal synthesis starting from Zn(NO32 and Zn(CH3COO2, respectively. The influence of synthetic procedure on the structural, microstructural, thermal and photocatalytic properties of the prepared ZnO powders was investigated. Both ZnO samples were further annealed at moderate conditions (300°C to avoid grain growth and to remove traces of impurities. In all four cases a single-phase hexagonal ZnO was confirmed by X-ray powder diffraction. The morphology of prepared ZnO powders was different and it varied from rounded nanograins to microrods. All prepared samples showed higher photocatalytic efficiency in degradation of textile azo-dye Reactive Orange 16(RO16 than the commercial ZnO. In addition, the non-annealed samples had better photocatalytic properties than the commercial Degussa P25 TiO2 powder. [Projekat Ministarstva nauke Republike Srbije, br. III45007, br. ON171032 i br. ON172013

  2. Solvothermal synthesis of discrete cages and extended networks comprising {Cr(III)3O(O2CR)3(oxime)3}2- (R = H, CH3, C(CH3)3, C14H9) building blocks

    DEFF Research Database (Denmark)

    Houton, Edel; Comar, Priyanka; Pitak, Mateusz B.

    2016-01-01

    The synthesis, structural and magnetic characterisation of a family of related Cr(iii) cages are reported. Each member comprises {Cr(iii)3O(O2CR1)3(R2-sao)3}2- (R1 = H, CH3, C(CH3)3, C14H9; R2 = Me, Ph, tBu, C10H8) triangles linked by Na+ cations, resulting in either the discrete complexes [H3O......][NEt4]2[NaCr(iii)6O2(O2C-C14H9)6(Naphth-sao)6] (1) and [Na4Cr(iii)6O2(O2CC(CH3)3)6(3,5-di-tBu-sao)6(MeCN)6] (3); or the extended networks [H3O]2[Na2Cr(iii)6O2(O2CH)6(Ph-sao)6(MeCN)2(H2O)2]n·4MeCN (2); [H3O][Na3Cr(iii)6O2(O2CCH3)6(Me-sao)6(MeCN)]n (4) and [Na2Cr(iii)3O(O2CCH3)3(Me-sao)3(H2O)6]n·3MeCN (5...

  3. Sodium-dodecyl-sulphate-assisted synthesis of Ni nanoparticles ...

    Indian Academy of Sciences (India)

    2017-11-20

    Nov 20, 2017 ... Abstract. Stabilized nickel nanoparticles (SNNPs) were prepared using Ni(acac)2 (acac = acetylacetonate) via a simple solvothermal method. The synthesis of the nickel nanoparticles was performed in the presence of sodium dodecyl sulphate. (SDS) of different concentrations (mole ratios of SDS:Ni(acac)2 ...

  4. Synthesis and optical characteristics of ZnO nanocrystals

    Indian Academy of Sciences (India)

    Administrator

    (Johnson et al 2001; Zhang et al 2002). Compared to other semiconductors, ZnO has wide bandgap of 3⋅37 eV and other large excitation binding energy, which makes excitation stable even at room temperature. There are various methods in order to synthesize ZnO nanomaterials viz. solvothermal synthesis, sol–gel (Li ...

  5. Investigation on development of advanced materials by solvothermal technique; Sorubo thermal hanno riyo senshin zairyo kaihatsu ni kansuru chosa

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1996-03-01

    Solvothermal reaction is reaction under high temperature and high pressure, which is expected to fabricate new functional materials. In this study, the materials are classified into two fields, i.e., inorganic materials, metals and their composites and organic materials and their composites. The current status of R and D of production and processing technology in each field is surveyed and the prospect of it is discussed. For the inorganic materials, metals and their composites, it is explained that very fine metal oxide particles, complex oxides, single crystals, whiskers, compounds with layer structure, metastable compounds, ion conductors and catalysts with high ability could be produced only by controlling the solvothermal reactions in atomic order. For the organic materials and their composites, surveyed results of the solvothermal technique using non-aqueous solutions are mainly provided. The necessity of a national project for researches on the solvothermal reactions is proposed from the viewpoint of resource, environment and energy. 777 refs., 38 figs., 26 tabs.

  6. Unprecedented connection mode of [V{sub 16}Sb{sub 4}O{sub 42}(H{sub 2}O)]{sup 8-} cluster anions by Mn{sup 2+} centered complexes. Solvothermal synthesis and properties of {[Mn(teta)]_4V_1_6Sb_4O_4_2(H_2O)}{sub n}.[(H{sub 2}O){sub 12}]{sub n}

    Energy Technology Data Exchange (ETDEWEB)

    Rasmussen, Maren; Naether, Christian; Bensch, Wolfgang [Institute of Inorganic Chemistry, Christian-Albrechts-University of Kiel (Germany); Leusen, Jan van; Koegerler, Paul [Institute of Inorganic Chemistry, RWTH Aachen University, Aachen (Germany)

    2017-11-17

    The new compound {[Mn(teta)]_4V_1_6Sb_4O_4_2}{sub n}.[(H{sub 2}O){sub 12}]{sub n} (teta = triethylenetetraamine) was synthesized under solvothermal conditions. The crystal structure features the high nuclearity [V{sub 16}{sup IV}Sb{sub 4}{sup III}O{sub 42}(H{sub 2}O)]{sup 8-} cluster anion, which consists of two rings composed of 8 edge-sharing VO{sub 5} polyhedra. The rings are perpendicular to each other generating four niches, which are occupied by two VO{sub 5} pyramids and two handle-like Sb{sub 2}O{sub 5} units. The two unique anions are each surrounded by eight Mn{sup 2+} centered complexes via Mn-O{sub term}-V bonds. Such an expansion has never been observed in heterometal polyoxovanadate chemistry. The connection mode between cluster anions and complex cations generates two individual layers stacked onto each other. Between the layers weak Sb..O contacts are observed. The crystal water molecules are mainly located in the empty space between the layers. Upon heating H{sub 2}O molecules are removed, while the crystal structure remains intact. The magnetic behavior is dominated by strong antiferromagnetic exchange interactions between the central V{sup 4+} ions, while the interaction between the cluster anion and central Mn{sup 2+} ions is significantly less pronounced. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  7. Solvothermal synthesis and characterization of acicular α-Fe2O3 ...

    Indian Academy of Sciences (India)

    Administrator

    the Fe 2p3/2 peak at 711⋅0 eV. C 1s peak of the carbon contamination over the sample is referenced at 284⋅6 eV. Shake up satellite ~ 8 eV above the Fe 2p1/2 and Fe 2p3/2 peaks are visible. Separation of the 2p doublet is ~ 13⋅6 eV. All these features are typical of Fe2O3. The peak maxi- mum for α and γ are reported to ...

  8. Solvothermal synthesis and characterization of acicular α-Fe2O3 ...

    Indian Academy of Sciences (India)

    ... X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transition electron microscopy (TEM), infrared spectroscopy (IR) and thermal analysis (TG–DTA). XRD indicates that the product is single-phase -Fe2O3 with rhombohedral structure. Bundles of acicular shaped nanoparticles are seen in TEM ...

  9. SCOPE OF VARIOUS SOLVENTS AND THEIR EFFECTS ON SOLVOTHERMAL SYNTHESIS OF Ni-BTC

    Directory of Open Access Journals (Sweden)

    Farrukh Israr

    2016-07-01

    Full Text Available Ni-BTC (BTC = 1,3,5-benzene tricarboxylate metal organic framework (MOF was synthesized using different solvent conditions. Solvent mixtures of water/N,N-dimethylformamide (DMF, water/ethanol, and water/ethanol/DMF were used for the reactions with or without a variety of bases at 160 ºC for 48 hours. Even with same green crystals, prepared MOFs show all different BET surface areas and different XRD patterns. The highest BET surface area of the crystals was 850 m2/g obtained from water/DMF solvent with NH4OH as a base. The measured surface areas of the crystals follows the order of Ni-BTC(water/DMF-NH4OH > Ni-BTC(water/DMF-TMA > Ni-BTC(water/DMF > Ni-BTC(water/DMF-Pyridine> Ni-BTC(water/ethanol> Ni-BTC(water/DMF-aniline> Ni-BTC(water/DMF-NaOH.

  10. Solvothermal synthesis and characterization of acicular α-Fe2O3 ...

    Indian Academy of Sciences (India)

    Administrator

    Cherepy N J, Liston D B, Lovejoy J A, Deng H and Zhang J Z. 1998 J. Phys. Chem. B102 770. Cornell R M and Schwertmann U 1996 The iron oxides: struc- ture, properties, reactions, occurrence and uses (VCH: Weinheim). Dawson W J 1988 Am. Ceram. Soc. Bull. 67 1673. Dow J D and Schuller I K 1987 Interfaces, ...

  11. Enhanced microbial electrosynthesis with three-dimensional graphene functionalized cathodes fabricated via solvothermal synthesis

    DEFF Research Database (Denmark)

    Aryal, Nabin; Halder, Arnab; Tremblay, Pier-Luc

    2016-01-01

    The biological reduction of CO2 into multicarbon chemicals can be driven by electrons derived from the cathode of a bioelectrochemical reactor via microbial electrosynthesis (MES). To increase MES productivity, conditions for optimal electron transfer between the cathode and the microbial catalys...... analysis, 3D-graphene/carbon felt composite cathode exhibited higher current response. The results indicate that the development of a 3D-network cathode is an effective approach to improve microbe-electrode interactions leading to productive MES systems....

  12. Electrochemical Li-uptake properties of nanosized NiSb2 prepared by solvothermal route

    International Nuclear Information System (INIS)

    Xie, J.; Zhao, X.B.; Cao, G.S.; Zhao, M.J.; Su, S.F.

    2005-01-01

    The nanosized intermetallic compound NiSb 2 was prepared by a solvothermal route and studied as a potential anode material for secondary lithium-ion batteries. The microstructure of the as-prepared NiSb 2 powder was characterized by X-ray diffraction, transmission electron microscopy. The electrochemical performances of the NiSb 2 electrode were investigated by galvanostatic charge and discharge cycling and by cyclic voltammogram. It was found that the nanosized NiSb 2 electrode shows improved cycling behavior, especially in the initial cycles, compared to the micrometer sized NiSb 2 prepared by a levitation-melting/ball-milling route

  13. Growth of ZnO nanoparticles from nanowhisker precursor with a simple solvothermal route

    International Nuclear Information System (INIS)

    Wang Chunlei; Wang Enbo; Shen Enhong; Gao Lei; Kang Zhenhui; Tian Chungui; Zhang Chao; Lan Yang

    2006-01-01

    Methods of preparing nanoparticles have long been a topic experiencing extensive investigation. Among those methods developed, using template or polymer and surfactant as capping reagents were often effective. However, obtaining nanoparticles in high amounts and high purity still remains an unresolved challenge. Here, a simple two-step solvothermal method without using any surfactant or coating reactant to prepare ZnO nanoparticles with high purity in large scale was developed. X-ray powder diffraction (XRD) and transmission electron microscopy (TEM) were used to characterize the as-prepared ZnO nanoparticles, and the formation process of the nanoparticles was discussed finally

  14. Rapid synthesis of zeolitic imidazolate framework-8 (ZIF-8) nanocrystals in an aqueous system

    KAUST Repository

    Pan, Yichang

    2011-01-01

    We report here the first example of ZIF materials synthesized in aqueous solution. The synthesis was performed at room temperature and typically took several minutes compared to hours and days in non-aqueous conditions. The obtained product were ZIF-8 nanocrystals having size of ∼85 nm and showed excellent thermal, hydrothermal and solvothermal stabilities. © 2011 The Royal Society of Chemistry.

  15. Solvothermally synthesized tungsten oxide nanowires/nanorods for NO2 gas sensor applications

    International Nuclear Information System (INIS)

    Qin Yuxiang; Li Xiao; Wang Fei; Hu Ming

    2011-01-01

    Highlights: → Tungsten oxide nanowires and nanorods were solvothermally synthesized by changing reaction solvent. → The sensing characteristics of the tungsten oxide nanowires and nanorods sensors to NO 2 gas were evaluated in detail. → The response time and recovery time for the nanowires or nanorods sensors are much shorter than the oxide nanoparticles or sputtered films. → The nanowires sensor shows a much shorter response time and a relative higher response value to NO 2 gas than the nanorods one. → The NO 2 -sensing mechanism and the possible reason for the better gas sensing properties of the nanowires are analyzed. - Abstract: One-dimensional nanorods or nanowires of W 18 O 49 were synthesized by solvothermal method at 200 deg. C with tungsten hexachloride (WCl 6 ) as precursor and cyclohexanol or 1-propanol as reaction solvent. Their morphology and structure properties were systematically characterized. The NO 2 -sensing properties of the sensors based on nanowires and nanorods were investigated at 100 deg. C up to 250 deg. C over NO 2 concentration ranging from 1 ppm to 20 ppm. The results indicate that both nanowires and nanorods exhibit reversible response to different concentrations of NO 2 , and the highest gas response is achieved at 150 deg. C. In comparison with nanorods, nanowires showed a much quicker response characteristic and a relative higher response value to the same concentration of NO 2 gas due to the smaller diameter and larger specific surface area.

  16. Solvo-thermal in situ transesterification of wet spent coffee grounds for the production of biodiesel.

    Science.gov (United States)

    Park, Jeongseok; Kim, Bora; Son, Jeesung; Lee, Jae W

    2018-02-01

    This work addresses non-catalytic biodiesel production from spent coffee ground (SCG) by integrating solvo-thermal effect of 1,2-dichloroethane (DCE) with in situ transesterification over 160 °C. The SCG water content has a positive effect on the DCE hydrolysis up to 60 wt% due to the bimolecular substitution mechanism. The hydrolysis gives an acidic environment favorable for cellulose decomposition, SCG particle size reduction and lipid conversion. The optimal fatty acid ethyl ester yield was 11.8 wt% based on the mass of dried SCG with 3.36 ml ethanol and 3.16 ml DCE at 196.8 °C through the response surface methodology. Using the solvo-thermal effect, direct utilization of wet SCG as a biodiesel feedstock provides not only economic feasibility without using drying process and additional acid catalyst but also environmental advantage of recycling the municipal waste. Copyright © 2017 Elsevier Ltd. All rights reserved.

  17. A Versatile Route for the Synthesis of Nickel Oxide Nanostructures Without Organics at Low Temperature

    Directory of Open Access Journals (Sweden)

    Shah MA

    2008-01-01

    Full Text Available AbstractNickel oxide nanoparticles and nanoflowers have been synthesized by a soft reaction of nickel powder and water without organics at 100 °C. The mechanism for the formation of nanostructures is briefly described in accordance with decomposition of metal with water giving out hydrogen. The structure, morphology, and the crystalline phase of resulting nanostructures have been characterized by various techniques. Compared with other methods, the present method is simple, fast, economical, template-free, and without organics. In addition, the approach is nontoxic without producing hazardous waste and could be expanded to provide a general and convenient strategy for the synthesis of nanostructures to other functional nanomaterials.

  18. RETRACTED: Facile, eco-friendly and template free photosynthesis of cauliflower like ZnO nanoparticles using leaf extract of Tamarindus indica (L.) and its biological evolution of antibacterial and antifungal activities.

    Science.gov (United States)

    Elumalai, K; Velmurugan, S; Ravi, S; Kathiravan, V; Ashokkumar, S

    2015-02-05

    In the present investigation, we chose the very simple and eco-friendly chemical method for synthesis of zinc oxide nanoparticles from leaf extract of Tamarindus indica (L.) (T. indica) and developed the new green route for synthesis of nanoparticles. Formed product has been studied by UV-vis absorption spectroscopy, Photoluminescence (PL) spectroscopy, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Field emission scanning electron microscopy (FE-SEM) and with corresponding energy dispersive X-ray analysis (EDX). Mainly, the present results depicted that the synthesized nanoproducts are moderately stable, hexagonal phase, roughly spherical with maximum particles in size range within 19-37 nm in diameter. The antibacterial and fungal activities of aqueous extracts of T. indica were ended with corresponding disk diffusion and Minimum Inhibitory Concentration (MIC). The highest mean zones of inhibition were observed in the ZnO NPs (200 μg/mL) against Staphylococcus aureus (13.1±0.28). Finally, it can be concluded that microbial activity of ZnO NPs has more susceptible S. aureus than the other micro organisms. Further, the present investigation suggests that ZnO NPs has the potential applications for various medical and industrial fields. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. RETRACTED: Facile, eco-friendly and template free photosynthesis of cauliflower like ZnO nanoparticles using leaf extract of Tamarindus indica (L.) and its biological evolution of antibacterial and antifungal activities

    Science.gov (United States)

    Elumalai, K.; Velmurugan, S.; Ravi, S.; Kathiravan, V.; Ashokkumar, S.

    2015-02-01

    This article has been retracted at the request of the Editor. The article contains an image (Fig. 5B) which was published later again in "Green synthesis of zinc oxide nanoparticles using Moringa oleifera leaf extract and evaluation of its antimicrobial activity" by K. Elumalai et al. in Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy 143 (2015) 158-164, http://dx.doi.org/10.1016/j.saa.2015.02.011 despite being attributed to different nanoparticles. Even though this represents the first publication of this image, the attribution to different sets of nanoparticles makes the dataset suspect. The scientific community takes a very strong view on this scientific misbehavior and apologies are offered to readers of the journal that this was not detected during the submission process.

  20. Study on structural, optical properties of solvothermally synthesized Ni doped CdS nanorods

    International Nuclear Information System (INIS)

    Kaur, Kamaldeep; Verma, N. K.

    2015-01-01

    Undoped and alkali metal i.e Ni doped CdS nanorods (Cd x Ni 1-x S) with (x = 0.0, 0.3,) has been synthesized by using a convenient solvothermal technique. In order to confirm the structure of the synthesized nanorods X-ray diffraction (XRD) has been done which reveals the formation of hexagonal phase of the dilute magnetic semiconducting nanorods having size of undoped 27.79nm and doped 17.49nm. Energy dispersive X-ray analysis depicts the presence of elements Cd, Ni and S in their stoichiometric ratio. Optical behavior of undoped and doped nanorods has been investigated. UV-visible spectra show the blue shift in the band gap, as compared to the bulk CdS which may be due the quantum confinement occurs in the nanostructures. Morphological analysis has been done with the help of Transmission electron microscope which confirms the polycrystalline nature of the synthesized nanorods

  1. High performance of solvothermally prepared VO2(B as anode for aqueous rechargeable lithium batteries

    Directory of Open Access Journals (Sweden)

    Milošević Sanja

    2015-01-01

    Full Text Available The VO2 (B was synthesized via a simple solvothermal route at 160oC in ethanol. The initial discharge capacity of VO2 (B anode, in saturated aqueous solution of LiNO3, was 177 mAh g-1 at a current rate of 50 mA g-1. After 50 cycles capacity fade was 4%, but from 20th-50th cycle no capacity drop was observed. The VO2 (B has shown very good cyclability at current rate of even 1000 mA g-1 with initial discharge capacity of 92 mAh g-1. The excellent electrochemical performance of VO2 (B was attributed to the stability of micro-nano structures to repeated intercalation /deintercalation process, very good electronic conductivity as well as the very low charge transfer resistance in the aqueous electrolyte. [Projekat Ministarstva nauke Republike Srbije, br. III45014

  2. Solvothermally synthesized tungsten oxide nanowires/nanorods for NO{sub 2} gas sensor applications

    Energy Technology Data Exchange (ETDEWEB)

    Qin Yuxiang, E-mail: qinyuxiang@tju.edu.cn [School of Electronics and Information Engineering, Tianjin University, No. 92, Weijin Road, Nankai District, Tianjin 300072 (China); Li Xiao; Wang Fei; Hu Ming [School of Electronics and Information Engineering, Tianjin University, No. 92, Weijin Road, Nankai District, Tianjin 300072 (China)

    2011-08-18

    Highlights: > Tungsten oxide nanowires and nanorods were solvothermally synthesized by changing reaction solvent. > The sensing characteristics of the tungsten oxide nanowires and nanorods sensors to NO{sub 2} gas were evaluated in detail. > The response time and recovery time for the nanowires or nanorods sensors are much shorter than the oxide nanoparticles or sputtered films. > The nanowires sensor shows a much shorter response time and a relative higher response value to NO{sub 2} gas than the nanorods one. > The NO{sub 2}-sensing mechanism and the possible reason for the better gas sensing properties of the nanowires are analyzed. - Abstract: One-dimensional nanorods or nanowires of W{sub 18}O{sub 49} were synthesized by solvothermal method at 200 deg. C with tungsten hexachloride (WCl{sub 6}) as precursor and cyclohexanol or 1-propanol as reaction solvent. Their morphology and structure properties were systematically characterized. The NO{sub 2}-sensing properties of the sensors based on nanowires and nanorods were investigated at 100 deg. C up to 250 deg. C over NO{sub 2} concentration ranging from 1 ppm to 20 ppm. The results indicate that both nanowires and nanorods exhibit reversible response to different concentrations of NO{sub 2}, and the highest gas response is achieved at 150 deg. C. In comparison with nanorods, nanowires showed a much quicker response characteristic and a relative higher response value to the same concentration of NO{sub 2} gas due to the smaller diameter and larger specific surface area.

  3. Challenges in TEM sample preparation of solvothermally grown CuInS2 films.

    Science.gov (United States)

    Frank, Anna; Changizi, Rasa; Scheu, Christina

    2018-06-01

    Transmission electron microscopy (TEM) is a widely used tool to characterize materials. The required samples need to be electron transparent which should be achieved without changing the microstructure. This work describes different TEM sample preparation techniques of nanostructured CuInS 2 thin films on fluorine-doped tin oxide substrates, synthesized solvothermally using l-cysteine as sulfur source. Focused ion beam lamellae, conventional cross section samples and scratch samples have been prepared and investigated. It was possible to prepare appropriate samples with each technique, however, each technique brings with it certain advantages and disadvantages. FIB preparation of solvothermally synthesized CuInS 2 suffers from two main drawbacks. First, the whole CuInS 2 layer displays a strongly increased Cu content caused by Cu migration and preferential removal of In. Further, electron diffraction shows the formation of an additional CuS phase after Ga + bombardment. Second, diffraction analysis is complicated by a strong contribution of crystalline Pt introduced during the FIB preparation and penetrating into the porous film surface. The conventional cross sectional CuInS 2 sample also shows a Cu signal enhancement which is caused by contribution of the brass tube material used for embedding. Additionally, Cu particles have been observed inside the CuInS 2 which have been sputtered on the film during preparation. Only the scratch samples allow an almost artefact-free and reliable elemental quantification using energy-dispersive X-ray spectroscopy. However, scratch samples suffer from the drawback that it is not possible to determine the layer thickness, which is possible for both cross sectional preparation techniques. Consequently, it is concluded that the type of sample preparation should be chosen dependent on the required information. A full characterization can only be achieved when the different techniques are combined. Copyright © 2018 Elsevier Ltd. All

  4. A Facile Synthesis of Hollow Palladium/Copper Alloy Nanocubes Supported on N-Doped Graphene for Ethanol Electrooxidation Catalyst

    OpenAIRE

    Zhengyu Bai; Rumeng Huang; Lu Niu; Qing Zhang; Lin Yang; Jiujun Zhang

    2015-01-01

    In this paper, a catalyst of hollow PdCu alloy nanocubes supported on nitrogen-doped graphene support (H-PdCu/ppy-NG) is successfully synthesized using a simple one-pot template-free method. Two other catalyst materials such as solid PdCu alloy particles supported on this same nitrogen-doped graphene support (PdCu/ppy-NG) and hollow PdCu alloy nanocubes supported on the reduced graphene oxide support (H-PdCu/RGO) are also prepared using the similar synthesis conditions for comparison. It is f...

  5. Pseudo template synthesis of poly (1-naphthylamine): effect of environment on nanostructured morphology

    International Nuclear Information System (INIS)

    Riaz, Ufana; Ahmad, Sharif; Ashraf, S. M.

    2008-01-01

    A template free approach was adopted to explore the effect of polymerization environment on the synthesis of nanostructured poly (1-naphthylamine) (PNA) using cupric chloride as oxidant and methyl alcohol as medium. The polymerization environment was varied by carrying out the synthesis in the presence of nitrogen and oxygen. The morphology of the synthesized nanostructured PNA was investigated using scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-vis and FT-IR spectroscopies. PNA nanorods of sizes varying between 50-100 nm were obtained in presence of nitrogen while in presence of oxygen, it formed aggregated globular particles of sizes varying between 80-100 nm. The results provide valuable information on controlling the synthesis of one-dimensional nanostructured conducting polymers that exhibit superior processibility as compared to the conventional conducting polymers.

  6. A strategy of combining SILAR with solvothermal process for In2S3 sensitized quantum dot-sensitized solar cells

    Science.gov (United States)

    Yang, Peizhi; Tang, Qunwei; Ji, Chenming; Wang, Haobo

    2015-12-01

    Pursuit of an efficient strategy for quantum dot-sensitized photoanode has been a persistent objective for enhancing photovoltaic performances of quantum dot-sensitized solar cell (QDSC). We present here the fabrication of the indium sulfide (In2S3) quantum dot-sensitized titanium dioxide (TiO2) photoanode by combining successive ionic layer adsorption and reaction (SILAR) with solvothermal processes. The resultant QDSC consists of an In2S3 sensitized TiO2 photoanode, a liquid polysulfide electrolyte, and a Co0.85Se counter electrode. The optimized QDSC with photoanode prepared with the help of a SILAR method at 20 deposition cycles and solvothermal method yields a maximum power conversion efficiency of 1.39%.

  7. CTAB-Assisted Solvothermal Growth and Optical Characterization of Flower-Like ZnS Structures

    Science.gov (United States)

    Roy, J. S.; Pal Majumder, T.

    2016-08-01

    Flower-like ZnS structures have been prepared by solvothermal method with the assistance of cetyl trimethyl ammonium bromide (CTAB). The effects of different experimental conditions on the morphology of ZnS structure have been investigated. The performances of ZnS structures have been analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), room temperature photoluminescence (PL), and UV-visible absorption spectroscopy. The XRD patterns indicate that the prepared ZnS structures are highly crystallized, which are of hexagonal phase. The SEM images indicate that the main role of CTAB is to assemble the ZnS flakes together to form the flower-like structures, and the reaction time affects the morphology of ZnS. The growth mechanism for the formation of flower-like ZnS structure is also described. The absorption and emission bands gradually shift towards longer wavelength due to the transformation of flower-like ZnS nanoflowers from ZnS flakes.

  8. Structure and optical properties of cubic gallium oxynitride synthesized by solvothermal route

    International Nuclear Information System (INIS)

    Oberländer, Andreas; Kinski, Isabel; Zhu, Wenliang; Pezzotti, Giuseppe; Michaelis, Alexander

    2013-01-01

    Cubic gallium oxynitride was synthesized using a solvothermal processing route. Crystal structure, chemical composition, optical properties and the influence of heat treatment in either reactive or inert atmospheres have been investigated. Despite a strongly distorted lattice revealed using X-ray diffraction, the Raman active modes of a cubic gallium oxynitride structure could be observed. With diffusive reflectance UV–Vis spectroscopy a band gap at around 4.8 eV has been observed. Additionally, cathodoluminescence spectroscopy exhibited observable luminescence caused by defect-related transitions within the optical gap. Cathodoluminescence and photoluminescence spectra collected after heat treatments showed significant changes in the defect structure. In particular, for annealing in ammonia the main spectral modifications were related to the substitution of oxygen by nitrogen on anion sites. - Graphical abstract: CL spectra of gallium oxynitride: As-prepared and heat-treated at temperatures of 500 °C in different atmospheres. Highlights: ► Raman spectrum of cubic gallium oxynitride. ► Experimental determination of optical band gap. ► Shift of band gap energy due to heat treatment. ► Nitrogen incorporation leads to deep level acceptor states. ► Red shifted luminescence spectrum

  9. Fabrication of Nanostructured TiO2 Using a Solvothermal Reaction for Lithium-ion Batteries

    Directory of Open Access Journals (Sweden)

    Jicai Liang

    2016-03-01

    Full Text Available Nanostructured TiO2 was successfully synthesized via a facile one-pot solvothermal reaction followed by calcina‐ tion. Hydrolysis and polycondensation of titanium butox‐ ide (Ti(OR4 were performed in the presence of sodium dodecylbenzenesulfonate (SDBS. The morphologies, crystallinity and compositions of obtained samples were identified by the methods of X-ray diffraction (XRD, Brunauer–Emmett–Teller (BET and transmission electron microscopy (TEM. It was found that the nanostructured TiO2 with an average diameter of 10±5 nm had the crystal type of anatase. A good specific surface was also obtained by the standard multipoint BET method (119.2 m2/g. As the anode materials for the lithium-ion batteries (LIBs, the anatase phase TiO2 demonstrated a relatively high gravi‐ metric specific capacity of 264.8 mAh g-1. The reversible capacity of TiO2 remained 196.4 mAh g-1 at a rate of 0.2 ̊C after 100 cycles. It indicated that this kind of TiO2 possessed a good electrochemical performance.

  10. Observation of magnetic anomalies in one-step solvothermally synthesized nickel-cobalt ferrite nanoparticles.

    Science.gov (United States)

    Datt, Gopal; Sen Bishwas, Mousumi; Manivel Raja, M; Abhyankar, A C

    2016-03-07

    Magnetic anomalies corresponding to the Verwey transition and reorientation of anisotropic vacancies are observed at 151 K and 306 K, respectively, in NiCoFe2O4 nanoparticles (NPs) synthesized by a modified-solvothermal method followed by annealing. Cationic disorder and spherical shape induced non-stoichiometry suppress the Verwey transition in the as-synthesized NPs. On the other hand, reorientation of anisotropic vacancies is quite robust. XRD and electron microscopy investigations confirm a single phase spinel structure and the surface morphology of the as-synthesized NPs changes from spherical to octahedral upon annealing. Rietveld analysis reveals that the Ni(2+) ions migrate from tetrahedral (A) to octahedral (B) sites upon annealing. The Mössbauer results show canted spins in both the NPs and the strength of superexchange is stronger in Co-O-Fe than Ni-O-Fe. Magnetic force images show that the as-synthesised NPs are single-domain whereas the annealed NPs are multi-domain octahedral particles. The FMR study reveals that both the NPs have a broad FMR line-width; and resonance properties are consistent with the random anisotropy model. The broad inhomogeneous FMR line-width, observation of the Verwey transition, tuning of the magnetic domain structure as well as the magnetic properties suggest that the NiCoFe2O4 ferrite NPs may be promising for future generation spintronics, magneto-electronics, and ultra-high-density recording media as well as for radar absorbing applications.

  11. Near UV excitable Eu-doped alumina nanophosphors synthesized by the microwave assisted solvothermal technique

    Science.gov (United States)

    Padilla-Rosales, I.; Cabañas-Moreno, J. G.; Jiménez, G. L.; Aguilar-Frutis, M. A.; Alarcón-Flores, G.; Falcony, C.

    2017-12-01

    Europium doped alumina nanophosphors have been synthesized by the microwave assisted solvothermal technique. The dependence of the photoluminescence response and structural features of these nanophosphors on the europium content and annealing temperature has been characterized for a wide range of compositions and thermal treatments. The nanophosphors are composed of a mixture of nanocrystalline γ-Al2O3 and EuAlO3, in addition to an amorphous alumina phase. The relative quantities of each phase depend on both the europium content and the annealing temperature. High europium content and/or annealing temperature lead to larger fractions of EuAlO3 nanocrystals having with poor luminescence characteristics, while lower temperatures and europium contents result in the predominance of γ-Al2O3 nanocrystals and amorphous alumina, showing much more efficient luminescent emission. The luminescence spectra from all samples show the characteristic red emission peaks from the Eu3+ ion associated with inter-electronic energy level transitions. However, the excitation spectra in these nanophosphors are dominated, by the 7F0–5L6 transition (395 nm), as opposed to the dominant charge-transfer related band at ~260 nm commonly reported for this material. The highest luminescence intensity was obtained for nanophosphors doped with 7.5 at.% of Eu, annealed at 900 °C, which exhibits a quantum yield of 45% when excited with 395 nm light.

  12. Assessment of CASP7 structure predictions for template free targets.

    Science.gov (United States)

    Jauch, Ralf; Yeo, Hock Chuan; Kolatkar, Prasanna R; Clarke, Neil D

    2007-01-01

    In CASP7, protein structure prediction targets that lacked substantial similarity to a protein in the PDB at the time of assessment were considered to be free modeling targets (FM). We assessed predictions for 14 FM targets as well as four other targets that were deemed to be on the borderline between FM targets and template based modeling targets (TBM/FM). GDT_TS was used as one measure of model quality. Model quality was also assessed by visual inspection. Visual inspection was performed by three independent assessors who were blinded to GDT_TS scores and other quantitative measures of model quality. The best models by visual inspection tended to rank among the top few percent by GDT_TS, but were typically not the highest scoring models. Thus, visual inspection remains an essential component of assessment for FM targets. Overall, group TS020 (Baker) performed best, but success on individual targets was widely distributed among many groups. Among these other groups, TS024 and TS025 (Zhang and Zhang server) performed notably well without exceptionally large computing resources. This should be considered encouraging for future CASPs. There was a sense of progress in template FM relative to CASP6, but we were unable to demonstrate this progress objectively. (c) 2007 Wiley-Liss, Inc.

  13. A simple solvothermal process for fabrication of a metal-organic framework with an iron oxide enclosure for the determination of organophosphorus pesticides in biological samples.

    Science.gov (United States)

    Zhang, Suling; Jiao, Zhe; Yao, Weixuan

    2014-12-05

    An active magnetic metal-organic framework (MOF) hybrid material was prepared using a novel in situ solvothermal method in the presence of magnetite (Fe3O4) particles, that holds much promise for large-scale synthesis. MIL-101(Fe), an iron terephthalate with pore structure and high resistance to water and common solvents, was functionalized as a model with superparamagnetic qualities, using Fe3O4. The electrostatic interaction between Fe3O4 and metal ions was thereby used to chemically stabilize magnetic nanoparticles, and thus MOF crystals were uniformly enclosed by Fe3O4 to form a homogeneous magnetic product identified as a Fe3O4/MIL-101 composite. This hybrid material with magnetic susceptibility but with the lowest possible loading amount of Fe3O4 was examined, and its potential application for magnetic solid-phase extraction of six organophosphorus pesticides (OPPs) from human hair and urine samples, followed by gas chromatography analysis, was assessed. The main effect parameters including solution ionic strength, desorption solvent, extraction time and desorption time were investigated in sequence. Under optimized conditions, this method showed low detection limits (0.21-2.28 ng/mL), wide linearity, and good precision (1.8-8.7% for intra-day, 2.9-9.4% for inter-day). The matrix interference produced by hair or urine could be effectively eliminated using this method, and satisfactory recoveries of the spiked samples were 76.8-94.5% and 74.9-92.1%, respectively, indicating that the Fe3O4/MIL-101 sorbents are feasible for the analysis of trace analytes from biological samples. Copyright © 2014. Published by Elsevier B.V.

  14. Novel multiform morphologies of hydroxyapatite: Synthesis and growth mechanism

    Energy Technology Data Exchange (ETDEWEB)

    Mary, I. Reeta [Department of Nanoscience and Technology, Bharathiar University, Coimbatore 641046 (India); Department of Physics, Government Arts College, Coimbatore 641018 (India); Sonia, S.; Viji, S.; Mangalaraj, D.; Viswanathan, C. [Department of Nanoscience and Technology, Bharathiar University, Coimbatore 641046 (India); Ponpandian, N., E-mail: ponpandian@buc.edu.in [Department of Nanoscience and Technology, Bharathiar University, Coimbatore 641046 (India)

    2016-01-15

    Graphical abstract: - Highlights: • Novel multiform morphologies of hydroxyapatite from nanoscale building blocks. • Facile hydro/solvothermal method under mild reaction conditions without the necessity of post-annealing treatment. • Growth mechanism by Ostwald ripening and self-assembly processes. - Abstract: Morphological evolution of materials becomes a prodigious challenge due to their key role in defining their functional properties and desired applications. Herein, we report the synthesis of hydroxyapatite (HAp) microstructures with multiform morphologies, such as spheres, cubes, hexagonal rods and nested bundles constructed from their respective nanoscale building blocks via a simple cost effective hydro/solvothermal method. A possible formation mechanism of diverse morphologies of HAp has been presented. Structural analysis based on X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy confirms the purity of the HAp microstructures. The multiform morphologies of HAp were corroborated by using Field emission scanning electron microscope (FESEM).

  15. Novel multiform morphologies of hydroxyapatite: Synthesis and growth mechanism

    International Nuclear Information System (INIS)

    Mary, I. Reeta; Sonia, S.; Viji, S.; Mangalaraj, D.; Viswanathan, C.; Ponpandian, N.

    2016-01-01

    Graphical abstract: - Highlights: • Novel multiform morphologies of hydroxyapatite from nanoscale building blocks. • Facile hydro/solvothermal method under mild reaction conditions without the necessity of post-annealing treatment. • Growth mechanism by Ostwald ripening and self-assembly processes. - Abstract: Morphological evolution of materials becomes a prodigious challenge due to their key role in defining their functional properties and desired applications. Herein, we report the synthesis of hydroxyapatite (HAp) microstructures with multiform morphologies, such as spheres, cubes, hexagonal rods and nested bundles constructed from their respective nanoscale building blocks via a simple cost effective hydro/solvothermal method. A possible formation mechanism of diverse morphologies of HAp has been presented. Structural analysis based on X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy confirms the purity of the HAp microstructures. The multiform morphologies of HAp were corroborated by using Field emission scanning electron microscope (FESEM).

  16. Continuous microwave flow synthesis of mesoporous hydroxyapatite

    Energy Technology Data Exchange (ETDEWEB)

    Akram, Muhammad; Alshemary, Ammar Z.; Goh, Yi-Fan; Wan Ibrahim, Wan Aini [Department of Chemistry, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor (Malaysia); Lintang, Hendrik O. [Centre for Sustainable Nanomaterials (CSNano), Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor (Malaysia); Hussain, Rafaqat, E-mail: rafaqat@kimia.fs.utm.my [Centre for Sustainable Nanomaterials (CSNano), Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor (Malaysia)

    2015-11-01

    We have successfully used continuous microwave flow synthesis (CMFS) technique for the template free synthesis of mesoporous hydroxyapatite. The continuous microwave flow reactor consisted of a modified 2.45 GHz household microwave, peristaltic pumps and a Teflon coil. This cost effective and efficient system was exploited to produce semi-crystalline phase pure nano-sized hydroxyapatite. Effect of microwave power, retention time and the concentration of reactants on the phase purity, degree of crystallinity and surface area of the final product was studied in detail. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) were used to study the phase purity and composition of the product, while transmission electron microscopy (TEM) was used to study the effect of process parameters on the morphology of hydroxyapatite. The TEM analysis confirmed the formation of spherical particles at low microwave power; however the morphology of the particles changed to mesoporous needle and rod-like structure upon exposing the reaction mixture to higher microwave power and longer retention time inside the microwave. The in-vitro ion dissolution behavior of the as synthesized hydroxyapatite was studied by determining the amount of Ca{sup 2+} ion released in SBF solution. - Highlights: • Continuous microwave flow synthesis method was used to prepare hydroxyapatite. • Increase in microwave power enhanced the degree of crystallinity. • TEM images confirmed the presence of mesopores on the surface of HA.

  17. Continuous microwave flow synthesis of mesoporous hydroxyapatite

    International Nuclear Information System (INIS)

    Akram, Muhammad; Alshemary, Ammar Z.; Goh, Yi-Fan; Wan Ibrahim, Wan Aini; Lintang, Hendrik O.; Hussain, Rafaqat

    2015-01-01

    We have successfully used continuous microwave flow synthesis (CMFS) technique for the template free synthesis of mesoporous hydroxyapatite. The continuous microwave flow reactor consisted of a modified 2.45 GHz household microwave, peristaltic pumps and a Teflon coil. This cost effective and efficient system was exploited to produce semi-crystalline phase pure nano-sized hydroxyapatite. Effect of microwave power, retention time and the concentration of reactants on the phase purity, degree of crystallinity and surface area of the final product was studied in detail. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) were used to study the phase purity and composition of the product, while transmission electron microscopy (TEM) was used to study the effect of process parameters on the morphology of hydroxyapatite. The TEM analysis confirmed the formation of spherical particles at low microwave power; however the morphology of the particles changed to mesoporous needle and rod-like structure upon exposing the reaction mixture to higher microwave power and longer retention time inside the microwave. The in-vitro ion dissolution behavior of the as synthesized hydroxyapatite was studied by determining the amount of Ca 2+ ion released in SBF solution. - Highlights: • Continuous microwave flow synthesis method was used to prepare hydroxyapatite. • Increase in microwave power enhanced the degree of crystallinity. • TEM images confirmed the presence of mesopores on the surface of HA

  18. One dimensional well-aligned CdO nanocrystal by solvothermal method

    International Nuclear Information System (INIS)

    Kaviyarasu, K.; Manikandan, E.; Paulraj, P.; Mohamed, S.B.; Kennedy, J.

