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Sample records for template-free solvothermal synthesis

  1. Green, one-step and template-free synthesis of silver spongelike networks via a solvothermal method

    International Nuclear Information System (INIS)

    Yi, Zao; Xu, Xibin; Zhang, Kuibao; Tan, Xiulan; Li, Xibo; Luo, Jiangshan; Ye, Xin; Wu, Weidong; Wu, Jie; Yi, Yougen; Tang, Yongjian

    2013-01-01

    Silver spongelike networks were synthesized from an alkaline pH solution of silver nitrate and glucose under solvothermal conditions. The products were characterized by X-ray powder diffraction, UV–visible spectroscopy, transmission electron microscopy, scanning electron microscopy and selected area electron diffraction. These Ag nanoparticles (NPs) appear to undergo sequentially linear aggregation and welding initially, and then, they randomly cross link into self-supporting, three-dimensional (3D) networks with time. The carboxylate groups, generated by glucose oxidation, interacted with the Ag nanostructures, resulting in formation of silver spongelike networks having very uniform wire diameters distributions (about 20 nm in diameter). A new plasmon band was observed in the longer-wavelengths region (565–912 nm) of the conventional transverse plasmon resonance band at 430 nm. In principle, this one-step, template-free approach can also be extended to large-scale 3D organizations of other transition/noble metal NPs. - Graphical abstract: Silver spongelike networks were synthesized from an alkaline pH solution of silver nitrate and glucose under solvothermal conditions, with any other reducing or capping agent. These Ag nanoparticles appear to undergo sequentially linear aggregation and welding initially, and then, they randomly cross link into self-supporting, three-dimensional spongelike networks with time. Highlights: ► Silver spongelike networks were synthesized using eco-friendly glucose. ► This synthesis was a seedless process, and did not need any other surfactant or capping agent. ► The process was initial reduction – nucleation – adsorption – growth – branching

  2. A template-free solvothermal synthesis and photoluminescence properties of multicolor Gd2O2S:xTb3+, yEu3+ hollow spheres

    Science.gov (United States)

    Sang, Xiaotong; Xu, Guangxi; Lian, Jingbao; Wu, Nianchu; Zhang, Xue; He, Jiao

    2018-06-01

    The multicolor Gd2O2S:xTb3+, yEu3+ hollow spheres were successfully synthesized via a template-free solvothermal route without the use of surfactant from commercially available Ln (NO3)3·6H2O (Ln = Gd, Tb and Eu), absolute ethanol, ethanediamine and sublimed sulfur as the starting materials. The phase, structure, particle morphology and photoluminescence (PL) properties of the as-obtained products were investigated by X-ray diffraction (XRD), fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM) and photoluminescence spectra. The influence of synthetic time on phase, structure and morphology was systematically investigated and discussed. The possible formation mechanism depending on synthetic time t for the Gd2O2S phase has been presented. These results demonstrate that the Gd2O2S hollow spheres could be obtained under optimal condition, namely solvothermal temperature T = 220 °C and synthetic time t = 16 h. The as-obtained Gd2O2S sample possesses hollow sphere structure, which has a typical size of about 2.5 μm in diameter and about 0.5 μm in shell thickness. PL spectroscopy reveals that the strongest emission peak for the Gd2O2S:xTb3+ and the Gd2O2S:yEu3+ samples is located at 545 nm and 628 nm, corresponding to 5D4→7F5 transitions of Tb3+ ions and 5D0→7F2 transitions of Eu3+ ions, respectively. The quenching concentration of Tb3+ ions and Eu3+ ions is 7%. In the case of Tb3+ and Eu3+ co-doped samples, when the concentration of Tb3+ or Eu3+ ions is 7%, the optimum concentration of Eu3+ or Tb3+ ions is determined to be 1%. Under 254 nm ultraviolet (UV) light excitation, the Gd2O2S:7%Tb3+, the Gd2O2S:7%Tb3+,1%Eu3+ and the Gd2O2S:7%Eu3+ samples give green, yellow and red light emissions, respectively. And the corresponding CIE coordinates vary from (0.3513, 0.5615), (0.4120, 0.4588) to (0.5868, 0.3023), which is also well consistent with their luminous photographs.

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

    Indian Academy of Sciences (India)

    Administrator

    2009), solar cells (Yuan et al 2011), transparent elec- trodes (Kim et al ... increasing the peak width, intensity and shifting the 2θ peak position. ... Facile template-free hydrothermal synthesis and microstrain measurement of ZnO nanorods. 399.

  4. organic template free synthesis of zsm11 from kaolinite clay

    African Journals Online (AJOL)

    user

    diffusion assistance and tortuosity, as depicted in Figure. 1. Hongyuan and others [6] .... characterized by nearly equal peak height of Al and Si, another means to ..... method for nanocrystalline zeolite synthesis. Chemical communication.

  5. Uniform hollow Fe3O4 spheres prepared by template-free solvothermal method as anode material for lithium-ion batteries

    International Nuclear Information System (INIS)

    Zhang Jingjing; Yao Yu; Huang Tao; Yu Aishui

    2012-01-01

    Graphical abstract: Unique hollow Fe 3 O 4 spheres assembled by Fe 3 O 4 nanoparticles prepared by a simple template-free solvothermal reaction are tested as anode material for lithium-ion batteries. The results show that the material delivers reversible specific capacities of 870 mA h g −1 even after 50 cycles at 100 mA g −1 and 836 mA h g −1 at 500 mA g −1 . The excellent electrochemical performance can be attributed to their hollow nanostructure and excellent structural stability. Highlights: ► Uniform hollow Fe 3 O 4 spheres were prepared by a template-free solvothermal method. ► The hollow Fe 3 O 4 spheres have the capacity of 870 mA h g −1 at 50th cycle. ► The specific capacity can be well maintained at a large current density. ► The hollow Fe 3 O 4 spheres exhibit enhanced rate capability. ► Electrochemical performance of hollow Fe 3 O 4 spheres is better than Fe 3 O 4 powders. - Abstract: Unique hollow Fe 3 O 4 spheres are prepared by a simple template-free solvothermal reaction. In the reaction, ethylene glycol (EG) and polyvinylpyrrolidone (PVP) serve as the reducing agent and surface stabilizer, respectively. NH 4 Ac plays the role of the structure-directing agent, which combines with the Ostwald ripening process, resulting in the favored formation of hollow structures. The morphologies and structures are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The hollow Fe 3 O 4 spheres exhibit excellent cycling and rate performance as anode material for lithium-ion batteries, delivering reversible specific capacities of 870 mA h g −1 even after 50 cycles at 100 mA g −1 and 836 mA h g −1 at 500 mA g −1 . The excellent electrochemical performance can be attributed to their hollow nanostructure and excellent structural stability.

  6. 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.

  7. Mesoporous Prussian blue analogues: template-free synthesis and sodium-ion battery applications.

    Science.gov (United States)

    Yue, Yanfeng; Binder, Andrew J; Guo, Bingkun; Zhang, Zhiyong; Qiao, Zhen-An; Tian, Chengcheng; Dai, Sheng

    2014-03-17

    The synthesis of mesoporous Prussian blue analogues through a template-free methodology and the application of these mesoporous materials as high-performance cathode materials in sodium-ion batteries is presented. Crystalline mesostructures were produced through a synergistically coupled nanocrystal formation and aggregation mechanism. As cathodes for sodium-ion batteries, the Prussian blue analogues all show a reversible capacity of 65 mA h g-1 at low current rate and show excellent cycle stability. The reported method stands as an environmentally friendly and low-cost alternative to hard or soft templating for the fabrication of mesoporous materials.

  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. Template-Free Synthesis of Nanoporous Nickel and Alloys as Binder- Free Current Collectors of Li Ion Batteries

    NARCIS (Netherlands)

    Lu, Liqiang; Andela, Paul; De Hosson, J.T.M.; Pei, Yutao T.

    2018-01-01

    This paper reports a versatile template-free method based on the hydrogen reduction of metallic salts for the synthesis of nanoporous Ni and alloys. The approach involves thermal decomposition and reduction of metallic precursors followed with metal cluster nucleation and ligament growth.

  10. A template-free solvent-mediated synthesis of high surface area boron nitride nanosheets for aerobic oxidative desulfurization.

    Science.gov (United States)

    Wu, Peiwen; Zhu, Wenshuai; Chao, Yanhong; Zhang, Jinshui; Zhang, Pengfei; Zhu, Huiyuan; Li, Changfeng; Chen, Zhigang; Li, Huaming; Dai, Sheng

    2016-01-04

    Hexagonal boron nitride nanosheets (h-BNNs) with rather high specific surface area (SSA) are important two-dimensional layer-structured materials. Here, a solvent-mediated synthesis of h-BNNs revealed a template-free lattice plane control strategy that induced high SSA nanoporous structured h-BNNs with outstanding aerobic oxidative desulfurization performance.

  11. Template-free synthesis of mesoporous nanoring-like Zn-Co mixed oxides with high lithium storage performance

    Science.gov (United States)

    Lu, Lun; Gao, Yan-Li; Yang, Zhi-Zheng; Wang, Cheng; Wang, Jin-Guo; Wang, Hui-Yuan; Jiang, Qi-Chuan

    2018-04-01

    Mesoporous nanoring-like Zn-Co mixed oxides are synthesized via a simple template-free solvothermal method with a subsequent annealing process. The ring-like nanostructures with hollow interiors are formed under the complexing effects of potassium sodium tartrate. Numerous mesopores are generated after the precursor is annealed at 500 °C. When applied as anode materials, the mesoporous nanoring-like Zn-Co mixed oxides can deliver a high discharge capacity of 1102 mAh g-1 after 200 cycles at 500 mA g-1. Even when the current density is increased to 2 A g-1, the mixed oxides can still retain a reversible capacity of 761 mAh g-1. Such high cycling stability and rate capability are mainly derived from the unique mesoporous ring-like nanostructures and the synergistic effects between Zn and Co based oxides.

  12. Template-free sonochemical synthesis of flower-like ZnO nanostructures

    Energy Technology Data Exchange (ETDEWEB)

    Yu, Huawa [State Key Laboratory of Solidification Processing, School of Materials Science and Engineering, Northwestern Polytechnical University, Xi' an 710072 (China); School of Science, Xi' an Polytechnic University, Xi' an 710048 (China); Fan, Huiqing, E-mail: hqfan3@163.com [State Key Laboratory of Solidification Processing, School of Materials Science and Engineering, Northwestern Polytechnical University, Xi' an 710072 (China); Wang, Xin [Shaanxi Province Thin Film Technology and Optical Test Open Key Laboratory, School of Photoelectrical Engineering, Xi' an Technological University, Xi' an 710032 (China); Wang, Jing [State Key Laboratory of Solidification Processing, School of Materials Science and Engineering, Northwestern Polytechnical University, Xi' an 710072 (China); Cheng, Pengfei; Zhang, Xiaojun [School of Science, Xi' an Polytechnic University, Xi' an 710048 (China)

    2014-10-03

    Flower-like ZnO nanostructures have been successfully synthesized via a facile and template-free sonochemical method, using zinc acetate and potassium hydroxide as reactants only. The as-synthesized flower-like ZnO nanostructures were composed of nanorods with the width of ∼300–400 nm and the length of ∼2–3 μm. The structures, morphologies and optical properties of the as-prepared products were characterized by X-ray diffraction, scanning electron microscope, transmission electron microscopy, UV-Vis spectrophotometry and Raman-scattering spectroscopy. A plausible formation mechanism of flower-like ZnO nanostructures was studied by SEM which monitors an intermediate morphology transformation of the product at the different ultrasonic time (t=80,90,95,105, and 120 min). - Highlights: • A facile and template-free sonochemical method to fabricate flower-like ZnO nanostructures was proposed. • The flower-like ZnO nanostructures follow the ingrowth of ZnO from the matrix of Zn(OH){sub 2} crystals. • The flower-like ZnO nanostructures are also expected to explore their application in the field of nano-electronic devices.