    2014-01-01

    Graphical abstract: - Highlights: • Cadmium oxide (CdO) emerged as one of the important semiconducting materials. • Iodine concentration increases intensity of the peak around 300 cm −1 becomes stronger. • Surface morphology of these crystals has been modified by varying complexing agent. • Nanofibers structure like CdO crystals first time achieved. • The diameters of these nanofibers range mostly between 40 nm and 70 nm. - Abstract: Cadmium oxide (CdO) is a category of the practical semiconductor metal oxides, which is widely applied in various scientific and industrial fields because of its catalytic, optical, and electrical properties. CdO nanocrystal was successfully synthesized by a virtue of a single source precursor method at mild reaction conditions between cadmium oxide, and element iodine by a solvothermal route. X-ray powder diffraction (XRD), ultraviolet spectroscopy studies (UV–vis), Fourier Transform Infrared analysis (FTIR), scanning electron microscopy (SEM), μ-Raman spectroscopy and cyclic voltammogram (CV) were used to characterize the CdO nanocrystals. The ultra-violet visible absorption peaks of CdO exhibited a large blue shift and the luminescent spectra had a strong and broad emission band centered at 228 nm. The various functional groups present in the CdO nanocrystals were identified by FTIR analysis. Intense PL was also observed with some spectral tuning possibly giving a range of emission photon energies approximately spanning from 2.5 to 3.4 eV. Scanning electron microscopy and μ-Raman microscopy images indicated that the morphology of the product is spherical nanoparticles with an average particle size of 46 nm with standard deviation. The electrochemical response of CdO which is proved the nano-cadmium has high functionality due to the small size and it has higher electrochemical activity without any modifications. The above studies demonstrate the potential for the utilization of cadmium nitrite nanocrystal in visible

  19. Efficient solvothermal wet in situ transesterification of Nannochloropsis gaditana for biodiesel production.

    Science.gov (United States)

    Kim, Bora; Chang, Yong Keun; Lee, Jae W

    2017-05-01

    In situ transesterification of wet microalgae is a promising, simplified alternative biodiesel production process that replaces multiple operations of cell drying, extraction, and transesterification reaction. This study addresses enhanced biodiesel production from Nannochloropsis gaditana at elevated temperatures. Compared with the previously reported in situ transesterification process of conducting the reaction at a temperature ranging from 95 to 125 °C, the present work employs higher temperatures of at least 150 °C. This relatively harsh condition allows much less acid catalyst with or without co-solvent to be used during this single extraction-conversion process. Without any co-solvent, 0.58% (v/v) of H 2 SO 4 in the reaction medium can achieve 90 wt% of the total lipid conversion to biodiesel at 170 °C when the moisture content of wet algal paste is 80 wt%. Here, the effects of temperature, acid catalyst, and co-solvent on the FAEE yield and specification were scrutinized, and the reaction kinetic was investigated to understand the solvothermal in situ transesterification reaction at the high temperature. Having a biphasic system (water/chloroform) during the reaction also helped to meet biodiesel quality standard EN 14214, as Na + , K + , Ca 2+ , Mg 2+ cations and phosphorus were detected only below 5 ppm. With highlights on the economic feasibility, wet in situ transesterification at the high temperature can contribute to sustainable production of biodiesel from microalgae by reducing the chemical input and relieve the burden of extensive post purification process, therefore a step towards green process.

  20. One dimensional well-aligned CdO nanocrystal by solvothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Kaviyarasu, K., E-mail: kaviyarasuloyolacollege@gmail.com [Materials Research Centre, Department of Physics, St. Xavier’s College, Tirunelveli (India); Manikandan, E., E-mail: maniphysics@gmail.com [Nano Research Centre, Department of Physics, B.S. Abdur Rahman University, Chennai (India); UNESCO–UNISA AFNET in Nanosciences/Nanotechnology Laboratories, Materials Research Department, iThemba LABS–National Research Foundation (NRF) (South Africa); Paulraj, P. [Department of Chemistry, B.S. Abdur Rahman University, Chennai (India); Mohamed, S.B. [Department of Mechanical Engineering, B.S. Abdur Rahman University, Chennai (India); Kennedy, J. [National Isotope Centre, GNS Science, Lower Hutt (New Zealand)

    2014-04-01

    Graphical abstract: - Highlights: • Cadmium oxide (CdO) emerged as one of the important semiconducting materials. • Iodine concentration increases intensity of the peak around 300 cm{sup −1} becomes stronger. • Surface morphology of these crystals has been modified by varying complexing agent. • Nanofibers structure like CdO crystals first time achieved. • The diameters of these nanofibers range mostly between 40 nm and 70 nm. - Abstract: Cadmium oxide (CdO) is a category of the practical semiconductor metal oxides, which is widely applied in various scientific and industrial fields because of its catalytic, optical, and electrical properties. CdO nanocrystal was successfully synthesized by a virtue of a single source precursor method at mild reaction conditions between cadmium oxide, and element iodine by a solvothermal route. X-ray powder diffraction (XRD), ultraviolet spectroscopy studies (UV–vis), Fourier Transform Infrared analysis (FTIR), scanning electron microscopy (SEM), μ-Raman spectroscopy and cyclic voltammogram (CV) were used to characterize the CdO nanocrystals. The ultra-violet visible absorption peaks of CdO exhibited a large blue shift and the luminescent spectra had a strong and broad emission band centered at 228 nm. The various functional groups present in the CdO nanocrystals were identified by FTIR analysis. Intense PL was also observed with some spectral tuning possibly giving a range of emission photon energies approximately spanning from 2.5 to 3.4 eV. Scanning electron microscopy and μ-Raman microscopy images indicated that the morphology of the product is spherical nanoparticles with an average particle size of 46 nm with standard deviation. The electrochemical response of CdO which is proved the nano-cadmium has high functionality due to the small size and it has higher electrochemical activity without any modifications. The above studies demonstrate the potential for the utilization of cadmium nitrite nanocrystal in

  1. Facile synthesis and reversible lithium insertion studies on hydrated iron trifluoride FeF3·0.33H2O

    Science.gov (United States)

    Rao, R. S.; Pralong, V.; Varadaraju, U. V.

    2016-05-01

    An original synthesis method for the synthesis of hydrated iron trifluoride is presented. This method, based on solvothermal process starting from iron salt and HF in alcool, is economic and simple. The electrochemical performances of the composite phase FeF3·0.33H2O/Graphitic oxide is showing enhanced capacity of 250 mAh/g at 0.05 °C.

  2. Facile synthesis of flexible macroporous polypropylene sponges for separation of oil and water

    Science.gov (United States)

    Wang, Guowei; Uyama, Hiroshi

    2016-02-01

    Oil spill disasters always occur accidentally, accompanied by the release of plenty of crude oil that could spread quickly over a wide area, creating enormous damage to the fragile marine ecological system. Therefore, the facile large-scale synthesis of hydrophobic three-dimensional (3-D) porous sorbents from low cost raw materials is in urgent demand. In this study, we report the facile template-free synthesis of polypropylene (PP) sponge by using a thermally-induced phase separation (TIPS) technique. The obtained sponge showed macroporous structure, excellent mechanical property, high hydrophobicity, and superoleophilicity. Oil could be separated from an oil/water mixture by simple immersing the sponge into the mixture and subsequent squeezing the sponge. All of these features make this sponge the most promising oil sorbent that will replace commercial non-woven PP fabrics.

  3. Metal Acetylacetonates as General Precursors for the Synthesis of Early Transition Metal Oxide Nanomaterials

    OpenAIRE

    Willis, Amanda L.; Chen, Zhuoying; He, Jiaqing; Zhu, Yimei; Turro, Nicholas J.; O'Brien, Stephen

    2007-01-01

    A versatile, convenient, and nontoxic solvothermal method for the synthesis of nanocrystalline iron, chromium, and manganese oxides is described. This method employs the reactions of metal acetylacetonate precursors and oxygen-containing solvents in a reaction to prepare metal oxide nanoparticles. Characterization of these nanocrystalline materials was carried out employing transmission electron microscopy (TEM), high-resolution TEM (HRTEM), X-ray diffraction (XRD), and elemental analysis.

  4. Metal Acetylacetonates as General Precursors for the Synthesis of Early Transition Metal Oxide Nanomaterials

    Directory of Open Access Journals (Sweden)

    Amanda L. Willis

    2007-01-01

    Full Text Available A versatile, convenient, and nontoxic solvothermal method for the synthesis of nanocrystalline iron, chromium, and manganese oxides is described. This method employs the reactions of metal acetylacetonate precursors and oxygen-containing solvents in a reaction to prepare metal oxide nanoparticles. Characterization of these nanocrystalline materials was carried out employing transmission electron microscopy (TEM, high-resolution TEM (HRTEM, X-ray diffraction (XRD, and elemental analysis.

  5. Preparation of flower-like CuS by solvothermal method and its photodegradation and UV protection

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Xiao-Sai; Shen, Yong, E-mail: shenyong@sues.edu.cn; Xu, Li-Hui; Wang, Li-Ming; Xing, Ya-Jun

    2016-07-25

    The flower-like CuS with hierarchical structures were synthesized by a solvothermal method. X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, UV–vis optical absorption spectroscopy and thermogravimetric analysis (TGA) and ultraviolet transmittance analyzer labsphere were used to characterize the as-prepared products. The results of photocatalytic degradation of Methylene blue (MB) demonstrated that the as-prepared flower-like CuS possessed high photocatalytic performance in UV and visible range and its band gap was 1.45 eV. The degradation rate of MB by CuS with the absence of H{sub 2}O{sub 2} was 98.23% and 100% under xenon lamp and Mercury tungsten blended lamp for 30 min, respectively. And a new approach for ultraviolet (UV) protection of cotton fabrics treated by flower-like CuS microspheres was innovatively investigated and the results showed that flower-like CuS was a good UV resistant material. - Highlights: • The flower-like CuS was prepared via solvothermal method. • The as-prepared CuS showed better photodegradation of MB solution under visible region. • The cotton fabric treated by the obtained flower-like CuS was proved to have a potential application in anti-UV field.

  6. Simple synthesis of porous melamine-formaldehyde resins by low temperature solvothermal method and its CO2 adsorption properties

    Directory of Open Access Journals (Sweden)

    F. Yin

    2017-11-01

    Full Text Available A simple and environmentally-friendly approach for the preparation of porous melamine-formaldehyde resins (PMFRs was developed by using low-boiling-point solvents, such as water, as pore-forming agent. With using dimethyl sulfoxide (DMSO and low-boiling solvents cosolvent method, PMFRs with a high specific surface area and well-defined pore structure can be synthesized at a low reaction temperature of 140 °C for a short reaction duration in 20 hours, which can replace the conventional methods that use dimethyl sulfoxide (DMSO as reaction medium and require 3 days at 170 °C to achieve similar surface area. When loaded with polyethylenimine (PEI, the PMFR-PEI-30% showed good CO2 adsorption performance with a capacity of up to 2.89 mmol/g at 30 °C. These results bring new perspectives for the development of lowcost and environmentally-friendly synthetic methods for porous materials, which can boost their widespread applications.

  7. Dialkylamide as Both Capping Agent and Surfactant in a Direct Solvothermal Synthesis of Magnetite and Titania Nanoparticles

    Czech Academy of Sciences Publication Activity Database

    Cara, C.; Musinu, A.; Mameli, V.; Ardu, A.; Nižňanský, D.; Buršík, Josef; Scorciapino, M. A.; Manzo, G.; Cannas, C.

    2015-01-01

    Roč. 15, č. 5 (2015), s. 2364-2372 ISSN 1528-7483 R&D Projects: GA ČR(CZ) GA14-18392S Institutional support: RVO:61388980 Keywords : Nanomagnetics * Nanoparticles * Nuclear magnetic resonance * Fourier transform infrared spectroscopy Subject RIV: CA - Inorganic Chemistry Impact factor: 4.425, year: 2015

  8. Continuous Solvothermal Synthesis and Surface Treatment for Improved and Scalable Processing of Ultra High Temperature Ceramic (UHTC) Nanopowders

    Science.gov (United States)

    2017-06-13

    The pressure-temperature relationship of Benzene in the high pressure reactor ... .. ...... ... 17 FTIR of commercial ZrB2 nanopowders and results...ZrCLJCCl,JNa. The identity of sharp absorbance at 1720 and 690 after heating the product to 1000 and 1500 °C is not clear...reacted first; BN7 = 1:2; BN8 = 1:2 with cat. ........................................................... 49 Figure 35. FTIR of polymer pyrolyzed in Ar

  9. Conducting polymer nanofibers: Synthesis, properties and applications

    Science.gov (United States)

    Huang, Jiaxing

    An interfacial polymerization method is described which enables the synthesis of polyaniline nanofibers with diameters tunable from 30 to 120 nm. This synthesis is template-free and readily scalable and can be applied to polyaniline derivatives and other conjugated polymers. Mechanistic studies reveal that nanofibers form naturally during the chemical oxidative polymerization of aniline in water without the need for any template, functional molecule or seed. In conventional polymerization, nanofibers are subject to secondary growth of amorphous particles which leads to irregularly shaped agglomerates. The key to producing pure nanofibers is to suppress secondary growth. This has been achieved with interfacial polymerization where the interface separates nanofiber formation from secondary growth and also by using rapidly mixed reactions where the initiator molecules are consumed before secondary growth begins. Polyaniline nanofibers dramatically enhance many applications of conventional polyaniline, such as in chemical sensors. Here, the small diameter, high surface area and water dispersibility of the nanofibers enable improved sensor performance and new sensing mechanisms. The nanofibers can also serve as a template to grow inorganic/polyaniline nanocomposites. Polyaniline nanofibers with 1--5 nm gold nanoparticles possess exciting applications such as in electronic non-volatile memory devices. Additionally, a novel flash welding technique for the nanofibers has been invented. A photographic camera flash sets off cross-linking reactions that can be used to make asymmetric polymer membranes, form patterned nanofiber films and create polymer based nanocomposites.

  10. Hollow Micro-/Nanostructures: Synthesis and Applications

    KAUST Repository

    Lou, Xiong Wen (David)

    2008-11-03

    Hollow micro-nanostructures are of great interest in many current and emerging areas of technology. Perhaps the best-known example of the former is the use of fly-ash hollow particles generated from coal power plants as partial replacement for Portland cement, to produce concrete with enhanced strength and durability. This review is devoted to the progress made in the last decade in synthesis and applications of hollow micro-nanostructures. We present a comprehensive overview of synthetic strategies for hollow structures. These strategies are broadly categorized into four themes, which include well-established approaches, such as conventional hard-templating and soft-templating methods, as well as newly emerging methods based on sacrificial templating and template-free synthesis. Success in each has inspired multiple variations that continue to drive the rapid evolution of the field. The Review therefore focuses on the fundamentals of each process, pointing out advantages and disadvantages where appropriate. Strategies for generating more complex hollow structures, such as rattle-type and nonspherical hollow structures, are also discussed. Applications of hollow structures in lithium batteries, catalysis and sensing, and biomedical applications are reviewed. © 2008 WILEY-VCH Verlag GmbH & Co. KGaA,.

  11. Continuous microwave flow synthesis of mesoporous hydroxyapatite.

    Science.gov (United States)

    Akram, Muhammad; Alshemary, Ammar Z; Goh, Yi-Fan; Wan Ibrahim, Wan Aini; Lintang, Hendrik O; Hussain, Rafaqat

    2015-11-01

    We have successfully used continuous microwave flow synthesis (CMFS) technique for the template free synthesis of mesoporous hydroxyapatite. The continuous microwave flow reactor consisted of a modified 2.45GHz household microwave, peristaltic pumps and a Teflon coil. This cost effective and efficient system was exploited to produce semi-crystalline phase pure nano-sized hydroxyapatite. Effect of microwave power, retention time and the concentration of reactants on the phase purity, degree of crystallinity and surface area of the final product was studied in detail. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) were used to study the phase purity and composition of the product, while transmission electron microscopy (TEM) was used to study the effect of process parameters on the morphology of hydroxyapatite. The TEM analysis confirmed the formation of spherical particles at low microwave power; however the morphology of the particles changed to mesoporous needle and rod-like structure upon exposing the reaction mixture to higher microwave power and longer retention time inside the microwave. The in-vitro ion dissolution behavior of the as synthesized hydroxyapatite was studied by determining the amount of Ca(2+) ion released in SBF solution. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Synthesis and growth mechanism of Bi2S3 nanoribbons.

    Science.gov (United States)

    Liu, Zhaoping; Liang, Jianbo; Li, Shu; Peng, Sheng; Qian, Yitai

    2004-02-06

    This article describes a facile solvothermal method by using mixed solvents for the large-scale synthesis of Bi(2)S(3) nanoribbons with lengths of up to several millimeters. These nanoribbons were formed by a solvothermal reaction between Bi(III)-glycerol complexes and various sulfur sources in a mixed solution of aqueous NaOH and glycerol. HRTEM (high-resolution transmission electron microscopy) and SAED (selective-area electron diffraction) studies show that the as-synthesized nanoribbons had predominately grown along the [001] direction. The Bi(2)S(3) nanoribbons prepared by the use of different sulfur sources have a common formation process: the initial formation of NaBiS(2) polycrystals, which serve as the precursors to Bi(2)S(3), the decomposition of NaBiS(2), and the formation of Bi(2)S(3) seeds in the solution through a homogeneous nucleation process; the growth of Bi(2)S(3) nanoribbons occurs at the expense of NaBiS(2) materials. The growth mechanism of millimeter-scale nanoribbons involves a special solid-solution-solid transformation as well as an Ostwald ripening process. Some crucial factors affect nanoribbon growth, such as, solvothermal temperature, volume ratio of glycerol to water, and the concentration of NaOH; these have also been discussed.

  13. Comparison of Two Novel Solution-Based Routes for the Synthesis of Equiaxed ZnO Nanoparticles

    Directory of Open Access Journals (Sweden)

    K. Elen

    2011-01-01

    Full Text Available Due to a dominant one-dimensional growth rate, nanoparticles of zinc oxide often show a rodlike morphology. As a result, the synthesis of small spherical nanoparticles of undoped ZnO remains challenging. This paper presents two procedures that successfully produce a powder consisting of equiaxed zinc oxide nanoparticles: one using a polyethylene glycol- (PEG- assisted solvothermal method and the other by calcination of zinc oxalate obtained from a microemulsion-mediated method. In the latter, zinc-substituted aerosol OT (AOT is used as a surfactant. The samples are characterized by inductively coupled plasma-atomic emission spectroscopy (ICP-AES, thermogravimetric analysis (TGA, X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FTIR, transmission electron microscopy (TEM, photon correlation spectroscopy (PCS, and photoluminescence (PL spectroscopy. Both synthesis techniques produce nanoparticles with similar sizes in the range of 10 to 20 nm. Dense aggregates observed in the calcined powder are infrequent in the case of the solvothermal method.

  14. Morphology-controlled synthesis of Ti3+ self-doped yolk–shell structure titanium oxide with superior photocatalytic activity under visible light

    International Nuclear Information System (INIS)

    Wang, Shixiong; Yang, Xiangjun; Wang, Yapeng; Liu, Lixiang; Guo, Yuanyuan; Guo, Hong

    2014-01-01

    Ti 3+ self-doped yolk–shell structure titanium oxide nanoparticle aggregates are fabricated through an environmental template-free route and the reduction reaction at low temperature subsequently. After the Ti 3+ doping, the reduced TiO 2 sample exhibits a wide visible-light absorption ranged from 400 nm to 800 nm. The intrinsic hollow core–shell microstructure can make multiple reflections of light within the chamber, and thus results in more efficient use of the light source compared with solid structure. Besides, the large surface area can render the sample with a high activity. Therefore, Ti 3+ self-doped yolk–shell structure titanium oxide exhibits a superior photocatalytic activity under visible light. This strategy is simple, cheap and mass-productive, which may shed light on a new avenue for large scale production of self-doped yolk–shell structural nano functional materials for catalyst, sensors, energy storage and other new applications. - Graphical abstract: A facile generic strategy is employed to prepare Ti 3+ self-doped yolk–shell structure titanium oxide nanoparticle aggregates with the superior photocatalytic activity under visible light. - Highlights: • Yolk–shell TiO 2 mesospheres are synthesized by solvothermal alcoholysis. • Ti 3+ self-doped yolk–shell structure titanium oxide is obtained at low temperature. • It exhibits a remarkable photocatalytic activity

  15. Solvothermal preparation of ZnO nanorods as anode material for improved cycle life Zn/AgO batteries.

    Directory of Open Access Journals (Sweden)

    Shafiq Ullah

    Full Text Available Nano materials with high surface area increase the kinetics and extent of the redox reactions, thus resulting in high power and energy densities. In this study high surface area zinc oxide nanorods have been synthesized by surfactant free ethylene glycol assisted solvothermal method. The nanorods thus prepared have diameters in the submicron range (300 ~ 500 nm with high aspect ratio. They have uniform geometry and well aligned direction. These nanorods are characterized by XRD, SEM, Specific Surface Area Analysis, solubility in alkaline medium, EDX analysis and galvanostatic charge/discharge studies in Zn/AgO batteries. The prepared zinc oxide nanorods have low solubility in alkaline medium with higher structural stability, which imparts the improved cycle life stability to Zn/AgO cells.

  16. Upconversion study of singly activator ions doped La2O3 nanoparticle synthesized via optimized solvothermal method

    Science.gov (United States)

    Tiwari, S. P.; Singh, S.; Kumar, A.; Kumar, K.

    2016-05-01

    In present work, an optimized solvothermal method has been chosen to synthesize the singly doped Er3+ activator ions with La2O3 host matrix. The sample is annealed at 500 °C in order to remove the moisture and other organic impurities. The sample is characterized by using XRD and FESEM to find out the phase and surface morphology. The observed particle size is found almost 80 nm with spherical agglomerated shape. Upconversion spectra are recorded at room temperature using 976 nm diode laser excitation sources and consequently the emission peaks in green and red region are observed. The color coordinate diagram shows the results that the present material may be applicable in different light emitting sources.

  17. Innovative biofilm inhibition and anti-microbial behavior of molybdenum sulfide nanostructures generated by microwave-assisted solvothermal route

    Science.gov (United States)

    Qureshi, Nilam; Patil, Rajendra; Shinde, Manish; Umarji, Govind; Causin, Valerio; Gade, Wasudev; Mulik, Uttam; Bhalerao, Anand; Amalnerkar, Dinesh P.

    2015-03-01

    The incessant use of antibiotics against infectious diseases has translated into a vicious circle of developing new antibiotic drug and its resistant strains in short period of time due to inherent nature of micro-organisms to alter their genes. Many researchers have been trying to formulate inorganic nanoparticles-based antiseptics that may be linked to broad-spectrum activity and far lower propensity to induce microbial resistance than antibiotics. The way-out approaches in this direction are nanomaterials based (1) bactericidal and (2) bacteriostatic activities. We, herein, present hitherto unreported observations on microbial abatement using non-cytotoxic molybdenum disulfide nanostructures (MSNs) which are synthesized using microwave assisted solvothermal route. Inhibition of biofilm formation using MSNs is a unique feature of our study. Furthermore, this study evinces antimicrobial mechanism of MSNs by reactive oxygen species (ROS) dependent generation of superoxide anion radical via disruption of cellular functions.

  18. Half opened microtubes of NaYF 4:Yb,Er synthesized in reverse microemulsion under solvothermal condition

    Science.gov (United States)

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

    2010-10-01

    NaYF 4:Yb,Er micro/nanocrystals with different sizes and morphologies such as nanospheres, short flexural nanorods, and half opened microtubes, were synthesized in reverse microemulsion under solvothermal condition using the quaternary reverse microemulsion system, CTAB/1-butanol/cyclohexane/aqueous solution. The X-ray diffraction analysis confirmed that cubic phase NaYF 4:Yb,Er can completely transform to hexagonal phase with increasing reaction time. The scanning electron microscope and transmission electron microscope images revealed that the morphology of the product can be tailored by varying the reaction time. A possible crystalline growth process of the NaYF 4:Yb,Er micro/nanocrystals was discussed. The obtained half opened microtubes exhibited an intense green upconversion luminescence, which may be attractive in novel optoelectronic devices.

  19. Preparation of flower-like CuS by solvothermal method for photocatalytic, UV protection and EMI shielding applications

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Xiao-Sai; Shen, Yong, E-mail: shenyong@sues.edu.cn; Xu, Li-Hui; Wang, Li-Ming; Lu, Li-sha; Zhang, Ya-ting

    2016-11-01

    Highlights: • The flower-like CuS was synthesized by a facil solvothermal method. • The as-prepared flower-like CuS showed better solar light-driven photocatalytic activity. • The as-prepared CuS could act as a novel UV blocker. • The flower-like CuS potentially hold promise as electromagnetic shielding material. - Abstract: The flower-like CuS hierarchical structures were synthesized by solvothermal method. The as-prepared products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared(FTIR) spectroscopy, UV–vis optical absorption spectroscopy and thermogravimetric analysis (TGA). The results demonstrated that the as-prepared flower-like CuS with the diameter of 1–5 um was pure hexagonal phase CuS and had well-defined flower-like structures. (1) The as-prepared CuS was proved to possess high photocatalytic performance with band gap of 1.45 eV. The degradation rate of Methylene blue (MB) was up to, 98.26%, 100% after 30 min under UV and visible irradiation. (2)The UPF of cotton fabric treated with CuS reached up to 174 compared with the original untreated fabric with the UPF 20.62. (3) The electromagnetic interference shielding effectiveness (EMI SE) of CuS coating was up to 27–31 dB when the content of CuS increased to 28.6%wt in the frequency of 300 KHz–3 GHz. Furthermore, the influence of reaction conditions on the morphology of the as-prepared CuS was investigated systematically and the possible formation mechanism of the CuS hierarchical structure was also proposed.

  20. Controlling the morphology and properties of solvothermal synthesized Cu2ZnSnS4 nanoparticles by solvent type

    International Nuclear Information System (INIS)

    Bahramzadeh, Saeid; Abdizadeh, Hossein; Golobostanfard, Mohammad Reza

    2015-01-01

    Highlights: • CZTS nanoparticles are fabricated by solvothermal method with different solvents. • Different morphologies are achieved by EDA, TETA, EG, and OA solvents. • Property and chelating ability of the solvents have a key role on nanoparticles formation. • TETA and OA are strongly recommended for solar cell applications. - Abstract: The copper–zinc–tin sulfide Cu 2 ZnSnS 4 (CZTS) semiconductors are recently considered as one of the favorable materials for application as absorber layers in solar cells due to their appropriate direct band gap energy and high optical absorption coefficient. In this study, the effect of solvent type on properties of solvothermal synthesized CZTS nanoparticles has been investigated. Ethylenediamine (EDA), triethylenetetramine (TETA), ethylene glycol (EG), and oleic acid (OA) have been used as the solvent. X-ray diffraction technique and Raman spectroscopy confirmed the formation of crystalline CZTS nanoparticles with kesterite crystal structure in these solvents with the exception of EDA, which forms wurtzite crystal structure. Morphological characterizations show that several distinct morphologies including spherical (70–160 nm), nanoplates (∼45 nm thickness and more than 1 μm length), peculiar flower-like particles (with diameter of ∼0.4–1.5 μm), truncated hexagonal disks, irregular particles, and hexagonal microdisks are obtained by varying the solvent type. Optical studies revealed broad absorption of the CZTS particles in the visible region. Compared with other solvents, OA synthesized CZTS particles show higher absorption in the visible region. However, CZTS nanoparticles synthesized by TETA solvent show the most appropriate properties for application as an absorber materials in solar cells due to high crystallinity, low impurity phases, suitable size, and proper band gap energy

  1. Novel multiform morphologies of hydroxyapatite: Synthesis and growth mechanism

    Science.gov (United States)

    Mary, I. Reeta; Sonia, S.; Viji, S.; Mangalaraj, D.; Viswanathan, C.; Ponpandian, N.

    2016-01-01

    Morphological evolution of materials becomes a prodigious challenge due to their key role in defining their functional properties and desired applications. Herein, we report the synthesis of hydroxyapatite (HAp) microstructures with multiform morphologies, such as spheres, cubes, hexagonal rods and nested bundles constructed from their respective nanoscale building blocks via a simple cost effective hydro/solvothermal method. A possible formation mechanism of diverse morphologies of HAp has been presented. Structural analysis based on X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy confirms the purity of the HAp microstructures. The multiform morphologies of HAp were corroborated by using Field emission scanning electron microscope (FESEM).

  2. Morphology-Controlled Synthesis of Hematite Nanocrystals and Their Optical, Magnetic and Electrochemical Performance

    Science.gov (United States)

    Li, Bangquan; Sun, Qian; Fan, Hongsheng; Cheng, Ming; Shan, Aixian; Cui, Yimin; Wang, Rongming

    2018-01-01

    A series of α-Fe2O3 nanocrystals (NCs) with fascinating morphologies, such as hollow nanoolives, nanotubes, nanospindles, and nanoplates, were prepared through a simple template-free hydrothermal synthesis process. The results showed that the morphologies could be easily controlled by SO42− and H2PO4−. Physical property analysis showed that the α-Fe2O3 NCs exhibited shape- and size-dependent ferromagnetic and optical behaviors. The absorption band peak of the α-Fe2O3 NCs could be tuned from 320 to 610 nm. Furthermore, when applied as electrode material for supercapacitor, the hollow olive-structure exhibited the highest capacitance (285.9 F·g−1) and an excellent long-term cycling stability (93% after 3000 cycles), indicating that it could serve as a candidate electrode material for a supercapacitor. PMID:29342929

  3. Preparation of weak-light-driven TiO2-based catalysts via adsorbed-layer nanoreactor synthesis and enhancement of their photo-degradation performance in seawater

    Science.gov (United States)

    Wang, Ting; Xu, Zhi-yong; Zhu, Yi-chen; Wu, Li-guang; Yuan, Hao-xuan; Li, Chang-chun; Liu, Ya-yu; Cai, Jing

    2017-11-01

    Graphene oxide (GO) was first employed as a support in preparing TiO2 nanoparticles by adsorbed-layer nanoreactor synthesis (ALNS). Both TiO2 crystallization and GO reduction simultaneously occurred during solvothermal treatment with alcohol as a solvent. By transmission electron microscopy, high resolution transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, and photoluminescence spectroscopy, the results showed that TiO2 nanoparticles with less than 10 nm of size distributed very homogeneously on the GO surface. Tight interaction between TiO2 particles and GO surface could effectively inhibit the aggregation of TiO2 particles, during solvothermal treatment for anatase TiO2 formation. Alcohol could also reduce oxygenated functional groups on GO surface after solvothermal treatment. TiO2 particles with small size and the decrease in oxygenated functional groups on the GO surface both caused high separation efficiency of photo-generated charge carriers, thus resulting in high photo-degradation performance of catalysts. Strong phenol adsorption on photocatalyst was key to enhancing photo-degradation efficiency for phenol in seawater. Moreover, the change in catalyst structure was minimal at different temperatures of solvothermal treatment. But, the degradation rate and efficiency for phenol in seawater were obviously enhanced because of the sensitive structure-activity relationship of catalysts under weak-light irradiation.

  4. Catalytic Activity of Urchin-like Ni nanoparticles Prepared by Solvothermal Method for Hydrogen Evolution Reaction in Alkaline Solution

    International Nuclear Information System (INIS)

    Abbas, Syed Asad; Iqbal, Muhammad Ibrahim; Kim, Seong-Hoon; Jung, Kwang-Deog

    2017-01-01

    Highlights: • Urchin-like Ni is prepared in solvothermal reaction. • Urchin-like Ni is formed via Ni(OH) 2 aggregates in ethanol and oleylamine. • Exchange current density of urchin-like Ni is 0.191 mA cm −2 . • Urchin-like Ni exceeds the catalytic performance of commercial Pt/C in HER. - Abstract: Ni nanoparticles with different morphologies were synthesized for hydrogen evolution reaction (HER) in alkaline solution. Here, Ni(acac) 2 was converted into Ni metal nanoparticles in solvothermal reactions with simple alcohols and oleylamine (OAm). The morphology of the resulting Ni nanoparticles was dependent mainly on the OAm/Ni molar ratio in alcohol solvent. Aggregates of spherical Ni nanoparticles (NiEt-OAm1) were observed at the OAm/Ni molar ratio of 1.0, whereas two echinoid Ni nanoparticles (NiEt-OAm4 and NiEt-OAm6) could be prepared in ethanol at the OAm/Ni molar ratios of 4.0 and 6.0. Ni(OH) 2 formed in ethanol during a reaction time of 5 h was then reduced into echinoid Ni nanoparticles after 8 h. Echinoid Ni nanoparticles were formed by atomic addition on the tops of the multipod Ni particles formed via Ni(OH) 2 /NiO aggregates. Webbed feet-like particles (NiIPA-OAm4) with plate edges were also observed in isopropanol under the same reaction conditions. The catalytic activities of the prepared Ni nanoparticles for the hydrogen evolution reaction were evaluated in alkaline solution. The NiEt-OAm4 with urchin-like morphology was much more active than the NiIPA-OAm4 with webbed feet-like morphology. The exchange current density of Ni catalysts was increased with increasing the OAm/Ni molar ratio. The NiEt-OAm6 exhibited an exchange current of 0.191 mA cm −2 and the NiEt-OAm4 exceeded electrocatalytic performance of a commercial Pt catalysts (40% Pt on Vulcan XC 72) in a stability test for 100 kiloseconds at −1.5 V (vs. Hg/HgO) in 1.0 M NaOH due to its high stability.

  5. Remarkable enhancement of the electrode performance of nanocrystalline LiMn2O4 via solvothermally-assisted immobilization on reduced graphene oxide nanosheets

    International Nuclear Information System (INIS)

    Jo, Kyung-Yeon; Han, Song-Yi; Lee, Jang Mee; Kim, In Young; Nahm, Sahn; Choi, Ji-Won; Hwang, Seong-Ju

    2013-01-01

    A facile solvothermal way to immobilize nanocrystalline LiMn 2 O 4 on the surface of graphene nanosheets is developed to improve the functionality of lithium manganate as lithium intercalation electrode. A solvothermal treatment for the colloidal mixture of graphene oxide (GO) nanosheets and LiMn 2 O 4 nanocrystals gives rise not only to the reduction of GO to reduced graphene oxide (RGO) but also to the immobilization of lithium manganate nanoparticles on the surface of RGO nanosheets. According to powder X-ray diffraction and electron microscopic analyses, the crystal structure and morphology of spinel lithium manganate remain intact upon the composite formation with the RGO nanosheets. The application of larger aldehyde molecule as a reductant leads to the increase of crystallinity and the lowering of Mn oxidation state for the pristine LiMn 2 O 4 and its nanocomposite with the RGO nanosheets. The present LiMn 2 O 4 –RGO nanocomposites display promising cathode performances for lithium rechargeable batteries, which are much superior to those of the pristine LiMn 2 O 4 nanocrystals. The observed enhancement of electrode performance upon the composite formation with the RGO nanosheets is attributable both to the improvement of the surface ion transport of nanocrystalline lithium manganate and to the increase of electrical conductivity. The present experimental findings demonstrate that the solvothermal treatment with RGO nanosheets provides an effective way of improving the electrochemical activity of nanocrystalline lithium metal oxides

  6. An Experimental Study on the Shape Changes of TiO2 Nanocrystals Synthesized by Microemulsion-Solvothermal Method

    Directory of Open Access Journals (Sweden)

    Wei Kong

    2011-01-01

    Full Text Available Titanium dioxide (TiO2 nanocrystals of different shape were successfully synthesized in a new microemulsion system through a solvothermal process. The TiO2 nanocrystals were prepared from the reaction of tetrabutyl titanate (TBT, H2O, and oleic acid (OA, which were used as solvent and surfactant at 300∘C and 240∘C in a stainless steel autoclave. The sphere, polygon, and rhombus-shaped nanocrystals have been prepared at 300∘C and the dot- and- rod shaped nanocrystals have been synthesized at 240∘C. The effect of the reaction time on the shape and size of TiO2 nanocrystals in this method was studied in the present paper. The size distribution of TiO2 nanocrystals prepared at 300∘C for different hours is also studied. In addition, an attempt to describe the mechanism of shape change of TiO2 nanocrystals was presented in this paper.

  7. Multicolor upconversion emission of dispersed ultrasmall cubic Sr2LuF7 nanocrystals synthesized by a solvothermal process

    International Nuclear Information System (INIS)

    Gong, Lunjun; Ma, Mo; Xu, Changfu; Li, Xujun; Wang, Suiping; Lin, Jianguo; Yang, Qibin

    2013-01-01

    Lanthanide (Ln 3+ ) doped Sr 2 LuF 7 (Ln 3+ =Er 3+ /Tm 3+ /Yb 3+ ) nanocrystals (NCs) were synthesized via a solvothermal process using oleate as stabilizing agent. The as-synthesized NCs with a mean diameter of sub-20 nm can be well dispersed in cyclohexane and show a pure cubic phase structure with space group Fm3 ¯ m. Following appropriate lanthanide ion doping, the NCs show intense red, green, blue and white-color upconversion emission (UC) under the excitation of a 980 nm laser. Predominant near-infrared UC can also be obtained in the Yb 3+ /Tm 3+ doped Sr 2 LuF 7 NCs. The energy transfer UC mechanisms for the fluorescent intensity were also investigated. The desirable property of the ultrasmall dispersed NCs makes them promising materials for the applications in miniaturized solid-state light sources, multicolor three-dimensional display devices and fluorescent labels for biomedical imaging. - Highlights: ► Cubic-structure (Fm3 ¯ m) Sr 2 LuF 7 nanocrystals were synthesized for the first time. ► Nanocrystals (sub-20 nm) with cubic or spherical shape can be well dispersed. ► By doping properly, the nanocrystals show intense multicolor upconversion. ► Predominant near-infrared upconversion can be obtained in Sr 2 LuF 7 nanocrystals. ► Upconversion mechanism for the fluorescent intensity is mainly energy transfer.

  8. Influence of reaction time on the structural, optical and electrical performance of copper antimony sulfide nanoparticles using solvothermal method

    Science.gov (United States)

    John, Bincy; Genifer Silvena, G.; Leo Rajesh, A.

    2018-05-01

    The less toxic and cost effective ternary Cu-Sb-S nanoparticles and thin films were synthesized and deposited using solvothermal and drop casting method. The reactions were carried out at different timings as 12-48 h, in steps of 12 h using ethylene glycol as solvent and polyvinylpyrrolidone (PVP) as surfactant. Systematic analysis revealed that due to the influence of different reaction time, significant and unique changes were occurring on the crystal structure, optical and electrical properties of the material. The synthesized nanopowders and deposited films were characterized by means of X-ray diffraction, Raman analysis, field emission scanning electron microscope with energy dispersive spectrometer, UV-Vis-NIR diffuse reflectance spectroscopy and hall measurement. XRD results showed that as the time increases crystallinity improves and phase transformation from chalcostibite to tetrahedrite occurs. The Optical performance revealed that the bandgap of nanoparticles were in the range of 1.21-1.49 eV. Hall measurements showed that the deposited Cu12Sb4S13 and CuSbS2 films exhibited p-type conductivity with carrier concentration ranging from 1016-1019 cm-3, indicating a promising p-type absorber material for photovoltaic applications.

  9. Pt nanoparticles supported over Ce-Ti-O: the solvothermal and photochemical approaches for the preparation of catalytic materials

    International Nuclear Information System (INIS)

    Silva, Adrian M. T.; Machado, Bruno F.; Gomes, Helder T.; Figueiredo, Jose L.; Drazic, Goran; Faria, Joaquim L.

    2010-01-01

    Ce-Ti-O supports with different Ce/Ti molar ratios were synthesized by the solvothermal method using hexadecyltrimethylammonium bromide. Pt nanoparticles were then supported by photochemical deposition. The shape, size, and structure of these materials were analyzed by high-resolution transmission electron microscopy. The single CeO 2 support was also prepared, consisting of agglomerated cubic particles ranging from ∼3 to 8 nm. When titania was combined with ceria, a nanostructured architecture was produced, evidencing the strong influence of Ti in the support structure. Photodeposition of Pt nanoparticles is more efficient on Ce-Ti-O supports than in pristine CeO 2 . Crystalline Pt nanoparticles (mainly of ∼2 to 4 nm) were detected. The catalytic properties of the materials were tested in the selective hydrogenation of cinnamaldehyde to cinnamyl alcohol. It was observed that Pt supported on Ce-Ti-O is more active and selective than Pt on CeO 2 or TiO 2 separately. The catalyst with 40 mol% Ce leads to total conversion of cinnamaldehyde in a few minutes; however, higher selectivity toward the desired product (cinnamyl alcohol) was obtained with higher amounts of Ce (50 mol%).

  10. Raman Spectroscopy of Two-Dimensional Bi2TexSe3 − x Platelets Produced by Solvothermal Method

    Directory of Open Access Journals (Sweden)

    Jian Yuan

    2015-08-01

    Full Text Available In this paper, we report a facile solvothermal method to produce both binary and ternary compounds of bismuth chalcogenides in the form of Bi2TexSe3 − x. The crystal morphology in terms of geometry and thickness as well as the stoichiometric ratio can be well controlled, which offers the opportunities to systematically investigate the relationship between microstructure and phonon scattering by Raman spectroscopy. Raman spectra of four compounds, i.e., Bi2Se3, Bi2Se2Te, Bi2SeTe2 and Bi2Te3, were collected at four different excitation photon energies (2.54, 2.41, 1.96, and 1.58 eV. It is found that the vibrational modes are shifted to higher frequency with more Se incorporation towards the replacement of Te. The dependence of Raman vibrational modes on excitation photon energy was investigated. As the excitation photon energy increases, three Raman vibrational modes (A1g1, Eg2 and A1g2 of the as-produced compounds move to low frequency. Three Infrared-active (IR-active modes were observed in thin topological insulators (TIs crystals.

  11. Fabrication of γ-MnS/rGO composite by facile one-pot solvothermal approach for supercapacitor applications

    Science.gov (United States)

    Li, Xianfu; Shen, Jianfeng; Li, Na; Ye, Mingxin

    2015-05-01

    γ-MnS/reduced graphene oxide (γ-MnS/rGO) composite was successfully fabricated via a facile one-pot solvothermal route using graphene oxide (GO), thioacetamide (TAA, CH3CSNH2) and MnCl2·4H2O as reactants. It reveals that TAA plays an important role in reducing GO and sulfurizing γ-MnS. The synthesized composite was characterized via X-ray diffraction and scanning electron microscopy for structural and morphological studies. Electrochemical performance was also investigated through cyclic voltammetry and galvanostatic charge-discharge. As for the application of supercapacitors, the γ-MnS/rGO composite shows a great value of 802.5 F g-1 at a current density of 5 A g-1. Furthermore, the capacitance of γ-MnS/rGO has no decrease of its initial values after 2000 cycles. The galvanostatic charge-discharge curve demonstrates the ideal capacitive behavior of γ-MnS/rGO composite electrodes.

  12. Synthesis, structural, optical and Raman studies of pure and lanthanum doped ZnSe nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Pushpendra, E-mail: push.nac@gmail.com [Department of Physics, Faculty of Science, Banaras Hindu University, Varanasi 221005 (India); Institute of Atomic and Molecular Sciences, Academia Sinica, Taipei 11529, Taiwan (China); Singh, Jai [Department of Physics, Faculty of Science, Banaras Hindu University, Varanasi 221005 (India); Department of Materials Science and Engineering, Pusan National University, 30 Jangjeon-dong, Geumjeong-gu, Busan 609-735 (Korea, Republic of); Pandey, Mukesh Kumar [Institute of Atomic and Molecular Sciences, Academia Sinica, Taipei 11529, Taiwan (China); Jeyanthi, C.E. [Research and Development Centre, Bharathiar University, Coimbatore 641 046 (India); Siddheswaran, R. [Department of Materials Science and Engineering, University of Concepcion, Concepcion (Chile); Paulraj, M. [Department of Physics, Faculty of Physical sciences and Mathematics, University of Concepcion, Casilla 160, Concepcion (Chile); Hui, K.N. [Department of Materials Science and Engineering, Pusan National University, 30 Jangjeon-dong, Geumjeong-gu, Busan 609-735 (Korea, Republic of); Hui, K.S., E-mail: kshui@hanyang.ac.kr [Department of Mechanical Engineering, Hanyang University, 17 Haengdang-dong, Seongdong-gu, Seoul 133-791 (Korea, Republic of)

    2014-01-01

    Graphical abstract: - Highlights: • Template-free synthesis of ZnSe and ZnSe:La nanoparticles was developed at low temperature 100 °C. • Cubic ZnSe and ZnSe:La nanoparticles were obtained by chemical route. • As-synthesized ZnSe:La nanoparticles showed higher emission intensity than ZnSe nanoparticles. • Band gap (E{sub g}) of ZnSe nanoparticles was bigger than ZnSe nanoparticles due to nanosized effect. - Abstract: In this work, a simple, effective and reproducible chemical synthetic route for the production of high-quality, pure ZnSe nanoparticles (NPs), and lanthanum-doped ZnSe (ZnSe:La) NPs is presented. The wide bandgap, luminescent pure ZnSe and ZnSe:La NPs has been synthesized at a low temperature (100 °C) in a single template-free step. The size and optical bandgap of the NPs was analyzed from powder X-ray diffraction (XRD), UV–visible (UV–vis) spectroscopy, transmission electron microscopy (TEM), and high resolution transmission electron microscopy (HRTEM). A broad photoluminescence (PL) emission across the visible spectrum has been demonstrated by a systematic blue-shift in emission due to the formation of small nanoparticles. Here, contribution to emission intensity from surface states of NPs increases with La doping. TEM data revealed that the average size of ZnSe and ZnSe:La NPs is 14 and 8 nm, respectively. On the other hand, band gap energy E{sub g} of ZnSe and ZnSe:La NPs were found to be 3.59 eV and 3.65 eV, respectively. Results showed that hydrazine hydrate played multiple roles in the formation of ZnSe and ZnSe:La NPs. A possible reaction mechanism for the growth of NPs is also discussed.

  13. Site selective Cu2+ substitution in single crystal Fe3O4 biocompatible nanospheres by solvothermal reflux method

    Science.gov (United States)

    Manohar, A.; Krishnamoorthi, C.

    2017-09-01

    Transition metal cations distribution among tetrahedral and octahedral sites in Fe3O4 has profound influence on it properties. The cations distribution among these sites were influenced by crystal field stabilization energy (CFSE) of a substituent ion. It was reported that Cu2+ substitutes both Fe3+ in tetrahedral and Fe2+ in octahedral sites of magnetite though it has high CFSE for octahedral sites. Thus it promotes mixed (normal & inverse) spinel structure and hence the properties deviate from the prediction. Here we show that selective octahedral site substitution of Fe2+ by Cu2+ in single crystal Fe3O4 nanoparticles was possible by solvothermal reflux method at moderate temperatures (≈300 °C). It was attributed to reduced energy barrier for crystallization and high diffusion coefficient of the metal cations at moderate temperature in low viscous organic solvents mixture, at ambient pressure, compared to coprecipitation and solid state reaction protocols. In addition, effective removal of exothermic crystal lattice energy, released during nucleation and growth process, by natural gas bubbles formed in the reflux organic solvent mixture. This promotes effective diffusion of cations during the growth process and easy octahedral occupation by Cu2+ in Fe1-xCuxFe2O4 (x = 0, 0.1, 0.2, 0.3, 0.4, 0.5 & 0.6) single crystal nanospheres. The octahedral substitution was confirmed by reduction of crystal lattice parameter as well as ferromagnetic strength of octahedral sublattice with enhanced Cu2+ concentration. In addition, morphology, lattice vibrational frequency and electron excitation spectra of the nanospheres were studied. The Langevin function fit analysis reveals that superparamagnetic domain diameter were slightly less than the particle diameter obtained from TEM micrograph.

  14. In-situ solvothermal processing of polycaprolactone/hydroxyapatite nanocomposites with enhanced mechanical and biological performance for bone tissue engineering

    Directory of Open Access Journals (Sweden)

    Saeed Moeini

    2017-09-01

    Full Text Available The interest in biodegradable polymer-matrix nanocomposites with bone regeneration potential has been increasing in recent years. In the present work, a solvothermal process is introduced to prepare hydroxyapatite (HA nanorod-reinforced polycaprolactone in-situ. A non-aqueous polymer solution containing calcium and phosphorous precursors is prepared and processed in a closed autoclave at different temperatures in the range of 60–150 °C. Hydroxyapatite nanorods with varying aspect ratios are formed depending on the processing temperature. X-ray diffraction analysis and field-emission scanning electron microscopy indicate that the HA nanorods are semi-crystalline. Energy-dispersive X-ray spectroscopy and Fourier transform infrared spectrometry determine that the ratio of calcium to phosphorous increases as the processing temperature increases. To evaluate the effect of in-situ processing on the mechanical properties of the nanocomposites, highly porous scaffolds (>90% containing HA nanorods are prepared by employing freeze drying and salt leaching techniques. It is shown that the elastic modulus and strength of the nanocomposites prepared by the in-situ method is superior (∼15% to those of the ex-situ samples (blended HA nanorods with the polymer solution. The enhanced bone regeneration potential of the nanocomposites is shown via an in vitro bioactivity assay in a saturated simulated body fluid. An improved cell viability and proliferation is also shown by employing (3-(4,5- dimethylthiazol-2-yl-2, 5-diphenyl tetrazolium bromide (MTT assay in human osteosarcoma cell lines. The prepared scaffolds with in vitro regeneration capacity could be potentially useful for orthopaedic applications and maxillofacial surgery.

  15. Synthesis and characterization of the ternary telluroargentate K4[Ag18Te11

    KAUST Repository

    Davaasuren, Bambar

    2014-10-19

    The ternary potassium telluroargentate(I), K4[Ag18Te11], was prepared by solvothermal synthesis in ethylenediamine at 160 °C. It crystallizes in the cubic space group Fm3¯ m (no. 225) with the cell parameter a = 18.6589(6) Å. The crystal structure can be described as a [Ag18Te11]4- three-dimensional anionic framework with the voids accommodating potassium cations. Chemical bonding analysis reveals polar covalent Ag-Te bonds and considerable Ag-Ag interactions, which support the complex anionic character of the structure. The compound is thermally stable up to 450 °C in an inert atmosphere.

  16. Synthesis of Highly Soluble TiO2 Nanoparticle with Narrow Size Distribution

    International Nuclear Information System (INIS)

    Baek, Seong Yong; Chai, Seung Yong; Hur, Kap Soo; Lee, Wan In

    2005-01-01

    The reverse micelle process has widely been applied to the syntheses of size-controlled nanoparticles for various metals and semiconductors. The carboxylic acids or amines with long hydrocarbon chains form a stable reverse micelle array in nonpolar ethers, and the cavities inside these arrays possibly be used as nanoreactors for the synthesis of nanoparticles. Moreover, it has been well-known that the carboxylic acids have strong binding affinity toward TiO 2 . Thus, the carboxylic acids with long hydrocarbon chain would be an appropriate surfactant for the synthesis of titania nanoparticles. Nonetheless, the synthesis of TiO 2 nanoparticle is still very complicated, and only a limited success has been achieved so far in controlling its shape and size. Under a typical synthetic condition, such as reflux of reactants in flask, the obtained titania nanoparticles are heavily aggregated and their crystallinities are not so high in most case. So far, the hydrothermal or solvothermal reaction has usually been applied for the syntheses of various metal oxides at relatively low temperatures. 20 Since the reaction is performed at an elevated pressure, more crystallized and denser structures have been obtained at a given temperature. Thus, in this work, we combined the solvothermal technique and reverse micelle method to obtain more crystallized and monodispersed titania nanoparticles without aggregation

  17. Self-assembly of Fe3O4 nanocrystal-clusters into cauliflower-like architectures: Synthesis and characterization

    International Nuclear Information System (INIS)

    Zhu Luping; Liao Guihong; Bing Naici; Wang Linlin; Xie Hongyong

    2011-01-01

    Large-scale cauliflower-like Fe 3 O 4 architectures consist of well-assembled magnetite nanocrystal clusters have been synthesized by a simple solvothermal process. The as-synthesized Fe 3 O 4 samples were characterized by XRD, XPS, FT-IR, SEM, TEM, etc. The results show that the samples exhibit cauliflower-like hierarchical microstructures. The influences of synthesis parameters on the morphology of the samples were experimentally investigated. Magnetic properties of the Fe 3 O 4 cauliflower-like hierarchical microstructures have been detected by VSM at room temperature, showing a relatively low saturation magnetization of 65 emu/g and an enhanced coercive force of 247 Oe. - Graphical Abstract: Cauliflower-like Fe 3 O 4 architectures consist of well-assembled magnetite nanocrystal clusters have been synthesized by a simple solvothermal process, using FeCl 3 .6H 2 O and EDA as the starting materials. Highlights: → Cauliflower-like Fe 3 O 4 architectures were successfully prepared by a simple solvothermal route. → The cauliflower-like Fe 3 O 4 architectures have a size in the range of 200-300 nm. → They show a low saturation magnetization of 65 emu/g and an enhanced coercive force of 247 Oe. → These Fe 3 O 4 architectures may have potential applications in catalysis and biological fields.

  18. Photocatalytic decomposition of dyes using ZnO doped SnO2 nanoparticles prepared by solvothermal method

    Directory of Open Access Journals (Sweden)

    Mohamed M. Rashad

    2014-01-01

    Full Text Available ZnO doped SnO2 has been successfully synthesized by the solvothermal method using methanol as organic solvent. The effect of ZnO/SnO2 molar ratios on the crystal structure, microstructure, optical and photocatalytic properties has been investigated. The synthesized samples are characterized by X-ray diffraction, transmission electron microscopy, N2 physical adsorption, FT-IR spectroscopy and UV–Vis spectroscopy. XRD results revealed that all diffraction peaks positions agree well with the reflection of a tetragonal rutile structure of SnO2 phase without extra peaks at 0.1ZnO:0.9SnO2 and 0.2ZnO:0.8SnO2 molar ratios. However, the secondary phase of ZnO at 0.3ZnO:0.7SnO2 molar ratio was investigated. TEM images revealed that the shape of SnO2 particles was spherical and the particle sizes of SnO2 and 0.3ZnO:0.7SnO2 molar ratio were 6.2 and 16.4 nm, respectively. The newly prepared samples have been tested by the determination of photocatalytic degradation of methylene blue (MB. The results indicated that Zn2+ doping at 0.3ZnO:0.7 SnO2 molar ratio showed the highest photocatalytic activity for the MB photodegradation. The heightened photocatalytic activity of ZnO/SnO2 could be ascribed to the enhanced charge separation derived from the coupling of ZnO with SnO2 due to the potential energy differences between SnO2 and ZnO. The recycling tests demonstrated that 0.3ZnO:0.7 SnO2 photocatalysts were quite stable during that liquid–solid heterogeneous photocatalysis since no decrease in activity in the first four cycles was observed.

  19. Facile synthesis of self-stabilized polyphenol nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Bilici, Ali, E-mail: alibilici66@hotmail.com [Lapseki Vocational School, Çanakkale Onsekiz Mart University, Lapseki, Çanakkale 17020 (Turkey); Department of Chemistry, Polymer Synthesis and Analysis Laboratory, Faculty of Science and Arts, Çanakkale Onsekiz Mart University, Çanakkale 17020 (Turkey); Doğan, Fatih, E-mail: fatihdogan@comu.edu.tr [Secondary Science and Mathematics Education, Faculty of Education, Canakkale Onsekiz Mart University, Canakkale 17100 (Turkey); Department of Chemistry, Polymer Synthesis and Analysis Laboratory, Faculty of Science and Arts, Çanakkale Onsekiz Mart University, Çanakkale 17020 (Turkey); Yıldırım, Mehmet [Department of Materials Science and Engineering, Faculty of Engineering, Çanakkale Onsekiz Mart University, Çanakkale 17020 (Turkey); Department of Chemistry, Polymer Synthesis and Analysis Laboratory, Faculty of Science and Arts, Çanakkale Onsekiz Mart University, Çanakkale 17020 (Turkey); Kaya, İsmet [Department of Chemistry, Polymer Synthesis and Analysis Laboratory, Faculty of Science and Arts, Çanakkale Onsekiz Mart University, Çanakkale 17020 (Turkey)

    2013-06-15

    We describe here the facile synthesis (in two-steps) of green light emitting phenol polymer with an azomethine side group. For this purpose, hydroxy functionalized-Schiff base monomer, HPMBT, was obtained by condensation of 2,3,4-trihydroxybenzaldehyde with 2-aminophenol. Subsequent oxidation of the monomer in alkaline medium by NaOCl yielded to corresponding phenol polymer (PHPMBT) with molecular weight ca. 34,500 Da. The characterizations were performed by NMR, FT-IR, UV–vis, gel permeation chromatography (GPC), thermogravimetry (TG), differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), cyclic voltammetry (CV), photoluminescence (PL), dynamic light scattering (DLS) and scanning electron microscope (SEM) analysis. PL analysis indicated that HPMBT was non-fluorescent whereas PHPMBT was a green light emitter. In addition, the redox behaviors of the polymer were explored by cyclic voltammetry (CV), assigned it's electroactive nature. The formation of nano-sized polyphenol particles was revealed by the SEM and DLS analyses. A possible mechanism for the formation and self-stabilization of the polyphenol nanoparticles was also suggested. - Highlights: • The nano-sized polyphenol particles were facilely obtained by a template-free oxidative polymerization process. • A possible mechanism for the formation and self-stabilization of the nanoparticles was proposed. • These electroactive particles emitted green light, efficiently. • The obtained polymer was well soluble in polar organic solvents.

  20. Facile synthesis of self-stabilized polyphenol nanoparticles

    International Nuclear Information System (INIS)

    Bilici, Ali; Doğan, Fatih; Yıldırım, Mehmet; Kaya, İsmet

    2013-01-01

    We describe here the facile synthesis (in two-steps) of green light emitting phenol polymer with an azomethine side group. For this purpose, hydroxy functionalized-Schiff base monomer, HPMBT, was obtained by condensation of 2,3,4-trihydroxybenzaldehyde with 2-aminophenol. Subsequent oxidation of the monomer in alkaline medium by NaOCl yielded to corresponding phenol polymer (PHPMBT) with molecular weight ca. 34,500 Da. The characterizations were performed by NMR, FT-IR, UV–vis, gel permeation chromatography (GPC), thermogravimetry (TG), differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), cyclic voltammetry (CV), photoluminescence (PL), dynamic light scattering (DLS) and scanning electron microscope (SEM) analysis. PL analysis indicated that HPMBT was non-fluorescent whereas PHPMBT was a green light emitter. In addition, the redox behaviors of the polymer were explored by cyclic voltammetry (CV), assigned it's electroactive nature. The formation of nano-sized polyphenol particles was revealed by the SEM and DLS analyses. A possible mechanism for the formation and self-stabilization of the polyphenol nanoparticles was also suggested. - Highlights: • The nano-sized polyphenol particles were facilely obtained by a template-free oxidative polymerization process. • A possible mechanism for the formation and self-stabilization of the nanoparticles was proposed. • These electroactive particles emitted green light, efficiently. • The obtained polymer was well soluble in polar organic solvents

  1. Solvothermal syntheses and characterization of three new silver(I)/copper(I)-thioarsenates based on As{sup 2+}/As{sup 3+} ions

    Energy Technology Data Exchange (ETDEWEB)

    Yao, Hua-Gang, E-mail: hgyao@gdpu.edu.cn [School of Chemistry and Chemical Engineering, Guangdong Pharmaceutical University, Zhongshan 528458 (China); Guangdong Cosmetics Engineering & Technology Research Center, Zhongshan 528458 (China); Tang, Cheng-Fei [School of Chemistry and Chemical Engineering, Guangdong Pharmaceutical University, Zhongshan 528458 (China); An, Yong-Lin [Department of Chemistry, Dalian University of Technology, Dalian 116024 (China); Ou, Zi-Jian; Wu, Guo-Hao; Lan, Pei; Zheng, Yi-Long [School of Chemistry and Chemical Engineering, Guangdong Pharmaceutical University, Zhongshan 528458 (China)

    2017-02-15

    Three new silver(I)/copper(I)-thioarsenates KAgAs{sup II}S{sub 2} (1), RbCu{sub 2}As{sup III}S{sub 3} (2) and RbCu{sub 4}As{sup III}S{sub 4} (3) have been solvothermally synthesized and structurally characterized. 1 exhibits a two-dimensional anionic network built up by As−As bond connecting the left- and right-handed helical [AgS{sub 2}]{sup 4−} chains, and represents the first examples of thioarsenates(II). The structure of 2 consists of two kinds of helical [Cu{sub 2}S{sub 3}]{sup 4–} chains linked by the arsenic atoms to form double layers with rubidium ions between the layers. Compound 3 is built up of infinite [Cu{sub 2}S{sub 2}]{sup 2–} chain and layered [Cu{sub 6}As{sub 2}S{sub 6}] linked to form a three-dimensional anionic framework, [Cu{sub 4}AsS{sub 4}]{sup –}, and containing channels in which the rubidium cations reside. The optical properties of 1–3 have been investigated by UV–vis spectroscopy. - Graphical abstract: Three new silver(I)/copper(I)-thioarsenates have been solvothermally synthesized and structurally characterized. 1 represents the first examples of thioarsenates(II) while compounds 2 and 3 possess noncondensed pyramidal AsS{sub 3}{sup 3–} unit.

  2. 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.

  3. Solid-Phase Synthesis of Molecularly Imprinted Polymer Nanoparticles with a Reusable Template - "Plastic Antibodies".

    Science.gov (United States)

    Poma, Alessandro; Guerreiro, Antonio; Whitcombe, Michael J; Piletska, Elena V; Turner, Anthony P F; Piletsky, Sergey A

    2013-06-13

    Molecularly Imprinted Polymers (MIPs) are generic alternatives to antibodies in sensors, diagnostics and separations. To displace biomolecules without radical changes in infrastructure in device manufacture, MIPs should share their characteristics (solubility, size, specificity and affinity, localized binding domain) whilst maintaining the advantages of MIPs (low-cost, short development time and high stability) hence the interest in MIP nanoparticles. Herein we report a reusable solid-phase template approach (fully compatible with automation) for the synthesis of MIP nanoparticles and their precise manufacture using a prototype automated UV photochemical reactor. Batches of nanoparticles (30-400 nm) with narrow size distributions imprinted with: melamine (d = 60 nm, K d = 6.3 × 10 -8 m), vancomycin (d = 250 nm, K d = 3.4 × 10 -9 m), a peptide (d = 350 nm, K d = 4.8 × 10 -8 m) and proteins have been produced. Our instrument uses a column packed with glass beads, bearing the template. Process parameters are under computer control, requiring minimal manual intervention. For the first time we demonstrate the reliable re-use of molecular templates in the synthesis of MIPs (≥ 30 batches of nanoMIPs without loss of performance). NanoMIPs are produced template-free and the solid-phase acts both as template and affinity separation medium.

  4. 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.

  5. A simple solvothermal route to synthesize graphene-modified LiFePO4 cathode for high power lithium ion batteries

    Science.gov (United States)

    Zhang, Yin; Wang, Wenchao; Li, Penghui; Fu, Yanbao; Ma, Xiaohua

    2012-07-01

    To improve the rate performance and cycling stability of LiFePO4, graphene-modified LiFePO4 composite has been developed as Li-ion battery cathode material. The composite is successfully prepared via a novel solvothermal route. C-LiFePO4/graphene, with structure of C-LiFePO4 nanoparticles embedded in graphene matrix, exhibits excellent electrochemical properties, including superior high-rate capability and favorable charge-discharge cycle performance under relative high current density. The size of LiFePO4 nanoparticles can be controlled below 30 nm with good reproducibility through this route and due to the synergism of thin carbon film and graphene matrix, the dual coatings exert a significant impact on the electronic conductivity. This novel composite presents excellent electrochemical properties: with reversible capacity of 90 mAh g-1 at 10C and 42 mAh g-1 at 40C achieved.

  6. Effect of electrolytes nature and concentration on the morphology and structure of MoS{sub 2} nanomaterials prepared using one-pot solvothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Akram, H., E-mail: akramhanane@yahoo.fr [Instituto de Catálisis y Petroleoquímica, CSIC, C/Marie Curie 2, Cantoblanco, 28049 Madrid (Spain); Laboratoire de Génie Chimique et Valorisation des Ressources, Faculté des Sciences et Techniques de Tanger, Université Abdelmalek Essâadi, B.P. 416 Tangier (Morocco); Mateos-Pedrero, C., E-mail: cmpedrero@yahoo.es [Laboratory for Process Engineering, Environment, Biotechnology and Energy, Faculdade de Engenharia da Universidade do Porto Rua Roberto Frias, s/n4200-465, Porto (Portugal); Gallegos-Suárez, E.; Guerrero-Ruíz, A. [Instituto de Catálisis y Petroleoquímica, CSIC, C/Marie Curie 2, Cantoblanco, 28049 Madrid (Spain); Grupo de Diseño y Aplicación de Catalizadores Heterogéneos, Unidad Asociada UNED—ICP (CSIC), Madrid (Spain); Chafik, T. [Laboratoire de Génie Chimique et Valorisation des Ressources, Faculté des Sciences et Techniques de Tanger, Université Abdelmalek Essâadi, B.P. 416 Tangier (Morocco); Rodríguez-Ramos, I. [Instituto de Catálisis y Petroleoquímica, CSIC, C/Marie Curie 2, Cantoblanco, 28049 Madrid (Spain); Grupo de Diseño y Aplicación de Catalizadores Heterogéneos, Unidad Asociada UNED—ICP (CSIC), Madrid (Spain)

    2014-07-01

    Different MoS{sub 2} nanostructures have been obtained following an innovative one-step solvothermal method by changing the concentration and type of the electrolyte while avoiding the use of surfactant. It was found that the chemical nature of the studied electrolyte ((NH{sub 4}){sub 2}CO{sub 3} or KCl) do not significantly affect the morphology and structure of the obtained MoS{sub 2} nanomaterials. Nevertheless, increasing the electrolyte concentration yields to a remarkable modification of the morphology of the resulting MoS{sub 2} from nanospheres to worm-shaped then finally to nanotubes. All the obtained nanomaterials were characterized by X-ray diffraction, (XRD), transmission electron microscopy (TEM, HRTEM), Fourier transformation infra-red spectroscopy (FTIR), thermogravimetric analysis (TGA) and X-ray photoelectron spectroscopy (XPS).

  7. Preparation of CoFeO Nanocrystallites by Solvothermal Process and Its Catalytic Activity on the Thermal Decomposition of Ammonium Perchlorate

    Directory of Open Access Journals (Sweden)

    Shusen Zhao

    2010-01-01

    Full Text Available Nanometer cobalt ferrite (CoFe2O4 was synthesized by polyol-medium solvothermal method and characterized by X-ray diffraction (XRD, transmission electron microscopy (TEM, and selected area electron diffraction (SAED. Further, the catalytic activity and kinetic parameters of CoFe2O4 nanocrystallites on the thermal decomposition behavior of ammonium perchlorate (AP have been investigated by thermogravimetry and differential scanning calorimetry analysis (TG-DSC. The results imply that the catalytic performance of CoFe2O4 nanocrystallites is significant and the decrease in the activation energy and the increase in the rate constant for AP further confirm the enhancement in catalytic activity of CoFe2O4 nanocrystallites. A mechanism based on an proton transfer process has also been proposed for AP in the presence of CoFe2O4 nanocrystallites.

  8. The effect of diethylenetriamine on the solvothermal reactions of polyethyleneimine-graphene oxide/lithium titanate nanocomposites for lithium battery anode

    Science.gov (United States)

    Rajagopalan, Balasubramaniyan; Oh, Eun Suok; Chung, Jin Suk

    2015-02-01

    A simple preparation of N-doped graphene/Li4Ti5O12-TiN (NG/LTO-TiN) from the polyethyleneimine-graphene oxide/Li4Ti5O12 (PEI-GO/LTO) is achieved through a solvothermal reaction in the presence of diethylenetriamine (DETA). The solvothermal reaction converts PEI-GO/LTO into corresponding NG/LTO-TiO2, which could be simultaneously converted into NG/LTO-TiN via reacting with DETA as an N source. It is proposed that the electrically conductive titanium nitride (TiN) is formed at the interface between the surfaces of Li4Ti5O12 (LTO) and nitrogen doped graphene (NG). When used as an anode material for lithium ion battery (LIB), the NG/LTO-TiN exhibited superior rate capability in comparison to LTO, reduced GO/Li4Ti5O12-TiO2 (RGO/LTO-TiO2) and NG/LTO-TiO2 nanocomposites, with excellent cyclic stability up to 100 cycles. Moreover, the ionic diffusion coefficient is 3.6 × 10-12 cm2 s-1 for NG/LTO-TiN-94.3%, which is a higher value than that of the LTO (8.85 × 10-13 cm2 s-1), RGO/LTO-TiO2-93.5% (1.48 × 10-12 cm2 s-1), and NG/LTO-TiO2-94.2% (2.51 × 10-12 cm2 s-1) nanocomposites studied.

  9. Facile in situ solvothermal method to synthesize MWCNT/SnIn4S8 composites with enhanced visible light photocatalytic activity

    International Nuclear Information System (INIS)

    Ding, Chaoying; Tian, Li; Liu, Bo; Liang, Qian; Li, Zhongyu; Xu, Song; Liu, Qiaoli; Lu, Dayong

    2015-01-01

    Highlights: • MWCNT/SnIn 4 S 8 composites were facilely fabricated via in situ solvothermal method. • MWCNT/SnIn 4 S 8 composites exhibited significantly enhanced visible-light activity. • MWCNT/SnIn 4 S 8 composites showed remarkable visible light photocatalytic activity. • MWCNT/SnIn 4 S 8 composites exhibited excellent photo-stability. • Possible photocatalytic mechanism under visible-light irradiation was proposed. - Abstract: Superior photocatalytic activity could be achieved by multi-walled carbon nanotube (MWCNT) incorporated in the porous assembly of marigold-like SnIn 4 S 8 heterostructures synthesized by a flexible in-situ solvothermal method. The as-prepared MWCNT/SnIn 4 S 8 composites were well-characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (FE-SEM) and UV–vis diffuse reflectance spectroscopy (DRS). The photocatalytic properties of the as-prepared samples were tested by photo-degradation of aqueous malachite green (MG) under the irradiation of visible light. It was found that the MWCNT/SnIn 4 S 8 composites showed enhanced visible light photocatalytic activity for dye degradation, and an optimum photocatalytic activity was observed over 3.0 wt.% MWCNT incorporated SnIn 4 S 8 composites. The superior photocatalytic activity of MWCNT/SnIn 4 S 8 composites could be ascribed to the existence of MWCNT which could serve as a good electron acceptor, mediator as well as the co-catalyst for dye degradation. The synergistic effect between SnIn 4 S 8 and MWCNT in the composites facilitated the interfacial charge transfer driven by the excitation of SnIn 4 S 8 under visible-light irradiation. Furthermore, a possible mechanism for the photocatalytic degradation of MWCNT/SnIn 4 S 8 composites was also discussed

  10. Solvothermal fabrication of TiO2/sepiolite composite gel with exposed {0 0 1} and {1 0 1} facets and its enhanced photocatalytic activity

    Science.gov (United States)

    Liu, Ruirui; Ji, Zhijiang; Wang, Jing; Zhang, Jinjun

    2018-05-01

    A novel TiO2/sepiolite composite gel (TiSG) was fabricated in the presence of cetyltrimethylammonium bromide (CTAB) through a simple solvothermal reaction in an acetic acid-water solvent. A homogeneous anchoring of TiO2 nanoparticles with exposed {0 0 1} and {1 0 1} facets on sepiolite nanofibers was achieved. CTAB content, solvothermal temperature/time, and HAc content play crucial roles in the morphological and facet formation of TiSG. A possible mechanism for the formation of TiSG was further proposed. CTAB as capping/shape-controlling agent can strongly bind to the more reactive (0 0 1) facet of TiO2 and then mitigate the thermodynamically favored (0 0 1) plane growth. Eventually, the truncated octahedral TiO2 was obtained by controlling the growth rates in 〈0 0 1〉 and 〈1 0 1〉 directions. Sepiolite as a cross-linking agent provides sufficient crosslinking sites for TiO2 to induce three-dimensional (3D) network formation, thereby generating the composite gel. The synthesized TiSG samples were then used as photocatalysts, which exhibited increased methyl orange removal under UV-vis light (350-780 nm) by the synergistic effect of adsorption and in-situ photocatalytic degradation as compared to P25 and bare TiO2. The excellent photocatalytic performance of TiSG was mainly ascribed to the formations of 3D gel structure and surface heterojunctions between (0 0 1) and (1 0 1) facets.

  11. Solvothermal fabrication and enhanced visible light photocatalytic activity of Cu{sub 2}O-reduced graphene oxide composite microspheres for photodegradation of Rhodamine B

    Energy Technology Data Exchange (ETDEWEB)

    Sun, Lingling [Hubei Collaborative Innovation Center for Rare Metal Chemistry, Hubei Normal University, Huangshi 435002 (China); Hubei Key Laboratory of Pollutant Analysis and Reuse Technology, Hubei Normal University, Huangshi 435002 (China); Wang, Guohong, E-mail: wanggh2003@163.com [Hubei Collaborative Innovation Center for Rare Metal Chemistry, Hubei Normal University, Huangshi 435002 (China); Hubei Key Laboratory of Pollutant Analysis and Reuse Technology, Hubei Normal University, Huangshi 435002 (China); Hao, Ruirui [Hubei Collaborative Innovation Center for Rare Metal Chemistry, Hubei Normal University, Huangshi 435002 (China); Hubei Key Laboratory of Pollutant Analysis and Reuse Technology, Hubei Normal University, Huangshi 435002 (China); Han, Deyan, E-mail: handeyan@sohu.com [Hubei Collaborative Innovation Center for Rare Metal Chemistry, Hubei Normal University, Huangshi 435002 (China); Hubei Key Laboratory of Pollutant Analysis and Reuse Technology, Hubei Normal University, Huangshi 435002 (China); Cao, Sheng [Hubei Collaborative Innovation Center for Rare Metal Chemistry, Hubei Normal University, Huangshi 435002 (China); Hubei Key Laboratory of Pollutant Analysis and Reuse Technology, Hubei Normal University, Huangshi 435002 (China)

    2015-12-15

    Graphical abstract: - Highlights: • Cu{sub 2}O-reduced graphene oxide composite spheres were successfully prepared. • The graphene oxide loading played an important role in photocatalytic activity. • A possible enhanced photocatalytic mechanism was proposed. - Abstract: The addition of graphene oxide (GO) in the semiconductors has been regarded as one of the effective methods to enhance their photocatalytic activity. In this study, Cu{sub 2}O-reduced graphene oxide (Cu{sub 2}O-rGO) composites with low loading (0–0.5 wt.%) of graphene oxide (GO) were produced by a one-step green solvothermal method in ethanol system by using Cu(NO{sub 3}){sub 2}·3H{sub 2}O and glutamic acid as copper precursor and reducing agent, respectively. During the solvothermal treatment, GO was reduced to rGO. The as-prepared Cu{sub 2}O-reduced graphene oxide composite microspheres exhibited enhanced photocatalytic activity toward the degradation of RhB aqueous solution under visible light irradiation. At the optimal loading of graphene oxide (0.05 wt.%), Cu{sub 2}O-rGO composites showed the highest photocatalytic activity, exceeding that of pure Cu{sub 2}O and commercial Degussa P25 by a factor of 2.9 and 7.9, respectively. The enhanced photocatalytic activity may be ascribed to the strong coupling interaction between Cu{sub 2}O particles and rGO nanosheets, which reduces the recombination of charge carriers.

  12. Water-n-BuOH solvothermal synthesis of ZnAl-LDHs with different morphologies and its calcined product in efficient dyes removal.

    Science.gov (United States)

    Huang, Gailing; Sun, Yingying; Zhao, Chencong; Zhao, Yifei; Song, Zhaoyuan; Chen, Junli; Ma, Shulan; Du, Junping; Yin, Zhigang

    2017-05-15

    In this study, water-n-BuOH mixed solvents were used to synthesize the ZnAl-layered double hydroxides (ZnAl-LDHs) via hydrothermal method. The XRD, FT-IR, SEM, ICP and CHN analyses revealed that the type of intercalated anions, the layer Zn/Al ratios, and morphologies of the LDHs depended on the ratio of V(water)/V(n-BuOH) in the mixed solvents. When the ratio of V(water)/V(n-BuOH) is 3 or 0.3, the as-prepared LDHs had 3D "silk flowers" (ZnAl-LDH-3) or "Sedimentary rock" morphology (ZnAl-LDH-0.3). Adsorption properties of dyes on calcined LDHs were studied. Compared with ZnAl-LDO-0.3 and ZnAl-LDO-w (calcined from the LDHs obtained in pure water), ZnAl-LDO-3 showed much better adsorption efficiency for anionic dyes thanks to its much larger BET-specific surface area. The sorption kinetics for dyes was appropriately described by the pseudo-second-order model and sorption isotherms can be fitted more satisfactorily by the Langmuir model. With the increasing concentrations of dyes from 10mg/L to 400mg/L, the maximum absorption capacities of ZnAl-LDO-3 were 1540mg/g (2.21mmol/g) for congo red, 1153mg/g (3.52mmol/g) for methyl orange and 390mg/g (0.63mmol/g) for active red (X-3B), respectively. The adsorption dyes onto the external surface is still the main mechanism for LDO adsorbents. The ZnAl-LDO-3 was a potential adsorbent for dyeing wastewater treatment. Copyright © 2017 Elsevier Inc. All rights reserved.

  13. A facile one-pot solvothermal method for synthesis of magnetically recoverable Pd-Fe3O4 hybrid nanocatalysts for the Mizoroki-Heck reaction

    Science.gov (United States)

    Zhen, Fangchen; Ran, Maofei; Chu, Wei; Jiang, Chengfa; Sun, Wenjing

    2018-03-01

    Pd-Fe3O4 hybrid nanostructures were prepared using a simple one-pot hydrothermal method. The prepared materials were characterized by Fourier transform-infrared spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, transmission electron microscopy, inductively coupled plasma, N2 adsorption-desorption, and vibrating sample magnetometry. This self-assembled nanosystem acted as an efficient magnetically recyclable noble metal-based multi-functional nanocatalyst. It showed excellent catalytic activity and stability for the Heck reaction of iodobenzene and styrene under mild conditions. The methods used to prepare the Pd-Fe3O4 catalysts were simple and low-cost, which will be useful for the large-scale development and application of a magnetically recoverable Pd catalyst.

  14. Microwave-assisted solvothermal synthesis of novel hierarchical BiOI/rGO composites for efficient photocatalytic degardation of organic pollutants

    Science.gov (United States)

    Niu, Jinfen; Dai, Peixuan; Zhang, Qian; Yao, Binghua; Yu, Xiaojiao

    2018-02-01

    In the present paper, a novel composite of BiOI/rGO with excellent visible-light photocatalytic activity was successfully fabricated via very different simple, fast and mild rapid microwave hydrothermal method. The BiOI/rGO -1(BG-1) was donated as a simple chemical mechanical and the BiOI/rGO -2(BG-2) was donated as one-step rapid microwave hydrothermal method. The BG-1 were composed of the BiOI microspheres with a diameter of about 1 μm and mixed heterogeneously with graphene. While, the BG-2 were consist of the BiOI nanoplates with the thickness of approximately 20 nm dispersed heterogeneously on the surface of rGO. The degradation of 40 mg/L methylene blue (MB) and 20 mg/L levofloxacin (LEV) under visible light irradiation can reach about 11 and 3 times than that of P25, respectively. Furthermore, the reactive species of hole was determined to dominant the photodegradation process. The intensive photocatlytic could ascribe to more effective electron transportation and separations, this conclusion was different with other studies. A possible photocatalytic mechanism of BG-2 was also proposed.