  13. Template-free sonochemical synthesis of flower-like ZnO nanostructures

    International Nuclear Information System (INIS)

    Yu, Huawa; Fan, Huiqing; Wang, Xin; Wang, Jing; Cheng, Pengfei; Zhang, Xiaojun

    2014-01-01

    Flower-like ZnO nanostructures have been successfully synthesized via a facile and template-free sonochemical method, using zinc acetate and potassium hydroxide as reactants only. The as-synthesized flower-like ZnO nanostructures were composed of nanorods with the width of ∼300–400 nm and the length of ∼2–3 μm. The structures, morphologies and optical properties of the as-prepared products were characterized by X-ray diffraction, scanning electron microscope, transmission electron microscopy, UV-Vis spectrophotometry and Raman-scattering spectroscopy. A plausible formation mechanism of flower-like ZnO nanostructures was studied by SEM which monitors an intermediate morphology transformation of the product at the different ultrasonic time (t=80,90,95,105, and 120 min). - Highlights: • A facile and template-free sonochemical method to fabricate flower-like ZnO nanostructures was proposed. • The flower-like ZnO nanostructures follow the ingrowth of ZnO from the matrix of Zn(OH) 2 crystals. • The flower-like ZnO nanostructures are also expected to explore their application in the field of nano-electronic devices

  14. Template-free hydrothermal synthesis and high photocatalytic activity of ZnWO4 nanorods

    International Nuclear Information System (INIS)

    Gao, Bin; Fan, Huiqing; Zhang, Xiaojun; Song, Lixun

    2012-01-01

    Highlights: ► ZnWO 4 nanorods with uniform diameter are successfully prepared through a template-free hydrothermal method. ► The crystallinity of the products is influenced by the pH value of initial precursor suspension. ► Photocatalytic activity of the ZnWO 4 nanorods for degradation of methylene blue is evaluated. ► The ZnWO 4 nanorods exhibit good stability of photocatalytic activity. - Abstract: ZnWO 4 nanorods are successfully synthesized by a template-free hydrothermal method, and are characterized in detail by X-ray diffractometer (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED). The results show that the ZnWO 4 nanorods with wolframite structure are well-crystallized single crystallites. The crystallinity of the products is influenced by the pH value of initial precursor suspension. The width and length of the synthesized samples increase with hydrothermal reaction temperature. The photocatalytic efficiency of the ZnWO 4 nanorods for degradation of methylene blue (MB) in aqueous solution under UV light irradiation declines greatly with increasing crystallinity. The ZnWO 4 nanorods prepared at pH of 4 have the best activity in photo-degradation of MB. After six recycles, photocatalytic activity loss of the catalyst is not obvious.

  15. Kinetically-controlled template-free synthesis of hollow silica micro-/nanostructures with unusual morphologies

    International Nuclear Information System (INIS)

    Zhang, An-Qi; Li, Hui-Jun; Qian, Dong-Jin; Chen, Meng

    2014-01-01

    We report a kinetically-controlled template-free room-temperature production of hollow silica materials with various novel morphologies, including tubes, crutches, ribbons, bundles and bells. The obtained products, which grew in a well-controlled manner, were monodispersed in shape and size. The role of ammonia, sodium citrate, polyvinylpyrrolidone, chloroauric acid and NaCl in shape control is discussed in detail. The oriented growth of these micro-/nanostructures directed by reverse micelles followed a solution–solution–solid (SSS) mechanism, similar to the classic vapor–liquid–solid mechanism. The evolution processes of silica rods, tubes, crutches, bundles and bells were recorded using transmission electron microscopy to prove the SSS mechanism. (paper)

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

    Energy Technology Data Exchange (ETDEWEB)

    Martinez-Castro, E. [Instituto de Ciencia de Materiales de Sevilla (CSIC-US), Americo Vespucio 49, Isla de La Cartuja, 41092 Sevilla (Spain); García-Sevillano, J.; Cussó, F. [Dpto. Física de Materiales, C-04, Universidad Autónoma de Madrid, Avda. Francisco Tomás y Valiente, 7, 28049 Madrid (Spain); Ocaña, M., E-mail: mjurado@icmse.csic.es [Instituto de Ciencia de Materiales de Sevilla (CSIC-US), Americo Vespucio 49, Isla de La Cartuja, 41092 Sevilla (Spain)

    2015-01-15

    Highlights: • Hollow lanthanide doped YOF spheres have been synthesised through a template-free procedure. • Strong red emissions are observed for Eu-doped spheres under UV illumination. • Concentration quenching of luminescence takes place in the spheres at very high Eu doping levels. • Bright red emission is observed for Er, Yb codoped spheres, making this matrix advantageous for biomedical imaging. - Abstract: 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 compared with other methods usually employed for the production of hollow spheres since it does not require the use of sacrificial templates. In addition, it is continuous, which is desirable because of practical reasons. The procedure is also suitable for doping the YOF spheres with europium cations resulting in down converting red phosphors when activated with UV light, or for co-doping with both Er{sup 3+} and Yb{sup 3+} giving rise to up-converting phosphors, which emit intense red light under near infrared (NIR) irradiation. Because of their optical properties and hollow architecture, the developed materials may find applications in optoelectronic devices and biotechnology.

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

    Science.gov (United States)

    An extremely simple single-step method is described for the bulk synthesis of nanofibers of the electronic polymer polyaniline in fully reduced state (leucoemarldine form) without using any reducing agents, surfactants, and/or large amounts of insoluble templates. Chemical oxida...

  18. 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.

  19. Silver nanoplates with ground or metastable structures obtained from template-free two-phase aqueous/organic synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Zhelev, Doncho V., E-mail: dontcho.jelev@nih.gov; Zheleva, Tsvetanka S. [Army Research Laboratory, 2800 Adelphi, Maryland 20783 (United States)

    2014-01-28

    Silver has unique electrical, catalytic, and plasmonic characteristics and has been widely sought for fabrication of nanostructures. The properties of silver nanostructures are intimately coupled to the structure of silver crystals. Two crystal structures are known for silver: the stable (ground) state cubic face centered 3C-Ag structure and the metastable hexagonal 4H-Ag structure. Recently, Chackraborty et al. [J. Phys.: Condens. Matter 23, 325401 (2011)] discovered a low density, highly reactive metastable hexagonal 2H-Ag structure accessible during electrodeposition of silver nanowires in porous anodic alumina templates. This 2H-Ag structure has enhanced electrical and catalytic characteristics. In the present work we report template-free synthesis of silver nanoplates with the metastable 2H-Ag crystal structure, which appears together with the ground 3C-Ag and the metastable 4H-Ag structures in a two-phase solution synthesis with citric acid as the capping agent. The capacity of citric acid to stabilize both the stable and the metastable structures is explained by its preferential binding to the close packed facets of Ag crystals, which are the (111) planes for 3C-Ag and the (0001) planes for 4H-Ag and 2H-Ag. Nanoplate morphology and structure are characterized using scanning electron microscopy, X-ray diffraction, and transmission electron microscopy. The synthesized nanoplates have thickness from 15 to 17 nm and edge length from 1 to 10 μm. Transmission electron microscopy selected area electron diffraction is used to uniquely identify and distinguish between nanoplates with 2H-Ag or 4H-Ag or 3C-Ag structures.

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

    International Nuclear Information System (INIS)

    Zhang, Yong-Xing; Jia, Yong

    2015-01-01

    Highlights: • Commercial Fe 2 O 3 and Al 2 O 3 powders were chosen to prepare Fe 2 O 3 /Al 2 O 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 2 O 3 /Al 2 O 3 catalyst was prepared by simply calcining the mixture of commercial Fe 2 O 3 and Al 2 O 3 powders at 1000 °C. The obtained Fe 2 O 3 /Al 2 O 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.

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

    Indian Academy of Sciences (India)

    polymers were synthesized by the solvothermal method. Optical ... compounds, especially to synthesize conjugated pol- ... analyses were performed under nitrogen flow using a .... Coffin R C, Peet J, Rogers J and Bazan G C 2009 Nat. Chem.

  2. 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.

  3. 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.

  4. 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.

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

    Indian Academy of Sciences (India)

    Effect of temperature and time study on solvothermal synthesis of BaTiO3 revealed that a moderate reaction temperature i.e. 185◦C and longer reaction time favour tetragonal phase stabiliza- tion. Dissolution–precipitation appears to be the transformation mechanism for the crystallization of BaTiO3 from particulate TiO2 ...

  6. 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.

  7. Facile solvothermal synthesis of graphene-MnOOH nanocomposites

    International Nuclear Information System (INIS)

    Chen Sheng; Zhu Junwu; Huang Huajie; Zeng Guiyu; Nie Fude; Wang Xin

    2010-01-01

    In this paper, we report a facile solvothermal route capable of aligning MnOOH nanocrystals on graphene. X-ray diffraction (XRD) and transmission electron microscopy (TEM) observations indicate that the exfoliated graphene sheets are decorated randomly by MnOOH nanocrystals, forming well-dispersed graphene-MnOOH nanocomposites. Dissolution-crystallization and oriented attachment are speculated to be the vital mechanisms in the synthetic process. The attachment of additives, such as MnOOH nanoparticles, are found to be beneficial for the exfoliation of GO as well as preventing the restack of graphene sheets. Moreover, cyclic voltammetry (CV) analyses suggest that the electrochemical reversibility is improved by anchoring MnOOH on graphene. Notably, the as-fabricated nanocomposites reveal unusual catalytic performance for the thermal decomposition of ammonium perchlorate (AP) due to the concerted effects of graphene and MnOOH. This template-free method is easy to reproduce, and the process proceeds at a low temperature and can be readily extended to prepare other graphene-based nanocomposites. - Graphical abstract: Manganese oxyhydroxide nanocrystals have been successfully attached onto the graphene sheets via an oriented attachment and dissolution-crystallization process, forming a nanocomposite with unusual catalytic capabilities. Display Omitted

  8. Synthesis of hierarchical porous materials with ZSM-5 structures via template-free sol–gel method

    Directory of Open Access Journals (Sweden)

    Wei Han et al

    2007-01-01

    Full Text Available Interests are focused on preparation of hierarchical porous materials with zeolite structures by using soft or rigid templates in order to solve diffusion and mass transfer limitations resulting from the small pore sizes of zeolites. Here we develop a convenient template-free sol–gel method to synthesize hierarchical porous materials with ZSM-5 structures. This method involves hydrothermal recrystallization of the xerogel converted from uniform ZSM-5 sol by a vacuum drying process. By utilizing this method we can manipulate the size of zeolite nanocrystals as building units of porous structures based on controlling temperature of recrystallization, consequently obtain hierarchical porous materials with different intercrystalline pore sizes and ZSM-5 structures.

  9. 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)

  10. Template-free synthesis of renewable macroporous carbon via yeast cells for high-performance supercapacitor electrode materials.

    Science.gov (United States)

    Sun, Hongmei; He, Wenhui; Zong, Chenghua; Lu, Lehui

    2013-03-01

    The urgent need for sustainable development has forced material scientists to explore novel materials for next-generation energy storage devices through a green and facile strategy. In this context, yeast, which is a large group of single cell fungi widely distributed in nature environments, will be an ideal candidate for developing effective electrode materials with fascinating structures for high-performance supercapacitors. With this in mind, herein, we present the first example of creating three-dimensional (3D) interpenetrating macroporous carbon materials via a template-free method, using the green, renewable, and widespread yeast cells as the precursors. Remarkably, when the as-prepared materials are used as the electrode materials for supercapacitors, they exhibit outstanding performance with high specific capacitance of 330 F g(-1) at a current density of 1 A g(-1), and good stability, even after 1000 charge/discharge cycles. The approach developed in this work provides a new view of making full use of sustainable resources endowed by nature, opening the avenue to designing and producing robust materials with great promising applications in high-performance energy-storage devices.