  15. Fast microwave-assisted solvothermal synthesis of metal nanoparticles (Pd, Ni, Sn) supported on sulfonated MWCNTs: Pd-based bimetallic catalysts for ethanol oxidation in alkaline medium

    CSIR Research Space (South Africa)

    Ramulifho, T

    2012-01-01

    Full Text Available -MWCNT-Pd and its "mixed" bimetallic electrocatalysts (i.e., SF-MWCNT-PdSn mix and SF-MWCNT-PdNi) towards ethanol oxidation in alkaline medium was investigated. The result shows that the mixed Pd-based catalysts (obtained by simple ultrasonic...

  16. Solvothermal fabrication of activated semi-coke supported TiO{sub 2}-rGO nanocomposite photocatalysts and application for NO removal under visible light

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Weiwei; Li, Chunhu, E-mail: lichunhu@ouc.edu.cn; Wang, Liang; Sun, ShengNan; Yan, Xin

    2015-10-30

    Highlights: • Activated semi-coke supported TiO{sub 2}-rGO photocatalysts were fabricated by one-step solvothermal method. • The photocatalytic performance for NO removal was studied under visible light irradiation. • The introduction of rGO is responsible for superior photocatalytic activity. • Optimum operational parameters at 70 °C, with 8% O{sub 2} and 8% relative humidity were obtained. • Thermal vapor regeneration is the most suitable generation method. - Abstract: The photocatalysts of activated semi-coke supported TiO{sub 2}-rGO nanocomposite (TiO{sub 2}-rGO/ASC) with different contents of reduced graphene oxide were fabricated by one-step solvothermal method for NO removal under visible light irradiation. It was confirmed that 8% content of reduced graphene oxide presented the best NO photooxidation performance under visible light irradiation at 70 °C with 350–400 mg/m{sup 3} NO,5% O{sub 2} and 5% relative humidity. The reasons for improved activity were discussed, alloyed with the mechanism of producing CO. Detailed structural information of TiO{sub 2}-rGO/ASC photocatalysts was characterized by scanning electron microscope (SEM), energy dispersive X-ray Spectroscopy (EDX), X-ray diffraction analysis (XRD), UV–Vis diffuse reflectance spectra (UV–Vis DRS) and photoluminescence (PL), which indicated that the introduction of rGO was responsible for well dispersion, smaller crystalline size, red shift of absorption band and suppressing quick photo-induced charges recombination of TiO{sub 2}-rGO/ASC photocatalysts. Optimization of operational parameters with 70 °C, 8% O{sub 2} and 8% relative humidity were also obtained. Deactivation of TiO{sub 2}-rGO/ASC photocatalysts for NO removal was investigated by Fourier-transform infrared (FTIR) analysis. Regeneration experiments showed that thermal vapor regeneration would be optimal method owing to excellent regenerative capacity and inexpensive procedure.

  17. Silicon hollow sphere anode with enhanced cycling stability by a template-free method.

    Science.gov (United States)

    Chen, Song; Chen, Zhuo; Luo, Yunjun; Xia, Min; Cao, Chuanbao

    2017-04-21

    Silicon is a promising alternative anode material since it has a ten times higher theoretical specific capacity than that of a traditional graphite anode. However, the poor cycling stability due to the huge volume change of Si during charge/discharge processes has seriously hampered its widespread application. To address this challenge, we design a silicon hollow sphere nanostructure by selective etching and a subsequent magnesiothermic reduction. The Si hollow spheres exhibit enhanced electrochemical properties compared to the commercial Si nanoparticles. The initial discharge and charge capacities of the Si hollow sphere anode are 2215.8 mAh g -1 and 1615.1 mAh g -1 with a high initial coulombic efficiency (72%) at a current density of 200 mA g -1 , respectively. In particular, the reversible capacity is 1534.5 mAh g -1 with a remarkable 88% capacity retention against the second cycle after 100 cycles, over four times the theoretical capacity of the traditional graphite electrode. Therefore, our work demonstrates the considerable potential of silicon structures for displacing commercial graphite, and might open up new opportunities to rationally design various nanostructured materials for lithium ion batteries.

  18. Silicon hollow sphere anode with enhanced cycling stability by a template-free method

    Science.gov (United States)

    Chen, Song; Chen, Zhuo; Luo, Yunjun; Xia, Min; Cao, Chuanbao

    2017-04-01

    Silicon is a promising alternative anode material since it has a ten times higher theoretical specific capacity than that of a traditional graphite anode. However, the poor cycling stability due to the huge volume change of Si during charge/discharge processes has seriously hampered its widespread application. To address this challenge, we design a silicon hollow sphere nanostructure by selective etching and a subsequent magnesiothermic reduction. The Si hollow spheres exhibit enhanced electrochemical properties compared to the commercial Si nanoparticles. The initial discharge and charge capacities of the Si hollow sphere anode are 2215.8 mAh g-1 and 1615.1 mAh g-1 with a high initial coulombic efficiency (72%) at a current density of 200 mA g-1, respectively. In particular, the reversible capacity is 1534.5 mAh g-1 with a remarkable 88% capacity retention against the second cycle after 100 cycles, over four times the theoretical capacity of the traditional graphite electrode. Therefore, our work demonstrates the considerable potential of silicon structures for displacing commercial graphite, and might open up new opportunities to rationally design various nanostructured materials for lithium ion batteries.

  19. Low temperature, template-free route to nickel thin films and nanowires.

    Science.gov (United States)

    Shviro, Meital; Zitoun, David

    2012-02-07

    In this manuscript, we report on the elaboration of nickel thin films, isolated clusters and nanowires on silicon, glass and polymers by a low temperature deposition technique. The process is based on the thermal decomposition of Ni (η(4)-C(8)H(12))(2) at temperatures as low as 80 °C, which exclusively yields metallic Ni and a volatile by-product. The low temperature of the process makes it compatible with most of the substrates, even polymers and organic layers. Several deposition techniques are explored, among them spin coating of the organometallic complex in solution, which allows controlling nickel film thickness down to several nanometers. The density of the film can be varied by the speed of the spin coater with the formation of nanowires being observed for an optimized speed. The nanowires form a network of parallel lines on silicon and the phenomenon will be discussed as a selective dewetting of the organometallic precursor. All samples are fully characterized by SEM, EDS, cross-sectional HRTEM, ellipsometry, AFM, MFM and SQUID magnetic measurements. This journal is © The Royal Society of Chemistry 2012

  20. Effect of oxidation degree on the synthesis and adsorption property of magnetite/graphene nanocomposites

    Science.gov (United States)

    Luo, Kun; Mu, Yuanying; Wang, Peng; Liu, Xiaoteng

    2015-12-01

    A facile approach is demonstrated to synthesize a series of magnetite/graphene nanocomposites by solvothermal method, which can be easily collected after removal of pollutants without secondary pollution of graphene powders. Raman and FT-IR analyses show that the reduction of the mixing vapor of ammonia and hydrazine at different reaction periods generates the discrepancy of oxidation degree for reduced graphene oxide (rGO), which can be kept after the solvothermal synthesis of Fe3O4/rGO nanocomposites. Batch adsorption experiments indicate that the nanocomposite with maximum oxidation degree of rGO presents the largest magnetization of 35.4 emu g-1 and adsorption capacity of 59.2 mg g-1 for Cu2+, while the one with minimum oxidation degree exhibits the strongest adsorption of 39.0 mg g-1 for methylene blue accompanied with appropriate magnetization of 9.0 emu g-1, and only 23% of initial capacity was lost after seven recycling use. The adsorption kinetics of the both composites follows the pseudo-second-order model, suggestive of physical and chemical interactions between the pollutants and adsorbent. The results suggest that the oxidation degree of the rGO substrate can apparently influence both the structure and the adsorbing behavior of Fe3O4/rGO nanocomposites, which allows the control over the adsorbent performance according to the pollutant of interest.

  1. Synthesis of uniform CdS nanowires in high yield and its single nanowire electrical property

    International Nuclear Information System (INIS)

    Yan Shancheng; Sun Litao; Qu Peng; Huang Ninping; Song Yinchen; Xiao Zhongdang

    2009-01-01

    Large-scale high quality CdS nanowires with uniform diameter were synthesized by using a rapid and simple solvothermal route. Field emission scan electron microscopy (FESEM) and transmission electron microscopy (TEM) images show that the CdS nanowires have diameter of about 26 nm and length up to several micrometres. High resolution TEM (HRTEM) study indicates the single-crystalline nature of CdS nanowires with an oriented growth along the c-axis direction. The optical properties of the products were characterized by UV-vis absorption spectra, photoluminescence spectra and Raman spectra. The resistivity, electron concentration and electron mobility of single NW are calculated by fitting the symmetric I-V curves measured on single NW by the metal-semiconductor-metal model based on thermionic field emission theory. - Graphical abstract: Large-scale high quality CdS nanowires (NWs) with uniform diameter were synthesized by using a rapid and simple solvothermal route. The reaction time is reduced to 2 h, comparing to other synthesis which needed long reaction time up to 12 h. In addition, the as-prepared CdS nanowires have more uniform diameter and high yield. More importantly, the I-V curve of present single CdS nanowire has a good symmetric characteristic as expected by the theory.

  2. A hollow nanogold/meso-magnetite composite: pulsed laser synthesis, properties, and biosensing application

    Science.gov (United States)

    Chaudhari, Nilima; Warule, Sambhaji; Agrawal, Shailaja; Thakare, Vishal; Jouen, Samuel; Hannoyer, Beatrice; Kale, Bharat; Paknikar, Kishore; Ogale, Satishchandra

    2013-12-01

    A facile and template-free UV (Excimer) laser photolysis process is demonstrated to transform a Fe-complex into unique hollow Fe3O4 nanosphere morphology with each sphere having nanometric pores and an opening. Depending on the Fe-complex concentration and processing time interesting configurations are seen to evolve. When an identical process is applied to a mixture of Fe-complex and chloroauric acid an enthrallingly decorated Au-Fe3O4 nanostructure evolves, with Au nanoparticles surface-loaded on mesospheric Fe3O4. This room temperature process implemented under normal laboratory conditions is clearly versatile and applicable to heterojunction nanomaterials synthesis in a single-step process. The potential application of these gold-decorated magnetic nanostructures was also investigated for immuno-magnetic capture of E. coli in biosensing and these were found to be sensitive even below 1,000 cfu/ml. The test results demonstrate linear sensing response in the range of 103-105 cfu/ml. We also show that these nanostructures can be used for simple electrical conductivity-based biosensing since they show dramatic conductivity change in a simple drop-cast test.

  3. A comparative study of magnetic properties of MnFe2O4 nanoparticles prepared by thermal decomposition and solvothermal methods

    Directory of Open Access Journals (Sweden)

    B Aslibeiki

    2017-09-01

    Full Text Available A comparative study of magnetic properties of MnFe2O4 ferrite nanoparticles prepared by two different methods has been reported. The first sample (S1 was synthesized by thermal decomposition of metal nitrates. And the second sample (S2 was prepared by solvothermal method using Tri-ethylene glycol (TEG. Magnetic hysteresis loops at 300 and 5 K; magnetization and AC susceptibility measurements versus temperature confirmed the effective role of TEG on the magnetic properties of nanoparticles. The results showed that, at 300 K the saturation magnetization (MS of S2 sample is 46% greater than that of S1 sample. At 5 K, the difference in MS of the samples raised to 60%. AC susceptibility measurements at different frequencies and also magnetization versus temperature under field cooling and zero field cooling processes revealed that, the TEG molecules influence the surface spins order of S2 sample. The sample S1 showed strongly interacting superspin glass state, while the sample S2 consists of weakly interacting superparamagnetic nanoparticles.

  4. The effect of structural and optical properties on the photocatalytic efficiency of Zinc Sulphide nanoparticles obtained by hydro/solvothermal decomposition of Zinc N,N-diethyldithiocarbamate

    Science.gov (United States)

    Siqueira, G. O.; de Morais, E. C. R.; da Silva, H. V.; Abelenda, A.; González, J. C.; Porto, A. O.

    2017-06-01

    Cubic and hexagonal zinc sulphide nanoparticles were prepared by hydro/solvothermal decomposition of Zinc N,N-diethyldithiocarbamate by using different experimental conditions such as pH values, solvents and the presence of a particle stabilizer, sodium polyacrylate. The effect of these different experimental conditions on the microstructure and photocatalytical efficiency of ZnS was investigated in this work. Microstructural parameters, such as, apparent mean crystal size, microstrain and crystal size distribution were determined by analysis of experimental X-ray diffraction. Apparent mean crystal sizes were in the range of 6.5-44 nm and the lattice microstrain varied from 0.24% to 0%. Dimethylformamide showed to be more suitable than water to form small particles with a very narrow size distribution. The obtained optical band gaps and Urbach energies were in range of 3.32-3.60 eV and 0.09-0.15 eV, respectively. Photoluminescence spectra showed strong visible light emissions (green, blue and white) associated to the electronic levels introduced by the presence of superficial defects. The photocatalytic efficiency of these samples was investigated towards methylene blue degradation and a correlation between this efficiency and the PL intensity was observed. This correlation was associated to the formation of surface active centres at catalyst surfaces and the local potential fluctuations of valence and conduction bands.

  5. Solvothermal fabrication of activated semi-coke supported TiO2-rGO nanocomposite photocatalysts and application for NO removal under visible light

    Science.gov (United States)

    Yang, Weiwei; Li, Chunhu; Wang, Liang; Sun, ShengNan; Yan, Xin

    2015-10-01

    The photocatalysts of activated semi-coke supported TiO2-rGO nanocomposite (TiO2-rGO/ASC) with different contents of reduced graphene oxide were fabricated by one-step solvothermal method for NO removal under visible light irradiation. It was confirmed that 8% content of reduced graphene oxide presented the best NO photooxidation performance under visible light irradiation at 70 °C with 350-400 mg/m3 NO,5% O2 and 5% relative humidity. The reasons for improved activity were discussed, alloyed with the mechanism of producing CO. Detailed structural information of TiO2-rGO/ASC photocatalysts was characterized by scanning electron microscope (SEM), energy dispersive X-ray Spectroscopy (EDX), X-ray diffraction analysis (XRD), UV-Vis diffuse reflectance spectra (UV-Vis DRS) and photoluminescence (PL), which indicated that the introduction of rGO was responsible for well dispersion, smaller crystalline size, red shift of absorption band and suppressing quick photo-induced charges recombination of TiO2-rGO/ASC photocatalysts. Optimization of operational parameters with 70 °C, 8% O2 and 8% relative humidity were also obtained. Deactivation of TiO2-rGO/ASC photocatalysts for NO removal was investigated by Fourier-transform infrared (FTIR) analysis. Regeneration experiments showed that thermal vapor regeneration would be optimal method owing to excellent regenerative capacity and inexpensive procedure.

  6. Structure-directing coordination template effect of ethylenediamine in formations of ZnS and ZnSe nanocrystallites via solvothermal route.

    Science.gov (United States)

    Deng, Zhao-Xiang; Wang, Cheng; Sun, Xiao-Ming; Li, Ya-Dong

    2002-02-25

    ZnS and ZnSe precursors (ZnS x 0.5en and ZnSe x 0.5en, en = ethylenediamine) were prepared via a solvothermal process using ethylenediamine as solvent. Phase-pure hexagonal wurtzite ZnS and ZnSe products were obtained by annealing the precursors in argon stream at temperatures above 350 degrees C. The role of ethylenediamine as a structure-directing coordination molecular template responsible for the morphologies of the annealed products was discussed. This work provided further insights into the solvent coordination molecular template (SCMT) mechanism previously proposed to explain the growth mechanism of CdE (E = S, Se, Te) nanorods in ethylenediamine (Inorg. Chem. 1999, 38, 1382). The as-prepared precursors as well as the annealed products were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), infrared absorbance spectroscopy (IR), thermogravimetric analysis (TGA), X-ray fluorescence (XRF) analysis, and combustion analysis for C, N, H contents.

  7. Solvothermal modification of BiOCl nanosheets with Bi nanoparticles using ascorbic acid as reductant and the superoxide radicals dominated photocatalytic performance

    Science.gov (United States)

    Cui, Zhankui; Gao, Keke; Ge, Suxiang; Fa, Wenjun

    2017-11-01

    BiOCl nanosheets were solvothermally modified with Bi nanoparticles (NPs) using ascorbic acid as the reductant. The structures of Bi/BiOCl composites were characterized by XRD, Raman spectroscopy, FTIR spectroscopy and SEM. The light absorption properties were measured by UV–vis–NIR spectroscopy. The photocatalytic performances were evaluated by photodegrading methyl orange (MO) and the photocatalytic mechanism was investigated using trapping experiments and a fluorescent probe method. The results show that Bi NPs are uniformly distributed on the surfaces of BiOCl nanosheets and the modification amount of Bi NPs could be well controlled because of the mild property of ascorbic acid as reducing agent. The photocatalytic activities for the composites are improved obviously and the best photocatalytic performance is obtained when the weight ratio of Bi and BiOCl is1:10 and the photochemical reaction rate is 3.5 times that of pure BiOCl nanosheets and 19.7 times of Bi powders. The enhanced photocatalytic efficiency is ascribed to the favorable formation of dominant \\cdot O2- radicals caused by the increased photoinduced electrons from both Bi NPs and BiOCl nanosheets.

  8. Sheet-on-sheet chrysanthemum-like C/FeS microspheres synthesized by one-step solvothermal method for high-performance sodium-ion batteries

    Science.gov (United States)

    Cao, Zhenjiang; Song, Huaihe; Cao, Bin; Ma, Jing; Chen, Xiaohong; Zhou, Jisheng; Ma, Zhaokun

    2017-10-01

    Chrysanthemum-like carbon/FeS microspheres (CL-C/FeS) are prepared from a one-step solvothermal method. The morphology and structure of the CL-C/FeS are characterized by X-ray diffraction, scanning electron microscopy and high-resolution transmission electron microscope. We note that the prepared CL-C/FeS microspheres exhibit the average diameter of 15 μm and possess a sheet-on-sheet structure. FeS nanosheets are stacked on the carbon sheets to form a 2D sheet-on-sheet structure, these 2D C/FeS nanosheets are self-assembled to form a 3D chrysanthemum-like morphology. Due to the unique structure, CL-C/FeS microspheres show the excellent sodium-storage performance of 500 mAh g-1 at 0.2 A g-1 and 260 mAh g-1 at 1 A g-1, which are higher than those of most reported values. Therefore, the CL-C/FeS with appropriate structure is expected to be a competitive choice for anode materials for sodium ion batteries.

  9. Effects of non-polar solvent on the morphology and property of three-dimensional hierarchical TiO2 nanostructures by one-step solvothermal route

    Science.gov (United States)

    Zhou, Yi; Wu, Hongyan; Zhong, Xian; Liu, Ce

    2014-07-01

    Three-dimensional (3D) hierarchical rutile TiO2 microspheres composed of nanorods with diameter of several-tens of nanometers, with different morphologies and with average size ranging from 1.3 to 1.8 μm, were successfully synthesized through a surfactant-free solvothermal route. The effects of the solvents n-hexane, chloroform, and cyclohexane on the microstructures of 3D hierarchical TiO2 nanostructures were investigated. Results of scanning electron microscopy showed that 3D sea-urchin like hierarchical TiO2 composed of nanorods with a diameter of 10 nm can only be prepared in the cyclohexane-water system. The growth mechanism of 3D sea-urchin like hierarchical TiO2 composed of numerous nanorods was further examined and found to differ from the well-known "growth → assembly" mode. The effects of surface tension and polarity of solvents on the morphology and crystal strength of 3D hierarchical TiO2 nanostructure were also investigated. In addition, the prepared 3D sea-urchin like hierarchical TiO2 showed highest photocatalytic activity compared with other 3D hierarchical TiO2 nanostructures in this study and Degussa P25 for the degradation of Rhodamine B solution under UV light irradiation, which could be attributed to its special hierarchical superstructure, the increase of surface catalytic sites and its special composition units.

  10. Rare Earth Ion-Doped Upconversion Nanocrystals: Synthesis and Surface Modification

    Directory of Open Access Journals (Sweden)

    Hongjin Chang

    2014-12-01

    Full Text Available The unique luminescent properties exhibited by rare earth ion-doped upconversion nanocrystals (UCNPs, such as long lifetime, narrow emission line, high color purity, and high resistance to photobleaching, have made them widely used in many areas, including but not limited to high-resolution displays, new-generation information technology, optical communication, bioimaging, and therapy. However, the inherent upconversion luminescent properties of UCNPs are influenced by various parameters, including the size, shape, crystal structure, and chemical composition of the UCNPs, and even the chosen synthesis process and the surfactant molecules used. This review will provide a complete summary on the synthesis methods and the surface modification strategies of UCNPs reported so far. Firstly, we summarize the synthesis methodologies developed in the past decades, such as thermal decomposition, thermal coprecipitation, hydro/solvothermal, sol-gel, combustion, and microwave synthesis. In the second part, five main streams of surface modification strategies for converting hydrophobic UCNPs into hydrophilic ones are elaborated. Finally, we consider the likely directions of the future development and challenges of the synthesis and surface modification, such as the large-scale production and actual applications, stability, and so on, of the UCNPs.

  11. Facile synthesis of 5 nm NaYF₄:Yb/Er nanoparticles for targeted upconversion imaging of cancer cells.

    Science.gov (United States)

    Hu, Yueli; Wu, Boyue; Jin, Qing; Wang, Xueyuan; Li, Yan; Sun, Yuxiu; Huo, Jianzhong; Zhao, Xiaojun

    2016-05-15

    5nm intense green emission NaYF4:Yb/Er upconversion nanoparticles (UCNPs) with pure β phase was synthesized with a simple "green" strategy for the first time. Traditional organic solvothermal method is often applied to prepare the high-quality and uniform UCNPs, but the preparation of lanthanide-oleate complexes is laborious as heating and multistep post-treatment for purification are often required. The water-alcohols solvothermal method is environmentally friendly, but the fabricated UCNPs have big size, poor biocompatibility and high cytotoxicity, which limited their application for cell imaging. Herein, NaYF4:Yb/Er UCNPs were prepared with rare-earth nitrates RE(NO3)3 (RE=Y0.80 Yb0.18 Er0.02) as precursors and diethylene glycol (DEG)/ethylene glycol (EG)/water as the solvent. A facile green solvothermal method with the temperature being controlled at 300°C was developed. The as-prepared NaYF4:Yb/Er UCNPs were characterized and were found to have enhanced UC emission and controllable particle size. The as-prepared UCNPs were further functionalized via folic acid coating for the targeted imaging and improved bio- compatibility. It was made the UCNPs potential for upconversion bioimaging of living cells by the strong upconversion luminescence, the excellent biocompatibility, and the super-small size. The good colloidal stability and low cell cytotoxicity of the as-prepared UCNPs and the developed synthesis protocol might advance both the fields of UCNPs and biomolecule-based nanotechnology for future studies. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Organic synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Thomas, S.E.

    1991-01-01

    This paper reports on reactions of organoboranes. Organoboron routes to unsaturated hydrocarbons. Boronic ester homologation. Properties of organosilicon compounds. Alkene synthesis (Peterson olefination). Allylsilanes and acylsilanes.

  13. Low temperature synthesis and characterization of Na–M–(O)–F phases with M=Ti, V

    Energy Technology Data Exchange (ETDEWEB)

    Nava-Avendaño, Jessica [Institut de Ciència de Materials de Barcelona (ICMAB-CSIC), Campus UAB, E-08193 Bellaterra, Catalonia (Spain); Ayllón, José A. [Departament de Química, Universitat Autònoma de Barcelona, Campus UAB, E-08193 Bellaterra, Catalonia (Spain); Frontera, Carlos; Oró-Solé, Judith [Institut de Ciència de Materials de Barcelona (ICMAB-CSIC), Campus UAB, E-08193 Bellaterra, Catalonia (Spain); Estruga, Marc [Departament de Química, Universitat Autònoma de Barcelona, Campus UAB, E-08193 Bellaterra, Catalonia (Spain); Molins, Elies [Institut de Ciència de Materials de Barcelona (ICMAB-CSIC), Campus UAB, E-08193 Bellaterra, Catalonia (Spain); Palacín, M. Rosa, E-mail: rosa.palacin@icmab.es [Institut de Ciència de Materials de Barcelona (ICMAB-CSIC), Campus UAB, E-08193 Bellaterra, Catalonia (Spain)

    2015-03-15

    Na{sub 5}Ti{sub 3}O{sub 3}F{sub 11} was prepared by the microwave assisted method, and presents a chiolite related structure with cell parameters a=10.5016(5), b=10.4025(5), and c=10.2911(5) Å and Cmca (no. 64) space group. From solvothermal synthesis at 100 °C the cryolite Na{sub 3−δ}VO{sub 1−δ}F{sub 5+δ} was prepared, which crystallizes in the monoclinic system with a=5.5403(2), b=5.6804(2), c=7.9523(2) Å, β=90.032(7)° cell parameters and P2{sub 1}/n (no. 14) space group. Under similar synthesis conditions but with higher HF concentration the chiolite-type phase Na{sub 5−δ}V{sub 3}F{sub 14} was achieved, which exhibits a=10.5482(2), b=10.4887(1) and c=10.3243(1) Å cell parameters and Cmc2{sub 1} (no. 36) space group. A single crystal also having the chiolite structure was synthesized at 200 °C which exhibits tetragonal symmetry (a=7.380(3) and c=10.381(11) Å and space group P4{sub 2}2{sub 1}2 (no. 94)). Bond valence sum indicates that it contains V{sup 4+} and therefore can be formulated as Na{sub 5}V{sub 3}O{sub 3}F{sub 11}. - Graphical abstract: Na{sub 5}M{sub 3}(O,F){sub 14} with M=Ti and V having chiolite structure and Na{sub 3−δ}VO{sub 1−δ}F{sub 5+δ} cryolite were prepared by means of microwave-assisted and solvothermal synthesis. - Highlights: • Na{sub 5}Ti{sub 3}O{sub 3}F{sub 11} chiolite was prepared by a microwave assisted method and characterized. • Na{sub 3−δ}VO{sub 1−δ}F{sub 5+δ} and Na{sub 5−δ}V{sub 3}F{sub 14} were prepared by solvothermal synthesis. • The compounds were structurally characterized by diffraction techniques. • O/F distribution was estimated by applying Pauling’s second rule.

  14. Multicolor upconversion emission of dispersed ultrasmall cubic Sr{sub 2}LuF{sub 7} nanocrystals synthesized by a solvothermal process

    Energy Technology Data Exchange (ETDEWEB)

    Gong, Lunjun; Ma, Mo [Key Laboratory of Low Dimensional Materials and Application Technology (Xiangtan University), Ministry of Education, Xiangtan 411105 (China); Institute of Modern Physics, Faculty of Materials, Optoelectronics and Physics, Xiangtan university, Xiangtan 411105 (China); Xu, Changfu, E-mail: xcfyang@yahoo.com.cn [Key Laboratory of Low Dimensional Materials and Application Technology (Xiangtan University), Ministry of Education, Xiangtan 411105 (China); Institute of Modern Physics, Faculty of Materials, Optoelectronics and Physics, Xiangtan university, Xiangtan 411105 (China); Li, Xujun [Key Laboratory of Low Dimensional Materials and Application Technology (Xiangtan University), Ministry of Education, Xiangtan 411105 (China); Wang, Suiping [Department of Food and Bioengineering, College of Chemical Engineering, Xiangtan University, Xiangtan 411105 (China); Lin, Jianguo [Key Laboratory of Low Dimensional Materials and Application Technology (Xiangtan University), Ministry of Education, Xiangtan 411105 (China); Yang, Qibin [Key Laboratory of Low Dimensional Materials and Application Technology (Xiangtan University), Ministry of Education, Xiangtan 411105 (China); Institute of Modern Physics, Faculty of Materials, Optoelectronics and Physics, Xiangtan university, Xiangtan 411105 (China)

    2013-02-15

    Lanthanide (Ln{sup 3+}) doped Sr{sub 2}LuF{sub 7} (Ln{sup 3+}=Er{sup 3+}/Tm{sup 3+}/Yb{sup 3+}) nanocrystals (NCs) were synthesized via a solvothermal process using oleate as stabilizing agent. The as-synthesized NCs with a mean diameter of sub-20 nm can be well dispersed in cyclohexane and show a pure cubic phase structure with space group Fm3{sup Macron }m. Following appropriate lanthanide ion doping, the NCs show intense red, green, blue and white-color upconversion emission (UC) under the excitation of a 980 nm laser. Predominant near-infrared UC can also be obtained in the Yb{sup 3+}/Tm{sup 3+} doped Sr{sub 2}LuF{sub 7} NCs. The energy transfer UC mechanisms for the fluorescent intensity were also investigated. The desirable property of the ultrasmall dispersed NCs makes them promising materials for the applications in miniaturized solid-state light sources, multicolor three-dimensional display devices and fluorescent labels for biomedical imaging. - Highlights: Black-Right-Pointing-Pointer Cubic-structure (Fm3{sup Macron }m) Sr{sub 2}LuF{sub 7} nanocrystals were synthesized for the first time. Black-Right-Pointing-Pointer Nanocrystals (sub-20 nm) with cubic or spherical shape can be well dispersed. Black-Right-Pointing-Pointer By doping properly, the nanocrystals show intense multicolor upconversion. Black-Right-Pointing-Pointer Predominant near-infrared upconversion can be obtained in Sr{sub 2}LuF{sub 7} nanocrystals. Black-Right-Pointing-Pointer Upconversion mechanism for the fluorescent intensity is mainly energy transfer.

  15. Aqueous hydrodechlorination of 4-chlorophenol over an Rh/reduced graphene oxide synthesized by a facile one-pot solvothermal process under mild conditions

    Energy Technology Data Exchange (ETDEWEB)

    Ren, Yanlin [Chemical Synthesis and Pollution Control, Key Laboratory of Sichuan Province, College of Chemistry and Chemical Industry, China West Normal University, Nanchong 637002 (China); Fan, Guangyin, E-mail: fanguangyin@cwnu.edu.cn [Chemical Synthesis and Pollution Control, Key Laboratory of Sichuan Province, College of Chemistry and Chemical Industry, China West Normal University, Nanchong 637002 (China); Wang, Chenyu [Department of Chemistry, State University of New York at Binghamton, Binghamton, NY 13902 (United States)

    2014-06-01

    Graphical abstract: The Rh nanoparticles/reduced graphene oxide (Rh NPs/RGO) nanocatalyst synthesized by a solvothermal technique showed high activity and stability for the hydrodechlorination of 4-chlorophenol under mild conditions. - Highlights: • Rh/RGO was synthesized through a one-pot polyol reduction of GO and RhCl{sub 3}. • Complete HDC of 4-chlorophenol was obtained in aqueous phase without any additive. • The Rh/RGO exhibited an excellent catalytic performance for HDC reaction. - Abstract: Reduced graphene oxide (RGO) supported rhodium nanoparticles (Rh-NPs/RGO) was synthesized through one-pot polyol co-reduction of graphene oxide (GO) and rhodium chloride. The catalytic property of Rh-NPs/RGO was investigated for the aqueous phase hydrodechlorination (HDC) of 4-chlorophenol (4-CP). A complete conversion of 4-CP into high valued products of cyclohexanone (selectivity: 23.2%) and cyclohexanol (selectivity: 76.8%) was successfully achieved at 303 K and balloon hydrogen pressure in a short reaction time of 50 min when 1.5 g/L of 4-CP was introduced. By comparing with Rh-NPs deposited on the other supports, Rh-NPs/RGO delivered the highest initial rate (111.4 mmol/g{sub Rh} min) for 4-CP HDC reaction under the identical conditions. The substantial catalytic activity of Rh-NPs/RGO can be ascribed to the small and uniform particle size of Rh (average particle size was 1.7 ± 0.14 nm) on the surface of the RGO sheets and an electron-deficient state of Rh in the catalyst as a result of the strong interaction between the active sites and the surface function groups of RGO.

  16. Visible light photocatalysts (Fe, N):TiO{sub 2} from ammonothermally processed, solvothermal self-assembly derived Fe-TiO{sub 2} mesoporous microspheres

    Energy Technology Data Exchange (ETDEWEB)

    Zou, Mingming; Xiong, Fengqiang; Ganeshraja, Ayyakannu Sundaram [Dalian Institute of Chemical Physics (DICP), Chinese Academy of Sciences, 457 Zhongshan Road, Dalian, Liaoning, 116023 (China); Feng, Xiaohua; Wang, Chuanxi [Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Ningbo, 315201 (China); Thomas, Tiju, E-mail: tijuthomas@iitm.ac.in [Department of Metallurgical and Materials Engineering, Indian Institute of Technology Madras, Chennai, 600036, Tamil Nadu (India); Yang, Minghui, E-mail: myang@dicp.ac.cn [Dalian Institute of Chemical Physics (DICP), Chinese Academy of Sciences, 457 Zhongshan Road, Dalian, Liaoning, 116023 (China)

    2017-07-01

    Iron (III) and nitrogen co-doped mesoporous TiO{sub 2} microspheres (Fe-N-TiO{sub 2}) are prepared using a self-assembly based solvothermal process followed by an ammonothermal method. Among all samples, 1 mol.% of Fe dopants and 500 °C nitridation (for 2 h) gives the highest visible light photoactivity. Results imply that the Fe{sup 3+}/Fe{sup 2+} dopant trap energy level introduced within the band gap in mildly Fe (∼1 at%) doped TiO{sub 2} and the mesoporous nature of the material, both aid in the observed catalytic performance. Subjecting Fe-TiO{sub 2} samples to ammonothermal process induces oxygen vancancies, and substitutional and interstitial N. This reduces optical band gap, and introduces local states. The lower band gap and local states together aid in the absorption of visible light and separation of charge carriers. Co-dopants are distributed uniformly in the best photocatalysts. The active species generated in the photocatalytic system is shown to be singlet molecular oxygen ({sup 1}O{sub 2}) using selective radical quenchers. - Highlights: • Iron (III) and nitrogen co-doped mesoporous TiO{sub 2} microspheres (Fe-N-TiO{sub 2}) are prepared. • Fe{sup 3+}/Fe{sup 2+} dopant trap energy level introduced within the band gap in Fe (∼1 at%) doped TiO{sub 2}. • Subjecting Fe-TiO{sub 2} samples to ammonothermal process induces oxygen vancancies, and causes substitutional and interstitial N. • Co-dopants are distributed uniformly in the best photocatalysts. • Active species generated is shown to be singlet molecular oxygen ({sup 1}O{sub 2}).

  17. A facile synthesis of gold micro/nanostructures at the interface of 1,3-dibutylimidazolium bis(trifluoromethylsulfonyl)imide and water.

    Science.gov (United States)

    Yao, Kaisheng; Huang, Qingling; Lu, Weiwei; Xu, Airong; Li, Xinying; Zhang, Hucheng; Wang, Jianji

    2016-10-15

    The development of a simple, template-free, and one-step strategy to synthesize nanostructured Au architectures with fascinating morphology is highly desirable and technically important due to their valuable applications in varied fields. In this work, the "green" strategy of "tunable ionic liquids-water (ILs-H2O) interfacial synthesis" developed previously by us is utilized for feasible synthesis of gold needle mushroom-like micro/nanostructures at the 1,3-dibutylimidazolium bis(trifluoromethylsulfonyl)imide ([C4bim][Tf2N]) - water interface and ambient conditions. The as-obtained gold needle mushrooms (AuNMs) have been characterized and analyzed systemically by scanning electron microscopy, X-ray powder diffraction, energy-dispersive X-ray spectroscopy, and transmission electron microscopy. It is shown that the as-prepared AuNMs can be used as substrates to perform surface enhanced Raman scattering (SERS) investigation with striking SERS sensitivity. By employing ILs with different alkyl chain lengths of the imidazolium cations and/or different nature of anions, Au nanomaterials with diverse morphologies can be easily prepared at different ILs-H2O interfaces. Based on the analysis of the control experiments, the growth and formation of AuNMs at the [C4bim][Tf2N]-H2O interface have been discussed. Copyright © 2016 Elsevier Inc. All rights reserved.

  18. Fire Synthesis

    Indian Academy of Sciences (India)

    1000ºC or special infrastructure which require careful maintenance. In such a situation fire synthesis is a simpler method that can be adopted for the bulk production of high purity alumina and related oxides. Fire Synthesis. Preparation of Alumina ...

  19. Controllable synthesis of TiO2 nanomaterials by assisting with l-cysteine and ethylenediamine

    KAUST Repository

    Tao, Yugui

    2013-11-21

    This paper reports a facile l-cysteine-assisted solvothermal synthesis of TiO2 nanomaterials using ethylenediamine (En) and distilled water as solvent. The influence of reaction time, temperature, l-cysteine and solvent was initially investigated. Results demonstrated the reaction temperature, l-cysteine and En significantly imposed impact on the phase and morphology of the particles. Amorphous nanosheets, mixed-crystal nanorods and pure anatase nanoparticles were controllably synthesized by varying reaction temperature. The formation of the amorphous nanosheets and mixed-crystal nanorods were directly affected by the presence of l-cysteine and En. And the presence of En distinctly affected the crystal phase of the products, which was rarely mentioned in other studies. Moreover, the photocatalytic activities of three typical samples were excellent. The possible formation mechanism of the sample was also discussed. © 2013 Springer Science+Business Media New York.

  20. Structural, optical and magnetic studies of CuFe2O4, MgFe2O4 and ZnFe2O4 nanoparticles prepared by hydrothermal/solvothermal method

    Science.gov (United States)

    Kurian, Jessyamma; Mathew, M. Jacob

    2018-04-01

    In this paper we report the structural, optical and magnetic studies of three spinel ferrites namely CuFe2O4, MgFe2O4 and ZnFe2O4 prepared in an autoclave under the same physical conditions but with two different liquid medium and different surfactant. We use water as the medium and trisodium citrate as the surfactant for one method (Hydrothermal method) and ethylene glycol as the medium and poly ethylene glycol as the surfactant for the second method (solvothermal method). The phase identification and structural characterization are done using XRD and morphological studies are carried out by TEM. Cubical and porous spherical morphologies are obtained for hydrothermal and solvothermal process respectively without any impurity phase. The optical studies are carried out using FTIR and UV-Vis reflectance spectra. In order to elucidate the nonlinear optical behaviour of the prepared nanomaterial, open aperture z-scan technique is used. From the fitted z-scan curves nonlinear absorption coefficient and the saturation intensity are determined. The magnetic characterization of the samples is performed at room temperature using vibrating sample magnetometer measurements. The M-H curves obtained are fitted using theoretical equation and the different components of magnetization are determined. Nanoparticles with high saturation magnetization are obtained for MgFe2O4 and ZnFe2O4 prepared under solvothermal reaction. The magnetic hyperfine parameters and the cation distribution of the prepared materials are determined using room temperature Mössbauer spectroscopy. The fitted spectra reveal the difference in the magnetic hyperfine parameters owing to the change in size and morphology.

  1. Synthesis, structural characterization and luminescent properties of a novel europium ternary complex Eu(2-A-4-CBA)3phen

    International Nuclear Information System (INIS)

    Chen, Yongjie; Wu, Shengnan; Xing, Zhenfang; Cao, Shuang; Geng, Xiujuan; Yang, Ying; Xiao, Linjiu

    2015-01-01

    The preparation of a novel europium ternary complex with the formula of Eu(2-A-4-CBA) 3 phen (where, 2-A-4-CBA = 2-amino-4-chlorobenzoic acid, phen = 1,10-phenanthroline) under solvothermal condition is described. The composition and structure of the resulting complex were investigated by elemental analysis, Fourier transform infrared (FT-IR) spectroscopy. The complex is polycrystalline, and the morphology is clean and regular as revealed by scanning electron microscope (SEM). The luminescent and thermal properties of the complex were researched by fluorescence spectroscopy and thermogravimetric analysis, respectively. Of importance here is that, the room-temperature luminescence spectra of the complex show strong characteristic emission of the corresponding Eu 3+ , which is attributed to the energy transfer from ligands to Eu 3+ via an Antenna effect. It is also found that the complex exhibits pure red light and high color purity. In addition, the complex does not decompose until 300 °C, so it exhibits good thermal stability. - Highlights: • A novel Eu(III) complex was synthesized by solvothermal synthesis method. • The structure and properties of complex were studied. • The complex can emits pure red light and has a high color purity. • The complex does not decompose until 300 °C and it has a good thermal stability

  2. A Facile Synthesis of Hollow Palladium/Copper Alloy Nanocubes Supported on N-Doped Graphene for Ethanol Electrooxidation Catalyst

    Directory of Open Access Journals (Sweden)

    Zhengyu Bai

    2015-04-01

    Full Text Available In this paper, a catalyst of hollow PdCu alloy nanocubes supported on nitrogen-doped graphene support (H-PdCu/ppy-NG is successfully synthesized using a simple one-pot template-free method. Two other catalyst materials such as solid PdCu alloy particles supported on this same nitrogen-doped graphene support (PdCu/ppy-NG and hollow PdCu alloy nanocubes supported on the reduced graphene oxide support (H-PdCu/RGO are also prepared using the similar synthesis conditions for comparison. It is found that, among these three catalyst materials, H-PdCu/ppy-NG gives the highest electrochemical active area and both the most uniformity and dispersibility of H-PdCu particles. Electrochemical tests show that the H-PdCu/ppy-NG catalyst can give the best electrocatalytic activity and stability towards the ethanol electrooxidation when compared to other two catalysts. Therefore, H-PdCu/ppy-NG should be a promising catalyst candidate for anodic ethanol oxidation in direct ethanol fuel cells.

  3. 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.

  4. Optimization on electrochemical synthesis of HKUST-1 as candidate catalytic material for Green diesel production

    Science.gov (United States)

    Lestari, W. W.; Nugraha, R. E.; Winarni, I. D.; Adreane, M.; Rahmawati, F.

    2016-04-01

    In the effort to support the discovery of new renewable energy sources in Indonesia, biofuel is one of promising options. The conversion of vegetable oil into ready-biofuel, especially green diesel, needs several steps, one of which is a hydrogenation or hydro-deoxygenation reaction. In this case, the catalyst plays a very important role regarding to its activity and selectivity, and Metal-Organic Frameworks (MOFs) becoming a new generation of heterogeneous catalyst in this area. In this research, a preliminary study to optimize electrochemical synthesis of the catalytic material based on MOFs, namely HKUST-1 [Cu3(BTC)2], has been conducted. Some electrochemical reaction parameters were tested, for example by modifying the electrochemical synthetic conditions, i.e. by performing variation of voltages (12, 13, 14, and 15 Volt), temperatures (RT, 40, 60, and 80 °C) and solvents (ethanol, water, methanol and dimethyl-formamide (DMF)). Material characterization was carried out by XRD, SEM, FTIR, DTA/TG and SAA. The results showed that the optimum synthetic conditions of HKUST-1 are performed at room temperature in a solvent combination of water: ethanol (1: 1) and a voltage of 15 Volt for 2 hours. The XRD-analysis revealed that the resulted peaks are identical to the simulated powder pattern generated from single crystal data and comparable to the peaks of solvothermal method. However, the porosity of the resulting material through electrochemical method is still in the range of micro-pore according to IUPAC and 50% smaller than the porosity resulted from solvothermal synthesis. The corresponding compounds are thermally stable until 300 °C according to TG/DTA.

  5. Organic synthesis

    International Nuclear Information System (INIS)

    Lallemand, J.Y.; Fetizon, M.

    1988-01-01

    The 1988 progress report of the Organic Synthesis Chemistry laboratory (Polytechnic School, France), is presented. The laboratory activities are centered on the chemistry of natural products, which have a biological activity and on the development of new reactions, useful in the organic synthesis. The research works involve the following domains: the natural products chemistry which are applied in pharmacology, the plants and insects chemistry, the organic synthesis, the radical chemistry new reactions and the bio-organic physicochemistry. The published papers, the congress communications and the thesis are listed [fr

  6. Structural diversity of four coordination polymers based on 5-nitro-1,2,3-benzenetricarboxylic acid (H3nbta): Solvothermal syntheses, structural characterizations and properties

    Science.gov (United States)

    Shi, Chenjie; Wang, Zikai; Chen, Yifan; Zhang, Xiaoyu; Zhao, Yue; Tao, Yuehong; Wu, Hua

    2017-09-01

    Four 3D coordination compounds, named [Cd3(nbta)2(bix)2(H2O)2]·H2O (1), Zn3(nbta)2(biim)3 (2), Zn6(nbta)4(btd)5 (3) and [Co3(nbta)2(bid)(H2O)8]·4H2O (4) (bix=1,4-bis(imidazole-1-ylmethyl)benzene, biim=1,1‧-(1,4-butanediyl)bis(imidazole), btd=1,10-bis(1,2,4-triazol-1-yl)decane, bid=1,10-bis(imidazole-1-yl)decane), and H3nbta=5-nitro-1,2,3-benzenetricarboxylic acid), have been synthesized by solvothermal methods and structurally characterized by X-ray diffraction studies. In compound 1, every nbta3- anion connects four CdII ions to give a 2D layer, and the layers are pillared by bix ligands to generate a 3D framework with a Schläfli symbol of (3·4·63·7)(4·64·8)(43·63)(34·42·66·76·88·92). For compound 2, every nbta3- anion connects three ZnII ions to give a 2D layer structure, the 2D layers are further connected into a facinating 3D framework by biim ligands with (3,4)-connected (3·6·7)(3·5·62·7·8)(3·52·6·8·9)(5·6·8·10·112) topology. In compound 3, the nbta3- anions are connected by ZnII ions to generate a 2D layer, and the layers are bridged by btd ligands to build a fascinating 3D framework with (4·6·7·8·92)(4·6·8·92·10)(4·93·102)(4·6·8·9·102)(4·6·7·8·9·10)(4·6·7·8·102)(42·6·7·8·9) topology. In compound 4, the nbta3- aions are connected by CoII ions into a 2D layer, the 2D layers are linked by bid ligands to generate a 3D 103 topological framework. Furthermore, the IR spectra, TGA, PXRD, elemental analyses, the solid-state luminescence of compounds 1-3 have been studied.

  7. Heterostructure of Au nanocluster tipping on a ZnS quantum rod: controlled synthesis and novel luminescence.

    Science.gov (United States)

    Tian, Yang; Wang, Ligang; Yu, Shanshan; Zhou, Weiwei

    2015-08-14

    Heterostructures of metal nanoparticles and semiconductors are widely studied for their unique properties. However, few reports are available on the heterostructure of metal nanoclusters and semiconductors. In the present study, a heterostructure, in which gold nanoclusters selectively locate at ZnS quantum rod (QR) tips, was fabricated using a two-step solvothermal route. The composition, intrinsic crystallography, and junction of the prepared heterostructure were thoroughly investigated, and it was observed to exhibit novel luminescent behaviours. By comparison with the individual components of ZnS QRs and gold clusters, the resultant heterostructure shows an enhanced exciton emission and complete depression of defect emission for the ZnS component, and a pronounced red emission for the gold nanocluster component. The mechanism of these properties and the charge transfer between gold nanoclusters and ZnS QRs were also explored. The size and location of gold in the heterostructure were also controlled during synthesis to study their effects on the luminescence.

  8. An Alternative Synthesis Route of LiFePO4-Carbon Composites for Li-Ion Cathodes

    Directory of Open Access Journals (Sweden)

    Yongbing Lou

    2013-01-01

    Full Text Available LiFePO4-Carbon (LFP/C composites with high purity and good crystallinity were prepared by an improved environmentally benign and low-cost solvothermal method. Capping agent polyvinylpyrrolidone (PVP and polyethylene glycol (PEG-400 showed no significant dispersive effect during the synthesis. These capping agents were converted into networking carbons after annealing, which consequently improved the charge and discharge performance. It was able to deliver a high initial discharge specific capacity of 154.1 mAh g−1 for sample prepared with PVP and 145.6 mAh g−1 for sample prepared with PEG-400 while having great capacity retention. The rate capability and cycling performance of LFP/C samples prepared with PVP or PEG-400 at high current rates were significantly improved compared to the LFP/C sample prepared without a capping agent.

  9. Nickel hydroxides and related materials: a review of their structures, synthesis and properties

    Science.gov (United States)

    Hall, David S.; Lockwood, David J.; Bock, Christina; MacDougall, Barry R.

    2015-01-01

    This review article summarizes the last few decades of research on nickel hydroxide, an important material in physics and chemistry, that has many applications in engineering including, significantly, batteries. First, the structures of the two known polymorphs, denoted as α-Ni(OH)2 and β-Ni(OH)2, are described. The various types of disorder, which are frequently present in nickel hydroxide materials, are discussed including hydration, stacking fault disorder, mechanical stresses and the incorporation of ionic impurities. Several related materials are discussed, including intercalated α-derivatives and basic nickel salts. Next, a number of methods to prepare, or synthesize, nickel hydroxides are summarized, including chemical precipitation, electrochemical precipitation, sol–gel synthesis, chemical ageing, hydrothermal and solvothermal synthesis, electrochemical oxidation, microwave-assisted synthesis, and sonochemical methods. Finally, the known physical properties of the nickel hydroxides are reviewed, including their magnetic, vibrational, optical, electrical and mechanical properties. The last section in this paper is intended to serve as a summary of both the potentially useful properties of these materials and the methods for the identification and characterization of ‘unknown’ nickel hydroxide-based samples. PMID:25663812

  10. An unconventional rapid synthesis of high performance metal-organic framework membranes.

    Science.gov (United States)

    Shah, Miral N; Gonzalez, Mariel A; McCarthy, Michael C; Jeong, Hae-Kwon

    2013-06-25

    Metal-organic frameworks (MOFs) are attractive for gas separation membrane applications due to their microporous channels with tunable pore shape, size, and functionality. Conventional MOF membrane fabrication techniques, namely in situ and secondary growth, pose challenges for their wider commercial applications. These challenges include reproducility, scalability, and high manufacturing cost. Recognizing that the coordination chemistry of MOFs is fundamentally different from the covalent chemistry of zeolites, we developed a radically different strategy for MOF membrane synthesis. Using this new technique, we were able to produce continuous well-intergrown membranes of prototypical MOFs, HKUST-1 and ZIF-8, in a relatively short period of time (tens of min). With a minimal consumption of precursors and a greatly simplified synthesis protocol, our new technique provides potential for a continuous, scalable, reproducible, and easily commercializable route for the rapid synthesis of MOF membranes. RTD-prepared MOF membranes show greatly improved gas separation performances as compared to those prepared by conventional solvothermal methods, indicating improved membrane microstructure.

  11. Synthesis of Metal-organic Frameworks Based on Zr4+ and Benzene 1,3,5-Tricarboxylate Linker as Heterogeneous Catalyst in the Esterification Reaction of Palmitic Acid

    Science.gov (United States)

    Larasati, I.; Winarni, D.; Putri, F. R.; Hanif, Q. A.; Lestari, W. W.

    2017-07-01

    The conversion of the biomass into biodiesels via catalytic esterification and trans-esterification became an interesting topic due to the depletion of fossil-based energy. Homogenous catalysts such as HCl, H2SO4 and NaOH commonly used as catalyst, however, the use of this kind of catalyst causes more problems, such as the difficulties on the separation from the product and the pollution effect on the environment. Heterogeneous catalysts, such as Metal-Organic Frameworks (MOFs) give an alternative promising way to substitute these limitations due to their strong catalytic site, porosity, high specific surface area, and easy-separation and reusable properties. Herein, we reported the synthesis of MOFs based on zirconium(IV) and H3BTC linker (H3BTC = benzene-1,3,5-tricarboxylic acid) by solvothermal and reflux method. Solvothermal reaction at 120 °C was found to be the optimum method, that was indicated by most crystalline product compared to the simulated pattern in XRD analysis. The formation of the framework was characterized by FTIR analysis, which showed a significant shift from 1722 cm-1 to 1620 cm-1. The synthesized Zr(IV)-BTC was thermally stable up to 322°C as shown by TG/DTA analysis. This high thermal stability was related to the high oxidation state of Zr(IV), which give a significant covalent character to the Zr-O bond.

  12. Synthesis of dual temperature - and pH-responsive yolk-shell nanoparticles by conventional etching and new deswelling approaches: DOX release behavior.

    Science.gov (United States)

    Nikravan, Goolia; Haddadi-Asl, Vahid; Salami-Kalajahi, Mehdi

    2018-05-01

    Dual stimuli-responsive yolk-shell nanoparticles with cross-linked poly(acrylic acid) (PAA) pH-responsive core and cross-linked poly(2-hydroxyethyl methacrylate) (PHEMA) temperature-responsive shell were synthesized via two different methods In the first method, silica encapsulated PAA (PAA@SiO 2 ) was used as seed in distillation precipitation polymerization (DPP) of HEMA to yield PAA@SiO 2 @PHEMA from which silica layer was etched by HF solution to produce yolk-shell PAA@air@PHEMA nanoparticles. In the second method, swollen PAA nanoparticles at pH = 10 were used as seeds in emulsion polymerization of HEMA to yield core-shell PAA@PHEMA nanoparticles. After dispersion of PAA@PHEMA nanoparticles in acidic medium at pH = 2, yolk-shell nanoparticles were formed through deswelling of pH-responsive cores due to protonation of carboxyl groups. Synthesized nanoparticles were characterized using FT-IR, FE-SEM and TEM methods to observe yolk-shell nanostructure for both synthesis routes. Stimuli-responsive behavior of the nanoparticles was investigated by UV-vis spectrometer where similar behaviors were obtained for template-assisted and template-free synthesized yolk-shell nanoparticles. Finally, both yolk-shell nanoparticles were examined as potential carriers for controlled release of doxorubicin hydrochloride (DOX) anti-cancer drug. Copyright © 2018 Elsevier B.V. All rights reserved.

  13. Fire Synthesis

    Indian Academy of Sciences (India)

    her PhD degree from. Bangalore University. She is currently working as a Research Associate at the Department of. Inorganic and Physical. Chemistry, Indian. Institute of Science,. Bangalore, on the synthesis of .... This method uses the experiences of propellant chemistry in making the redox mixture. The . stoichiometry or ...

  14. Fire Synthesis

    Indian Academy of Sciences (India)

    special infrastructure which require careful maintenance. In such situation fire synthesis is a simpler method that can be adopted for the bulk production of high purity .... reaction between Ti and B to form titanium boride. The reaction between titanium (fuel- electron donor) and boron (oxidiser-electron acceptor) once initiated ...

  15. Fire Synthesis

    Indian Academy of Sciences (India)

    Home; Journals; Resonance – Journal of Science Education; Volume 16; Issue 12. Fire Synthesis - Preparation of Alumina Products. Tanu Mimani. Volume 16 Issue 12 December 2011 pp 1324-1332. Fulltext. Click here to view fulltext PDF. Permanent link: http://www.ias.ac.in/article/fulltext/reso/016/12/1324-1332 ...

  16. Fire Synthesis

    Indian Academy of Sciences (India)

    Home; Journals; Resonance – Journal of Science Education; Volume 5; Issue 2. Fire Synthesis - Preparation of Alumina Products. Tanu Mimani. General Article Volume 5 Issue 2 February 2000 pp 50-57. Fulltext. Click here to view fulltext PDF. Permanent link: http://www.ias.ac.in/article/fulltext/reso/005/02/0050-0057 ...

  17. Synthesis engineering of iron oxide raspberry-shaped nanostructures.

    Science.gov (United States)

    Gerber, O; Pichon, B P; Ihiawakrim, D; Florea, I; Moldovan, S; Ersen, O; Begin, D; Grenèche, J-M; Lemonnier, S; Barraud, E; Begin-Colin, S

    2017-01-07

    Magnetic porous nanostructures consisting of oriented aggregates of iron oxide nanocrystals display very interesting properties such as a lower oxidation state of magnetite, and enhanced saturation magnetization in comparison with individual nanoparticles of similar sizes and porosity. However, the formation mechanism of these promising nanostructures is not well understood, which hampers the fine tuning of their magnetic properties, for instance by doping them with other elements. Therefore the formation mechanism of porous raspberry shaped nanostructures (RSNs) synthesized by a one-pot polyol solvothermal method has been investigated in detail from the early stages by using a wide panel of characterization techniques, and especially by performing original in situ HR-TEM studies in temperature. A time-resolved study showed the intermediate formation of an amorphous iron alkoxide phase with a plate-like lamellar structure (PLS). Then, the fine investigation of PLS transformation upon heating up to 500 °C confirmed that the synthesis of RSNs involves two iron precursors: the starting one (hydrated iron chlorides) and the in situ formed iron alkoxide precursor which decomposes with time and heating and contributes to the growth step of nanostructures. Such an understanding of the formation mechanism of RSNs is necessary to envision efficient and rational enhancement of their magnetic properties.

  18. Synthesis and characterization of pharmaceutical surfactant templated mesoporous silica: Its application to controlled delivery of duloxetine

    Energy Technology Data Exchange (ETDEWEB)

    Mani, Ganesh; Pushparaj, Hemalatha; Peng, Mei Mei; Muthiahpillai, Palanichamy [Department of Chemical Engineering, Hanseo University, Seosan-si 356 706 (Korea, Republic of); Udhumansha, Ubaidulla [Department of Chemical Engineering, Hanseo University, Seosan-si 356 706 (Korea, Republic of); Department of Pharmaceutics, C.L. Baid Metha College of Pharmacy, Chennai (India); Jang, Hyun Tae, E-mail: htjang@hanseo.ac.kr [Department of Chemical Engineering, Hanseo University, Seosan-si 356 706 (Korea, Republic of)

    2014-03-01

    Graphical abstract: - Highlights: • Usefulness of dual pharmaceutical surfactants in silica synthesis was evaluated. • Effects of concentration of secondary template (Tween-40) were studied. • Effects of fixed solvothermal condition on mesostructure formation were studied. • Duloxetine drug loading capability was studied. • Sustained release of duloxetine was evaluated. - Abstract: A new group of mesoporous silica nanoparticles (MSNs) were synthesized using combination pharmaceutical surfactants, Triton X-100 and Tween-40 as template and loaded with duloxetine hydrochloride (DX), for improving the sustained release of DX and patterns with high drug loading. Agglomerated spherical silica MSNs were synthesized by sol–gel and solvothermal methods. The calcined and drug loaded MSNs were characterized using X-ray diffraction (XRD), Braunner–Emmett–Teller (BET), thermogravimetric analysis (TGA), Fourier-transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), diffuse reflectance ultraviolet–visible (DRS-UV–vis) spectroscopy. MSNs with high surface area and pore volume were selected and studied for their DX loading and release. The selected MSNs can accommodate a maximum of 34% DX within it. About 90% was released at 200 h and hence, the synthesized MSNs were capable of engulfing DX and sustain its release. Further form the Ritger and Peppas, Higuchi model for mechanism drug release from all the MSN matrices follows anomalous transport or Non-Fickian diffusion with the ‘r’ and ‘n’ value 0.9 and 0.45 < n < 1, respectively. So, from this study it could be concluded that the MSNs synthesized using pharmaceutical templates were better choice of reservoir for the controlled delivery of drug which requires sustained release.

  19. Synthesis, characterization, and applications of electroactive polymeric nanostructures for organic coatings

    Science.gov (United States)

    Suryawanshi, Abhijit Jagnnath

    Electroactive polymers (EAP) such as polypyrrole (PPy) and polyaniline (PANI) are being explored intensively in the scientific community. Nanostructures of EAPs have low dimensions and high surface area enabling them to be considered for various useful applications. These applications are in several fields including corrosion inhibition, capacitors, artificial muscles, solar cells, polymer light emitting diodes, and energy storage devices. Nanostructures of EAPs have been synthesized in different morphologies such as nanowires, nanorods, nanotubes, nanospheres, and nanocapsules. This variety in morphology is traditionally achieved using soft templates, such as surfactant micelles, or hard templates, such as anodized aluminum oxide (AAO). Templates provide stability and groundwork from which the polymer can grow, but the templates add undesirable expense to the process and can change the properties of the nanoparticles by integrating its own properties. In this study a template free method is introduced to synthesize EAP nanostructures of PPy and PANI utilizing ozone oxidation. The simple techniques involve ozone exposure to the monomer solution to produce aqueous dispersions of EAP nanostructures. The synthesized nanostructures exhibit uniform morphology, low particle size distribution, and stability against agglomeration. Ozone oxidation is further explored for the synthesis of silver-PPy (Ag-PPy) core-shell nanospheres (CSNs). Coatings containing PPy nanospheres were formulated to study the corrosion inhibition efficiency of PPy nanospheres. Investigation of the coatings using electrochemical techniques revealed that the PPy nanospheres may provide corrosion inhibition against filiform corrosion by oxygen scavenging mechanism. Finally, organic corrosion inhibitors were incorporated in PPy to develop efficient corrosion inhibiting systems, by using the synergistic effects from PPy and organic corrosion inhibitors.

  20. Solvothermal syntheses of Bi and Zn co-doped TiO2 with enhanced electron-hole separation and efficient photodegradation of gaseous toluene under visible-light

    International Nuclear Information System (INIS)

    Li, Juan-Juan; Cai, Song-Cai; Xu, Zhen; Chen, Xi; Chen, Jin; Jia, Hong-Peng; Chen, Jing

    2017-01-01

    Highlights: • Bi-Zn co-doped TiO 2 catalysts were prepared by solvothermal route. • The incorporation of Bi doping into the TiO 2 generates intermediate energy levels. • Bi and Zn doping showed the enhanced absorption in visible-light region. • Zn dopant acts as a mediator of interfacial charge transfer. • TiBi 1.9% Zn 1% O 2 exhibited high photocatalytic degradation for toluene. - Abstract: This study investigated the effects of Bi doped and Bi-Zn co-doped TiO 2 on photodegradation of gaseous toluene. The doped TiO 2 with various concentration of metal was prepared using the solvothermal route and characterized by SEM, XRD, Raman, BET, DRS, XPS, PL and EPR. Their photocatalytic activities under visible-light irradiation were drastically influenced by the dopant content. The results showed that moderate metal doping levels were obviously beneficial for the toluene degradation, while high doping levels suppressed the photocatalytic activity. The photocatalytic degradation of toluene over TiBi 1.9% O 2 and TiBi 1.9% Zn 1% O 2 can reach to 51% and 93%, respectively, which are much higher than 25% of TiO 2 . Bi doping into TiO 2 lattice generates new intermediate energy level of Bi below the CB edge of TiO 2 . The electron excitation from the VB to Bi orbitals results in the decreased band gap, extended absorption of visible-light and thus enhances its photocatalytic efficiency. Zn doping not only further enhances the absorption in this visible-light region, but also Zn dopant exists as the form of ZnO crystallites located on the interfaces of TiO 2 agglomerates and acts as a mediator of interfacial charge transfer to suppress the electron-hole recombination. These synergistic effects are responsible for the enhanced photocatalytic performance.

  1. Structure-directing effects of ionic liquids in the ionothermal synthesis of metal–organic frameworks

    Directory of Open Access Journals (Sweden)

    Thomas P. Vaid

    2017-07-01

    Full Text Available Traditional synthesis of metal–organic frameworks (MOFs involves the reaction of a metal-containing precursor with an organic linker in an organic solvent at an elevated temperature, in what is termed a `solvothermal' reaction. More recently, many examples have been reported of MOF synthesis in ionic liquids (ILs, rather than an organic solvent, in `ionothermal' reactions. The high concentration of both cations and anions in an ionic liquid allows for the formation of new MOF structures in which the IL cation or anion or both are incorporated into the MOF. Most commonly, the IL cation is included in the open cavities of the MOF, countering the anionic charge of the MOF framework itself and acting as a template around which the MOF structure forms. Ionic liquids can also serve other structure-directing roles, for example, when an IL containing a single enantiomer of a chiral anion leads to a homochiral MOF, even though the IL anion is not itself incorporated into the MOF. A comprehensive review of ionothermal syntheses of MOFs, and the structure-directing effects of the ILs, is given.

  2. Acid and redox activity of template-free Al-rich H-BEA* and Fe-BEA* zeolites

    Czech Academy of Sciences Publication Activity Database

    Sazama, Petr; Wichterlová, Blanka; Sklenák, Štěpán; Parvulescu, V. I.; Candu, N.; Sádovská, Galina; Dědeček, Jiří; Klein, Petr; Pashková, Veronika; Šťastný, Petr

    2014-01-01

    Roč. 318, OCT 2014 (2014), s. 22-33 ISSN 0021-9517 R&D Projects: GA ČR GAP106/11/0624; GA ČR(CZ) GA14-10251S; GA TA ČR TA01021377 Institutional support: RVO:61388955 Keywords : Acid strength * Alkylation of aromatics * Beta zeolite Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 6.921, year: 2014

  3. Corona protein composition and cytotoxicity evaluation of ultra-small zeolites synthesized from template free precursor suspensions

    NARCIS (Netherlands)

    Laurent, S.; Ng, E. -P.; Thirifays, C.; Lakiss, L.; Goupil, G. -M.; Mintova, S.; Burtea, C.; Oveisi, E.; Hebert, C.; de Vries, M.; Motazacker, M. M.; Rezaee, F.; Mahmoudi, M.

    2013-01-01

    The toxicity of two types of ultra-small zeolites (8-18 nm) with LTL-and EMT-type structures is reported. Both the LTL- and EMT-type zeolites belong to the same group of molecular sieves; they have large pores (7.1-7.5 angstrom) and low silica content (Si/Al = 1.2-2.3). The zeolites are prepared by

  4. Size-tunable TiO2 nanorod microspheres synthesised via a one-pot solvothermal method and used as the scattering layer for dye-sensitized solar cells

    Science.gov (United States)

    Rui, Yichuan; Li, Yaogang; Zhang, Qinghong; Wang, Hongzhi

    2013-11-01

    TiO2 microspheres assembled by single crystalline rutile TiO2 nanorods were synthesized by one-pot solvothermal treatment at 180 °C based on an aqueous-organic mixture solution containing n-hexane, distilled water, titanium n-butoxide and hydrochloric acid. The spheres had a radiative structure from the center, and their diameters were controlled in the range from 1 to 5 μm by adjusting the volume of the reactant water. Nitrogen adsorption-desorption isotherms showed that all the as-prepared microspheres had relatively high specific surface areas of about 50 m2 g-1. The 1 μm sized TiO2 nanorod microspheres were fabricated as a scattering overlayer in DSSCs, leading to a remarkable improvement in the power conversion efficiency: 8.22% of the bi-layer DSSCs versus 7.00% for the reference cell made of a single-layer film prepared from nanocrystalline TiO2. Such improvement was mainly attributed to the enhanced light harvesting and dye loading brought by the effective scattering centers.TiO2 microspheres assembled by single crystalline rutile TiO2 nanorods were synthesized by one-pot solvothermal treatment at 180 °C based on an aqueous-organic mixture solution containing n-hexane, distilled water, titanium n-butoxide and hydrochloric acid. The spheres had a radiative structure from the center, and their diameters were controlled in the range from 1 to 5 μm by adjusting the volume of the reactant water. Nitrogen adsorption-desorption isotherms showed that all the as-prepared microspheres had relatively high specific surface areas of about 50 m2 g-1. The 1 μm sized TiO2 nanorod microspheres were fabricated as a scattering overlayer in DSSCs, leading to a remarkable improvement in the power conversion efficiency: 8.22% of the bi-layer DSSCs versus 7.00% for the reference cell made of a single-layer film prepared from nanocrystalline TiO2. Such improvement was mainly attributed to the enhanced light harvesting and dye loading brought by the effective scattering

  5. A facile solvothermal approach of novel Bi{sub 2}S{sub 3}/TiO{sub 2}/RGO composites with excellent visible light degradation activity for methylene blue

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Ya; Shi, Yidan [The Laboratory of Food Colloids and Biotechnology, Ministry of Education, School of Chemical and Material Engineering, Jiangnan University, Wuxi 214122 (China); Liu, Xiang, E-mail: liuxiang@jiangnan.edu.cn [The Laboratory of Food Colloids and Biotechnology, Ministry of Education, School of Chemical and Material Engineering, Jiangnan University, Wuxi 214122 (China); Li, Hexing, E-mail: hexing-li@shnu.edu.cn [The Key Laboratory of the Chinese Ministry of Education in Resource Chemistry, Shanghai Normal University, Shanghai 200234 (China)

    2017-02-28

    Highlights: • Solvothermal approach of novel Bi{sub 2}S{sub 3}/TiO{sub 2}/RGO composites is simple. • Introduction of graphene enhanced the adsorption capacity and conductivity of Bi{sub 2}S{sub 3}/TiO{sub 2}/RGO. • Bi{sub 2}S{sub 3}/TiO{sub 2}/RGO shows high photocatalytic activity under simulated solar light. • Bi{sub 2}S{sub 3}/TiO{sub 2}/RGO exhibits excellent durability and reusability. - Abstract: In this paper, novel photocatalyst Bi{sub 2}S{sub 3}/TiO{sub 2}/RGO composites were successfully fabricated by a facile solvothermal method. During this process, TiO{sub 2} was coupled with Bi{sub 2}S{sub 3} to generate Bi{sub 2}S{sub 3} sensitized TiO{sub 2} nanoparticles, and graphene oxide (GO) was reduced to reduced graphene oxide (RGO), which was uniformly covered with plenty of Bi{sub 2}S{sub 3} and TiO{sub 2}. The as-prepared samples were characterized by scanning electron microscope (SEM), transmission electron microscopy (TEM), specific surface areas (BET), X-ray diffraction (XRD), Fourier transform infrared (FTIR), Raman, X-ray photoelectron spectroscopy (XPS), UV–vis diffuse reflectance spectroscopy (UV–vis DRS) and photoluminescence (PL) spectroscopy. The results confirmed that Bi{sub 2}S{sub 3} could act as an optical filter, which could be activated under visible light. And the introduction of Bi{sub 2}S{sub 3} could improve the response of TiO{sub 2} nanoparticles for visible light. In addition, the Bi{sub 2}S{sub 3}/TiO{sub 2} in Bi{sub 2}S{sub 3}/TiO{sub 2}/RGO composites had more uniform dispersion on the surface of graphene with less agglomeration in comparison with the Bi{sub 2}S{sub 3}/TiO{sub 2}. Graphene can provide conductive electron channels for separation of the electrons and inhibit the recombination of electrons and holes. Furthermore, the photocatalytic activity of Bi{sub 2}S{sub 3}/TiO{sub 2}/RGO composites was evaluated through the degradation of methylene blue (MB) under visible light irradiation. The Bi{sub 2}S{sub 3}/Ti

  6. In Situ Studies and Magnetic Properties of the Cmcm Polymorph of LiCoPO4 with a Hierarchical Dumbbell-Like Morphology Synthesized by Easy Single-Step Polyol Synthesis

    Directory of Open Access Journals (Sweden)

    Carlos Alarcón-Suesca

    2016-11-01

    Full Text Available LiCoPO4 (LCP exists in three different structural modifications: LCP-Pnma (olivine structure, LCP-Pn21a (KNiPO4 structure type, and LCP-Cmcm (Na2CrO4 structure type. The synthesis of the LCP-Cmcm polymorph has been reported via high pressure/temperature solid-state methods and by microwave-assisted solvothermal synthesis. Phase transitions from both LCP-Pn21a and LCP-Cmcm to LCP-Pnma upon heating indicates a metastable behavior. However, a precise study of the structural changes during the heating process and the magnetic properties of LCP-Cmcm are hitherto unknown. Herein, we present the synthesis and characterization of LCP-Cmcm via a rapid and facile soft-chemistry approach using two different kinetically controlled pathways, solvothermal and polyol syntheses, both of which only require relatively low temperatures (~200 °C. Additionally, by polyol, method a dumbbell-like morphology is obtained without the use of any additional surfactant or template. A temperature-dependent in situ powder XRD shows a transition from LCP-Cmcm at room temperature to LCP-Pnma and finally to LCP-Pn21a at 575 and 725 °C, respectively. In addition to that, the determination of the magnetic susceptibility as a function of temperature indicates a long-range antiferromagnetic order below TN = 11 K at 10 kOe and 9.1 K at 25 kOe. The magnetization curves suggests the presence of a metamagnetic transition.

  7. Solvothermal Synthesis, Crystal Structure, and Magnetic Properties of [Co3(SDA)3(DMF)2]: 2-D Layered Metal-organic Framework Derived from 4,4'-Stilbenedicarboxylic Acid (H2SDA)

    International Nuclear Information System (INIS)

    Park, Gyung Se; Kim, Hyun Uk; Kim, Ki Moon; Lee, Gang Ho; Park, Sang Kyu

    2006-01-01

    A new 2-D coordination polymer has been synthesized and characterized by using a novel 4,4'-stilbene dicarboxylic acid and Co(ClO 4 ) 2 ·6H 2 O. The title complex has an unique Co 3 pin-wheel cluster in which central Co has octahedral geometry and two surrounding Co have tetrahedral geometry. The Co 3 pin-wheel clusters, the building unit, are linked through carboxylate oxygens to generate a 2-D layered coordination polymer in ABCABC packing mode. Variable-temperature magnetic susceptibility data of the title compound confirms the high spin splitting of Co with S=3/2. Syntheses of MOF by using SDA and other transition metal ions, Zn, Cd, and Mn, are on progress in this lab. Metal-organic frameworks (MOF) have attracted much more attention in the past decade owing to their various intriguing framework topologies and potential applications as functional materials in gas storage, separation, and catalysis. Because high framework stability is fundamental and essential property for many practical applications, multi-dentate linkers such as carboxylates have been extensively investigated for the formation of more rigid frameworks due to their ability to aggregate metal ions into M-O-C clusters called secondary building units (SBUs) rather than N-bound organic linkers such as 4,4-bipyridine (bipy)

  8. Two new two-dimensional organically templated phosphite compounds: (C6H16N2)0.5[M(HPO3)F], M=Fe(II) and Co(II): Solvothermal synthesis, crystal structures, thermal, spectroscopic, and magnetic properties

    International Nuclear Information System (INIS)

    Fernandez-Armas, Sergio; Mesa, Jose L.; Pizarro, Jose L.; Chung, U-Chan; Arriortua, Maria I.; Rojo, Teofilo

    2005-01-01

    The organically templated (C 6 H 16 N 2 ) 0.5 [M(HPO 3 )F] [M(II)=Fe (1) and Co (2)] compounds have been synthesized by using mild hydrothermal conditions under autogeneous pressure. The crystal structures have been determined from X-ray single-crystal diffraction data. The compounds are isostructural and crystallize in the C2/c monoclinic space group. The unit-cell parameters are a=5.607(1), b=21.276(4), c=11.652(1)A, β=93.74(1) deg. for the iron phase and a=5.5822(7), b=21.325(3), c=11.4910(1)A, β=93.464(9) o for the cobalt compound with Z=4. The crystal structure of these compounds consists of [M(HPO 3 )F] - anionic sheets. The layers are constructed from chains which contain [M 2 O 6 F 3 ] dimeric units linked by fluoride ions. The trans-1,4-diaminocyclohexane cations are placed in the interlayer space. The IR and Raman spectra show the bands corresponding to the phosphite oxoanion and organic dication. The Dq and Racah (B and C) parameters have been calculated from the diffuse reflectance spectra in the visible region. Dq parameter is 790cm -1 for compound (1). For phase (2) the Dq value is 725cm -1 and B and C are 930 and 4100cm -1 , respectively. The thermal evolution of the molar magnetic susceptibilities of these compounds show maxima at 20.0 and 6.0K for the iron(II) and cobalt(II) phases, respectively. These results indicate the existence of antiferromagnetic interactions in both compounds

  9. [C 6H 21N 4][Sb 9S 14O]: Solvothermal synthesis, crystal structure and characterization of the first non-centrosymmetric open Sb-S-O framework containing the new [SbS 2O] building unit

    Science.gov (United States)

    Kiebach, Ragnar; Näther, Christian; Peter Sebastian, C.; Mosel, Bernd D.; Pöttgen, Rainer; Bensch, Wolfgang

    2006-10-01

    [C 6H 21N 4][Sb 9S 14O] represents the first known oxo-thioantimonate with an organic ion acting as structure director. The compound crystallizes in the non-centrosymmetric space group Cmc2 1 with a=29.679(2), b=9.9798(6), c=11.7155(7) Å, V=3470.1(4) Å3, Z=4. The structure contains the hitherto unknown [SbS 2O] unit as a structural motif. The [SbS 3] trigonal pyramids and [SbS 2O] units are joined to form a 10-membered ring with large pores having a diameter of 7.7 Å×8.3 Å. The organic template molecule acts like a tetra-dentate ligand around the O atom of the [SbS 2O] group. Depending on the value chosen for the Sb-S bond lengths, the material contains a 1-, 2- or 3-dimensional anion. The optical band gap of 2.03 eV demonstrates that the material is an optical semi-conductor. Upon heating, the compound decomposes in two steps yielding finally a mixture of Sb and Sb 2S 3. The 121Sb Mössbauer spectrum shows a relative large line width in accordance with the superposition of the five signals.

  10. X-ray excited photoluminescence near the giant resonance in solid-solution Gd(1-x)Tb(x)OCl nanocrystals and their retention upon solvothermal topotactic transformation to Gd(1-x)Tb(x)F3.

    Science.gov (United States)

    Waetzig, Gregory R; Horrocks, Gregory A; Jude, Joshua W; Zuin, Lucia; Banerjee, Sarbajit

    2016-01-14

    Design rules for X-ray phosphors are much less established as compared to their optically stimulated counterparts owing to the absence of a detailed understanding of sensitization mechanisms, activation pathways and recombination channels upon high-energy excitation. Here, we demonstrate a pronounced modulation of the X-ray excited photoluminescence of Tb(3+) centers upon excitation in proximity to the giant resonance of the host Gd(3+) ions in solid-solution Gd1-xTbxOCl nanocrystals prepared by a non-hydrolytic cross-coupling method. The strong suppression of X-ray excited optical luminescence at the giant resonance suggests a change in mechanism from multiple exciton generation to single thermal exciton formation and Auger decay processes. The solid-solution Gd1-xTbxOCl nanocrystals are further topotactically transformed with retention of a nine-coordinated cation environment to solid-solution Gd1-xTbxF3 nanocrystals upon solvothermal treatment with XeF2. The metastable hexagonal phase of GdF3 can be stabilized at room temperature through this topotactic approach and is transformed subsequently to the orthorhombic phase. The fluoride nanocrystals indicate an analogous but blue-shifted modulation of the X-ray excited optical luminescence of the Tb(3+) centers upon X-ray excitation near the giant resonance of the host Gd(3+) ions.

  11. Photoluminescence Study of the Photoinduced Phase Separation in Mixed-Halide Hybrid Perovskite CH3NH3Pb(BrxI1-x)3 Crystals Synthesized via a Solvothermal Method.

    Science.gov (United States)

    Zhang, Baohua; Guo, Fuqiang; Xue, Junjun; Yang, Lianhong; Zhao, Yafei; Ge, Mei; Cai, Qing; Liu, Bin; Xie, Zili; Chen, Dunjun; Lu, Hai; Zhang, Rong; Zheng, Youdou

    2017-12-18

    We systematically synthesized mixed-halide hybrid perovskite CH 3 NH 3 Pb(Br x I 1-x ) 3 (0 ≤ x ≤ 1) crystals in the full composition range by a solvothermal method. The as-synthesized crystals retained cuboid shapes, and the crystalline structure transitioned from the tetragonal phase to the cubic phase with an increasing Br-ion content. The photoluminescence (PL) of CH 3 NH 3 Pb(Br x I 1-x ) 3 crystals exhibited a continuous variation from red (768 nm) to green (549 nm) with increasing the volume ratio of HBr (V HBr %), corresponding to a variation in the bandgap from 1.61 eV to 2.26 eV. Moreover, the bandgap of the crystals changed nonlinearly as a quadratic function of x with a bowing parameter of 0.53 eV. Notably, the CH 3 NH 3 Pb(Br x I 1-x ) 3 (0.4 ≤ x ≤ 0.6) crystals exhibited obvious phase separation by prolonged illumination. The cause for the phase separation was attributed to the formation of small clusters enriched in lower-band-gap, iodide-rich and higher-band-gap, bromide-rich domains, which induced localized strain to promote halide phase separation. We also clarified the relationship between the PL features and the band structures of the crystals.