  11. Solvothermal synthesis and characterization of ceria with solid and hollow spherical and multilayered morphologies

    International Nuclear Information System (INIS)

    He, Lei; Li, Junping; Feng, Zhihai; Sun, Dongfeng; Wang, Tingyu; Li, Ruixing; Xu, Yaohui

    2014-01-01

    Highlights: • Various morphologies of CeO 2 are gotten by controlling the solvothermal conditions. • The various morphologies are synthesized without any template or surfactant. • The chemical mechanisms for the formation of the products in the solvothermal process are discussed. • The morphology evolution from solid spheres to multilayered structures is supposed. • The as-synthesized CeO 2 samples possess excellent adsorption capacities. - Abstract: Ceria powders with different morphologies were synthesized using a facile template-free solvothermal process combined with calcination. The influence of solvothermal temperature and time on the powder was studied. Solid spheres, hollow spheres, and multilayered structures were controlled by adjusting the solvothermal conditions. The possible mechanisms for the formation of the precursors under the solvothermal conditions employed and the evolution of the powder from solid spherical to multilayered structures were discussed. Ethylene glycol played a key role in the morphology evolution of the powder. Cerium catalyzed the Guerbet-like reaction and reacted with ethylene glycol to produce ceria (CeO 2 ), Ce(HCOO) 3 , and Ce(OH)CO 3 . The redox-assisted dissolution–recrystallization process significantly contributed to the morphology transformation from solid spheres to multilayered structures. Moreover, the samples synthesized at different temperatures for 24 h possessed excellent adsorption capacities towards the removal of acid orange 7 when compared with commercial ceria

  12. 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.

  13. 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.

  14. 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.

  15. Template-free synthesis of novel SnS2 array and its superior performances for lithium ion battery

    Science.gov (United States)

    Zhu, Anquan; Qiao, Lulu; Tan, Pengfei; Ma, Yongjin; Liu, Yi; Pan, Jun

    2018-05-01

    A kind of novel three-dimensional SnS2 array was fabricated by an ethylenediamine (EDA) assisting low-temperature solvothermal method. It was observed that as-obtained SnS2 array was composed of numerous SnS2 nanosheets with the thickness of about 22 nm. When used as lithium ion batteries (LIBs) anode, the SnS2 array displayed remarkable capacities on rate and cycling performances, delivering the rates with reversible capacities of 763.3, 658.6, 593.6, 554.4 and 450.3 mAh g-1 at the current densities of 0.2, 0.5, 1, 2 and 5 A g-1, respectively. Moreover, the satisfactory cycling performance was also disclosed, remaining capacity of 547.8 mAh g-1 after 100th cycle at 0.2 A g-1, better than some reported pure SnS2 nanostructures. Based on the characterization and experimental results, the reasons of such superior electrochemical performances were determined and elaborated. It means that the SnS2 array possesses promising potential on the renewable energy field.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. Mesoporous anatase TiO2/reduced graphene oxide nanocomposites: A simple template-free synthesis and their high photocatalytic performance

    International Nuclear Information System (INIS)

    Zhou, Qi; Zhong, Yong-Hui; Chen, Xing; Huang, Xing-Jiu; Wu, Yu-Cheng

    2014-01-01

    Graphical abstract: - Highlights: • Mesoporous TiO 2 nanoparticles with anatase phase were assembled on reduced graphene oxide via a template-free one-step hydrothermal method. • The TiO 2 /rGO nanocomposites have better adsorption capacity and photocatalytic degradation efficiency for dyes removal. • Improved dye adsorption and photogenerated charge separation are responsible for enhanced activity. - Abstract: Mesoporous anatase phase TiO 2 was assembled on reduced graphene oxide (rGO) using a template-free one-step hydrothermal process. The nanocomposites were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and Brunauer–Emmett–Teller (BET) surface area. Morphology of TiO 2 was related to the content of graphene oxide. TiO 2 /rGO nanocomposites exhibited excellent photocatalytic activity for the photo-degradation of methyl orange. The degradation rate was 4.5 times greater than that of pure TiO 2 nanoparticles. This difference was attributed to the thin two-dimensional graphene sheet. The graphene sheet had a large surface area, high adsorption capacity, and acted as a good electron acceptor for the transfer of photo-generated electrons from the conduction band of TiO 2 . The enhanced surface adsorption characteristics and excellent charge transport separation were independent properties of the photocatalytic degradation process

  1. 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.

  2. 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.

  3. 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.

  4. Solvothermal Synthesis of Copper Indium Diselenide in Toluene

    International Nuclear Information System (INIS)

    Chang, Ju Yeon; Han, Jae Eok; Jung, Duk Young

    2011-01-01

    Polycrystalline CuInSe 2 (CIS) was synthesized through solvothermal reactions in toluene with selected alkyl amines as complexing agents. The alkyl amines were used as reducing agent of selenium and catalytic ligands, enhancing the formation of CIS compounds in the colloidal solution. Toluene does not contribute the syntheses directly but minimizes the amounts of amines required for single phase CIS. We systematically studied the reactivity of amine compounds for the solovothermal syntheses, determined critical concentration of amine and the shortest reaction time. Crystallinity, morphology, chemical composition, and band gap of the prepared CuInSe 2 were respectively measured by X-ray diffraction, scanning electron microscopy, inductively coupled plasma atomic emission spectroscopy and UV-vis spectroscopy

  5. Solvothermal synthesis of copper sulfide semiconductor micro/nanostructures

    International Nuclear Information System (INIS)

    Liu, Jun; Xue, Dongfeng

    2010-01-01

    Covellite copper sulfide (CuS) micro/nanometer crystals in the shape of hierarchical doughnut-shaped, superstructured spheric-shaped and flowerlike architectures congregated from those nanoplates with the thickness of 20-100 nm have been prepared by a solvothermal method. The as-obtained CuS products were characterized by means of scanning electron microscopy (SEM), X-ray diffractometry (XRD) and energy-dispersive X-ray spectroscopy (EDS). A systematic investigation has been carried out to understand the factors influencing the evolution of CuS particle morphology which found to be predominant by solvent, surfactant, sulfur resource and copper salt. The possible formation mechanism for the nanostructure formation was also discussed. These CuS products show potential applications in solar cell, photothermal conversion and chemical sensor.

  6. TiO2/carbon nanotube hybrid nanostructures: Solvothermal synthesis and their visible light photocatalytic activity

    International Nuclear Information System (INIS)

    Tian Lihong; Ye Liqun; Deng Kejian; Zan Ling

    2011-01-01

    MWCNT/TiO 2 hybrid nanostructures were prepared via solvothermal synthesis and sol-gel method with benzyl alcohol as a surfactant. As-prepared hybrid materials were characterized by X-ray diffraction, transmission electron microscopy, UV-vis diffuse reflectance spectra and X-ray photoelectron spectroscopy. The results showed that MWCNTs were uniformly decorated with anatase nanocrystals in solvothermal condition, but MWCNTs were embedded in a majority of TiO 2 nanoparticles by sol-gel method. When the weight ratio of MWCNTs to TiO 2 was 20%, MWCNT/TiO 2 hybrid nanostructures prepared by solvothermal synthesis exhibited higher visible-light-driven photocatalytic activity than that prepared by sol-gel method. Post-annealing of MWCNT/TiO 2 nanostructures at 400 deg. C resulted in the formation of the carbonaceous Ti-C bonds on the interface between TiO 2 and MWCNTs, which enhanced the photoabsorbance of the hybrid materials in the visible light region and improved the visible-light degradation efficiency of methylene blue. - Graphical abstract: MWCNT/TiO 2 nanostructures have been prepared by solvothermal method, which exhibited higher visible-light-driven photocatalytic activity than that prepared by sol-gel method. The carbonaceous Ti-C bonds on the interface between TiO 2 and MWCNTs enhanced the photoabsorbance of the hybrid materials in the visible light region. Highlights: → Anatase TiO 2 nanoparticles were anchored on CNTs surface uniformly via solvothermal method → The morphology facilitated the electron transfer between CNTs and TiO 2 → Ti-C bonds extended the absorption of MWCNT/TiO 2 to the whole visible light region. → The hybrid nanostructures showed enhanced visible-light induced photocatalytic activity.

  7. Silver nanoparticles: Large scale solvothermal synthesis and optical properties

    Energy Technology Data Exchange (ETDEWEB)

    Wani, Irshad A.; Khatoon, Sarvari [Nanochemistry Laboratory, Department of Chemistry, Jamia Millia Islamia, New Delhi 110025 (India); Ganguly, Aparna [Nanochemistry Laboratory, Department of Chemistry, Jamia Millia Islamia, New Delhi 110025 (India); Department of Chemistry, Indian Institute of Technology, Hauz Khas, New Delhi 110016 (India); Ahmed, Jahangeer; Ganguli, Ashok K. [Department of Chemistry, Indian Institute of Technology, Hauz Khas, New Delhi 110016 (India); Ahmad, Tokeer, E-mail: tokeer.ch@jmi.ac.in [Nanochemistry Laboratory, Department of Chemistry, Jamia Millia Islamia, New Delhi 110025 (India)

    2010-08-15

    Silver nanoparticles have been successfully synthesized by a simple and modified solvothermal method at large scale using ethanol as the refluxing solvent and NaBH{sub 4} as reducing agent. The nanopowder was investigated by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), dynamic light scattering (DLS), UV-visible and BET surface area studies. XRD studies reveal the monophasic nature of these highly crystalline silver nanoparticles. Transmission electron microscopic studies show the monodisperse and highly uniform nanoparticles of silver of the particle size of 5 nm, however, the size is found to be 7 nm using dynamic light scattering which is in good agreement with the TEM and X-ray line broadening studies. The surface area was found to be 34.5 m{sup 2}/g. UV-visible studies show the absorption band at {approx}425 nm due to surface plasmon resonance. The percentage yield of silver nanoparticles was found to be as high as 98.5%.

  8. Indium telluride nanotubes: Solvothermal synthesis, growth mechanism, and properties

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Liyan [National Laboratory of Solid State Microstructures, School of Electronic Science and Engineering, Nanjing University, Nanjing 210093 (China); Yan, Shancheng, E-mail: yansc@njupt.edu.cn [National Laboratory of Solid State Microstructures, School of Electronic Science and Engineering, Nanjing University, Nanjing 210093 (China); School of Geography and Biological Information, Nanjing University of Posts and Telecommunications, Nanjing 210046 (China); Lu, Tao; Shi, Yi; Wang, Jianyu [National Laboratory of Solid State Microstructures, School of Electronic Science and Engineering, Nanjing University, Nanjing 210093 (China); Yang, Fan [School of Geography and Biological Information, Nanjing University of Posts and Telecommunications, Nanjing 210046 (China)

    2014-03-15

    A convenient solvothermal approach was applied for the first time to synthesize In{sub 2}Te{sub 3} nanotubes. The morphology of the resultant nanotubes was studied by scanning electron microscopy and transmission electron microscopy. Nanotubes with a relatively uniform diameter of around 500 nm, tube wall thickness of 50–100 nm, and average length of tens of microns were obtained. X-ray diffraction, X-ray photoelectron spectroscopy, and Raman spectroscopy were used to study the crystal structures, composition, and optical properties of the products. To understand the growth mechanism of the In{sub 2}Te{sub 3} nanotubes, we studied the influences of temperature, reaction time, and polyvinylpyrrolidone (PVP) and ethylene diamine (EDA) dosages on the final products. Based on the experimental results, a possible growth mechanism of In{sub 2}Te{sub 3} nanotubes was proposed. In this mechanism, TeO{sub 3}{sup −2} is first reduced to allow nucleation. Circumferential edges of these nucleated molecules attract further deposition, and nanotubes finally grow rapidly along the c-axis and relatively slowly along the circumferential direction. The surface area of the products was determined by BET and found to be 137.85 m{sup 2} g{sup −1}. This large surface area indicates that the nanotubes may be suitable for gas sensing and hydrogen storage applications. The nanotubes also showed broad light detection ranging from 300 nm to 1100 nm, which covers the UV–visible–NIR regions. Such excellent optical properties indicate that In{sub 2}Te{sub 3} nanotubes may enable significant advancements in new photodetection and photosensing applications. -- Graphical abstract: A convenient solvothermal approach was applied to synthesize In{sub 2}Te{sub 3} nanotubes, which has not been reported in the literature for our knowledge. Surface area of this material is 137.85 m{sup 2} g{sup −1} from the BET testing, and such a high value makes it probably suitable for gas sensing and

  9. 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)

  10. 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.