  12. Total synthesis of ciguatoxin.

    Science.gov (United States)

    Hamajima, Akinari; Isobe, Minoru

    2009-01-01

    Something fishy: Ciguatoxin (see structure) is one of the principal toxins involved in ciguatera poisoning and the target of a total synthesis involving the coupling of three segments. The key transformations in this synthesis feature acetylene-dicobalthexacarbonyl complexation.

  13. Synthesis of highly c-oriented ZIF-69 membranes by secondary growth and their gas permeation properties

    KAUST Repository

    Liu, Yunyang

    2011-09-01

    A seeded growth procedure was successfully developed to synthesize highly c-oriented and well-intergrown zeolitic imidazolate framework-69 (ZIF-69) membranes on porous α-alumina substrates. The synthesis conditions were optimized both for seed preparation and for secondary growth. For seeding, a facile method was developed to prepare smaller and flat ZIF-69 microcrystals in order to make thin and c-oriented seed layers. While for secondary growth, a synthesis condition that favored the growth along the c-direction was chosen in order to form highly c-oriented ZIF-69 membranes after growth. As a result, the majority of ZIF-69 grains inside the membrane have their straight channels along the crystallographic c-axis aligned perpendicularly to the substrate surface. Such alignment was confirmed by both XRD and pole figure analysis. The mixture-gas separation studies that were carried out at room temperature and 1atm gave separation factors of 6.3, 5.0, 4.6 for CO2/N2, CO2/CO and CO2/CH4 respectively, and a permeance of ∼1.0×10-7molm-2s-1Pa-1 for CO2 in almost all mixtures. Both the separation factor and permeance were better than the performance of the ZIF-69 membranes prepared by the in situ solvothermal method due to improvement in the membrane microstructure by the seeded growth method. © 2011 Elsevier B.V.

  14. Synthesis of Uniform Rare Earth Doped Gd2O2S Sub-micron Sized Spheres Using Gas-Aided Sulfurization and their Optical Characteristics.

    Science.gov (United States)

    He, Shuqing; Zhao, Xinyu; Tan, Mei Chee

    2017-01-01

    In this work, we report a detailed study of the synthesis of sub-micron sized Gd 2 O 2 S spheres using a two-step process: (1) amorphous precursor synthesis using the solvothermal method where a surfactant was used to control particle morphology, followed by (2) crystallization to form Gd 2 O 2 S polycrystalline spheres in a sulfur-rich environment. The crystallization and sulfurization processes are investigated by monitoring the crystal growth at different temperatures and under different environments using mainly x-ray diffraction and analysis of the precursor's thermal decomposition profile. The optical emissions of the Er and Yb-Er doped Gd 2 O 2 S upon excitation at 975 nm were investigated to identify the optimal dopant concentrations, optimal heat treatment temperature as well as to further elucidate any fine structure changes. Our results also show that the maximum emission intensities were obtained for a heat treatment temperature of 800 °C, where increased dopant diffusion coupled with non-uniform surface segregation at much higher temperatures led to non-uniform dopant distribution and reduced emission intensities. Our findings from these studies would be useful towards the synthesis of brightly-emitting Gd 2 O 2 S based luminescent materials as well as for the controlled gas-aided sulfurization of other metal oxysulfides.

  15. Microwave-assisted synthesis of C-doped TiO2 and ZnO hybrid nanostructured materials as quantum-dots sensitized solar cells

    Science.gov (United States)

    Rangel-Mendez, Jose R.; Matos, Juan; Cházaro-Ruiz, Luis F.; González-Castillo, Ana C.; Barrios-Yáñez, Guillermo

    2018-03-01

    The microwave-assisted solvothermal synthesis of C-doped TiO2 and ZnO hybrid materials was performed. Saccharose, titanium isopropoxide and zinc acetate were used as organic and inorganic sources for the synthesis. The influence of temperature and reaction time on the textural and optoelectronic properties of the hybrid materials was verified. Carbon quantum-dots of TiO2 and ZnO nanostructured spheres were obtained in a second pot by controlled calcination steps of the precursor hybrid materials. A carefully characterization by adsorption-desorption N2 isotherms, XRD, XPS, SEM, UV-vis/DR and electro- and photo-electrochemistry properties of the carbon quantum-dots TiO2 and ZnO spheres was performed. The photoelectrochemical activity of TiO2-C and ZnO-C films proved to be dependent on the conditions of synthesis. It was found a red-shift in the energy band gap of the semiconductors with values of 3.02 eV and 3.13 eV for the TiO2-C and ZnO-C, respectively, clearly lower than those on bare semiconductors, which is associated with the C-doping effect. From the photo-electrochemistry characterization of C-doped TiO2 and ZnO films can be concluded that the present materials have potential applications as photoelectrodes for quantum-dots sensitized solar cells.

  16. X-ray excited photoluminescence near the giant resonance in solid-solution Gd1-xTbxOCl nanocrystals and their retention upon solvothermal topotactic transformation to Gd1-xTbxF3

    Science.gov (United States)

    Waetzig, Gregory R.; Horrocks, Gregory A.; Jude, Joshua W.; Zuin, Lucia; Banerjee, Sarbajit

    2015-12-01

    Design rules for X-ray phosphors are much less established as compared to their optically stimulated counterparts owing to the absence of a detailed understanding of sensitization mechanisms, activation pathways and recombination channels upon high-energy excitation. Here, we demonstrate a pronounced modulation of the X-ray excited photoluminescence of Tb3+ centers upon excitation in proximity to the giant resonance of the host Gd3+ ions in solid-solution Gd1-xTbxOCl nanocrystals prepared by a non-hydrolytic cross-coupling method. The strong suppression of X-ray excited optical luminescence at the giant resonance suggests a change in mechanism from multiple exciton generation to single thermal exciton formation and Auger decay processes. The solid-solution Gd1-xTbxOCl nanocrystals are further topotactically transformed with retention of a nine-coordinated cation environment to solid-solution Gd1-xTbxF3 nanocrystals upon solvothermal treatment with XeF2. The metastable hexagonal phase of GdF3 can be stabilized at room temperature through this topotactic approach and is transformed subsequently to the orthorhombic phase. The fluoride nanocrystals indicate an analogous but blue-shifted modulation of the X-ray excited optical luminescence of the Tb3+ centers upon X-ray excitation near the giant resonance of the host Gd3+ ions.Design rules for X-ray phosphors are much less established as compared to their optically stimulated counterparts owing to the absence of a detailed understanding of sensitization mechanisms, activation pathways and recombination channels upon high-energy excitation. Here, we demonstrate a pronounced modulation of the X-ray excited photoluminescence of Tb3+ centers upon excitation in proximity to the giant resonance of the host Gd3+ ions in solid-solution Gd1-xTbxOCl nanocrystals prepared by a non-hydrolytic cross-coupling method. The strong suppression of X-ray excited optical luminescence at the giant resonance suggests a change in mechanism

  17. Synthesis of grape-like carbon nanospheres and their application as photocatalyst and electrocatalyst

    Energy Technology Data Exchange (ETDEWEB)

    Mahajan, Mani, E-mail: manimahajan86@gmail.com; Singla, Gourav, E-mail: gsinghla@gmail.com; Singh, K., E-mail: kusingh@thapar.edu; Pandey, O.P., E-mail: oppandey@thapar.edu

    2015-12-15

    Carbon nanospheres of grape-like structure (CNS) with diameter ranging from 40 to 50 nm and wall thickness of 6–8 nm were synthesized by solvothermal route. The phase structure, morphology, microstructure, thermal stability, disorder and optical properties of synthesized CNS were investigated by various characterization techniques. The possible formation and growth mechanism for CNS were discussed on the basis of the in-build reaction conditions. The degradation study of organic pollutants (methylene blue) in UV light in the presence of synthesized CNS was done. The stability of the CNS in electrochemical performance was also discussed at the different potential window and compared its electrocatalytic activity with platinum supported on CNS which shows the better response for oxygen reduction reactions (ORR) at an optimized potential window (–0.2 to 1.0 V vs SCE). - Graphical abstract: A representative synthesis mechanism of carbon nano sphere (CNS) showing spherical morphology with its photo as well as electrocatalyst properties. - Highlights: • Carbon nanospheres (CNS) have been synthesized using in situ chemical-reduction route. • The bare CNS shows good luminescence and photocatalytic applications. • The Pt/CNS shows better electrochemical performance than the reported Pt/C.

  18. Controlled synthesis and structure characterization of nanostructured MnWO{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Hu, W.B., E-mail: w.hu@tom.com [Hubei Institute for Nationalities, Enshi 445000 (China); Nie, X.L.; Mi, Y.Zh. [Hubei Institute for Nationalities, Enshi 445000 (China)

    2010-01-15

    Using Mn to partly substitute the W in W{sub 18}O{sub 49} nanowires, the synthesis of MnWO{sub 4} hubnerite nano-cocoons is described in this paper, by using mixed MnCl{sub 2} and WCl{sub 6} as the precursors and cyclohexanol as the solvent, in a simple solvothermal process. Detailed characterization of the resulting products, using electron microscopy and spectroscopy, has shown that the gradual increase of MnCl{sub 2} concentration changes the long W{sub 18}O{sub 49} nanowires to cocoon-like nanomaterials of stable MnWO{sub 4} phase. The driving force for such transformations is attributed to the Mn{sup 2+} inclusion within the W{sub 18}O{sub 49}. At low Mn{sup 2+} concentration, internal stresses would be introduced to the W{sub 18}O{sub 49} nanowires; whilst at high Mn{sup 2+} concentration close to the stoichiometric composition of MnWO{sub 4}, the formation of the nano-cocoons is triggered by the intrinsic crystalline feature of the hubnerite. It is believed that a combination of the initial nanowire nucleation and competing growth, and of self-assembly of neighboring parallel nanowires, leads to the final structure.

  19. Controlled synthesis and structure characterization of nanostructured MnWO4

    International Nuclear Information System (INIS)

    Hu, W.B.; Nie, X.L.; Mi, Y.Zh.

    2010-01-01

    Using Mn to partly substitute the W in W 18 O 49 nanowires, the synthesis of MnWO 4 hubnerite nano-cocoons is described in this paper, by using mixed MnCl 2 and WCl 6 as the precursors and cyclohexanol as the solvent, in a simple solvothermal process. Detailed characterization of the resulting products, using electron microscopy and spectroscopy, has shown that the gradual increase of MnCl 2 concentration changes the long W 18 O 49 nanowires to cocoon-like nanomaterials of stable MnWO 4 phase. The driving force for such transformations is attributed to the Mn 2+ inclusion within the W 18 O 49 . At low Mn 2+ concentration, internal stresses would be introduced to the W 18 O 49 nanowires; whilst at high Mn 2+ concentration close to the stoichiometric composition of MnWO 4 , the formation of the nano-cocoons is triggered by the intrinsic crystalline feature of the hubnerite. It is believed that a combination of the initial nanowire nucleation and competing growth, and of self-assembly of neighboring parallel nanowires, leads to the final structure.

  20. Stable and Controllable Synthesis of Silver Nanowires for Transparent Conducting Film

    Science.gov (United States)

    Liu, Bitao; Yan, Hengqing; Chen, Shanyong; Guan, Youwei; Wu, Guoguo; Jin, Rong; Li, Lu

    2017-03-01

    Silver nanowires without particles are synthesized by a solvothermal method at temperature 150 °C. Silver nanowires are prepared via a reducing agent of glycerol and a capping agent of polyvinylpyrrolidone ( M w ≈ 1,300,000). Both of them can improve the purity of the as-prepared silver nanowires. With controllable shapes and sizes, silver nanowires are grown continuously up to 10-20 μm in length with 40-50 nm in diameter. To improve the yield of silver nanowires, the different concentrations of AgNO3 synthesis silver nanowires are discussed. The characterizations of the synthesized silver nanowires are analyzed by UV-visible absorption spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), and atomic force microscope (AFM), and silver nanowires are pumped on the cellulose membrane and heated stress on the PET. Then, the cellulose membrane is dissolved by the steam of acetone to prepare flexible transparent conducting thin film, which is detected 89.9 of transmittance and 58 Ω/□. Additionally, there is a close loop connected by the thin film, a blue LED, a pair of batteries, and a number of wires, to determinate directly the film if conductive or not.

  1. Synthesis and characterization of ZIF-69 membranes and separation for CO2/CO mixture

    KAUST Repository

    Liu, Yunyang

    2010-05-01

    Continuous and c-oriented ZIF-69 membranes were successfully synthesized on porous alpha-alumina substrates by an in situ solvothermal method. The membranes were characterized by XRD, SEM and single-gas permeation tests. The BET measurements on crystals taken from the same mother liquor that was used for membrane synthesis yield a Langmuir surface area of 1138 m(2)/g. The stability of the membrane towards heat and different solvents were studied. Single-gas permeation experiments through ZIF-69 membranes were carried out by a vacuum method at room temperature using H-2, CH4, CO, CO2 and SF6, respectively. The permeances were in the order of H-2 > CO2 > CH4 > CO > SF6. The separation of CO2/CO gas mixture was investigated by gas chromatograph (GC) and the permselectivity of CO2/CO was 3.5 +/- 0.1 with CO2 permeance of 3.6 +/- 0.3 x 10(-8) mol m(-2) s(-1) Pa-1 at room temperature. (C) 2010 Elsevier B.V. All rights reserved.

  2. Synthesis, Characterization and Ferroelectric Properties of LN-Type ZnSnO3 Nanostructures

    Science.gov (United States)

    Kons, Corisa

    With increasing focus on the ill health and environmental effects of lead there is a greater push to develop Pb-free devices and materials. To this extent, ecofriendly and earth abundant LiNbO3-type ZnSnO3, a derivative of the ABO3 perovskite structure, has a high theoretically predicted polarization making it an excellent choice as a suitable alternative to lead based material such as PZT. In this work we present a novel synthesis procedure for the growth of various ZnSnO3 nanostructures by combined physical/chemical processes. Various ZnSnO3 nanostructures of different dimensions were grown from a ZnO:Al template layer on a Si (100) substrate deposited by pulsed laser deposition followed by a strategic solvothermal process. The ferroelectric properties of each sample were explored and a remanent polarization as high as nearly 30 muC/cm2 was found in aligned nanowire arrayed films. An in-depth understanding of the structure-property relationship is key to the future development of this material and is the subject of future investigations.

  3. Study on the synthesis and excitation-powerdependent photoluminescence spectrum of ZnSe nanoparticles

    Science.gov (United States)

    Feng, Bo; Cao, Jian; Yang, Jinghai; Han, Donglai; Yang, Shuo

    2015-02-01

    Zinc selenide (ZnSe) nanoparticles with the cubic zinc blende structure were successfully prepared by a solvothermal method without any surface-active agents. The as-obtained sample was characterized by X-ray diffraction, transmission electron microscopy (TEM), selected area electron diffraction, high-resolution TEM, and room-temperature photoluminescence (PL) techniques. It was proved that EDTA played a significant role during the synthesis of ZnSe nanoparticles. The room-temperature PL spectrum of the ZnSe nanoparticles showed a strong near-band-edge emission peak at 472 nm and a weak defect-related emission band in the range of 600-650 nm. Excitation-powerdependent PL spectrum of the ZnSe nanoparticles showed that the near-band-edge emission peak displayed an evident redshift with increasing the excitation power, and the corresponding energy shift might be as large as 51 meV. In addition, the integrated intensity of the near-band-edge emission peak increased with increasing the excitation power, which indicated the competition between the radiative recombination process and the nonradiative recombination process of photogenerated carriers.

  4. Design, Synthesis and Characterization of Novel Graphene-Based Nanoarchitectures for Sustainability

    Science.gov (United States)

    Bay, Hamed Hosseini

    The unique structure and properties of graphene initiated broad fundamental and technological research in recent years, and highlighted graphene as an alternative for various applications such as energy storage and nanoelectronics. Chemical vapor deposition (CVD) of graphene on copper is believed to be the most promising method for large-scale synthesis of continuous sheets. The exceptional properties of graphene however, are governed by its microstructure. The size of graphene grains and the grain boundaries affect the carrier mobility. Therefore understanding the formation mechanism of graphene is critical to control the microstructure and physical properties. We implemented Fluorescence Quenching Microscopy (FQM) in conjunction with other methods to understand a trend which is pertinent in large-scale. In order to investigate the nucleation and growth mechanism of graphene on copper and its subsequent microstructure, effect of key parameters such as density of defects in copper foils and growth pressure in the CVD chamber have been altered. Results point out that microstructure of copper regulates the structure and properties of graphene and heat treatment and electropolishing of the foil substrates as well as controlling the saturation pressure of the carbon precursor yield to large graphene domains. Water decontamination and oil/water separation are principal motives in the surge to develop novel means for sustainability. In this prospect, supplying clean water for the ecosystems is as important as the recovery of the oil spills since the supplies are scarce. Inspired to design an engineering material which not only serves this purpose, but can also be altered for other applications to preserve natural resources, a facile template-free process is suggested to fabricate a superporous, superhydrophobic graphene-based sponge. Moreover, the process is designed to be inexpensive and scalable. The fabricated sponge can be used to clean up different types of oil

  5. Synthesis of Mechanisms

    DEFF Research Database (Denmark)

    Hansen, John Michael

    1999-01-01

    These notes describe an automated procedure for analysis and synthesis of mechanisms. The analysis method is based on the body coordinate formulation, and the synthesis is based on applying optimization methods, used to minimize the difference between an actual and a desired behaviour......These notes describe an automated procedure for analysis and synthesis of mechanisms. The analysis method is based on the body coordinate formulation, and the synthesis is based on applying optimization methods, used to minimize the difference between an actual and a desired behaviour...

  6. One-step synthesis for FeBTC-MOF/iron oxide composite

    Energy Technology Data Exchange (ETDEWEB)

    Nascimento, R.F.F. do; Gentil, G.; Junior, S.A.; Azevedo, W.M. de; Rodrigues, A.R.; Campello, S.L. [Universidade Federal de Pernambuco (UFPE), PE (Brazil)

    2016-07-01

    Full text: In this work we present the assisted ultrasonic radiation synthesis for f Fe(BTC) (BTC = 1,3,5-benzenetricarboxilic acid) metal organic framework preparation. By definition Metal-organic frameworks (MOFs) belongs to a class of material prepared by the combination of metal ions and organic linkers to form a tridimensional framework which presents defined characteristics like crystallinity, high porosity and the presence of strong metal-ligand interaction. In the last decades the MOFs materials have received considerable attention not only due to scientific interest, but also because of their high potential for applications in several technological areas such as in gas storage, catalysis and drug delivery [1]. Among several Metal-organic frameworks (MOFs) the Fe-BTC structure seems to be one of promising materials, mainly due to their chemical and thermal stability, presents biocompatibility, can be used as drug delivery and as a contrast agent for magnetic resonance. Its functionalization has been reported in the literature by several works where the methods consist to mix the iron oxide Fe3O4 nanoparticles, in the solution contained the MOF'S precursor and the synthesis is prepared by solvothermal method. Typically, it has core-shell Fe3O4@MOF structures and exhibit magnetic properties. Our experimental technique proposed for the synthesis of the composite consists to use iron powder (?-Fe) as a target material dispersed in a solution of DMF/H2O (1:1) containing benzene 1,3,5 tricarboxilic acid and NaNO3. The synthesis was performed using a Ultrasound equipment model GEX500 500 W operating at 80 kHz, pulse 1s intervals for 60 min. The x-ray diffraction patterns and SEM measurements shown that the obtained materials are similar to those found in the literature and presents a rods likes morphology. The BET analysis indicate that the surface area is 1257 m²g-1 and pore volume 1.4 cm³g-1. Also the magnetic measurements indicates a paramagnetic

  7. Synthesis and electrochemical performance of hierarchical nano-vanadium oxide.

    Science.gov (United States)

    Mjejri, I; Sediri, F

    2016-10-15

    Hierarchically structured nano-vanadium oxides with different morphologies have been synthesized via a template-free hydrothermal route by adjusting the organic precursor quantities. The effects of molar ratio on structure, morphology and crystallite sized were investigated. The possible growth mechanism is also proposed. When evaluated as a cathode material for lithium-ion batteries, the vanadium oxyhydroxide H2V3O8 samples deliver very high charging capacity, good reversibility and a better cycling stability. The excellent electrochemical performance is attributed to multiple advantageous structural features. Copyright © 2016 Elsevier Inc. All rights reserved.

  8. Synthesis of Co9S8 and CoS nanocrystallites using Co(II ...

    Indian Academy of Sciences (India)

    Department of Chemistry, University of Mumbai, Vidyanagari, Santacruz (East), Mumbai 400 098, India. MS received 20 June 2015; ... Keywords. Cobalt sulphide; single-source precursors; pyrolysis and solvothermal decomposition. 1. Introduction ..... with ligand coordination through azomethine nitrogen and sulphur atoms.

  9. One-pot synthesis and bioapplication of amine-functionalized magnetite nanoparticles and hollow nanospheres.

    Science.gov (United States)

    Wang, Leyu; Bao, Jie; Wang, Lun; Zhang, Fang; Li, Yadong

    2006-08-16

    To demonstrate their applications in biological and medical fields such as in immunoassays, magnetic separation of cells or proteins, drug or gene delivery, and magnetic resonance imaging, the template-free syntheses of water-soluble and surface functionalized magnetic nanomaterials have become essential and are challenging. Herein, we developed a facile one-pot template-free method for the preparation of amine-functionalized magnetite nanoparticles and hollow nanospheres by using FeCl(3)6 H(2)O as single iron source. These magnetic nanomaterials were characterized by TEM, SEM, XRD, and FTIR technologies. Their magnetic properties were also studied by using a superconducting quantum interference device (SQUID) magnetometer at room temperature. Then the amine-functionalized magnetite nanoparticles were applied to immunoassays and magnetic resonance imaging in live mice.

  10. Total Synthesis of Avrainvilleol.

    Science.gov (United States)

    Wegener, Aaron; Miller, Kenneth A

    2017-11-03

    The first total synthesis of the marine natural product avrainvilleol is reported. The total synthesis features the first application of the transition-metal-free coupling of a tosyl hydrazone and a boronic acid to the preparation of a complex natural product, and the first example of this coupling with a hindered diortho substituted hydrazone substrate.

  11. Difluoromethylenephosphonates: synthesis and transformations

    International Nuclear Information System (INIS)

    Chunikhin, Konstantin S; Kadyrov, A A; Pasternak, P V; Chkanikov, Nikolai D

    2010-01-01

    The data on the synthesis of organic compounds containing the difluoromethylenephosphonate group are analyzed and generalized. The attention is focused on the introduction of this group into various organic molecules and subsequent transformations of the compounds thus formed. Individual sections are devoted to the synthesis of heterocyclic compounds and analogues of natural substances containing difluoromethylenephosphonate groups.

  12. Synthesis of Isoiminosugars

    DEFF Research Database (Denmark)

    Hyldtoft, Lene; Godskesen, Michael Anders; Lundt, Inge

    1998-01-01

    A short synthesis of isoiminosugars have been developed. Bromolactones are diastereoselectively alkylated at C-2 followed by ring closure to the corresponding lactams. Reduction of these then gives isoiminosugars......A short synthesis of isoiminosugars have been developed. Bromolactones are diastereoselectively alkylated at C-2 followed by ring closure to the corresponding lactams. Reduction of these then gives isoiminosugars...

  13. Synthesis of oligonucleotide phosphorodithioates

    DEFF Research Database (Denmark)

    Beaton, G.; Brill, W. K D; Grandas, A.

    1991-01-01

    The synthesis of DNA containing sulfur at the two nonbonding internucleotide valencies is reported. Several different routes using either tervalent or pentavalent mononucleotide synthons are described.......The synthesis of DNA containing sulfur at the two nonbonding internucleotide valencies is reported. Several different routes using either tervalent or pentavalent mononucleotide synthons are described....

  14. VHDL for logic synthesis

    CERN Document Server

    Rushton, Andrew

    2011-01-01

    Many engineers encountering VHDL (very high speed integrated circuits hardware description language) for the first time can feel overwhelmed by it. This book bridges the gap between the VHDL language and the hardware that results from logic synthesis with clear organisation, progressing from the basics of combinational logic, types, and operators; through special structures such as tristate buses, register banks and memories, to advanced themes such as developing your own packages, writing test benches and using the full range of synthesis types. This third edition has been substantially rewritten to include the new VHDL-2008 features that enable synthesis of fixed-point and floating-point hardware. Extensively updated throughout to reflect modern logic synthesis usage, it also contains a complete case study to demonstrate the updated features. Features to this edition include: * a common VHDL subset which will work across a range of different synthesis systems, targeting a very wide range of technologies...

  15. Solvothermal syntheses, crystal structures, optical and thermal ...

    Indian Academy of Sciences (India)

    The dimeric [Ge₂Se₆] ⁴⁻ anion acts as a bridging ligand via the trans terminal Se atoms to link two [Ni(tepa)] ²⁺ cations, resulting in neutral complex 3. The Ni²⁺ ion in 2 is coordinated by two tridentate dien ... in the presence of transition metal ions. Thecompounds 1–3 exhibit optical band gaps between 2.06 and 2.35 eV.

  16. Solvothermal syntheses, crystal structures, optical and thermal ...

    Indian Academy of Sciences (India)

    and [Ni(dien)2]2+ counter cations, respectively. The [Ge2Se6]4− anion is constructed by two tetrahedral GeSe4 building units via edge-sharing. In 2, two tetra- hedral GeSe4 units are linked by a corner and a Se–Se bond to form a polyselenidogermanate anion [Ge2Se7]4− containing a five-membered ring Ge2Se3.

  17. Synthesis and spectral studies on Cd(II) dithiocarbamate complexes and their use as precursors for CdS nanoparticles

    Science.gov (United States)

    Sathiyaraj, Ethiraj; Padmavathy, Krishnaraj; Kumar, Chandran Udhaya; Krishnan, Kannan Gokula; Ramalingan, Chennan

    2017-11-01

    Bis(N-cyclopropyl-N-4-chlorobenzyldithiocarbamato-S,S‧)cadmium(II) (1) and (2,2‧-bipyridine) bis(N-cyclopropyl-N-4-chlorobenzyldithiocarbamato-S,S‧)cadmium(II) (2) have been synthesized and characterized by FT-IR, 1HNMR and 13C NMR analyses. For the complex 2, single crystal X-ray diffraction analysis and computational studies (optimized geometry, HOMO-LUMO and MEP) have been executed employing DFT/B3LYP method with LANL 2DZ basic set. The optimized bond lengths and bond angles agree well with the experimental results. The complexes 1 and 2 have been used as single source precursors for the synthesis of ethyleneglycol capped CdS1 and CdS2 nanoparticles, respectively. CdS1 and CdS2 nanoparticles have been synthesized by solvothermal method. PXRD, SEM, Elemental colour mapping, EDAX, TEM and UV-Vis spectroscopy have been used to characterize the as-prepared CdS nanoparticles. The X-ray diffraction pattern confirms both their hexagonal structures.

  18. Asymmetric synthesis v.4

    CERN Document Server

    Morrison, James

    1984-01-01

    Asymmetric Synthesis, Volume 4: The Chiral Carbon Pool and Chiral Sulfur, Nitrogen, Phosphorus, and Silicon Centers describes the practical methods of obtaining chiral fragments. Divided into five chapters, this book specifically examines initial chiral transmission and extension. The opening chapter describes the so-called chiral carbon pool, the readily available chiral carbon fragments used as building blocks in synthesis. This chapter also provides a list of 375 chiral building blocks, along with their commercial sources, approximate prices, and methods of synthesis. Schemes involving

  19. Designed synthesis of tunable amorphous carbon nanotubes (a ...

    Indian Academy of Sciences (India)

    Administrator

    nanoelectronics and sensor devices (Zhao et al 2009). Thus, a-CNTs become another focus of research. So far, some methods including CVD, arc discharge, anodic aluminium oxide (AAO) template, solvothermal method, etc., have been developed to synthesize a-CNTs (Ci et al. 2001, 2003; Nishino et al 2003; Zhao et al ...

  20. SYNTHESIS, CHARACTERIZATION AND ANTIBACTERIAL ...

    African Journals Online (AJOL)

    Preferred Customer

    E-mail: a-ahmadi@kiau.ac.ir; ahmadikiau@yahoo.com. SYNTHESIS, CHARACTERIZATION AND ANTIBACTERIAL EVALUATION OF. SOME NOVEL DERIVATIVES OF 2-BROMOMETHYL-BENZIMIDAZOLE. Abbas Ahmadi*. Department of Medicinal Chemistry, Pharmaceutical Sciences Branch, Islamic Azad University,.

  1. 2002 Annual report: synthesis

    International Nuclear Information System (INIS)

    2003-01-01

    This synthesis of the Annual Report 2002 presents information of the main activities on the scope of the radiation protection and nuclear safety of the Nuclear Regulatory Authority (ARN) of the Argentina during 2002

  2. 2001 Annual report: synthesis

    International Nuclear Information System (INIS)

    2001-01-01

    This synthesis of the Annual Report 2001 presents information of the main activities on the scope of the radiation protection and nuclear safety of the Nuclear Regulatory Authority (ARN) of the Argentina during 2001

  3. 2000 Annual report: synthesis

    International Nuclear Information System (INIS)

    2001-01-01

    This synthesis of the Annual Report 2000 present information of the main activities on the scope of the radiation protection and nuclear safety of the Nuclear Regulatory Authority (NRA) of the Argentina during 2000

  4. Synthesis of Acetylhomoagmatine

    Directory of Open Access Journals (Sweden)

    Carmenza Duque

    2006-08-01

    Full Text Available Abstract: The first total synthesis of acetylhomoagmatine, a natural product isolated form the methanolic extracts from the sponge Cliona celata, is performed in four steps in a very high yield.

  5. Instrument Modeling and Synthesis

    Science.gov (United States)

    Horner, Andrew B.; Beauchamp, James W.

    During the 1970s and 1980s, before synthesizers based on direct sampling of musical sounds became popular, replicating musical instruments using frequency modulation (FM) or wavetable synthesis was one of the “holy grails” of music synthesis. Synthesizers such as the Yamaha DX7 allowed users great flexibility in mixing and matching sounds, but were notoriously difficult to coerce into producing sounds like those of a given instrument. Instrument design wizards practiced the mysteries of FM instrument design.

  6. Lanthanide(III) complexes with μ-SnSe{sub 4} and μ-Sn{sub 2}Se{sub 6} linkers. Solvothermal syntheses and properties of new Ln(III) selenidostannates decorated with linear polyamine

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Shuzhen; Sun, Peipei; Shen, Yali; Han, Jingyu; Sun, Hui; Jia, Dingxian [Soochow Univ., Suzhou (China). College of Chemistry, Chemical Engineering and Materials Science

    2017-06-01

    New lanthanide-selenidostannate complexes [{La(peha)(Cl)}{La(peha)(NO_3)}(μ-1κ{sup 2}:2κ{sup 2}-SnSe{sub 4})] (1), [H{sub 2}trien][{La(trien)_2}{sub 2}(μ-1-κ:2κ-Sn{sub 2}Se{sub 6})][Sn{sub 2}Se{sub 6}].H{sub 2}O (2) and [{Ln(tepa)(μ-OH)}{sub 2}(μ-1κ:2κ-Sn{sub 2}Se{sub 6})]{sub n}.nH{sub 2}O (Ln=Sm(3), Eu(4)) were prepared by solvothermal methods in pentaethylenehexamine (peha), triethylenetetramine (trien) and tetraethylenepentamine (tepa), respectively. Acting as a tetradentate chelating and bridging ligand, μ-1κ{sup 2}:2κ{sup 2}-SnSe{sub 4}, the tetrahedral SnSe{sub 4} unit joins {La(peha)(Cl)}{sup 2+} and {La(peha)(NO_3)}{sup 2+} complex fragments to generate the neutral coordination compound 1. The tetradentate μ-1κ{sup 2}:2κ{sup 2} bridge in 1 represents a new coordination mode for the SnSe{sub 4} tetrahedron. In 2, dinuclear [Sn{sub 2}Se{sub 6}]{sup 4-} anions are formed of SnSe{sub 4} tetrahedra via edge-sharing. One [Sn{sub 2}Se{sub 6}]{sup 4-} anion acts as a bidentate bridging ligand in a μ-1κ:2κ coordination mode to join two {La(trien)_2}{sup 3+} units, and the other [Sn{sub 2}Se{sub 6}]{sup 4-} anion exists as a free charge compensating ion. In 3 and 4, the [Sn{sub 2}Se{sub 6}]{sup 4-} anion connects binuclear [{Ln(tepa)(μ-OH)}{sub 2}]{sup 2+}(Ln=Sm, Eu) units with a bidentate μ-1κ:2κ mode, giving neutral coordination polymers [{Ln(tepa)(μ-OH)}{sub 2}(μ-1κ:2κ-Sn{sub 2}Se{sub 6})]{sub n}. The La(2){sup 3+} ion in 1 is in a 10-fold coordination environment of LaN{sub 6}O{sub 2}Se{sub 2}, whereas the La(1){sup 3+} ions in 1 and 2 are in 9-fold coordinated environments forming polyhedra LaN{sub 6}ClSe{sub 2} and LaN{sub 8}Se, respectively. The Sm{sup 3+} and Eu{sup 3+} ions in 3 and 4 are both in an 8-fold coordination environment of LnN{sub 5}O{sub 2}Se. Compounds 1-4 exhibit optical band gaps between 2.21 and 2.42 eV. Their thermal stabilities were investigated by thermogravimetric analyses.

  7. Detonation-synthesis nanodiamonds: synthesis, structure, properties and applications

    International Nuclear Information System (INIS)

    Dolmatov, Valerii Yu

    2007-01-01

    The review outlines the theoretical foundations and industrial implementations of modern detonation synthesis of nanodiamonds and chemical purification of the nanodiamonds thus obtained. The structure, key properties and promising fields of application of detonation-synthesis nanodiamonds are considered.

  8. Synthesis of phenanthrenes

    International Nuclear Information System (INIS)

    Clarke, C.

    1983-01-01

    A new and improved synthesis of 7-methoxy-12-methyl-2-oxo-2,3,4,9,10,12-hexahydrophenanthrene has been described. The compound is an important intermediate for the synthesis of many di- and tri-terpenes, and was required in this work for the synthesis of 17-acetyl-5α-etiojerva-12,14,16-trien-3β-ol. This compound is a known starting material for the synthesis of the veratrum alkaloids jervine, veratramine and verarine. Two synthetic routes to the synthesis of 7-methoxy-12-methyl-2-oxo-2,3,4,9,10,12-hexahydrophenanthrene were investigated. The first route required preparation of the intermediate 1-(5-methyl-2-furyl)-3-(3'-methoxyphenyl)propane which, by simple manipulation involving mainly the furan ring, gave the desired compound in 33% yield. All of the reactions involved are suitable for both large and small scale preparations. The synthesis of 17-acetyl-5α-etiojerva-12,14,16-trien-3B-ol can be achieved by the hyde and 3-methoxyacetophenone, followed by hydrogeneration and Wolff-Kishner reduction. A less successful synthesis of the above compound was achieved by condensing the Grignard derivative of 2-(3'-methoxyphenyl)ethyl bromide with 5-methylfurfuraldehyde to form a furyl alcohol, which was oxidized and reduced to give 1-(5-methyl-2-furyl)-3-(3'-methoxyphenyl)propane in only 7% overall yield, but the starting materials are inexpensive and readily available. The compound was also prepared in 40% yield by condensing 2-lithio-5-methylfuran with 3-(3'methoxyphenyl)propyl bromide. An appendix describes the reaction of 3-ethoxy-cyclohex-2-en-1-one with ethylmagnesium bromide, followed by aromatization. A second appendix describes the reductive alkylation of 8-methoxy-12-methyl-2-oxo-2,3,4,9,10,12-hexahydrophenanthrene

  9. Facile synthesis of N-rich carbon quantum dots by spontaneous polymerization and incision of solvents as efficient bioimaging probes and advanced electrocatalysts for oxygen reduction reaction

    Science.gov (United States)

    Lei, Zhouyue; Xu, Shengjie; Wan, Jiaxun; Wu, Peiyi

    2016-01-01

    In this study, uniform nitrogen-doped carbon quantum dots (N-CDs) were synthesized through a one-step solvothermal process of cyclic and nitrogen-rich solvents, such as N-methyl-2-pyrrolidone (NMP) and dimethyl-imidazolidinone (DMEU), under mild conditions. The products exhibited strong light blue fluorescence, good cell permeability and low cytotoxicity. Moreover, after a facile post-thermal treatment, it developed a lotus seedpod surface-like structure of seed-like N-CDs decorating on the surface of carbon layers with a high proportion of quaternary nitrogen moieties that exhibited excellent electrocatalytic activity and long-term durability towards the oxygen reduction reaction (ORR). The peak potential was -160 mV, which was comparable to or even lower than commercial Pt/C catalysts. Therefore, this study provides an alternative facile approach to the synthesis of versatile carbon quantum dots (CDs) with widespread commercial application prospects, not only as bioimaging probes but also as promising electrocatalysts for the metal-free ORR.In this study, uniform nitrogen-doped carbon quantum dots (N-CDs) were synthesized through a one-step solvothermal process of cyclic and nitrogen-rich solvents, such as N-methyl-2-pyrrolidone (NMP) and dimethyl-imidazolidinone (DMEU), under mild conditions. The products exhibited strong light blue fluorescence, good cell permeability and low cytotoxicity. Moreover, after a facile post-thermal treatment, it developed a lotus seedpod surface-like structure of seed-like N-CDs decorating on the surface of carbon layers with a high proportion of quaternary nitrogen moieties that exhibited excellent electrocatalytic activity and long-term durability towards the oxygen reduction reaction (ORR). The peak potential was -160 mV, which was comparable to or even lower than commercial Pt/C catalysts. Therefore, this study provides an alternative facile approach to the synthesis of versatile carbon quantum dots (CDs) with widespread

  10. Synthesis and photocatalytic activity of mesoporous – (001) facets TiO{sub 2} single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Dong, Yeshuo [School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072 (China); Fei, Xuening, E-mail: xueningfei@126.com [School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072 (China); School of Science, Tianjin Chengjian University, Tianjin 300384 (China); Zhou, Yongzhu [School of Science, Tianjin Chengjian University, Tianjin 300384 (China)

    2017-05-01

    Highlights: • The (001) facets of TiO{sub 2} single crystals with mesoporous structure. • The (010) and (100) facets of TiO{sub 2} single crystals were covered by the flower – shaped TiO{sub 2} crystals. • This special structure could promote charge separation and provide more active sites, which will lead to a substantial increase in photocatalytic activity. - Abstract: In this work, the mesoporous – (001) facets TiO{sub 2} single crystals have been successfully synthesized through a two-step solvothermal route without any template. Their structure and morphology were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), ultraviolet-visible (UV–vis) diffuse reflectance spectroscopy and energy dispersive X-ray spectrometer (EDX). Based on the different characteristics and atomic arrangements on each facet of anatase TiO{sub 2} single crystals, we synthesized these mesoporous – (001) facets TiO{sub 2} single crystals by controlling the interaction characteristics of hydrofluoric acid (HF) and isopropanol (i-PrOH) on the crystal facets. It can been seen that the (001) facets of these as-synthesized TiO{sub 2} single crystals have a clear mesoporous structure through the SEM images and BET methods. Moreover, the other four facets were covered by the flower – shaped TiO{sub 2} crystals with the generation of the mesoporous – (001) facets. This special and interesting morphology could promote charge separation and provide more active sites, which will lead to a substantial increase in photocatalytic activity. Moreover, it is more intuitive to reflect that the different crystal facets possess the different properties due to their atomic arrangement. Besides, according to the different synthetic routes, we proposed and discussed a plausible synthesis mechanism of these mesoporous – (001) facets TiO{sub 2} single crystals.

  11. Polyethylene Glycol-Mediated Synthesis of Cubic Iron Oxide Nanoparticles with High Heating Power

    Science.gov (United States)

    Iacovita, Cristian; Stiufiuc, Rares; Radu, Teodora; Florea, Adrian; Stiufiuc, Gabriela; Dutu, Alina; Mican, Sever; Tetean, Romulus; Lucaciu, Constantin M.

    2015-10-01

    Iron oxide magnetic nanoparticles (IOMNPs) have been successfully synthesized by means of solvothermal reduction method employing polyethylene glycol (PEG200) as a solvent. The as-synthesized IOMNPs are poly-dispersed, highly crystalline, and exhibit a cubic shape. The size of IOMNPs is strongly dependent on the reaction time and the ration between the amount of magnetic precursor and PEG200 used in the synthesis method. At low magnetic precursor/PEG200 ratio, the cubic IOMNPs coexist with polyhedral IOMNPs. The structure and morphology of the IOMNPs were thoroughly investigated by using a wide range of techniques: TEM, XRD, XPS, FTIR, and RAMAN. XPS analysis showed that the IOMNPs comprise a crystalline magnetite core bearing on the outer surface functional groups from PEG200 and acetate. The presence of physisorbed PEG200 on the IOMNP surface is faintly detected through FT-IR spectroscopy. The surface of IOMNPs undergoes oxidation into maghemite as proven by RAMAN spectroscopy and the occurrence of satellite peaks in the Fe2p XP spectra. The magnetic studies performed on powder show that the blocking temperature (TB) of IOMNPs is around 300 K displaying a coercive field in between 160 and 170 Oe. Below the TB, the field-cooled (FC) curves turn concave and describe a plateau indicating that strong magnetic dipole-dipole interactions are manifested in between IOMNPs. The specific absorption rate (SAR) values increase with decreasing nanoparticle concentrations for the IOMNPs dispersed in water. The SAR dependence on the applied magnetic field, studied up to magnetic field amplitude of 60 kA/m, presents a sigmoid shape with saturation values up to 1700 W/g. By dispersing the IOMNPs in PEG600 (liquid) and PEG1000 (solid), it was found that the SAR values decrease by 50 or 75 %, indicating that the Brownian friction within the solvent was the main contributor to the heating power of IOMNPs.

  12. Behavioral synthesis of asynchronous circuits

    DEFF Research Database (Denmark)

    Nielsen, Sune Fallgaard

    2005-01-01

    This thesis presents a method for behavioral synthesis of asynchronous circuits, which aims at providing a synthesis flow which uses and tranfers methods from synchronous circuits to asynchronous circuits. We move the synchronous behavioral synthesis abstraction into the asynchronous handshake...... is idle. This reduces unnecessary switching activity in the individual functional units and therefore the energy consumption of the entire circuit. A collection of behavioral synthesis algorithms have been developed allowing the designer to perform time and power constrained design space exploration...

  13. Synthesis of organosilicon compounds

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, G. [Iowa State Univ., Ames, IA (United States)

    1996-01-01

    Silicon-containing polymers have been a focus of synthesis and study in Dr. Barton`s group because of their chemistry and properties which are not offered by other systems or materials. For example, the polymer -[-SiMe2C≡C-]n-can be easily processed to films or fibers from melt or solution, and thermally converted to a SiC-containing ceramic in high yield at high temperature. In recent years, carbosilane dendritic polymers have been of great interests in many research groups. However, no synthesis of carbosilane dendrimers with functionalties both inside and outside the dendrimer has been reported. Functionality is very important in the synthesis of preceramic polymers. This thesis will be devoted to exploring several new organosilicon polymer systems.

  14. Total Synthesis of Strychnine.

    Science.gov (United States)

    Lee, Geun Seok; Namkoong, Gil; Park, Jisook; Chen, David Y-K

    2017-11-16

    The total synthesis of the flagship Strychnos indole alkaloid, strychnine, has been accomplished. The developed synthetic sequence features a novel vinylogous 1,4-addition, a challenging iodinium salt mediated silyl enol ether arylation, a palladium-catalyzed Heck reaction, and a streamlined late-stage conversion to strychnine. Furthermore, an application of asymmetric counterion-directed catalysis (ACDC) in the context of target-oriented organic synthesis has been rendered access to an optically active material. The synthetic sequence described herein represents the most concise entry to optically active strychnine to date. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. 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.

  16. Direct dimethyl ether synthesis from synthesis gas: The influence of methanol dehydration on methanol synthesis reaction

    OpenAIRE

    Dadgar, Farbod; Myrstad, Rune; Pfeifer, Peter; Holmen, Anders; Venvik, Hilde Johnsen

    2016-01-01

    Direct dimethyl ether (DME) synthesis from synthesis gas is studied with regard to potential effects of methanol dehydration on methanol formation and copper-based catalyst performance. For this, the influence of the operating conditions (space velocity, temperature, pressure, time-on-stream and syngas composition) on activity, selectivity and stability of the catalyst was studied and compared for methanol synthesis and direct DME synthesis. The advantage of the direct over the two-step DME s...

  17. An Approach to Interface Synthesis

    DEFF Research Database (Denmark)

    Madsen, Jan; Hald, Bjarne

    1995-01-01

    Presents a novel interface synthesis approach based on a one-sided interface description. Whereas most other approaches consider interface synthesis as optimizing a channel to existing client/server modules, we consider the interface synthesis as part of the client/server module synthesis (which...... may contain the re-use of existing modules). The interface synthesis approach describes the basic transformations needed to transform the server interface description into an interface description on the client side of the communication medium. The synthesis approach is illustrated through a point......-to-point communication, but is applicable to synthesis of a multiple client/server environment. The interface description is based on a formalization of communication events....

  18. Enzymatic synthesis of vanillin

    NARCIS (Netherlands)

    van den Heuvel, RHH; Fraaije, MW; Laane, C; van Berkel, WJH; Heuvel, Robert H.H. van den; Berkel, Willem J.H. van

    Due to increasing interest in natural vanillin, two enzymatic routes for the synthesis of vanillin were developed. The flavoprotein vanillyl alcohol oxidase (VAO) acts on a wide range of phenolic compounds and converts both creosol and vanillylamine to vanillin with high yield. The VAO-mediated

  19. Enzymatic synthesis of vanillin

    NARCIS (Netherlands)

    Heuvel, van den R.H.H.; Fraaije, M.W.; Laane, C.; Berkel, van W.J.H.

    2001-01-01

    Due to increasing interest in natural vanillin, two enzymatic routes for the synthesis of vanillin were developed. The flavoprotein vanillyl alcohol oxidase (VAO) acts on a wide range of phenolic compounds and converts both creosol and vanillylamine to vanillin with high yield. The VAO-mediated

  20. Design synthesis exercise 2012

    NARCIS (Netherlands)

    Melkert, J.A.

    2013-01-01

    The design synthesis exercise forms the closing piece of the third year of the Bachelor degree curriculum of the Faculty of Aerospace Engineering at TU Delft. In this exercise the students learn to apply their acquired knowledge from all aerospace disciplines in one complete design. The object of

  1. Asymmetric synthesis of acetomycin

    NARCIS (Netherlands)

    Kinderman, S.S.; Feringa, B.L.

    1998-01-01

    The synthesis of (-)-acetomycin, a highly functionalized γ-lactone with antitumor activity, was achieved in five steps with nearly complete enantioselectivity. The key step was realized by a large scale lipase R catalyzed esterification of 5-hydroxy-4-methyl-2(5H)-furanone providing

  2. Synthesis de 1-dotriacotanol

    International Nuclear Information System (INIS)

    Hernandez, L.; Gonzalez, J.C.

    1996-01-01

    In order to prepare isotopic labeled long chain aliphatic primary alcohol's, the synthesis overall yielding and chemical purity of 1-dotriacotanol were 41% and 98%, respectively. This procedure is very useful for carbon-14 and tritium labeling at Beta position of saturated fatty alcohol's

  3. Synthesis of Camalexin

    Directory of Open Access Journals (Sweden)

    V. Kovacik

    2001-08-01

    Full Text Available In this paper we describe a new method for the synthesis of camalexin (1 based on the reaction of 1-(tert-butoxycarbonylindole-3-carboxaldehyde with methyl Lcysteinate hydrochloride, followed by oxidation and decarboxylation. Compounds 1, and intermediates 5-7 were identified by elemental analysis, 1H NMR, 13C NMR and mass spectroscopy.

  4. Synthesis of Camalexin

    OpenAIRE

    Dzurilla, M.; Kutschy, P.; Zaletova, J.; Ruzinsky, M.; Kovacik, V.

    2001-01-01

    In this paper we describe a new method for the synthesis of camalexin (1) based on the reaction of 1-(tert-butoxycarbonyl)indole-3-carboxaldehyde with methyl Lcysteinate hydrochloride, followed by oxidation and decarboxylation. Compounds 1, and intermediates 5-7 were identified by elemental analysis, 1H NMR, 13C NMR and mass spectroscopy.

  5. Synthesis of acrylic prepolymer

    International Nuclear Information System (INIS)

    Hussin bin Mohd Nor; Dahlan bin Haji Mohd; Mohamad Hilmi bin Mahmood.

    1988-04-01

    An acrylic prepolymer was synthesized from glycidyl methacrylate (GMA), butyl methacrylate (BMA), methyl methacrylate (MMA) and acrylic acid (AA). Butyl acetate (BAc), benzoyl peroxide (BzO), 4-methoxyphenol (MPh) and triethylamine (TEA) were used as solvent, initiator, inhibitor and catalyst respectively. Observations of the synthesis leading to the formation of acrylic prepolymer are described. (author)

  6. Synthesis, characterization and properties

    Indian Academy of Sciences (India)

    Unknown

    C−H⋅⋅⋅O bonds leading to an intricate hydrogen bonding network. Keywords. Synthesis .... in the refinement riding on their respective parent atoms. ..... nent peaks at 326 and 255 nm which can be assigned to transitions of the intramolecularly hydrogen-bon- ded salicylidenimino chromophore. Cotton effects of negative ...

  7. Synthesis of new radiotracers

    International Nuclear Information System (INIS)

    Chahed, Ahlem

    2008-01-01

    The brain's sensibility besides to the rigorous selectivity of changes taking place on brain's barriers leads us to synthesis specifics radiotracers based on diamine ethylene and marked with technetium radioisotope to form a radiotracer able to pass these barriers and diagnose illnesses in an early stage. These radiotracers are tested by a biodistribution on a small animal to be ratified. (Author)

  8. Synthesis of arabinoxylan fragments

    DEFF Research Database (Denmark)

    Underlin, Emilie Nørmølle; Böhm, Maximilian F.; Madsen, Robert

    , or production of commercial chemicals which are mainly obtained from fossil fuels today.The arbinoxylan fragments have a backbone of β-1,4-linked xylans with α-L-arabinose units attached at specific positions. The synthesis ultilises an efficient synthetic route, where all the xylan units can be derived from D...

  9. Total synthesis of aquatolide

    NARCIS (Netherlands)

    Saya, J.M.; Vos, K.; Klein Nijenhuis, R.A.; van Maarseveen, J.H.; Ingemann, S.; Hiemstra, H.

    2015-01-01

    A total synthesis of the sesquiterpene lactone aquatolide has been accomplished. The central step is an intramolecular [2 + 2]-photocycloaddition of an allene onto an alpha,beta-unsaturated delta-lactone. Other key steps are an intramolecular Horner-Wadsworth-Emmons reaction to close the lactone and

  10. The synthesis of gemcitabine.

    Science.gov (United States)

    Brown, Kylie; Dixey, Michael; Weymouth-Wilson, Alex; Linclau, Bruno

    2014-03-31

    Gemcitabine is a fluorinated nucleoside currently administered against a number of cancers. It consists of a cytosine base and a 2-deoxy-2,2-difluororibose sugar. The synthetic challenges associated with the introduction of the fluorine atoms, as well as with nucleobase introduction of 2,2-difluorinated sugars, combined with the requirement to have an efficient process suitable for large scale synthesis, have spurred significant activity towards the synthesis of gemcitabine exploring a wide variety of synthetic approaches. In addition, many methods have been developed for selective crystallisation of diastereomeric (including anomeric) mixtures. In that regard, the 2-deoxy-2,2-difluororibose sugar is one of the most investigated fluorinated carbohydrates in terms of its synthesis. The versatility of synthetic methods employed is illustrative of the current state of the art of fluorination methodology for the synthesis of CF2-containing carbohydrates, and involves the use of fluorinated building blocks, as well as nucleophilic and electrophilic fluorination of sugar precursors. Copyright © 2014. Published by Elsevier Ltd.

  11. Synthesis of the catalyst

    Indian Academy of Sciences (India)

    Admin

    62 11; Palhagen S, Canger R, Henriksen O, Van Parys J A, Riviere M E and Karolchyk M A 2001 Rufinamide: a double-blind, placebo-controlled proof of principle trial in patients with epilepsy; Epilepsy Res. 43, 115; Bakunov S A, Bakunova S M, Wenzler T, Ghebru M, Werbovetz K A, Brun R and Tidwell R R 2010 Synthesis ...

  12. Industrial scale gene synthesis.

    Science.gov (United States)

    Notka, Frank; Liss, Michael; Wagner, Ralf

    2011-01-01

    The most recent developments in the area of deep DNA sequencing and downstream quantitative and functional analysis are rapidly adding a new dimension to understanding biochemical pathways and metabolic interdependencies. These increasing insights pave the way to designing new strategies that address public needs, including environmental applications and therapeutic inventions, or novel cell factories for sustainable and reconcilable energy or chemicals sources. Adding yet another level is building upon nonnaturally occurring networks and pathways. Recent developments in synthetic biology have created economic and reliable options for designing and synthesizing genes, operons, and eventually complete genomes. Meanwhile, high-throughput design and synthesis of extremely comprehensive DNA sequences have evolved into an enabling technology already indispensable in various life science sectors today. Here, we describe the industrial perspective of modern gene synthesis and its relationship with synthetic biology. Gene synthesis contributed significantly to the emergence of synthetic biology by not only providing the genetic material in high quality and quantity but also enabling its assembly, according to engineering design principles, in a standardized format. Synthetic biology on the other hand, added the need for assembling complex circuits and large complexes, thus fostering the development of appropriate methods and expanding the scope of applications. Synthetic biology has also stimulated interdisciplinary collaboration as well as integration of the broader public by addressing socioeconomic, philosophical, ethical, political, and legal opportunities and concerns. The demand-driven technological achievements of gene synthesis and the implemented processes are exemplified by an industrial setting of large-scale gene synthesis, describing production from order to delivery. Copyright © 2011 Elsevier Inc. All rights reserved.

  13. Facile synthesis of N-rich carbon quantum dots by spontaneous polymerization and incision of solvents as efficient bioimaging probes and advanced electrocatalysts for oxygen reduction reaction.

    Science.gov (United States)

    Lei, Zhouyue; Xu, Shengjie; Wan, Jiaxun; Wu, Peiyi

    2016-01-28

    In this study, uniform nitrogen-doped carbon quantum dots (N-CDs) were synthesized through a one-step solvothermal process of cyclic and nitrogen-rich solvents, such as N-methyl-2-pyrrolidone (NMP) and dimethyl-imidazolidinone (DMEU), under mild conditions. The products exhibited strong light blue fluorescence, good cell permeability and low cytotoxicity. Moreover, after a facile post-thermal treatment, it developed a lotus seedpod surface-like structure of seed-like N-CDs decorating on the surface of carbon layers with a high proportion of quaternary nitrogen moieties that exhibited excellent electrocatalytic activity and long-term durability towards the oxygen reduction reaction (ORR). The peak potential was -160 mV, which was comparable to or even lower than commercial Pt/C catalysts. Therefore, this study provides an alternative facile approach to the synthesis of versatile carbon quantum dots (CDs) with widespread commercial application prospects, not only as bioimaging probes but also as promising electrocatalysts for the metal-free ORR.

  14. Solvent transfer of graphene oxide for synthesis of tin mono-sulfide graphene composite and application as anode of lithium-ion battery

    International Nuclear Information System (INIS)

    Tripathi, Alok M.; Mitra, Sagar

    2016-01-01

    Graphical abstract: Destabilization of graphene oxide colloid and SnS graphene composite preparation for lithium-ion battery. - Abstract: Tin mono sulfide (SnS) graphene composite has been synthesized for anode of lithium-ion battery. For synthesis of composite, graphene oxide (GO)-water (H 2 O) colloid has been destabilized and ensured the complete transfer of graphene oxide into another organic solvent N, N-dimethyl formamide (DMF). Mechanism for the destabilization of GO-H 2 O colloid is established. Surface to surface attachment of SnS on graphene sheet is achieved by solvothermal solution phase assembly of graphene sheets and SnS nanoparticles in DMF solvent. Graphene plays role in nanoparticle formation in composite. Such confined composite has been cycled reversibly at current rate of 160 mA g −1 , in voltage region of 0.01–2.5 V and exhibit a superior discharge capacity of 630 mAh g −1 after 50th cycle. Ex situ TEM analysis of used electrode reveal that the SnS nanoparticle-graphene composite with CMC binder perform better due to proper shape retention of electroactive materials during electrochemical cycling.

  15. Facile synthesis of yeast cross-linked Fe3O4nanoadsorbents for efficient removal of aquatic environment contaminated with As(V).

    Science.gov (United States)

    Rajesh Kumar, S; Jayavignesh, V; Selvakumar, R; Swaminathan, K; Ponpandian, N

    2016-12-15

    A facile solvothermal method was adopted to prepare monodispersed surface functionalized Fe 3 O 4 nanoparticles via self assembly process. The pure yeast, diethylamine functionalized Fe 3 O 4 nanoparticles (DMNPs) and yeast cross-linked Fe 3 O 4 nanoparticles (YcMNPs) were used for the efficient removal of arsenate from aqueous solution. The crystal structure, morphology and magnetic properties of these nanoparticles were characterized by using X-ray diffraction, field emission scanning electron microscopy and vibrating sample magnetometer. The observed physico-chemical properties confirms the metal binding nature of prepared samples. The adsorption of As(V) on the functionalized magnetite nanoparticles was tested under different operating conditions like contact time, adsorbate dosage, adsorbate concentration and pH. The faster removal of As(V) was obtained using YcMNPs (99%) than DMNPs and pure yeast. The adsorption equilibrium data obeys Langmuir isotherm than Freundlich model and the kinetics data well depicts the pseudo-second-order model. The batch column experiment confirms the adequate desorption as well as reusability without significant loss of efficiency. The results reveal the technical feasibility of the prepared nanoparticles for their easy synthesis, recovery, cost effective, eco-friendly and a promising advanced adsorbent for environmental pollution. Copyright © 2016 Elsevier Inc. All rights reserved.

  16. A dechlorination pathway for synthesis of horn shaped carbon nanotubes and its adsorption properties for CO2, CH4, CO and N2.

    Science.gov (United States)

    Sawant, Sandesh Y; Somani, Rajesh S; Bajaj, Hari C; Sharma, Sangita S

    2012-08-15

    Using metallic copper as reductant and tetrachloroethylene as carbon precursor, a simple, low temperature solvothermal method for the synthesis of horn shaped carbon nanotubes is reported. The detail study of reaction parameters such as temperature, time, carbon precursor amount, type and catalyst proportion has been carried out to optimize the conditions wherein that the copper metal (10 g) mediated reduction of tetrachloroethylene (25 mL) at 200°C for 5h resulted in the horn shaped carbon nanotubes with high yield and structural selectivity. The adsorption properties of horn shaped carbon nanotubes were investigated for carbon dioxide, methane, carbon monoxide and nitrogen as adsorbate by volumetric measurements up to 850 mm Hg. The prepared horn shaped carbon nanotubes showed good adsorption capacity for CO(2) (45 cm(3)/g) and CO (17 cm(3)/g), at 303 K and 850 mm Hg pressure, with high equilibrium selectivity (73.3 for CO(2) and 110.7 for CO at 318 K) and capacity selectivity (9.1 for CO(2) and 3.1 for CO at 850 mm Hg and 318 K) over nitrogen which provides the tool for the separation of CO(2) from its mixture with nitrogen observed in flue gas of thermal power plants and boilers, as well as with CO such as syngas. Copyright © 2012 Elsevier B.V. All rights reserved.

  17. Synthesis of Zn-Cu-Cd sulfide nanospheres with controlled copper locations and their effects on photocatalytic activities for H{sub 2} production

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Yabo; Xu, Rong [School of Chemical and Biomedical Engineering, Nanyang Technological University, 62 Nanyang Drive, Singapore 637459 (Singapore); Wang, Yongsheng [School of Mechanical and Aerospace Engineering, Nanyang Technological University, 50 Nanyang Avenue, Singapore 639798 (Singapore)

    2010-06-15

    In this work, a two-step solvothermal method was used to synthesize Zn-Cu-Cd sulfide nanospheres with controlled copper locations. The structural and other physical properties of the nanospheres were investigated by XRD, FESEM, TEM, energy-filtered TEM, XPS, ICP and UV-vis DRS methods. By varying the addition of the copper precursor during the two synthesis steps, Zn-Cu-Cd sulfide nanospheres with three distinctive copper distribution patterns can be obtained with copper (i) only in the core, (ii) only on the surface shell, and (iii) both in the core and on the surface shell. The influence of the location and concentration of copper on the photocatalytic activity for hydrogen production from water under visible light was investigated. It was found that the activity of the sample with copper only on the surface shell is about two times of that with copper only in the core. The highest hydrogen production rate was obtained on the nanosphere sample with copper both in the core and on the surface shell. The possible mechanism was discussed. The findings from this study are important for the development of efficient photocatalysts based on ternary or multinary systems. (author)

  18. Template-free construction of hollow α-Fe2O3 hexagonal nanocolumn particles with an exposed special surface for advanced gas sensing properties.

    Science.gov (United States)

    Sun, Linqiang; Han, Xiao; Liu, Kai; Yin, Shan; Chen, Qiaoli; Kuang, Qin; Han, Xiguang; Xie, Zhaoxiong; Wang, Chao

    2015-06-07

    Hollow α-Fe2O3 hexagonal nanocolumn particles (HHCPs) with exposed (101[combining macron]0) and (112[combining macron]5) facets have been synthesized through a hydrothermal method in the absence of templates. The time-dependent experimental results demonstrate that the formation of HHCPs includes four main steps: (1) formation of nanowire precursors, (2) aggregation and conversion to Fe1.833(OH)0.5O2 solid ellipsoid particles (SEPs), (3) dehydration to form hollow ellipsoid particles (HEPs), and (4) recrystallization to HHCPs. Due to their advantages of the hollow structure and the exposed special external and internal surface on the pore structure, the HHCPs exhibit higher gas sensing ability than that of calcined SEPs (CSEPs) and HEPs.

  19. Interface-defect-mediated photocatalysis of mesocrystalline ZnO assembly synthesized in-situ via a template-free hydrothermal approach

    Science.gov (United States)

    Wang, Hui; Wang, Cuicui; Chen, Qifeng; Ren, Baosheng; Guan, Ruifang; Cao, Xiaofeng; Yang, Xiaopeng; Duan, Ran

    2017-08-01

    Both architecture construction and defects engineering of photocatalysts are highly vital in the photocatalytic activity. We report herein that the interface-defect-mediated photocatalytic activity of pompon-like ZnO (P-ZnO) mesocrystal photocatalyst synthesized via an aqueous approach, in the presence of sodium citrate without any other organic templates. The microstructure and defects of the diverse ZnO photocatalysts were examined with various techniques. The results indicated that the P-ZnO assemblies were composed of mesocrystal nanosheets exposed high energy (002) facet with high crystallinity. More importantly, the defects located at the interfaces among the nanocrystals in ZnO mesocrystals played an important role in the photocatalytic activity than that of interstitial zinc vacancies in bulk, which was confirmed by photocatalytic degradation of organic pollutants, such as methylene blue (MB) and 2,4,6-trichlorophenol (2,4,6-TCP). The results showed that the P-ZnO exhibited higher photocatalytic activity than that of the nanosized ZnO (N-ZnO), which could be attributed to not only the unique mesocrystal structure and high energy (002) facet exposed, but also the defects located at interfaces among nanocrystals in ZnO mesocrystals. In addition, the formation mechanism of the P-ZnO was investigated via a time-dependent method. It was found that the formation of P-ZnO hierarchical architecture assembled with ZnO mesocrystals involved a nonclassical crystallization growth and Ostwald Ripening process. This study provides a perspective on the improvement in photocatalytic activity via adjusting the bulk and interface defects and construction of hierarchical architectures of semiconductors.

  20. Template Free and Binderless NiO Nanowire Foam for Li-ion Battery Anodes with Long Cycle Life and Ultrahigh Rate Capability.

    Science.gov (United States)

    Liu, Chueh; Li, Changling; Ahmed, Kazi; Mutlu, Zafer; Ozkan, Cengiz S; Ozkan, Mihrimah

    2016-07-18

    Herein, NiO-decorated Ni nanowires with diameters ca. 30-150 nm derived from Ni wire backbone (ca. 2 μm in diameter) is directly synthesized on commercially available Ni foam as a renovated anode for Li-ion batteries. Excellent stability with capacity 680 mAh g(-1) at 0.5C (1C = 718 mA g(-1)) is achieved after 1000 cycles. Superior rate capability is exhibited by cycling at extremely high current rates, such as 20C and 50C with capacities ca. 164 and 75 mAh g(-1), respectively. The capacity can be recovered back to ca. 430 mAh g(-1) in 2 cycles when lowered to 0.2C and stably cycled for 430 times with capacity 460 mAh g(-1). The NiO nanowire foam anode possesses low equivalent series resistance ca. 3.5 Ω, resulting in superior power performance and low resistive losses. The NiO nanowire foam can be manufactured with bio-friendly chemicals and low temperature processes without any templates, binders and conductive additives, which possesses the potential transferring from lab scale to industrial production.

  1. Template-free fabrication of hierarchical MoS2/MoO2 nanostructures as efficient catalysts for hydrogen production

    Science.gov (United States)

    Zhang, Xiangyong; Du, Zijie; Luo, Xiaonan; Sun, Aokui; Wu, Zhuangzhi; Wang, Dezhi

    2018-03-01

    A hierarchical MoS2/MoO2 nanostructure is presented as a highly efficient catalyst for the hydrogen evolution reaction (HER), which is prepared via a facile hydrothermal route in the absence of templates. The influence of various Mo sources has been studied and the roles of MoS2 shell and MoO2 core are discussed. It is found that the MoS2/MoO2 nanostructures derived from the MoO2 nanobelts exhibit the best HER activity, and the HER performance is strongly affected by the relative contents of MoS2 shell and MoO2 core, which correspond to the mass transport ability and the electron transfer ability, respectively.

  2. Growth of raspberry-, prism- and flower-like ZnO particles using template-free low-temperature hydrothermal method and their application as humidity sensors

    International Nuclear Information System (INIS)

    Pál, Edit; Hornok, Viktória; Kun, Robert; Chernyshev, Vladimir; Seemann, Torben; Dékány, Imre; Busse, Matthias

    2012-01-01

    Zinc oxide particles with different morphologies were prepared by hydrothermal method at 60–90 °C. The structure formation was controlled by the addition rate and temperature of hydrolyzing agent, while the particles size (10 nm–2.5 μm) was influenced by the preparation (hydrothermal) temperature. Scanning electron microscopy studies showed that raspberry-, prism- and flower-like ZnO particles were prepared, whose average size decreased with increasing reaction temperature. X-ray diffraction investigations confirmed that ZnO particles with hexagonal crystal structure formed in all syntheses. The raspberry-, prism- and flower-like ZnO particles showed a weak UV-emission in the range of 390–395 nm and strong visible emission with a maximum at 586, 593 and 598 nm, respectively. Morphology effect on electrical and water vapour sensing properties of ZnO samples was investigated by impedance spectroscopy and quartz crystal microbalance, respectively. The absolute impedance of raspberry-, prism- and flower-like ZnO particles was found to be strong dependent on the morphology. Space-charge-limited conductivity transport mechanism was proved by the oscillatory behaviour of impedance. Humidity sensor tests also revealed morphology and specific surface area dependency on the sensitivity and water vapour adsorption property.

  3. 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.

  4. Voice synthesis application

    Science.gov (United States)

    Lightstone, P. C.; Davidson, W. M.

    1982-04-01

    The military detection assessment laboratory houses an experimental field system which assesses different alarm indicators such as fence disturbance sensors, MILES cables, and microwave Racons. A speech synthesis board which could be interfaced, by means of a computer, to an alarm logger making verbal acknowledgement of alarms possible was purchased. Different products and different types of voice synthesis were analyzed before a linear predictive code device produced by Telesensory Speech Systems of Palo Alto, California was chosen. This device is called the Speech 1000 Board and has a dedicated 8085 processor. A multiplexer card was designed and the Sp 1000 interfaced through the card into a TMS 990/100M Texas Instrument microcomputer. It was also necessary to design the software with the capability of recognizing and flagging an alarm on any 1 of 32 possible lines. The experimental field system was then packaged with a dc power supply, LED indicators, speakers, and switches, and deployed in the field performing reliably.

  5. Synthesis of quantum dots

    Science.gov (United States)

    McDaniel, Hunter

    2017-10-17

    Common approaches to synthesizing alloyed quantum dots employ high-cost, air-sensitive phosphine complexes as the selenium precursor. Disclosed quantum dot synthesis embodiments avoid these hazardous and air-sensitive selenium precursors. Certain embodiments utilize a combination comprising a thiol and an amine that together reduce and complex the elemental selenium to form a highly reactive selenium precursor at room temperature. The same combination of thiol and amine acts as the reaction solvent, stabilizing ligand, and sulfur source in the synthesis of quantum dot cores. A non-injection approach may also be used. The optical properties of the quantum dots synthesized by this new approach can be finely tuned for a variety of applications by controlling size and/or composition of size and composition. Further, using the same approach, a shell can be grown around a quantum dot core that improves stability, luminescence efficiency, and may reduce toxicity.

  6. Prebiotic synthesis of histidine

    Science.gov (United States)

    Shen, C.; Yang, L.; Miller, S. L.; Oro, J.

    1990-01-01

    The prebiotic formation of histidine (His) has been accomplished experimentally by the reaction of erythrose with formamidine followed by a Strecker synthesis. In the first step of this reaction sequence, the formation of imidazole-4-acetaldehyde took place by the condensation of erythrose and formamidine, two compounds that are known to be formed under prebiotic conditions. In a second step, the imidazole-4-acetaldehyde was converted to His, without isolation of the reaction products by adding HCN and ammonia to the reaction mixture. LC, HPLC, thermospray liquid chromatography-mass spectrometry, and tandem mass spectrometry were used to identify the product, which was obtained in a yield of 3.5% based on the ratio of His/erythrose. This is a new chemical synthesis of one of the basic amino acids which had not been synthesized prebiotically until now.

  7. Distributed PROMPT-LTL Synthesis

    Directory of Open Access Journals (Sweden)

    Swen Jacobs

    2016-09-01

    Full Text Available We consider the synthesis of distributed implementations for specifications in Prompt Linear Temporal Logic (PROMPT-LTL, which extends LTL by temporal operators equipped with parameters that bound their scope. For single process synthesis it is well-established that such parametric extensions do not increase worst-case complexities. For synchronous systems, we show that, despite being more powerful, the distributed realizability problem for PROMPT-LTL is not harder than its LTL counterpart. For asynchronous systems we have to consider an assume-guarantee synthesis problem, as we have to express scheduling assumptions. As asynchronous distributed synthesis is already undecidable for LTL, we give a semi-decision procedure for the PROMPT-LTL assume-guarantee synthesis problem based on bounded synthesis.

  8. Microwave multicomponent synthesis.

    Science.gov (United States)

    Hügel, Helmut M

    2009-12-01

    In the manner that very important research is often performed by multidisciplinary research teams, the applications of multicomponent reactions involving the combination of multiple starting materials with different functional groups leading to the higher efficiency and environmentally friendly construction of multifunctional/complex target molecules is growing in importance. This review will explore the advances and advantages in microwave multicomponent synthesis (MMS) that have been achieved over the last five years.

  9. Microwave Multicomponent Synthesis

    Directory of Open Access Journals (Sweden)

    Helmut M. Hügel

    2009-12-01

    Full Text Available In the manner that very important research is often performed by multidisciplinary research teams, the applications of multicomponent reactions involving the combination of multiple starting materials with different functional groups leading to the higher efficiency and environmentally friendly construction of multifunctional/complex target molecules is growing in importance. This review will explore the advances and advantages in microwave multicomponent synthesis (MMS that have been achieved over the last five years.

  10. Microwave Multicomponent Synthesis

    OpenAIRE

    Helmut M. Hügel

    2009-01-01

    In the manner that very important research is often performed by multidisciplinary research teams, the applications of multicomponent reactions involving the combination of multiple starting materials with different functional groups leading to the higher efficiency and environmentally friendly construction of multifunctional/complex target molecules is growing in importance. This review will explore the advances and advantages in microwave multicomponent synthesis (MMS) that have been achiev...

  11. Synthesis of functionalised sulfonamides

    OpenAIRE

    Mok, B. L.

    2008-01-01

    Sulfonamides are important therapeutic agents and have a diverse array of biological functions in biology and medicine. Their means of synthesis has often involved the use of unstable sulfonyl chloride species; however, recent research has established pentafluorophenyl (PFP) sulfonate esters as a useful stable alternative to such species. This thesis describes the use of PFP vinyl sulfonate in a [3+2] cycloaddition with a variety of N-methyl-nitrones, providing access to the corresponding...

  12. Phase contrast image synthesis

    DEFF Research Database (Denmark)

    Glückstad, J.

    1996-01-01

    A new method is presented for synthesizing arbitrary intensity patterns based on phase contrast imaging. The concept is grounded on an extension of the Zernike phase contrast method into the domain of full range [0; 2 pi] phase modulation. By controlling the average value of the input phase funct...... function and by choosing appropriate phase retardation at the phase contrast filter, a pure phase to intensity imaging is accomplished. The method presented is also directly applicable in dark field image synthesis....

  13. Integrated methanol synthesis

    International Nuclear Information System (INIS)

    Jaeger, W.

    1982-01-01

    This invention concerns a plant for methanol manufacture from gasified coal, particularly using nuclear power. In order to reduce the cost of the hydrogen circuits, the methanol synthesis is integrated in the coal gasification plant. The coal used is gasified with hydration by means of hydrogen and the crude gas emerging, after cooling and separating the carbon dioxide and hydrogen sulphide, is mixed with the synthetic gas leaving the methane cracking furnace. This mixture is taken to the methanol synthesis and more than 90% is converted into methanol in one pass. The gas mixture remaning after condensation and separation of methanol is decomposed into three fractions in low temperature gas decomposition with a high proportion of unconverted carbon monoxide. The flow of methane is taken to the cracking furnace with steam, the flow of hydrogen is taken to the hydrating coal gasifier, and the flow of carbon monoxide is taken to the methanol synthesis. The heat required for cracking the methane can either be provided by a nuclear reactor or by the coke left after hydrating gasification. (orig./RB) [de

  14. Gold Nanoparticle Microwave Synthesis

    International Nuclear Information System (INIS)

    Krantz, Kelsie E.; Christian, Jonathan H.; Coopersmith, Kaitlin; Washington II, Aaron L.; Murph, Simona H.

    2016-01-01

    At the nanometer scale, numerous compounds display different properties than those found in bulk material that can prove useful in areas such as medicinal chemistry. Gold nanoparticles, for example, display promise in newly developed hyperthermia therapies for cancer treatment. Currently, gold nanoparticle synthesis is performed via the hot injection technique which has large variability in final particle size and a longer reaction time. One underdeveloped area by which these particles could be produced is through microwave synthesis. To initiate heating, microwaves agitate polar molecules creating a vibration that gives off the heat energy needed. Previous studies have used microwaves for gold nanoparticle synthesis; however, polar solvents were used that partially absorbed incident microwaves, leading to partial thermal heating of the sample rather than taking full advantage of the microwave to solely heat the gold nanoparticle precursors in a non-polar solution. Through this project, microwaves were utilized as the sole heat source, and non-polar solvents were used to explore the effects of microwave heating only as pertains to the precursor material. Our findings show that the use of non-polar solvents allows for more rapid heating as compared to polar solvents, and a reduction in reaction time from 10 minutes to 1 minute; this maximizes the efficiency of the reaction, and allows for reproducibility in the size/shape of the fabricated nanoparticles.

  15. Gold Nanoparticle Microwave Synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Krantz, Kelsie E. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Christian, Jonathan H. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Coopersmith, Kaitlin [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Washington, II, Aaron L. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Murph, Simona H. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2016-07-27

    At the nanometer scale, numerous compounds display different properties than those found in bulk material that can prove useful in areas such as medicinal chemistry. Gold nanoparticles, for example, display promise in newly developed hyperthermia therapies for cancer treatment. Currently, gold nanoparticle synthesis is performed via the hot injection technique which has large variability in final particle size and a longer reaction time. One underdeveloped area by which these particles could be produced is through microwave synthesis. To initiate heating, microwaves agitate polar molecules creating a vibration that gives off the heat energy needed. Previous studies have used microwaves for gold nanoparticle synthesis; however, polar solvents were used that partially absorbed incident microwaves, leading to partial thermal heating of the sample rather than taking full advantage of the microwave to solely heat the gold nanoparticle precursors in a non-polar solution. Through this project, microwaves were utilized as the sole heat source, and non-polar solvents were used to explore the effects of microwave heating only as pertains to the precursor material. Our findings show that the use of non-polar solvents allows for more rapid heating as compared to polar solvents, and a reduction in reaction time from 10 minutes to 1 minute; this maximizes the efficiency of the reaction, and allows for reproducibility in the size/shape of the fabricated nanoparticles.

  16. Structure and magnetic properties evolution of rod-like Co{sub 0.5}Ni{sub 0.25}Zn{sub 0.25}Dy{sub x}Fe{sub 2−x}O{sub 4} synthesized by solvothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Wen; Liu, Dongsheng [School of Chemistry and Chemical Engineering, Guangxi University, Nanning, 530004 (China); Wu, Wenwei, E-mail: gxuwuwenwei@aliyun.com [School of Chemistry and Chemical Engineering, Guangxi University, Nanning, 530004 (China); Guangxi Colleges and Universities Key Laboratory of Applied Chemistry Technology and Resource Development, Nanning, 530004 (China); Zhang, Huaxin; Wu, Juan [School of Chemistry and Chemical Engineering, Guangxi University, Nanning, 530004 (China)

    2017-01-15

    A series of Dy{sup 3+} doped Co–Ni–Zn ferrites with the formula Co{sub 0.5}Ni{sub 0.25}Zn{sub 0.25}Dy{sub x}Fe{sub 2−x}O{sub 4} 0≤x≤0.24) have been successfully synthesized using the solvothermal method. X-ray diffraction and scanning electron microscope examinations indicate that a highly-crystallized cubic Co{sub 0.5}Ni{sub 0.25}Zn{sub 0.25}Dy{sub x}Fe{sub 2−x}O{sub 4} with rod-like morphology is obtained when the precursor is calcined at 1000 °C in air for 3 h. Single phase Co{sub 0.5}Ni{sub 0.25}Zn{sub 0.25}Fe{sub 2}O{sub 4} is obtained at 650 °C, but all samples consist of the main spinel phase in combination of a small amount of a foreign Dy{sub 2}O{sub 3} phase after doping Dy. When the precursor is calcined at 1000 °C, the lattice parameter of the ferrites initially increase after doping Dy, but then become smaller with increasing Dy content. The addition of Dy content results in a reduction of crystallite size, attributed that the binding energy of Dy{sup 3+}–O{sup 2−} is larger than that of Fe{sup 3+}–O{sup 2−}. Dy{sup 3+} substitution can decrease the remanence (Mr) and coercivity (Hc) of Co{sub 0.5}Ni{sub 0.25}Zn{sub 0.25}Dy{sub x}Fe{sub 2−x}O{sub 4} samples, which are very desirable characteristics for high density data storage devices. - Highlights: • Rod-like Co{sub 0.5}Ni{sub 0.25}Zn{sub 0.25}Dy{sub x}Fe{sub 2−x}O{sub 4} was synthesized by solvothermal method. • Magnetic properties evolution for Co{sub 0.5}Ni{sub 0.25}Zn{sub 0.25}Dy{sub x}Fe{sub 2−x}O{sub 4} was explained. • Dy{sup 3+} substitution can decrease the remanence and coercivity of Co{sub 0.5}Ni{sub 0.25}Zn{sub 0.25}Dy{sub x}Fe{sub 2−x}O{sub 4}.