  11. Solvothermal synthesis of Li–Al layered double hydroxides and their electrochemical performance

    International Nuclear Information System (INIS)

    Wei, Jinbo; Gao, Zan; Song, Yanchao; Yang, Wanlu; Wang, Jun; Li, Zhanshuang; Mann, Tom; Zhang, Milin; Liu, Lianhe

    2013-01-01

    In this paper, for the first time, Li/Al layered double hydroxides (LDHs) were synthesized by a facile and environment-friendly solvothermal approach. X-ray diffraction patterns show that the as-prepared products belong to the hexagonal phase. Well-defined LDHs particles with spiral-shape (1–2 μm), hexagonal (2–3 μm) and petal-like structures (10–15 μm) have been successfully fabricated by adjusting the content of water/ethanol in the synthesis process. A possible growth mechanism was proposed for the formation of these structures. Their electrochemical performances were investigated by cyclic voltammetry, galvanostatic charge/discharge test and electrochemical impedance spectroscopy. The hexagonal Li/Al LDHs calcined at 450 °C exhibit the specific capacitance of 848 F g −1 at a current density of 1.25 A g −1 . The high specific capacitance and remarkable rate capacity of Li/Al LDHs are promising for applications in capacitors and low-cost aqueous lithium ion batteries. - Graphical abstract: Hexagonal Li/Al layered double hydroxides (LDHs) with high specific surface area and remarkable rate capacity via a facile and environmentally friendly solvothermal approach. Highlights: ► Li/Al LDHs with different morphologies were fabricated by a solvothermal method. ► Hexagonal Li/Al LDHs display better electrochemical performance. ► A possible growth mechanism to explain the different morphology is proposed

  12. Synthesis of nano γ-alumina by the solvothermal technique

    International Nuclear Information System (INIS)

    Meor Yusoff Meor Sulaiman; Masliana Muslimin

    2006-01-01

    The paper describes work done on synthesis of γ-alumina by using the solvo thermal technique. Synthesis of γ-alumina involves the transition reactions of the aluminium hydroxide into alumina by a dehydroxylation process. As there are many forms of transition aluminas produced during this process, a x-ray diffraction (XRD) technique was used to identify γ-alumina and the other forms of alumina. After establishing the optimum conditions for the production of a single-phase γ-alumina, characteristic study on the product was performed. An important parameter in establishing nanosized powders is their crystallite size and analysis of the γ-alumina shows that it is a nanosized powder with a size of 28 nm. Other properties analysed include morphology, surface area and particle size. (Author)

  13. High-Quality ZnCdS Nanosheets Prepared Using Solvothermal Synthesis

    International Nuclear Information System (INIS)

    Mahdi, M.A.; Hassan, J.J.; Ng, S.S.; Hassan, Z.

    2013-01-01

    For the first time, Zn X Cd 1-X S nanosheets with different Zn and Cd ion concentrations were prepared using solvothermal synthesis at 200 degree C for 4 and 24 h. The crystalline structure of the nanosheets was wurtzite. The optical band gaps of the nanosheets increased with increasing Zn ratio; this increase is consistent with the band gaps estimated using Vegard’s formula. The photoluminescence spectra for the 24 h nanosheets had higher emission intensities than those for the 4 h nanosheets. The emission band corresponding to intrinsic near-band-edge emission and a broad peak associated with extrinsic deep-level emission were observed in the photoluminescence spectra.

  14. Large-scale solvothermal synthesis of fluorescent carbon nanoparticles

    International Nuclear Information System (INIS)

    Ku, Kahoe; Park, Jinwoo; Kim, Nayon; Kim, Woong; Lee, Seung-Wook; Chung, Haegeun; Han, Chi-Hwan

    2014-01-01

    The large-scale production of high-quality carbon nanomaterials is highly desirable for a variety of applications. We demonstrate a novel synthetic route to the production of fluorescent carbon nanoparticles (CNPs) in large quantities via a single-step reaction. The simple heating of a mixture of benzaldehyde, ethanol and graphite oxide (GO) with residual sulfuric acid in an autoclave produced 7 g of CNPs with a quantum yield of 20%. The CNPs can be dispersed in various organic solvents; hence, they are easily incorporated into polymer composites in forms such as nanofibers and thin films. Additionally, we observed that the GO present during the CNP synthesis was reduced. The reduced GO (RGO) was sufficiently conductive (σ ≈ 282 S m −1 ) such that it could be used as an electrode material in a supercapacitor; in addition, it can provide excellent capacitive behavior and high-rate capability. This work will contribute greatly to the development of efficient synthetic routes to diverse carbon nanomaterials, including CNPs and RGO, that are suitable for a wide range of applications. (paper)

  15. Solvothermal synthesis and analysis of Bi1-xSbx nanoparticles

    International Nuclear Information System (INIS)

    Sumithra, S.; Misra, D.K.; Wei, C.; Gabrisch, H.; Poudeu, P.F.P.; Stokes, K.L.

    2011-01-01

    Bismuth-antimony alloy nanoparticles have been synthesized by a facile solvothermal method using N,N-dimethylformamide and ethylene glycol as solvent/reducing agent; BiCl 3 , SbCl 3 and Bi(NO 3 ) 3 as precursors; and citric acid as a surface modifier/stabilizing agent. The particle size and size distribution of Bi nanoparticles were analyzed as a function of the synthesis conditions: molar ratio of precursor to surfactant, precursor concentration and reducing agent. Synthesis of Sb and Bi 0.88 Sb 0.12 under similar conditions was also investigated. The phase purity of nanoparticles was confirmed from X-ray diffraction and thermogravimetry and the nanoparticle morphology was investigated by transmission electron microscopy. A case study of Bi nanoparticles with detailed analysis of the particle morphology and size distribution of the nanoparticles is reported.

  16. Scalable and template-free synthesis of nanostructured Na{sub 1.08}V{sub 6}O{sub 15} as high-performance cathode material for lithium-ion batteries

    Energy Technology Data Exchange (ETDEWEB)

    Zheng, Shili, E-mail: slzheng@ipe.ac.cn [National Engineering Laboratory for Hydrometallurgical Cleaner Production Technology, Key Laboratory of Green Process and Engineering, Institute of Process Engineering, Chinese Academy of Sciences, Beijing (China); Wang, Xinran; Yan, Hong [National Engineering Laboratory for Hydrometallurgical Cleaner Production Technology, Key Laboratory of Green Process and Engineering, Institute of Process Engineering, Chinese Academy of Sciences, Beijing (China); University of Chinese Academy of Sciences, No. 19A Yuquan Road, Beijing (China); Du, Hao; Zhang, Yi [National Engineering Laboratory for Hydrometallurgical Cleaner Production Technology, Key Laboratory of Green Process and Engineering, Institute of Process Engineering, Chinese Academy of Sciences, Beijing (China)

    2016-09-15

    Highlights: • Nanostructured Na{sub 1.08}V{sub 6}O{sub 15} was synthesized through additive-free sol-gel process. • Prepared Na{sub 1.08}V{sub 6}O{sub 15} demonstrated high capacity and sufficient cycling stability. • The reaction temperature was optimized to allow scalable Na{sub 1.08}V{sub 6}O{sub 15} fabrication. - Abstract: Developing high-capacity cathode material with feasibility and scalability is still challenging for lithium-ion batteries (LIBs). In this study, a high-capacity ternary sodium vanadate compound, nanostructured NaV{sub 6}O{sub 15}, was template-free synthesized through sol-gel process with high producing efficiency. The as-prepared sample was systematically post-treated at different temperature and the post-annealing temperature was found to determine the cycling stability and capacity of NaV{sub 6}O{sub 15}. The well-crystallized one exhibited good electrochemical performance with a high specific capacity of 302 mAh g{sup −1} when cycled at current density of 0.03 mA g{sup −1}. Its relatively long-term cycling stability was characterized by the cell performance under the current density of 1 A g{sup −1}, delivering a reversible capacity of 118 mAh g{sup −1} after 300 cycles with 79% capacity retention and nearly 100% coulombic efficiency: all demonstrating its significant promise of proposed strategy for large-scale synthesis of NaV{sub 6}O{sub 15} as cathode with high-capacity and high energy density for LIBs.

  17. 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.

  18. Synthesis and optical properties of CuS nanoplate-based architectures by a solvothermal method

    International Nuclear Information System (INIS)

    Li Fei; Kong Tao; Bi Wentuan; Li Dachang; Li Zhen; Huang Xintang

    2009-01-01

    The controlled synthesis of copper sulfide (CuS) nanoplate-based architectures in different solvents has been realized at low cost by simply reaction of Cu(NO 3 ) 2 .3H 2 O and S under solvothermal conditions without the use of any template. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-vis spectrometer and fluorescence measurement were used to characterize the products. The products were all in hexagonal phase with high crystallinity and the morphology was significantly influenced by the solvents. The CuS products synthesized in dimethylformamide (DMF) were nanoplates and the samples prepared in ethanol were flower-like morphology composed of large numbers of nanoplates, but those synthesized in ethylene glycol (EG) were CuS architectures with high symmetry made up of several nanoplates arranged in a certain mode. The optical properties were investigated and the growth mechanisms of these CuS crystals were also proposed.

  19. One-pot solvothermal synthesis of three-dimensional (3D) BiOI/BiOCl composites with enhanced visible-light photocatalytic activities for the degradation of bisphenol-A

    International Nuclear Information System (INIS)

    Xiao, Xin; Hao, Rong; Liang, Min; Zuo, Xiaoxi; Nan, Junmin; Li, Laisheng; Zhang, Weide

    2012-01-01

    Highlights: ► Synthesis of 3D BiOI/BiOCl microspheres by a one-pot template-free solvothermal method. ► Photocatalyst is BiOI/BiOCl composites. ► BiOI/BiOCl composites have enhanced visible-light photocatalytic ability to bisphenol-A. ► A simple and direct photodegradation pathway of bisphenol-A is proposed. - Abstract: Three-dimensional (3D) BiOI/BiOCl composite microspheres with enhanced visible-light photodegradation activity of bisphenol-A (BPA) are synthesized by a simple, one-pot, template-free, solvothermal method using BiI 3 and BiCl 3 as precursors. These 3D hierarchical microspheres with heterojunction structures are composed of 2D nanosheets and have composition-dependent absorption properties in the ultraviolet and visible light regions. The photocatalytic oxidation of BPA over BiOI/BiOCl composites followed pseudo first-order kinetics according to the Langmuir–Hinshelwood model. The highest photodegradation efficiency of BPA, i.e., nearly 100%, was observed with the BiOI/BiOCl composite (containing 90% BiOI) using a catalyst dosage of 1 g L −1 in the BPA solution (C 0 = 20 mg L −1 , pH = 7.0) under visible light irradiation for 60 min. Under these conditions, the reaction rate constant was more than 4 and 20 times greater than that of pure BiOI and the commercially available Degussa P25, respectively. The superior photocatalytic activity of this composite catalyst is attributed to the suitable band gap energies and the low recombination rate of the photogenerated electron–hole pairs due to the presence of BiOI/BiOCl heterostructures. Only one intermediate at m/z 151 was observed in the photodegradation process of BPA by liquid chromatography combined with mass spectrometry (LC–MS) analysis, and a simple and hole-predominated photodegradation pathway of BPA was subsequently proposed. Furthermore, this photocatalyst exhibited a high mineralization ratio, high stability and easy separation for recycling use, suggesting that it is a

  20. One-pot solvothermal synthesis of three-dimensional (3D) BiOI/BiOCl composites with enhanced visible-light photocatalytic activities for the degradation of bisphenol-A

    Energy Technology Data Exchange (ETDEWEB)

    Xiao, Xin [School of Chemistry and Environment, South China Normal University, Key Lab of Theoretical Chemistry of Environment, Guangzhou 510006 (China); Nano Science Research Center, School of Chemistry and Chemical Engineering, South China University of Technology, Guangzhou 510640 (China); Hao, Rong; Liang, Min; Zuo, Xiaoxi [School of Chemistry and Environment, South China Normal University, Key Lab of Theoretical Chemistry of Environment, Guangzhou 510006 (China); Nan, Junmin, E-mail: jmnan@scnu.edu.cn [School of Chemistry and Environment, South China Normal University, Key Lab of Theoretical Chemistry of Environment, Guangzhou 510006 (China); Li, Laisheng [School of Chemistry and Environment, South China Normal University, Key Lab of Theoretical Chemistry of Environment, Guangzhou 510006 (China); Zhang, Weide [Nano Science Research Center, School of Chemistry and Chemical Engineering, South China University of Technology, Guangzhou 510640 (China)

    2012-09-30

    Highlights: Black-Right-Pointing-Pointer Synthesis of 3D BiOI/BiOCl microspheres by a one-pot template-free solvothermal method. Black-Right-Pointing-Pointer Photocatalyst is BiOI/BiOCl composites. Black-Right-Pointing-Pointer BiOI/BiOCl composites have enhanced visible-light photocatalytic ability to bisphenol-A. Black-Right-Pointing-Pointer A simple and direct photodegradation pathway of bisphenol-A is proposed. - Abstract: Three-dimensional (3D) BiOI/BiOCl composite microspheres with enhanced visible-light photodegradation activity of bisphenol-A (BPA) are synthesized by a simple, one-pot, template-free, solvothermal method using BiI{sub 3} and BiCl{sub 3} as precursors. These 3D hierarchical microspheres with heterojunction structures are composed of 2D nanosheets and have composition-dependent absorption properties in the ultraviolet and visible light regions. The photocatalytic oxidation of BPA over BiOI/BiOCl composites followed pseudo first-order kinetics according to the Langmuir-Hinshelwood model. The highest photodegradation efficiency of BPA, i.e., nearly 100%, was observed with the BiOI/BiOCl composite (containing 90% BiOI) using a catalyst dosage of 1 g L{sup -1} in the BPA solution (C{sub 0} = 20 mg L{sup -1}, pH = 7.0) under visible light irradiation for 60 min. Under these conditions, the reaction rate constant was more than 4 and 20 times greater than that of pure BiOI and the commercially available Degussa P25, respectively. The superior photocatalytic activity of this composite catalyst is attributed to the suitable band gap energies and the low recombination rate of the photogenerated electron-hole pairs due to the presence of BiOI/BiOCl heterostructures. Only one intermediate at m/z 151 was observed in the photodegradation process of BPA by liquid chromatography combined with mass spectrometry (LC-MS) analysis, and a simple and hole-predominated photodegradation pathway of BPA was subsequently proposed. Furthermore, this photocatalyst

  1. Modified solvothermal synthesis and characterization of CdS/ZnS core/shell nanorods

    International Nuclear Information System (INIS)

    Baby Suganthi, A.R.; Sagayaraj, P.

    2013-01-01

    Core/shell CdS/ZnS nanorods were synthesized using a two-step solvothermal approach. The first step is the formation of CdS nanoparticles initiated using nucleation followed by growth through coalescence-exchange and particle coagulation. The second step leads to the formation of ZnS and further coalescence-exchange leading to deposition and growth of a ZnS shell around CdS nanoparticles. The structural, morphological and chemical studies were performed using X-ray diffraction, Energy Dispersive X-ray spectroscopy (EDX) Scanning electron Microscopy (SEM), UV–vis absorption spectra and Transmission Electron Microscopy (TEM), provide direct evidence for shell growth. The present synthesis provides a rational approach to the design of novel core/shell nanomaterials with appealing applications in optoelectronic devices. - Graphical abstract: From the resulting TEM images, the formation of core/shell could be observed. The apparent microscopy contrast between the CdS core and the ZnS shell offers evidence for the formation of CdS/ZnS core/shell nanostructures. It is clearly evident that the surfaces of the nanorods became rough after coating and also the diameter of the nanorod is seen increased up to 40–50 nm. Highlights: ► CdS/ZnS core/shell nanorods were synthesized using two-step solvothermal approach. ► The nanoparticles were characterized by XRD, EDX, SEM, UV–vis and TEM. ► SEM images revealed the surface roughness after ZnS shell growth. ► TEM microscopy offers evidence for the formation of core/shell nanostructures

  2. Synthesis of the Complex Fluoride LiBaF3 through a Solvothermal Process

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    The complex fluoride LiBaF3 is solvothermally synthesized at 180℃ and characterized by means of X-ray powder diffraction, scanning electron microscopy, thermogravimetric analysis and infrared spectroscopy. In the solvothermal process, the solvents, mole ratios of initial mixtures and reaction temperature play important roles in the growth of the single crystal.

  3. 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.

  4. 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.

  5. Solvothermal synthesis of gallium-indium-zinc-oxide nanoparticles for electrolyte-gated transistors.

    Science.gov (United States)

    Santos, Lídia; Nunes, Daniela; Calmeiro, Tomás; Branquinho, Rita; Salgueiro, Daniela; Barquinha, Pedro; Pereira, Luís; Martins, Rodrigo; Fortunato, Elvira

    2015-01-14

    Solution-processed field-effect transistors are strategic building blocks when considering low-cost sustainable flexible electronics. Nevertheless, some challenges (e.g., processing temperature, reliability, reproducibility in large areas, and cost effectiveness) are requirements that must be surpassed in order to achieve high-performance transistors. The present work reports electrolyte-gated transistors using as channel layer gallium-indium-zinc-oxide nanoparticles produced by solvothermal synthesis combined with a solid-state electrolyte based on aqueous dispersions of vinyl acetate stabilized with cellulose derivatives, acrylic acid ester in styrene and lithium perchlorate. The devices fabricated using this approach display a ION/IOFF up to 1 × 10(6), threshold voltage (VTh) of 0.3-1.9 V, and mobility up to 1 cm(2)/(V s), as a function of gallium-indium-zinc-oxide ink formulation and two different annealing temperatures. These results validates the usage of electrolyte-gated transistors as a viable and promising alternative for nanoparticle based semiconductor devices as the electrolyte improves the interface and promotes a more efficient step coverage of the channel layer, reducing the operating voltage when compared with conventional dielectrics gating. Moreover, it is shown that by controlling the applied gate potential, the operation mechanism of the electrolyte-gated transistors can be modified from electric double layer to electrochemical doping.

  6. 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

  7. Surfactant-assisted mild solvothermal synthesis of nanostructured LiFePO4/C cathodes evidencing ultrafast rate capability

    International Nuclear Information System (INIS)

    Di Lupo, F.; Meligrana, G.; Gerbaldi, C.; Bodoardo, S.; Penazzi, N.

    2015-01-01

    Highlights: • Nanostructured LiFePO 4 /C by surfactant assisted solvothermal synthesis. • Novel and simple preparation method, with no critical parameters. • Noticeable stability, good capacity values and capacity retention after prolonged cycling. • Improved rate capability at a very high C-rate (100C). • High performance for the next generation of advanced high power Li-ion batteries. - Abstract: A surfactant-assisted solvothermal synthesis is hereby applied to produce carbon-coated LiFePO 4 /C nanostructured Li-ion battery cathodes. The use of different mixed alcohol/water solutions for the dissolution of a cationic surfactant is absolutely peculiar in this field and herewith exploited to tailor-make the properties of the active material particles (e.g., morphology and electrochemical behaviour). Thorough investigation is carried out by means of X-ray powder diffraction, scanning and transmission electron microscopy, cyclic voltammetry and constant current charge-discharge cycling. The best performing sample, obtained in a 20:80 w/w ethanol:water solution, demonstrates good specific capacity values, high Coulombic efficiency and rate capability, with stable behaviour upon long-term cycling even at ultrafast 100C discharge regime. This is definitely remarkable for a nanosized powder specifically conceived for high power applications obtained by means of low cost raw materials, simple and reliable procedures

  8. Synthesis of mesoporous TiO(2-x)N(x) spheres by template free homogeneous co-precipitation method and their photo-catalytic activity under visible light illumination.

    Science.gov (United States)

    Parida, K M; Naik, Brundabana

    2009-05-01

    The article presents preparation, characterization and catalytic activity evaluation of an efficient nitrogen doped mesoporous titania sphere photo-catalyst for degradation of methylene blue (MB) and methyl orange (MO) under visible light illumination. Nitrogen doped titania was prepared by soft chemical route i.e. template free, slow and controlled homogeneous co-precipitation from titanium oxysulfate sulfuric acid complex hydrate, urea, ethanol and water. The molar composition of TiOSO(4) to urea was varied to prepare different atomic % nitrogen doped titania. Mesoporous anatase TiO(2-x)N(x) spheres with average crystallite size of 10 nm and formation of titanium oxynitride center were confirmed from HRTEM, XRD and XPS study. UV-vis DRS showed a strong absorption in the range of 400-500 nm which supports its use in visible spectrum of light. Nitrogen adsorption-desorption study supports the porous nature of the doped material. All the TiO(2-x)N(x) samples showed higher photo-catalytic activity than Degussa P(25) and undoped mesoporous titania. Sample containing around one atomic % nitrogen showed highest activity among the TiO(2-x)N(x) samples.

  9. Simple extraction-solvothermal synthesis of single-crystalline silver microplates

    Energy Technology Data Exchange (ETDEWEB)

    You, Ting; Sun, Sixiu; Song, Xinyu; Xu, Shuling [Department of Chemistry and Chemical Engineering, Shandong University (China)

    2009-08-15

    Single-crystalline silver microplates, with average edge length of about 1.5{mu}m and thickness of 100 nm, have been synthesized by a simple extraction-solvothermal method. Samples were characterized in detail by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and High-resolution transmission electron microscopy (HRTEM) technologies. Extractant primary amine N1923 can also act as reducing agent. It has been found that microstructure of the silver can be controlled by the n-octanol during the solvothermal treatment. Based on a series of experimental analysis, the possible formation mechanism of these microplates was discussed briefly. (copyright 2009 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  10. Water-assisted and surfactant-free synthesis of cobalt ferrite nanospheres via solvothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Bi, Yiqing [CAS Laboratory of Nanosystem and Hierarchical Fabrication, National Center for Nanoscience and Technology, Beijing 100190 (China); University of the Chinese Academy of Sciences, Beijing 100049 (China); Ren, Yanan [CAS Laboratory of Nanosystem and Hierarchical Fabrication, National Center for Nanoscience and Technology, Beijing 100190 (China); Bi, Feng [CAS Laboratory of Nanosystem and Hierarchical Fabrication, National Center for Nanoscience and Technology, Beijing 100190 (China); University of the Chinese Academy of Sciences, Beijing 100049 (China); He, Tao, E-mail: het@nanoctr.cn [CAS Laboratory of Nanosystem and Hierarchical Fabrication, National Center for Nanoscience and Technology, Beijing 100190 (China)

    2015-10-15

    With ethylene glycol as the solvent, monodispersed cobalt ferrite nanospheres were prepared via a solvothermal method assisted by water. The samples were mainly characterized by X-ray diffraction, scanning electron microscope, and transmission electron microscope. The size of as-prepared products ranges from 10 nm to 200 nm. Size distribution and chemical composition were controlled by the amount of water and pH value in the reaction system. More important, suitable amount of water can avoid the use of surfactant. - Highlights: • Cobalt ferrite nanospheres were synthesized via solvothermal method assisted by water. • An introduction of suitable amount of water can avoid the use of surfactant. • The pH value of the precursor can be used to adjust the product composition.

  11. Polyol-mediated synthesis of copper indium sulphide by solvothermal process

    International Nuclear Information System (INIS)

    Gorai, S.; Chaudhuri, S.