  17. Mesoporous silicon synthesis and applications in Li-ion batteries and solar hydrogen fuel cells

    Science.gov (United States)

    Wang, Donghai; Dai, Fang; Yi, Ran; Zai, Jianto

    2017-05-23

    We provide a mesoporous silicon material (PSi) prepared via a template-free and HF-free process. The production process is facile and scalable, and it may be conducted under mild reaction conditions. The silicon may be produced directly by the reduction of a silicon-halogenide precursor (for example, SiCl.sub.4) with an alkaline alloy (for example, NaK alloy). The resulting Si-salt matrix is then annealed for the pore formation and crystallite growth. Final product is obtained by removal of the salt by-products with water.

  18. Multifunctional role of rare earth doping in optical materials: nonaqueous sol-gel synthesis of stabilized cubic HfO2 luminescent nanoparticles.

    Science.gov (United States)

    Lauria, Alessandro; Villa, Irene; Fasoli, Mauro; Niederberger, Markus; Vedda, Anna

    2013-08-27

    In this work a strategy for the control of structure and optical properties of inorganic luminescent oxide-based nanoparticles is presented. The nonaqueous sol-gel route is found to be suitable for the synthesis of hafnia nanoparticles and their doping with rare earths (RE) ions, which gives rise to their luminescence either under UV and X-ray irradiation. Moreover, we have revealed the capability of the technique to achieve the low-temperature stabilization of the cubic phase through the effective incorporation of trivalent RE ions into the crystal lattice. Particular attention has been paid to doping with europium, causing a red luminescence, and with lutetium. Structure and morphology characterization by XRD, TEM/SEM, elemental analysis, and Raman/IR vibrational spectroscopies have confirmed the occurrence of the HfO2 cubic polymorph for dopant concentrations exceeding a threshold value of nominal 5 mol %, for either Lu(3+) or Eu(3+). The optical properties of the nanopowders were investigated by room temperature radio- and photoluminescence experiments. Specific features of Eu(3+) luminescence sensitive to the local crystal field were employed for probing the lattice modifications at the atomic scale. Moreover, we detected an intrinsic blue emission, allowing for a luminescence color switch depending on excitation wavelength in the UV region. We also demonstrate the possibility of changing the emission spectrum by multiple RE doping in minor concentration, while deputing the cubic phase stabilization to a larger concentration of optically inactive Lu(3+) ions. The peculiar properties arising from the solvothermal nonaqueous synthesis here used are described through the comparison with thermally treated powders.

  19. Application of chalcones in heterocycles synthesis: Synthesis of 2 ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 125; Issue 3. Application of chalcones in heterocycles synthesis: Synthesis of 2-(isoxazolo, pyrazolo and pyrimido) substituted analogues of 1,4-benzodiazepin-5-carboxamides linked through an oxyphenyl bridge. N Kaur D Kishore. Volume 125 Issue 3 May 2013 pp ...

  20. Superparamagnetic plasmonic nanohybrids: shape-controlled synthesis, TEM-induced structure evolution, and efficient sunlight-driven inactivation of bacteria.

    Science.gov (United States)

    Zhai, Yueming; Han, Lei; Wang, Ping; Li, Gaiping; Ren, Wen; Liu, Ling; Wang, Erkang; Dong, Shaojun

    2011-11-22

    Magnetic materials and noble metal-based multifunctional hybrids have attracted much attention recently due to their unique properties and potential applications in a variety of fields. However, substantial challenges remain to directly obtain water-soluble hybrids with well-defined structures and to directly combine magnetic nanoparticles with nonspherical noble metals. We describe here for the first time a simple solvothermal method to synthesize a series of novel water-soluble nanohybrids composed of shape-tuned Ag cores and a Fe(3)O(4) shell. We found that small Fe(3)O(4) grains can be well-distributed directly on the surface on the Ag seeds. Such hybrids have both plasmonic and significant superparamagnetic properties, enabling magnetic separation. The plasmon resonance frequency of Ag nanostructures can be fine-tuned through the interactions between the two components. In addition, the decorated Fe(3)O(4) nanoparticles stabilized the Ag nanostructures when exposed to air and natural light for a long time. Furthermore, an interesting structural transformation is observed in the one-dimensional Ag-Fe(3)O(4) nanowires under high-energy electron beam. The Ag core can diffuse through the porous iron oxide shell, break away, and result in the formation of Ag nanocluster-decorated iron oxide tubes. Finally, the hybrids acted as a chemical template for the synthesis of Fe(3)O(4)/Au-AgCl double-layer nanotubes that display obvious near-infrared absorption. Importantly, the double-layer nanotubes exhibited enhanced photocatalytic inactivation of bacteria at very low concentrations under natural sunlight. © 2011 American Chemical Society

  1. The synthesis of magnetic lysozyme-imprinted polymers by means of distillation-precipitation polymerization for selective protein enrichment.

    Science.gov (United States)

    Cao, Jiali; Zhang, Xihao; He, Xiwen; Chen, Langxing; Zhang, Yukui

    2014-02-01

    A protein imprinting approach for the synthesis of core-shell structure nanoparticles with a magnetic core and molecularly imprinted polymer (MIP) shell was developed using a simple distillation-precipitation polymerization method. In this work, Fe3O4 magnetic nanoparticles were first synthesized through a solvothermal method and then were conveniently surface-modified with 3-(methacryloyloxy)propyltrimethoxylsilane as anchor molecules to donate vinyl groups. Next a high-density MIP shell was coated onto the surface of the magnetic nanoparticles by the copolymerization of functional monomer acrylamide (AAm), cross-linking agent N,N'-methylenebisacrylamide (MBA), the initiator azodiisobutyronitrile (AIBN), and protein in acetonitrile heated at reflux. The morphology, adsorption, and recognition properties of the magnetic molecularly imprinted nanoparticles were investigated by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), vibrating sample magnetometer (VSM), and rebinding experiments. The resulting MIP showed a high adsorption capacity (104.8 mg g(-1)) and specific recognition (imprinting factor=7.6) to lysozyme (Lyz). The as-prepared Fe3O4@Lyz-MIP nanoparticles with a mean diameter of 320 nm were coated with an MIP shell that was 20 nm thick, which enabled Fe3O4@Lyz-MIP to easily reach adsorption equilibrium. The high magnetization saturation (40.35 emu g(-1)) endows the materials with the convenience of magnetic separation under an external magnetic field and allows them to be subsequently reused. Furthermore, Fe3O4@Lyz-MIP could selectively extract a target protein from real egg-white samples under an external magnetic field. Copyright © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Recycling of iron and silicon from drinking water treatment sludge for synthesis of magnetic iron oxide@SiO₂ composites.

    Science.gov (United States)

    Meng, Lingyou; Chan, Yingzi; Wang, Han; Dai, Ying; Wang, Xue; Zou, Jinlong

    2016-03-01

    More attention has been paid to the deterioration of water bodies polluted by drinking water treatment sludge (DWTS) in recent years. It is important to develop methods to effectively treat DWTS by avoiding secondary pollution. We report herein a novel investigation for recovery of Si and Fe from DWTS, which are used for the synthesis of two iron oxide@SiO2 composites for adsorption of reactive red X-3B (RRX-3B) and NaNO2. The results show that Fe(3+) (acid-leaching) and Si(4+) (basic-leaching) can be successfully recovered from roasted DWTS. Whether to dissolve Fe(OH)3 precipitation is the key point for obtaining Fe3O4 or γ-Fe2O3 particles using the solvothermal method. The magnetic characteristics of Fe3O4@SiO2 (390.0 m(2) g(-1)) or Fe2O3@SiO2 (220.9 m(2) g(-1)) are slightly influenced by the coated porous SiO2 layer. Peaks of Fe-O stretching vibration (580 cm(-1)) and asymmetric Si-O-Si stretching vibrations (1080 cm(-1)) of Fe3O4@SiO2 indicate the successful coating of a thin silica layer (20-150 nm). The adsorption capacity of RRX-3B and NaNO2 by Fe3O4@SiO2 is better than that of Fe2O3@SiO2, and both composites can be recycled through an external magnetic field. This method is an efficient and environmentally friendly method for recycling DWTS.

  3. The effect of phase interface on the synthesis of SnS{sub 2}-Cu{sub 2}S

    Energy Technology Data Exchange (ETDEWEB)

    Yazdani, Ahmad, E-mail: Yazdania@modares.ac.ir [Department of Physics, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Shadrokh, Zohreh [Department of Physics, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Department of Physics, University of Shahrood, P.O. Box 316-36155, Shahrood (Iran, Islamic Republic of); Eshghi, Hosein [Department of Physics, University of Shahrood, P.O. Box 316-36155, Shahrood (Iran, Islamic Republic of)

    2016-08-15

    Highlights: • Opto-crystalline character of the composition of Cu{sub 2}S and S{sub 2}Sn was considered. • The formation Cu{sub 2}SnS{sub 3} is strongly related to phase separation at interface. • The entanglement of phases is strongly due to the chemical bond competition. • The suggested fluctuation region is approved by PL spectra. • Reconstruction and cluster formation is evident by formation of flat-spiral flowers. - Abstract: Optical character of crystal structure of the composition of two different semiconducting metallic sulfides, Cu{sub 2}S and S{sub 2}Sn, in pure phase formation of the ternary chalcogenide Cu{sub 2}SnS{sub 3} was considered. Because of the difficulties related to the phase separation at the definite Eutectic temperature for the composite formation, which is evident in optical absorption fluctuations, solvothermal synthesis in the intermediate temperature range 180–220 °C seems convenient where tetragonal crystal structure is investigated by XRD. Absorption fluctuations below E = E{sub g} were more pronounced for the lower limit case (180 °C) reflected in a sharp peak located at 1.48 eV on S1 as seen in UV-PL measurement. The characteristic behavior of the interface, resulting in the reconstruction and cluster formation due to the offset of bond rupturing displacement of atomic positions, is in favor of aggregation instead of agglomeration, which is evident by formation of small flat-spiral flowers in SEM images.

  4. Metal oxide blended ZSM-5 nanocomposites as ethanol sensors

    Indian Academy of Sciences (India)

    ZSM-5 zeolite crystals are synthesized via microwave- assisted template-free hydrothermal method as per the method described in literature to reduce the synthesis time. [17]. Sodium aluminate (aluminium source), sodium hydrox- ide and silica sol (silica source) are used as the starting chem- icals to obtain synthesis sol.

  5. Preparation of CuS nanoparticles embedded in poly(vinyl alcohol ...

    Indian Academy of Sciences (India)

    WINTEC

    of methods have been developed for the synthesis of CuS nanostructures including hydrothermal route (Zhang et al. 2004a,b; Ji et al 2005; Zhu et al 2005; Roy and. Srivastava 2006), organogel (Xue et al 2004), hydrogel- assisted synthesis (Kalyanikutty et al 2006), template- free chemical route (Gautam et al 2004), ...

  6. Gene Synthesis with HG Khorana

    Indian Academy of Sciences (India)

    Home; Journals; Resonance – Journal of Science Education; Volume 17; Issue 12. Gene Synthesis with H G Khorana. Marvin H Caruthers. General Article Volume 17 Issue 12 December 2012 pp ... Keywords. Chemical synthesis of genes for yeast alanine tRNA and E. coli supressor tRNA; Khorana's philosophy on science.

  7. Organic synthesis with stable isotopes

    International Nuclear Information System (INIS)

    Blazer, R.M.; Daub, G.H.; Kerr, V.N.; Williams, D.L.; Whaley, T.W.

    1982-01-01

    Described is a scheme for the synthesis of L-arginine-1- 13 C utilizing methods developed for the synthesis of L-ornithine-1- 13 C from L-ornithine-2- 13 C and then converting ornithine into arginine with the enzyme acylase

  8. Chemical synthesis on SU-8

    DEFF Research Database (Denmark)

    Qvortrup, Katrine; Taveras, Kennedy; Thastrup, Ole

    2011-01-01

    In this paper we describe a highly effective surface modification of SU-8 microparticles, the attachment of appropriate linkers for solid-supported synthesis, and the successful chemical modification of these particles via controlled multi-step organic synthesis leading to molecules attached...

  9. Organic Synthesis using Clay Catalysts

    Indian Academy of Sciences (India)

    His work includes organic synthesis and reaction mechanisms mainly in the area of organosilicon chemistry. Presently he is also working on organic synthesis under solvent- free conditions and using clay-catalyses. Keywords. Montmorillonite, ion-exchange, clay-nanomaterials, dehydration pyrolysis, rearrangement, steric.

  10. First total synthesis of Boehmenan

    Indian Academy of Sciences (India)

    The first total synthesis of dilignan Boehmenan has been achieved. A biomimetic oxidative coupling of the ferulic acid methyl ester in the presence of silver oxide is the crucial step in the synthesis sequence, generating the dihydrobenzofuran skeleton. Hydroxyl group was protected with DHP and reducted with LiAlH4 to ...

  11. SHORT COMMUNICATION SYNTHESIS AND ANTIBACTERIAL ...

    African Journals Online (AJOL)

    Admin

    a. sodium nitrite, b. ethylacetoacetate, c. phenyl hydrazine, d. hydrazine hydrate, e. hydroxyl- amine hydrochloride, f. Salycylaldehye, g. chloroacetyl chloride, h. thioglycollic acid. Scheme 1. Synthesis of heterocyclic derivatives of sulfanilamide. Synthesis of compound 1 and 2a-e were done as per the reported method [7-8] ...

  12. Total synthesis of proposed auranthine.

    Science.gov (United States)

    Kshirsagar, Umesh A; Puranik, Vedavati G; Argade, Narshinha P

    2010-04-16

    Starting from CBz-protected glutamic anhydride and Boc-protected o-aminobenzyl amine, the first total synthesis of proposed structure of auranthine has been reported. An intramolecular aza-Wittig reaction involving a lactam carbonyl group that delivered the diazepine core unit was the key step in the synthesis.

  13. First total synthesis of Boehmenan

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 126; Issue 3 ... The first total synthesis of dilignan Boehmenan has been achieved. A biomimetic oxidative coupling of the ferulic acid methyl ester in the presence of silver oxide is the crucial step in the synthesis sequence, generating the dihydrobenzofuran skeleton.

  14. Stereoselective total synthesis of sphingolipids

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 128; Issue 11. Stereoselective total synthesis of sphingolipids. PARAMESH JANGILI PERLA ... Keywords. 1,2-Diacetyl D-erythro-sphinganine; 1,2-diacetyl L-threo-sphinganine; D-erythro-sphinganine triacetate; sphingolipids; total synthesis; Garner aldehyde.

  15. Chemical Synthesis of Antimicrobial Peptides.

    Science.gov (United States)

    Münzker, Lena; Oddo, Alberto; Hansen, Paul R

    2017-01-01

    Solid-phase peptide synthesis (SPPS) is the method of choice for chemical synthesis of peptides. In this nonspecialist review, we describe commonly used resins, linkers, protecting groups, and coupling reagents in 9-fluorenylmethyloxycarbonyl (Fmoc) SPPS. Finally, a detailed protocol for manual Fmoc SPPS is presented.

  16. Methyltrioctylammonium chloride catalysed sonochemical synthesis ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 125; Issue 5. Methyltrioctylammonium chloride catalysed sonochemical synthesis of acridine diones ... The greener, clean and efficient protocol for the synthesis of acridine diones derivatives has been achieved by reacting aromatic aldehyde, dimedone and amines ...

  17. Lactobacillusassisted synthesis of titanium nanoparticles

    Directory of Open Access Journals (Sweden)

    Jha Anal

    2007-01-01

    Full Text Available AbstractAn eco-friendlylactobacillussp. (microbe assisted synthesis of titanium nanoparticles is reported. The synthesis is performed at room temperature. X-ray and transmission electron microscopy analyses are performed to ascertain the formation of Ti nanoparticles. Individual nanoparticles as well as a number of aggregates almost spherical in shape having a size of 40–60 nm are found.

  18. Microemulsion Synthesis of Nanoparticles

    Directory of Open Access Journals (Sweden)

    Gotić, M.

    2013-11-01

    Full Text Available Nanoparticles and nanomaterials have wide applications in electronics, physics, material design, being also utilized as sensors, catalysts, and more and more in biomedicine. Microemulsions are an exceptionally suitable medium for the synthesis of nanoparticles due to their thermodynamical stability, great solubility of both polar and nonpolar components, as well as their ability to control the size, dispersity and shape of the particles. This review presents microemulsion techniques for the synthesis of inorganic nanoparticles. It takes place in water-in-oil microemulsions by mixing one microemulsion with a cationic precursor, and the other with a precipitating or reducing agent, or by direct addition of reducing agents or gas (O2, NH3 ili CO2 into microemul sion (Fig. 1. Metal nanoparticles are used as catalysts, sensors, ferrofluids etc. They are produced by reducing the metal cation with a suitable reducing agent. In a similar way, one can prepare nanoparticles of alloys from the metal salts, provided that the metals are mutually soluble. The microemulsion technique is also suitable for depositing nanoparticles onto various surfaces. Highly active catalysts made from nanoparticles of Pt, Pd, Rh and other noble metals may be obtained in this way. Metal oxides and hydroxides may be prepared by hydrolysis or precipitation in the water core of microemulsion. Precipitation can be initiated by adding the base or precipitating agent into the microemulsion with water solution of metal ions. Similarly, nanoparticles may be prepared of sulphides, halogenides, cyanides, carbonates, sulphates and other insoluble metal salts. To prevent oxidation of nanoparticles, especially Fe, the particles are coated with inert metals, oxides, various polymers etc. Coating may provide additional functionality; e.g. coating with gold allows subsequent functionalization with organic compounds containing sulphur, due to the strong Au–S bond. Polymer coatings decrease

  19. Total Synthesis of Hyperforin.

    Science.gov (United States)

    Ting, Chi P; Maimone, Thomas J

    2015-08-26

    A 10-step total synthesis of the polycyclic polyprenylated acylphloroglucinol (PPAP) natural product hyperforin from 2-methylcyclopent-2-en-1-one is reported. This route was enabled by a diketene annulation reaction and an oxidative ring expansion strategy designed to complement the presumed biosynthesis of this complex meroterpene. The described work enables the preparation of a highly substituted bicyclo[3.3.1]nonane-1,3,5-trione motif in only six steps and thus serves as a platform for the construction of easily synthesized, highly diverse PPAPs modifiable at every position.

  20. Dibutylphosphoric acid synthesis

    International Nuclear Information System (INIS)

    Elias, H.; Boumaout, R.; Kellou, N.; Amedjkouh, A.; Hamidi, A.

    1995-09-01

    This work consists on the synthesis of dibutylphosphoric acis (DBP) by reaction of butanol with phosphorus pentoxid and on its separation by liquid-liquid extraction. It also deals with the characterization of DBP by some physicochemical analysis methods such as : chromatography, pH-metry and infrared and ultraviolet spectrophotometries. this study showed essentialy, that DBP can be formed in an appreciable amount (55%) when the reaction is realised with butanol/pentoxid molar ratio upper than 3 at temperature of 95 C

  1. Catalytic Oligopeptide Synthesis.

    Science.gov (United States)

    Liu, Zijian; Noda, Hidetoshi; Shibasaki, Masakatsu; Kumagai, Naoya

    2018-02-02

    Waste-free catalytic assembly of α-amino acids is fueled by a multiboron catalyst that features a characteristic B 3 NO 2 heterocycle, providing a versatile catalytic protocol wherein functionalized natural α-amino acid units are accommodated and commonly used protecting groups are tolerated. The facile dehydrative conditions eliminate the use of engineered peptide coupling reagents, exemplifying a greener catalytic alternative for peptide coupling. The catalysis is sufficiently robust to enable pentapeptide synthesis, constructing all four amide bond linkages in a catalytic fashion.

  2. Learning via Query Synthesis

    KAUST Repository

    Alabdulmohsin, Ibrahim Mansour

    2017-05-07

    Active learning is a subfield of machine learning that has been successfully used in many applications. One of the main branches of active learning is query synthe- sis, where the learning agent constructs artificial queries from scratch in order to reveal sensitive information about the underlying decision boundary. It has found applications in areas, such as adversarial reverse engineering, automated science, and computational chemistry. Nevertheless, the existing literature on membership query synthesis has, generally, focused on finite concept classes or toy problems, with a limited extension to real-world applications. In this thesis, I develop two spectral algorithms for learning halfspaces via query synthesis. The first algorithm is a maximum-determinant convex optimization method while the second algorithm is a Markovian method that relies on Khachiyan’s classical update formulas for solving linear programs. The general theme of these methods is to construct an ellipsoidal approximation of the version space and to synthesize queries, afterward, via spectral decomposition. Moreover, I also describe how these algorithms can be extended to other settings as well, such as pool-based active learning. Having demonstrated that halfspaces can be learned quite efficiently via query synthesis, the second part of this thesis proposes strategies for mitigating the risk of reverse engineering in adversarial environments. One approach that can be used to render query synthesis algorithms ineffective is to implement a randomized response. In this thesis, I propose a semidefinite program (SDP) for learning a distribution of classifiers, subject to the constraint that any individual classifier picked at random from this distributions provides reliable predictions with a high probability. This algorithm is, then, justified both theoretically and empirically. A second approach is to use a non-parametric classification method, such as similarity-based classification. In this

  3. Synthesis of deuterated clenbuterol

    Energy Technology Data Exchange (ETDEWEB)

    Joergensen, Ole [Risoe National Lab., Roskilde (Denmark). Solid State Physics Dept.; Egsgaard, Helge; Larsen, Elfinn [Risoe National Lab., Roskilde (Denmark). Science and Technology Dept.

    1996-11-01

    The synthesis of D{sub 9}-clenbuterol (I) and D{sub 3}-clenbuterol (II) is described. D{sub 9}-clenbuterol (I) was prepared from 4-amino-{alpha}-bromo-3, 5-dichloroacetophenone by reaction with D{sub 9}-tert-butylamine followed by reduction of the keto group with NaBH{sub 4}. D{sub 3}-clenbuterol (II) was prepared from 4-amino-{alpha}-tert-butylamino-3, 5-dichloroacetophenone by an exchange reaction of the {alpha}-hydrogens with deuterium followed by reduction of the keto group with NaBD{sub 4}. The eventual products were characterized by mass spectrometry and NMR. (author).

  4. Synthesis in land change science

    DEFF Research Database (Denmark)

    Magliocca, Nicholas R.; Rudel, Thomas K.; Verburg, Peter H.

    2015-01-01

    of these changes, land change science (LCS) draws on a wide array synthetic and meta-study techniques to generate global and regional knowledge from local case studies of land change. Here, we review the characteristics and applications of synthesis methods in LCS and assess the current state of synthetic research...... based on a meta-analysis of synthesis studies from 1995 to 2012. Publication of synthesis research is accelerating, with a clear trend toward increasingly sophisticated and quantitative methods, including meta-analysis. Detailed trends in synthesis objectives, methods, and land change phenomena......, synthesis methods based on local case studies will remain essential for generating systematic global and regional understanding of local land change for the foreseeable future, and multiple opportunities exist to accelerate and enhance the reliability of synthetic LCS research in the future. Demand...

  5. Sonochemical synthesis of versatile hydrophilic magnetite nanoparticles.

    Science.gov (United States)

    Marchegiani, G; Imperatori, P; Mari, A; Pilloni, L; Chiolerio, A; Allia, P; Tiberto, P; Suber, L

    2012-07-01

    Hydrophilic magnetite nanoparticles in the size range 30-10nm are easily and rapidly prepared under ultrasonic irradiation of Fe(OH)(2) in di- and tri-ethylene glycol/water solution with volume ratio varying between 7:3 and 3:7. Structural (XRD) and morphological (SEM) characterization reveal good crystalline and homogeneous particles whereas, when solvothermally prepared, the particles are inhomogeneous and aggregated. The sonochemically prepared particles are versatile, i.e. well suited to covalently bind molecules because of the free glycol hydroxylic groups on their surface or exchange the diethylene or triethylene glycol ligand. They can be easily transferred in hydrophobic solvents too. Room-temperature magnetic hysteresis properties measured by means of Vibrating Sample Magnetometer (VSM) display a nearly superparamagnetic character. The sonochemical preparation is easily scalable to meet industrial demand. Copyright © 2011 Elsevier B.V. All rights reserved.

  6. Reevaluating synthesis by biology.

    Science.gov (United States)

    Yadav, Vikramaditya G; Stephanopoulos, Gregory

    2010-06-01

    The two cornerstones of synthetic biology are the introduction of the new technology of chemical DNA synthesis and its subsequent emphasis on the use of standardized biological parts in the construction of genetic systems aimed at eliciting of desired cellular behavior. A number of high-impact applications have been proposed for this technology, notable among them being the biological synthesis of valuable compounds for chemical or pharmaceutical use. To this end, synthetic biologists propose assembling metabolic pathways in toto by combining genes isolated from a variety of sources. While pathway construction is similar to approaches established long ago by Metabolic Engineering, the two methods deviate significantly when it comes to pathway optimization. Synthetic biologists opt for gene-combinatorial methods whereby large numbers of pathways, comprising several combinations of genes from different sources, and their mutants, are evaluated in search for an optimal pathway configuration. Metabolic engineering, on the contrary, aims to optimize pathways by tuning the activity of the intermediate reaction steps. Both, rational methods based on kinetics and regulation, as well as combinatorial methods, typically in this order, are used to this end. We argue that a systematic approach consisting of fine-tuning the properties of individual pathway components, prominently enzymes, is a superior strategy to searches spanning large genetic spaces in engineering optimal microbes for the production of chemical and pharmaceutical products. Copyright 2010 Elsevier Ltd. All rights reserved.

  7. Synthesis of Lysophospholipids

    Directory of Open Access Journals (Sweden)

    Paola D’Arrigo

    2010-03-01

    Full Text Available New synthetic methods for the preparation of biologically active phospholipids and lysophospholipids (LPLs are very important in solving problems of membrane–chemistry and biochemistry. Traditionally considered just as second-messenger molecules regulating intracellular signalling pathways, LPLs have recently shown to be involved in many physiological and pathological processes such as inflammation, reproduction, angiogenesis, tumorogenesis, atherosclerosis and nervous system regulation. Elucidation of the mechanistic details involved in the enzymological, cell-biological and membrane-biophysical roles of LPLs relies obviously on the availability of structurally diverse compounds. A variety of chemical and enzymatic routes have been reported in the literature for the synthesis of LPLs: the enzymatic transformation of natural glycerophospholipids (GPLs using regiospecific enzymes such as phospholipases A1 (PLA1, A2 (PLA2 phospholipase D (PLD and different lipases, the coupling of enzymatic processes with chemical transformations, the complete chemical synthesis of LPLs starting from glycerol or derivatives. In this review, chemo-enzymatic procedures leading to 1- and 2-LPLs will be described.

  8. Oxygenates vs. synthesis gas

    Energy Technology Data Exchange (ETDEWEB)

    Kamil Klier; Richard G. Herman; Alessandra Beretta; Maria A. Burcham; Qun Sun; Yeping Cai; Biswanath Roy

    1999-04-01

    Methanol synthesis from H{sub 2}/CO has been carried out at 7.6 MPa over zirconia-supported copper catalysts. Catalysts with nominal compositions of 10/90 mol% and 30/70 mol% Cu/ZrO{sub 2} were used in this study. Additionally, a 3 mol% cesium-doped 10/90 catalyst was prepared to study the effect of doping with heavy alkali, and this promoter greatly increased the methanol productivity. The effects of CO{sub 2} addition, water injection, reaction temperature, and H{sub 2}/C0 ratio have been investigated. Both CO{sub 2} addition to the synthesis gas and cesium doping of the catalyst promoted methanol synthesis, while inhibiting the synthesis of dimethyl ether. Injection of water, however, was found to slightly suppress methanol and dimethyl ether formation while being converted to CO{sub 2} via the water gas shift reaction over these catalysts. There was no clear correlation between copper surface area and catalyst activity. Surface analysis of the tested samples revealed that copper tended to migrate and enrich the catalyst surface. The concept of employing a double-bed reactor with a pronounced temperature gradient to enhance higher alcohol synthesis was explored, and it was found that utilization of a Cs-promoted Cu/ZnO/Cr{sub 2}O{sub 3} catalyst as a first lower temperature bed and a Cs-promoted ZnO/Cr{sub 2}O{sub 3} catalyst as a second high-temperature bed significantly promoted the productivity of 2-methyl-1-propanol (isobutanol) from H{sub 2}/CO synthesis gas mixtures. While the conversion of CO to C{sub 2+} oxygenates over the double-bed configuration was comparable to that observed over the single Cu-based catalyst, major changes in the product distribution occurred by the coupling to the zinc chromite catalyst; that is, the productivity of the C{sub 1}-C{sub 3} alcohols decreased dramatically, and 2-methyl branched alcohols were selectively formed. The desirable methanol/2-methyl oxygenate molar ratios close to 1 were obtained in the present double

  9. Synthesis, structure of [H3 dien].(MF6).H2O (M=Cr, Fe) and 57Fe Moessbauer study of [H3 dien].(FeF6).H2O

    International Nuclear Information System (INIS)

    Ben Ali, Amor; Trang Dang, Minh; Greneche, Jean-Marc; Hemon-Ribaud, Annie; Leblanc, Marc; Maisonneuve, Vincent

    2007-01-01

    Single crystals of [H 3 dien].(FeF 6 ).H 2 O (I) and [H 3 dien].(CrF 6 ).H 2 O (II) are obtained by solvothermal synthesis under microwave heating. I is orthorhombic (Pna2 1 ) with a=11.530(2) A, b=6.6446(8) A, c=13.787(3) A, V=1056.3(2) A 3 and Z=4. II is monoclinic (P2 1 /c) with a=13.706(1) A, b=6.7606(6) A, c=11.3181(9) A, β=99.38(1) o , V=1034.7(1) A 3 and Z=4. The structure determinations, performed from single crystal X-ray diffraction data, lead to the R 1 /wR 2 reliability factors 0.028/0.066 for I and 0.035/0.102 for II. The structures of I and II are built up from isolated FeF 6 or CrF 6 octahedra, water molecules and triprotonated amines. In both structures, each octahedron is connected by hydrogen bonds to six organic cations and two water molecules. The iron-based compound is also characterized by 57 Fe Moessbauer spectrometry: the hyperfine structure confirms the presence of Fe 3+ in octahedral coordination and reveals the existence of paramagnetic spin fluctuations. - Graphical abstract: Moessbauer spectra of [H 3 dien].(FeF 6 ).H 2 O

  10. Sustainable, Rapid Synthesis of Bright-Luminescent CuInS2-ZnS Alloyed Nanocrystals: Multistage Nano-xenotoxicity Assessment and Intravital Fluorescence Bioimaging in Zebrafish-Embryos.

    Science.gov (United States)

    Chetty, S Shashank; Praneetha, S; Basu, Sandeep; Sachidanandan, Chetana; Murugan, A Vadivel

    2016-05-18

    Near-infrared (NIR) luminescent CuInS2-ZnS alloyed nanocrystals (CIZS-NCs) for highly fluorescence bioimaging have received considerable interest in recent years. Owing, they became a desirable alternative to heavy-metal based-NCs and organic dyes with unique optical properties and low-toxicity for bioimaging and optoelectronic applications. In the present study, bright and robust CIZS-NCs have been synthesized within 5 min, as-high-as 230 °C without requiring any inert-gas atmosphere via microwave-solvothermal (MW-ST) method. Subsequently, the in vitro and in vivo nano-xenotoxicity and cellular uptake of the MUA-functionalized CIZS-NCs were investigated in L929, Vero, MCF7 cell lines and zebrafish-embryos. We observed minimal toxicity and acute teratogenic consequences upto 62.5 μg/ml of the CIZS-NCs in zebrafish-embryos. We also observed spontaneous uptake of the MUA-functionalized CIZS-NCs by 3 dpf older zebrafish-embryos that are evident through bright red fluorescence-emission at a low concentration of 7.8 μg/mL. Hence, we propose that the rapid, low-cost, large-scale "sustainable" MW-ST synthesis of CIZS-NCs, is an ideal bio-nanoprobe with good temporal and spatial resolution for rapid labeling, long-term in vivo tracking and intravital-fluorescence-bioimaging (IVBI).

  11. Sustainable, Rapid Synthesis of Bright-Luminescent CuInS2-ZnS Alloyed Nanocrystals: Multistage Nano-xenotoxicity Assessment and Intravital Fluorescence Bioimaging in Zebrafish-Embryos

    Science.gov (United States)

    Chetty, S. Shashank; Praneetha, S.; Basu, Sandeep; Sachidanandan, Chetana; Murugan, A. Vadivel

    2016-05-01

    Near-infrared (NIR) luminescent CuInS2-ZnS alloyed nanocrystals (CIZS-NCs) for highly fluorescence bioimaging have received considerable interest in recent years. Owing, they became a desirable alternative to heavy-metal based-NCs and organic dyes with unique optical properties and low-toxicity for bioimaging and optoelectronic applications. In the present study, bright and robust CIZS-NCs have been synthesized within 5 min, as-high-as 230 °C without requiring any inert-gas atmosphere via microwave-solvothermal (MW-ST) method. Subsequently, the in vitro and in vivo nano-xenotoxicity and cellular uptake of the MUA-functionalized CIZS-NCs were investigated in L929, Vero, MCF7 cell lines and zebrafish-embryos. We observed minimal toxicity and acute teratogenic consequences upto 62.5 μg/ml of the CIZS-NCs in zebrafish-embryos. We also observed spontaneous uptake of the MUA-functionalized CIZS-NCs by 3 dpf older zebrafish-embryos that are evident through bright red fluorescence-emission at a low concentration of 7.8 μg/mL. Hence, we propose that the rapid, low-cost, large-scale “sustainable” MW-ST synthesis of CIZS-NCs, is an ideal bio-nanoprobe with good temporal and spatial resolution for rapid labeling, long-term in vivo tracking and intravital-fluorescence-bioimaging (IVBI).

  12. Synthesis of 2-phosphaadamantane derivatives

    International Nuclear Information System (INIS)

    Zemlyanoi, V.N.; Aleksandrov, A.M.; Kukhar', V.P.

    1986-01-01

    The authors describe the synthesis and properties of 2-phosphadamantane derivatives. For the synthesis of 2-phosphaadamantane derivatives they decided to use the methodology of the synthesis of 2-thiaadamantane. The IR spectra were determined on CHCl 3 solutions with a Specord 711R spectrometer, the PMR spectra were determined on Tesla BS-467 (60 MHz) and Bruker WP-200 (200 MHz) spectrometers, external standard hexamethyldisiloxane, the 31 P NMR spectra were determined on Tesla BS-487 C (30 MHz) and Bruker WP-200 (81 MHz) spectrometers, external standard 85% phosphoric acid, and the mass spectra were determined on an MS-1302 spectrometer

  13. Synthesis of C-vinylpyrroles

    International Nuclear Information System (INIS)

    Sobenina, Lyubov N; Demenev, Andrei P; Mikhaleva, Albina I; Trofimov, Boris A

    2002-01-01

    The latest advances in the synthesis of C-vinylpyrroles are generalised and systematised. Methods for the synthesis based on reactions of acylpyrroles and dicarbonyl compounds or their synthetic equivalents are still of most importance. New promising methods for the synthesis of C-vinylpyrroles are considered, among them the reactions of alkenyl ketone oximes with acetylene in the KOH-DMSO system and base-catalysed condensation of pyrrolecarbodithioates, which have recently become available, with CH-acids. The bibliography includes 195 references.

  14. Hypericin: chemical synthesis and biosynthesis.

    Science.gov (United States)

    Huang, Lin-Fang; Wang, Zeng-Hui; Chen, Shi-Lin

    2014-02-01

    Hypericin is one of the most important phenanthoperylene quinones extracted mainly from plants of the genus Hypericum belonging to the sections Euhypericum and Campylosporus of Keller's classification. Widespread attention to the antiviral and anti-tumor properties of hypericin has spurred investigations of the chemical synthesis and biosynthesis of this unique compound. However, the synthetic strategies are challenging for organic and biological chemists. In this review, specific significant advances in total synthesis, semi-synthesis, and biosynthesis in the past decades are summarized. Copyright © 2014 China Pharmaceutical University. Published by Elsevier B.V. All rights reserved.

  15. Co9S8 nanotubes: facile synthesis and application in the catalytic ...

    Indian Academy of Sciences (India)

    step solvothermal method with- out the assistance of any template or surfactant, using cobalt sulphate (CoSO4·7H2O), urea and sodium sulphide. (Na2S·9H2O) as starting reactants, and deionized water and glycol as the reactive medium.

  16. Co9S8 nanotubes: facile synthesis and application in the catalytic ...

    Indian Academy of Sciences (India)

    Co 9 S 8 nanotubes have been successfully synthesized via a facile two-step solvothermal method without the assistance of any template or surfactant, using cobalt sulphate (CoSO 4 ·7H 2 O), urea and sodium sulphide (Na 2 S·9H 2 O) as starting reactants, and deionized water and glycol as the reactive medium.

  17. Synthesis and characterization of ester and amide derivatives of titanium(IV) carboxymethylphosphonate

    Czech Academy of Sciences Publication Activity Database

    Melánová, Klára; Beneš, L.; Trchová, Miroslava; Svoboda, Jan; Zima, Vítězslav

    2013-01-01

    Roč. 202, June (2013), s. 93-98 ISSN 0022-4596 R&D Projects: GA ČR GA203/08/0208 Institutional support: RVO:61389013 Keywords : layered titanium organohphosphonates * solvothermal treatment IR spectroscopy * grafting Subject RIV: CA - Inorganic Chemistry Impact factor: 2.200, year: 2013

  18. Synthesis of radium silicate

    International Nuclear Information System (INIS)

    Garibov, A.A; Agayev, T.N; Mansimov, Z.A

    2010-01-01

    Full text :One of the possible ways of implementation of the processes of molecular hydrogen radiologic of the elements in the differential heat of water as a catalyst for the collapse of the creation of a special nuclear reactors. A chemical process in radiation-4-oxide-silicon compounds, which is one of the radium, is of great importance. Research in the silicon-oxide-radiumun different activity-4 has been synthesized. As initial substances for the synthesis of tetra etiolate silicate and radium chloride solutions were used. At the same time to remove reaction products from the reaction intermediate in acetate acid was used. The intermediate product was reacted with ethyl alcohol ethyl acetate ether acetate acid that forms from the reaction of the temperature effect is broken. As a result, 4-oxide was initially pure silicon.

  19. The synthesis of clopidogrel

    Science.gov (United States)

    Huang, Yuanjun; Zhu, Qingxin

    2017-12-01

    Cardiac and cerebrovascular disease is a common disease. It is well recognized that antiplatelet agent is effective in the prevention and treatment of thrombosis. Clopidogrel is one of thieno pyridine derivatives, which can inhibit ADP-induced platelet aggregation. The preparation methods of Clopidogrel were reviewed and Clopidogrel was finally synthesized from 2-chlorobenzyl cyanide via bromination, condensation, hydrolyze, esterification, resolution, Finally with the sulfate, re-crystallization product of the target compound clopidogrel. The overall yield is 16%. Synthesis of the intermediate product and finally the structure of the product through ESI and 1H-NMR corroboration. The improved synthetic procedure has the advantage of low cost and is suitable for industrial production.

  20. Synthesis of cyclododeciptycene quinones.

    Science.gov (United States)

    Lou, Kaiyan; Prior, Allan M; Wiredu, Bernard; Desper, John; Hua, Duy H

    2010-12-15

    Cycloiptycenes are elusive and synthetically challenging molecules. We report the first synthesis of two substituted cyclododeciptycene tetraquinones via a sequence of intermolecular and intramolecular Diels-Alder reactions from cis,cis-heptiptycene tetraquinone 2 and substituted 7,16-dihydro-7,16-(o-benzeno)heptacenes 3. Heptiptycene tetraquinone 2 was made from triptycene bisquinone 4 and 1,4-dimethoxyanthracene in three steps, and 6,8,15,17-tetramethoxy-7,16-dihydro-7,16-(o-benzeno)heptacene (3a) was synthesized from triptycene bisquinone 4 and 1,4-dihydro-2,3-benzoxathiin-3-oxide in four steps. The structure of a cyclododeciptycene, 1a, was determined by a single-crystal X-ray analysis. The synthetic sequence is general and should allow the incorporation of various alkoxy and acetoxy substituents appended to the cycloiptycene framework.