    2005-01-01

    A simple polyol-mediated solvothermal method has been proposed to synthesize copper indium sulphide. XRD studies reveal that the products are well crystallized. SEM indicates rod-like (with different aspect ratio) and star-shaped flake-like morphology of the products. The products are also characterized by optical studies and compositional analysis (XRF). XRF results show the formation of stoichiometric and non-stoichiometric copper indium sulphides depending on the reaction conditions

  12. Facile Solvothermal Synthesis of BiOCl/ZnO Heterostructures with Enhanced Photocatalytic Activity

    Directory of Open Access Journals (Sweden)

    Yong-Fang Li

    2014-01-01

    Full Text Available Well-defined nanosheet-assembled (BiOClx(ZnO1−x nanoflowers were synthesized by a solvothermal method. It was found that ZnO nanoparticles were anchored on the flower-like BiOCl nanostructures, as demonstrated by varying the initial compositions of the Bi precursor and the volume ratios of mixed solvents (ethylene glycol to water. The as-prepared (BiOCl0.6(ZnO0.4 nanocomposites showed enhanced photocatalytic activity toward rhodamine B degradation under ultraviolet (UV irradiation. And the photocatalytic mechanism was discussed in detail.

  13. Facile Synthesis of Long, Straight and Uniform Copper Nanowires via a Solvothermal Method

    Institute of Scientific and Technical Information of China (English)

    Chunfu Lin; Hong Lin; Ning Wang; Xing Zhang; Jun Yang; Jianbo Li; Xiaozhan Yang

    2006-01-01

    Copper nanowires were facilely prepared via a solvothermal method. In this method, cetyltrimethylammonium bromide (CTAB) was used as a soft template, copper nitrate was an inorganic precursor, and absolute ethanol served as a reducing agent as well as a solvent. X-ray diffraction (XRD) and scanning electron microscopy (SEM) were used to characterize the as-prepared copper nanowires. The as-prepared copper nanowires are fairly uniform and long. The majority of them are longer than 100 μm and some even longer than 200 μm. Furthermore, most nanowires are quite straight. In addition,The mechanism of the growth process of copper nanowires was discussed.

  14. Ultra-flexible lithium ion batteries fabricated by electrodeposition and solvothermal synthesis

    International Nuclear Information System (INIS)

    Wang, Jian; Zhang, Lei; Zhou, Qingwen; Wu, Wenlu; Zhu, Chao; Liu, Ziqiang; Chang, Shaozhong; Pu, Jun; Zhang, Huigang

    2017-01-01

    Cathodes have been one of the major challenges of flexible batteries. The traditional slurry-based technologies lead to loose interparticle connection, which is vulnerable upon bending. The direct fabrication of cathode materials requires high temperatures, which may destroy flexible substrates. Here we developed an electrodepostion and solvothermal route to conformally coat cathode material on a flexible scaffold. The monolithic electrode enables an ultra-flexible lithium ion battery because of the close attachment of active materials to flexible scaffolds and the interlock effect between the hard shell and soft core. This ultra-flexible battery retains 58.8% of initial capacity even after bending 4000 cycles.

  15. Solvothermal synthesis and enhanced CO2 adsorption ability of mesoporous graphene oxide-ZnO nanocomposite

    International Nuclear Information System (INIS)

    Li, Weidong; Jiang, Xia; Yang, Huayun; Liu, Qi

    2015-01-01

    Highlights: • GO–ZnO nanocomposite was prepared by solvothermal method. • Several technologies have been used to ensure and analyze the composite. • GO–ZnO has CO 2 adsorption capacity of up to 44.8 cm 3 /g at 298 K and 1 bar. • The composite has excellent adsorption/desorption recycling ability. - Abstract: Mesoporous graphene oxide–ZnO (GO–ZnO) nanocomposite has been synthesized by GO and ZnO which was prepared by solvothermal method. Power X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) have been used to characterize the structure and morphology of the porous GO–ZnO hybrid. With visible porosity of ZnO and GO–ZnO, N 2 adsorption–desorption measurements and pore size analysis have been investigated and compared. Comparing to ZnO, GO–ZnO showed larger Brunauer–Emmett–Teller (BET) surface area and enhanced ability on capturing CO 2 at different temperatures. Several cycles of adsorption–desorption experiments on CO 2 have been tested and it proved GO–ZnO to be potential adsorbent material with excellent cycling stability.

  16. Solvothermal synthesis and electrochemical performance of hollow LiFePO{sub 4} nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Zheng, Zhenmiao [School of Chemistry and Chemical Engineering, Central South University, Changsha 410083 (China); Pang, Wei Kong [Institute for Superconducting and Electronic Materials, University of Wollongong, Wollongong, NSW 2522 (Australia); Australian Nuclear Science and Technology Organization, Locked Bag 2001, Kirrawee DC, NSW 2232 (Australia); Tang, Xincun, E-mail: tangxincun@163.com [School of Chemistry and Chemical Engineering, Central South University, Changsha 410083 (China); Jia, Dianzeng; Huang, Yudai [Institute of Applied Chemistry, Xinjiang University, Urumqi 840046 (China); Guo, Zaiping [Institute for Superconducting and Electronic Materials, University of Wollongong, Wollongong, NSW 2522 (Australia)

    2015-08-15

    Highlights: • Hollow LiFePO{sub 4} nanoparticles were successfully synthesized via solvothermal method. • The shorter b lattice parameter allows the shorter diffusion path of lithium ion. • Hollow LiFePO{sub 4} nanoparticles show better rate capability than solid LiFePO{sub 4}. - Abstract: Hollow LiFePO{sub 4} nanoparticles were synthesized via a solvothermal technique, using ammonium tartrate as additive and carbon source, and ethylene glycol/water as solvent. The as-prepared samples were characterized by X-ray diffraction, Fourier-transform infrared spectroscopy, Raman spectroscopy, scanning and transmission electron microscopies, and Brunauer–Emmett–Teller specific surface area measurements. The electrochemical properties of the LiFePO{sub 4} cathode were examined in coin-type cell configuration and the cathode exhibited excellent rate capability (i.e., discharge capacity of 120.9 mA h g{sup −1} at 10 C) and cycling performance (i.e., >98% of capacity retention rate after 50 cycles). It is believed that the enhanced performance is correlated to the hollow structure, small crystallite and particle sizes, and relatively shorter lattice parameter b.

  17. 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.

  18. 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

  19. Surfactant-free solvothermal synthesis of Hydroxyapatite nested bundles for the effective photodegradation of cationic dyes

    Science.gov (United States)

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

    2018-05-01

    In this study, hydroxyapatite nested bundles (HNBs) were successfully constructed from nanosticks as nanoscale building blocks via a facile, solvothermal process without using any surfactant. The fabricated HNBs were structurally analyzed using X-ray diffraction and Fourier transform infrared spectroscopy, which confirmed the purity of the HNBs. The surface characteristics were determined by field emission scanning electron microscopy and Brunauer-Emmett-Teller analysis, and the optical characteristics by ultraviolet (UV)-visible spectroscopy. The synthesized HNBs were tested to determine their activity during the degradation of methylene blue, methylene violet, and rhodamine B via photocatalysis under UV irradiation. The degradation efficiency of HNBs and the rate of degradation can be explained based on the properties of the HNBs and cationic dyes.

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

    Energy Technology Data Exchange (ETDEWEB)

    Chang Xin [Nanomaterials Research Institute, College of Material Science and Technology, Nanjing University of Aeronautics and Astronautics, Nanjing 210016 (China); Cao Jieming [Nanomaterials Research Institute, College of Material Science and Technology, Nanjing University of Aeronautics and Astronautics, Nanjing 210016 (China)]. E-mail: jmcao@nuaa.edu.cn; Ji Hongmei [Nanomaterials Research Institute, College of Material Science and Technology, Nanjing University of Aeronautics and Astronautics, Nanjing 210016 (China); Fang Baoqing [Nanomaterials Research Institute, College of Material Science and Technology, Nanjing University of Aeronautics and Astronautics, Nanjing 210016 (China); Feng Jie [Nanomaterials Research Institute, College of Material Science and Technology, Nanjing University of Aeronautics and Astronautics, Nanjing 210016 (China); Pan Lijia [Nanomaterials Research Institute, College of Material Science and Technology, Nanjing University of Aeronautics and Astronautics, Nanjing 210016 (China); Zhang Fang [Nanomaterials Research Institute, College of Material Science and Technology, Nanjing University of Aeronautics and Astronautics, Nanjing 210016 (China); Wang, Haiyan [Nanomaterials Research Institute, College of Material Science and Technology, Nanjing University of Aeronautics and Astronautics, Nanjing 210016 (China)

    2005-01-15

    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.

  1. 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

  2. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Zhong Shengliang, E-mail: zslxhx@yahoo.com.cn [College of Chemistry and Chemical Engineering, Jiangxi Normal University, Nanchang 330022 (China); Zhang Linfei; Huang Zhenzhong; Wang Shangping [College of Chemistry and Chemical Engineering, Jiangxi Normal University, Nanchang 330022 (China)

    2011-01-15

    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{sub 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.

  4. 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.

  5. Fabrication of mesoporous polymer monolith: a template-free approach.

    Science.gov (United States)

    Okada, Keisuke; Nandi, Mahasweta; Maruyama, Jun; Oka, Tatsuya; Tsujimoto, Takashi; Kondoh, Katsuyoshi; Uyama, Hiroshi

    2011-07-14

    Mesoporous polyacrylonitrile (PAN) monolith has been fabricated by a template-free approach using the unique affinity of PAN towards a water/dimethyl sulfoxide (DMSO) mixture. A newly developed Thermally Induced Phase Separation Technique (TIPS) has been used to obtain the polymer monoliths and their microstructures have been controlled by optimizing the concentration and cooling temperature.

  6. Solvothermal synthesis of Zinc sulfide decorated Graphene (ZnS/G) nanocomposites for novel Supercapacitor electrodes

    International Nuclear Information System (INIS)

    Ramachandran, Rajendran; Saranya, Murugan; Kollu, Pratap; Raghupathy, Bala P.C.; Jeong, Soon Kwan; Grace, Andrews Nirmala

    2015-01-01

    Highlights: • ZnS/G nanocomposites were prepared by a simple solvothermal process. • Electrochemical measurements were carried out in 6 M KOH electrolyte. • Cyclic voltammetry showed the excellent capacitive behavior of the composites. • A specific capacitance of 197.1 F/g was observed for ZnS/G-60 nanocomposites. - Abstract: Zinc sulfide decorated graphene nanocomposites are synthesized by a facile solvothermal approach and the prepared composites are analyzed by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), High Resolution Transmission electron microscopy (HRTEM), Fourier transform infrared (FTIR), Ultraviolet visible spectroscopy (UV), Photoluminescence spectroscopy (PL) and Raman spectrum. Results show the effective reduction of graphene oxide (GO) to graphene and decoration of ZnS nanoparticles on graphene sheets. Towards supercapacitor applications, the electrochemical measurements of different electrodes are performed in 6 M KOH electrolyte. A series of composites with different loadings of graphene is synthesized and tested for its electrochemical properties. The specific capacitance of the electrodes are evaluated from cyclic voltammetry (CV) studies and a maximum specific capacitance of 197.1 F/g is achieved in ZnS/G-60 electrode (60 indicates the weight ratio of GO) at scan rate of 5 mV s"−"1. A capacitance retention of about 94.1% is observed even after 1000 cycles for ZnS/G-60 electrode, suggesting the long time cyclic stability of the composite electrode. Galvanostatic charge–discharge curves show the highly reversible process of ZnS/G-60 electrode. Electrochemical Impedance Spectrum (EIS) shows a high conductivity of composite electrode suggesting that the composites are good candidates for energy storage.

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

    KAUST Repository

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

    2016-01-01

    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.

  8. Solvothermal Synthesis of Zn2SnO4 Nanocrystals and Their Photocatalytic Properties

    Directory of Open Access Journals (Sweden)

    Guang Sun

    2014-01-01

    Full Text Available Crystalline Zn2SnO4 nanoparticles were successfully synthesized via a simple solvothermal route by using Zn(CH3COO2·2H2O and SnCl4·5H2O as source materials, NaOH as mineralizing agent, and water and ethanol as mixed solvents. The used amount of NaOH was found to have an important influence on the formation of Zn2SnO4. When the molar ratio of OH− : Zn2+ : Sn4+ was set in the range from 4 : 2 : 1 to 8 : 2 : 1, Zn2SnO4 nanoparticles with different shape and size were obtained. However, when the molar ratio of OH− : Zn2+ : Sn4+ was set as 10 : 2 : 1, a mixture phase of ZnO and ZnSn(OH6 instead of Zn2SnO4 was obtained. Photodegradation measurements indicated that the Zn2SnO4 nanoparticles own better photocatalytic property to depredate methyl orange than the Zn2SnO4 nanopolyhedrons. The superior photocatalytic properties of Zn2SnO4 nanoparticles may be contributed to their small crystal size and high surface area.

  9. 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 .

  10. 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.

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

    International Nuclear Information System (INIS)

    Wang Huanwen; Hu Zhongai; Chang Yanqin; Chen Yanli; Lei Ziqiang; Zhang Ziyu; Yang Yuying

    2010-01-01

    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 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 -1 (based on composite) is obtained at a specific current of 1 A g -1 as compared with 71 F g -1 for pure graphene. The loaded-bismuth oxide achieves a specific capacitance as high as 757 F g -1 even at 10 A g -1 . In addition, the graphene nanosheet-bismuth oxide composite electrode exhibits the excellent rate capability and well reversibility.

  12. 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

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

    Energy Technology Data Exchange (ETDEWEB)

    Shen, Peng; Zhang, Haitao, E-mail: htzhang@ipe.ac.cn; Zhang, Suojiang, E-mail: sjzhang@ipe.ac.cn; Yuan, Pei [Chinese Academy of Sciences, Beijing Key Laboratory of Ionic Liquids Clean Process Institute of Process Engineering, Key Laboratory of Green Process and Engineering, Institute of Process Engineering (China); Yang, Yang [China Building Materials Academy, State Key Laboratory of Green Building Materials (China); Zhang, Qiang; Zhang, Xixiang [King Abdullah University of Science and Technology, Physical Science and Engineering (Saudi Arabia)

    2016-05-15

    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 m{sup 2}/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.

  14. 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.

  15. Facile solvothermal synthesis of abnormal growth of one-dimensional ZnO nanostructures by ring-opening reaction of polyvinylpyrrolidone

    Energy Technology Data Exchange (ETDEWEB)

    Xu, G., E-mail: gxu@alum.imr.ac.cn; Wang, X.L.; Liu, G.Z.

    2015-02-28

    Graphical abstract: - Highlights: • Facile solvothermal synthesis of ZnO nanostructures in super high alkaline alcoholic condition. • The exact role and chemical transformations of PVP in solvothermal synthesis of ZnO nanostructures was revealed. • Mechanism of abnormal growth of ZnO nanopyramids was proposed based on ring-opening reaction of PVP. - Abstract: Abnormal growth of one-dimensional (1-D) ZnO nanostructures (NSs) have been accomplished with the assistance of polyvinylpyrrolidone (PVP) under a super high alkaline alcoholic solvothermal condition. The products were characterized by transmission electron microscopy (TEM), thermogravimetric analysis (TGA), X-ray diffraction (XRD), Fourier transform infrared (FT-IR) and proton nuclear magnetic resonance ({sup 1}H NMR) spectroscopy. The effect of synthetic conditions, such as reaction temperature and the addition of PVP, on the morphologies of ZnO products were investigated. The results show that PVP molecules had the significant role in the transformation of morphologies of ZnO NSs ranging from nanorods, nanoparticles to pyramids, as well as flower-like assembly features. The possible growth mechanism of ZnO pyramids was proposed based on ring-opening reaction of PVP.

  16. Facile and low temperature route to synthesis of CuS nanostructure in mesoporous material by solvothermal method.

    Science.gov (United States)

    Sohrabnezhad, Sh; Zanjanchi, M A; Hosseingholizadeh, S; Rahnama, R

    2014-04-05

    The synthesis of CuS nanomaterial in MCM-41 matrix has been realized by chemical synthesis between MCM-41, copper sulfate pentahydrate and thiourea via a solvothermal method in ethylene glycol and water, separately. X-ray diffraction analysis (XRD), diffuse reflectance spectroscopy (DRS), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and fourier transform infrared (FT-IR) were used to characterize the products. At synthesized CuS/MCM-41 sample in ethylene glycol, X-ray diffraction and diffuse reflectance spectroscopy showed pure covellite phase of copper sulfide with high crystality. But prepared CuS/MCM-41 sample in water shows the covellite, chalcocite and the djurleite phase of copper sulfide nanostructures. The formation of CuS nanostructures was confirmed by FT-IR. Photocatalytic activity of CuS/MCM-41 nanocomposites was studied for degradation of Methylene Blue (MB) under visible light. The CuS/MCM-41 nanocomposite is more effective nanocatalyst than synthesized CuS/MCM-41 sample in water for degradation of methylene blue. Several parameters were examined, catalyst amount (0.1-1gL(-1)), pH (1-13) and initial concentration of MB (0.96-10ppm). The extent of degradation was estimated from the residual concentration by spectrophotometrically. The support size was obtained in the range 60-145nm by TEM. In the same way, the average size of copper sulfide in CuSMCM-41E and CuS/MCM-41W nanostructures were obtained about 10nm and 16nm, respectively. Copyright © 2013 Elsevier B.V. All rights reserved.

  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. 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.

  19. Solvothermal Synthesis of Fe2O3 Loaded Activated Carbon as Electrode Materials for High-performance Electrochemical Capacitors

    International Nuclear Information System (INIS)

    Li, Ying; Kang, Litao; Bai, Gailing; Li, Peiyang; Deng, Jiachun; Liu, Xuguang; Yang, Yongzhen; Gao, Feng; Liang, Wei

    2014-01-01

    This article describes a facile solvothermal synthesis method to prepare Fe 2 O 3 /AC composites for electrochemical capacitors from Iron (III) chloride hexahydrate (FeCl 3 ·6H 2 O), activated carbon (AC, from petroleum coke), and four different precipitants (i.e., NaOH, CH 3 COONa, HMT, CO(NH 2 ) 2 ). X-ray powder diffraction (XRD), Scanning electron microscopy (SEM), Energy dispersive spectroscopy (EDS) and Thermogravimetric (TG) analysis show that the products consisted of nanosized α-Fe 2 O 3 (weight ratios: 48.1, 47.9, 44.2, 44.3%) loaded onto AC particles (∼ 20 μm). Significantly, both kind and dosage of precipitants exhibit effects on the specific capacitances of Fe 2 O 3 /AC composites. The highest specific capacitance reaches up to 240 F g −1 (at a current density of 1 A g −1 in 6 M KOH aqueous electrolyte) when the molar ratio of CH 3 COONa: FeCl 3 is 9. On the other hand, the sample prepared with NaOH: FeCl 3 molar ratio being 1.5 exhibits excellent rate capability with specific capacitance of 215 F g −1 at 1 A g −1 , and 89.3, 82.3, 78.1, 72.6 and 65.1% capacity retention at 2, 5, 10, 20, and 40 A g −1 , respectively. These electrochemical performances are superior to other materials consisted of Fe 2 O 3 /carbon nanotube (CNT), graphene oxide (GO) or reduced graphene oxide (rGO) composites, demonstrating the great potential of Fe 2 O 3 /AC composites in the development of high-performance electrode materials for electrochemical capacitors

  20. 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.

  1. Template-free synthesis of multifunctional carbonaceous microcone forests

    Science.gov (United States)

    Wang, Qiang; Yang, Lei; Dai, Bing; Bai, Jie; Yang, Zhenhuai; Guo, Shuai; He, Yurong; Han, Jiecai; Zhu, Jiaqi

    2018-01-01

    Forests of vertically aligned carbonaceous microcones are fabricated directly on a nickel mesh by microwave-plasma-assisted chemical vapor deposition. The microstructure is formed through a simple one-step process involving self-assembly. The fabricated composite exhibits superhydrophobicity and superoleophilicity as well as low density, owing to which it floats on water and can be used for the in-situ separation of oil from water at the oil/water interface. Furthermore, the composite exhibits pH responsivity, and its water permeability can be varied simply by altering the pH of the aqueous solution. In addition, the composite is suitable for use as an electrode material for supercapacitors owing to its large geometric surface area, porous structure, and superior electrical properties, which allow for fast ion and electron transportation. Thus, this composite consisting of forests of vertically aligned carbonaceous microcones on a nickel mesh is expected to find use in a wide range of fields and applications, including in environmental cleanup, flow switches, and energy storage devices.

  2. Solvothermal synthesis of nanorods of ZnO, N-doped ZnO and CdO

    International Nuclear Information System (INIS)

    Varghese, Neenu; Panchakarla, L.S.; Hanapi, M.; Govindaraj, A.; Rao, C.N.R.

    2007-01-01

    ZnO nanorods with diameters in the 80-800 nm range are readily synthesized by the reaction of zinc acetate, ethanol and ethylenediamine under solvothermal conditions. The best products are obtained at 330 deg. C with a slow heating rate. Addition of the surfactant Triton -X 100 gave nanorods of uniform (300 nm) diameter. By adding a small amount of liquid NH 3 to the reaction mixture, N-doped ZnO nanorods, with distinct spectroscopic features are obtained. CdO nanorods of 80 nm diameter have been prepared under solvothermal conditions using a mixture of cadmium cupferronate, ethylenediamine and ethanol at 330 deg. C. Similarly, Zn 1-x Cd x O nanorods of a 70 nm diameter are obtained under solvothermal conditions starting with a mixture of zinc acetate, cadmium cupferronate, ethanol and ethylenediamine

  3. 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.

  4. 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.

  5. One-pot, template- and surfactant-free solvothermal synthesis of high-crystalline Fe{sub 3}O{sub 4} nanostructures with adjustable morphologies and high magnetization

    Energy Technology Data Exchange (ETDEWEB)

    Zong, Yan; Xin, Hongna; Zhang, Jiarui [School of Physics, Northwest University, Xi’an 710000 (China); Li, Xinghua, E-mail: lixinghua04@gmail.com [School of Physics, Northwest University, Xi’an 710000 (China); Feng, Juan [School of Physics, Northwest University, Xi’an 710000 (China); Deng, Xia [School of Physical Science and Technology, Lanzhou University, Lanzhou 730000 (China); Sun, Yong [School of Physics, Northwest University, Xi’an 710000 (China); Zheng, Xinliang, E-mail: zhengxl@nwu.edu.cn [School of Physics, Northwest University, Xi’an 710000 (China)

    2017-02-01

    In the present study, high-crystalline and well-defined Fe{sub 3}O{sub 4} nanostructures with tunable morphologies were fabricated through a facile one-pot solvothermal approach. The morphology, crystal structure and chemical compositions of the products were characterized at the nanoscale. X-ray diffraction and selected area electron diffraction patterns indicate that the products have a pure spinel phase without the presence of any other impurity. Based on the transmission electron microscope technology, shape evolution of the products were investigated. Several morphologies including irregular particles, clusters, hollow sphere and octahedrons can be obtained by only adjusting the amount of NaOH without using any surfactant. Magnetism investigations show that all the products perform ferromagnetic behavior with high saturation magnetization at room temperature, which mainly originates from their high crystalline nature and template-free fabrication process. - Highlights: • Fe{sub 3}O{sub 4} were prepared by a template- and surfactant-free solvothermal route. • The shapes of Fe{sub 3}O{sub 4} nanostructures can be controlled by changing the amount of NaOH. • All the Fe{sub 3}O{sub 4} nanostructures with different shapes have high magnetization values.

  6. Solvothermal synthesis of LiFePO4 nanoplates with (010) plane and the uniform carbon coated on their surface by esterification reaction

    International Nuclear Information System (INIS)

    Ma, Zhipeng; Shao, Guangjie; Wang, Xu; Song, Jianjun; Wang, Guiling; Liu, Tingting

    2014-01-01

    A facile solvothermal synthesis and esterification reaction combined with a high temperature calcination technique has been developed to prepare the uniform carbon coating LiFePO 4 nanoplates. The carbon coating LiFePO 4 nanoplates are investigated by X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscope (SEM), transmission electron microscope (TEM), galvanostatic intermittent titration technique (GITT) and galvanostatic charge–discharge test. A reasonable growth mechanism of LiFePO 4 nanoplates is proposed on the basis of time dependent experimental results. The results show that each nanoplate is a LiFePO 4 single crystal with the large (010) plane. According to Raman spectroscopy analysis, carbon is uniformly coated on the surface of LiFePO 4 nanoplates. Electrochemical test results also indicate that the carbon coating LiFePO 4 nanoplates exhibit a high reversible specific capacity of 144.8 mAh g −1 at 0.5 C and 116.9 mAh g −1 under lower discharging rate at −20 °C. - Highlights: • LiFePO 4 nanoplates prepared by facile solvothermal synthesis expose large (010) plane. • The polyester network formed by the esterification reaction could entirely wrap LiFePO 4 . • The polyester wrapped on the surface of LiFePO 4 transformed into the uniform carbon layer after calcination. • LiFePO 4 /C nanoplates have good high-rate and low-temperature performance

  7. 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.

  8. Solvothermal Synthesis of One-Dimensional Transition Metal Doped ZnO Nanocrystals and Their Applications in Smart Window Devices

    OpenAIRE

    Šutka, A; Timusk, M; Kisand, V; Saal, K; Joost, U; Lõhmus, R

    2015-01-01

    Oxide semiconductor nanowire (NW) suspension based devices have been attracted growing interest in smart window applications due to their great controllability of light transmittance, simplicity and long term stability. Recently, we demonstrated smart window device using the suspension of electrospun TiO2 or solvothermally synthesized ZnO NWs in viscous polydimethylsiloxane (PDMS) matrix. The operating principle of the oxide semiconductor NW and PDMS device is based on the alterable orientati...

  9. 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.

  10. 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.

  11. 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.

  12. Surfactant-ligand co-assisted solvothermal technique for the synthesis of different-shaped CdS nanorod-based materials

    International Nuclear Information System (INIS)

    Bao Chunyan; Jin Ming; Lu Ran; Xue Pengchong; Zhang Qinglin; Wang Dejun; Zhao Yingying

    2003-01-01

    1-D nanorods, twinrods, golfclubs, and tripods of CdS were prepared via a surfactant-ligand co-assisted solvothermal method at 160 deg. C. The surfactant of S-dodecylisothiounium bromide (C 12 ) used in the process was favorable for synthesis of different-shaped CdS nanorod with high aspect ratio. X-ray diffraction (XRD) and TEM images showed that the 1-D nanorods had wurtzite phase and others had a zinc blende core and wurtzite arms. The morphologies of CdS prepared under different conditions suggested the 'template-assistance' of the surfactant and that the nonaqueous organic media are important for the self-assembling of inorganic components at atomic level

  13. 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.

  14. Solvothermal synthesis and high optical performance of three-dimensional sea-urchin-like TiO2

    International Nuclear Information System (INIS)

    Zhou, Yi; Wang, Yutang; Li, Mengyao; Li, Xuzhi; Yi, Qin; Deng, Pan; Wu, Hongyan

    2015-01-01

    Graphical abstract: I–V characteristics of different TiO 2 microspheres based DSSCs (a) 3D sphere-like, (b) 3D flower-like, (c) 3D sea-urchin-like. - Highlights: • 3D sea-urchin-like TiO 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 2 were studied upon DSSCs. • The PCE of the 3D sea-urchin-like TiO 2 was higher than that of other morphologies. - Abstract: Three-dimensional (3D) sea-urchin-like TiO 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 2 . In addition, when the sea-urchin-like TiO 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 2 nanostructures

  15. Solvothermal synthesis of uranium(VI) phases with aromatic carboxylate ligands: A dinuclear complex with 4-hydroxybenzoic acid and a 3D framework with terephthalic acid

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Yingjie, E-mail: yzx@ansto.gov.au [Australian Nuclear Science and Technology Organisation, Locked Bag 2001, Kirrawee DC, NSW 2232 (Australia); Karatchevtseva, Inna [Australian Nuclear Science and Technology Organisation, Locked Bag 2001, Kirrawee DC, NSW 2232 (Australia); Bhadbhade, Mohan [Mark Wainwright Analytical Centre, University of New South Wales, Kensington, NSW 2052 (Australia); Tran, Toan Trong; Aharonovich, Igor [School of Physics and Advanced Materials, University of Technology Sydney, Ultimo, NSW 2007 (Australia); Fanna, Daniel J.; Shepherd, Nicholas D. [School of Science and Health, Western Sydney University, Locked Bag 1797, Penrith, NSW 2751 (Australia); Lu, Kim [Australian Nuclear Science and Technology Organisation, Locked Bag 2001, Kirrawee DC, NSW 2232 (Australia); Li, Feng [School of Science and Health, Western Sydney University, Locked Bag 1797, Penrith, NSW 2751 (Australia); Lumpkin, Gregory R. [Australian Nuclear Science and Technology Organisation, Locked Bag 2001, Kirrawee DC, NSW 2232 (Australia)

    2016-02-15

    With the coordination of dimethylformamide (DMF), two new uranium(VI) complexes with either 4-hydroxybenzoic acid (H{sub 2}phb) or terephthalic acid (H{sub 2}tph) have been synthesized under solvothermal conditions and structurally characterized. [(UO{sub 2}){sub 2}(Hphb){sub 2}(phb)(DMF)(H{sub 2}O){sub 3}]·4H{sub 2}O (1) has a dinuclear structure constructed with both pentagonal and hexagonal bipyramidal uranium polyhedra linked through a µ{sub 2}-bridging ligand via both chelating carboxylate arm and alcohol oxygen bonding, first observation of such a coordination mode of 4-hydroxybenzoate for 5 f ions. [(UO{sub 2})(tph)(DMF)] (2) has a three-dimensional (3D) framework built with pentagonal bipyramidal uranium polyhedra linked with µ{sub 4}-terephthalate ligands. The 3D channeled structure is facilitated by the unique carboxylate bonding with nearly linear C–O–U angles and the coordination of DMF molecules. The presence of phb ligands in different coordination modes, uranyl ions in diverse environments and DMF in complex 1, and tph ligand, DMF and uranyl ion in complex 2 has been confirmed by Raman spectroscopy. In addition, their thermal stability and photoluminescence properties have been investigated. - Graphical abstract: With the coordination of dimethylformamide, two new uranyl complexes with either 4-hydroxybenzoate or terephthalate have been synthesized under solvothermal conditions and structurally characterized. - Highlights: • Solvent facilitates the synthesis of two new uranium(VI) complexes. • A dinuclear complex with both penta- and hexagonal bipyramidal uranium polyhedral. • A unique µ{sub 2}-bridging mode of 4-hydroxybenzoate via alcohol oxygen for 5 f ions. • A 3D framework with uranium polyhedra and µ{sub 4}-terephthalate ligands. • Vibration modes and photoluminescence properties are reported.

  16. 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.

  17. 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.

  18. Shape-Evolution Control of hybrid perovskite CH3NH3PbI3 crystals via solvothermal synthesis

    Science.gov (United States)

    Zhang, Baohua; Guo, Fuqiang; Yang, Lianhong; Jia, Xiuling; Liu, Bin; Xie, Zili; Chen, Dunjun; Lu, Hai; Zhang, Rong; Zheng, Youdou

    2017-02-01

    We systematically synthesized CH3NH3PbI3 crystals using solvothermal process, and the reaction conditions such as concentration of the precursor, temperature, time, and lead source have been comprehensively investigated to obtain shape-controlled CH3NH3PbI3 crystals. The results showed that the CH3NH3PbI3 crystals exhibit tetragonal phase and the crystals change from nanoparticles to hopper-faced cuboids. Photoluminescence spectra of the crystals obtained with different lead sources show a blue shift due to the presence of defects in the crystals, and the peak intensity is very sensitive to the lead sources. Moreover, impurities (undesirable byproducts and excess components like HI or CH3NH2) presented during crystal growth can result in hopper growth.

  19. Solvothermal synthesis of graphene-Sb2S3 composite and the degradation activity under visible light

    International Nuclear Information System (INIS)

    Tao, Wenguang; Chang, Jiuli; Wu, Dapeng; Gao, Zhiyong; Duan, Xiaoli; Xu, Fang; Jiang, Kai

    2013-01-01

    Graphical abstract: Display Omitted Highlights: ► Graphene-Sb 2 S 3 composites were synthesized through a facile solvothermal method. ► Hydroxyl radicals are the main species responsible for the photodegradation activity. ► Graphene-Sb 2 S 3 demonstrated dramatically improved visible light degradation activity. -- Abstract: Novel graphene-Sb 2 S 3 (G-Sb 2 S 3 ) composites were synthesized via a facile solvothermal method with graphene oxide (GO), SbCl 3 and thiourea as the reactants. GO played an important role in controlling the size and the distribution of the formed Sb 2 S 3 nanoparticles on the graphene sheets with different density. Due to the negative surface charge, smaller Sb 2 S 3 particles size and efficient electrons transfer from Sb 2 S 3 to graphene, the composites demonstrated improved photodegradation activity on rhodamine B (RhB). Among these composites, the product G-Sb 2 S 3 0.1, which was synthesized with the GO concentration of 0.1 mg/mL, exhibited the highest photodegradation activity owing to the considerable density of Sb 2 S 3 nanoparticles onto graphene sheet free of aggregation. Hydroxyl radicals (·OH) derived from conduction band (CB) electrons of Sb 2 S 3 is suggested to be responsible for the photodegradation of RhB. The high visible light degradation activity and the satisfactory cycling stability made the as-prepared G-Sb 2 S 3 0.1 an applicable photocatalyst.

  20. Facile solvothermal synthesis of highly active and robust Pd1.87Cu0.11Sn electrocatalyst towards direct ethanol fuel cell applications

    Science.gov (United States)

    Jana, Rajkumar; Dhiman, Shikha; Peter, Sebastian C.

    2016-08-01

    Ordered intermetallic Pd1.87Cu0.11Sn ternary electrocatalyst has been synthesized by sodium borohydride reduction of precursor salts Pd(acac)2, CuCl2.2H2O and SnCl2 using one-pot solvothermal synthesis method at 220 °C with a reaction time of 24 h. To the best of our knowledge, here for the first time we report surfactant free synthesis of a novel ordered intermetallic ternary Pd1.87Cu0.11Sn nanoparticles. The ordered structure of the catalyst has been confirmed by powder x-ray diffraction, transmission electron microscopy (TEM). Composition and morphology of the nanoparticles have been confirmed through field emission scanning electron microscopy, energy-dispersive spectrometry and TEM. The electrocatalytic activity and stability of the ternary electrocatalyst towards ethanol oxidation in alkaline medium was investigated by cyclic voltammetry and chronoamperometry techniques. The catalyst is proved to be highly efficient and stable upto 500th cycle and even better than commercially available Pd/C (20 wt%) electrocatalysts. The specific and mass activity of the as synthesized ternary catalyst are found to be ∼4.76 and ∼2.9 times better than that of commercial Pd/C. The enhanced activity and stability of the ordered ternary Pd1.87Cu0.11Sn catalyst can make it as a promising candidate for the alkaline direct ethanol fuel cell application.

  1. 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 .

  2. Solvothermal synthesis of carbon coated N-doped TiO{sub 2} nanostructures with enhanced visible light catalytic activity

    Energy Technology Data Exchange (ETDEWEB)

    Yan Xuemin, E-mail: yanzhangmm2002@163.com [College of Chemistry and Environmental Engineering, Yangtze University, Jingzhou 434023 (China); Kang Jialing; Gao Lin; Xiong Lin; Mei Ping [College of Chemistry and Environmental Engineering, Yangtze University, Jingzhou 434023 (China)

    2013-01-15

    Highlights: Black-Right-Pointing-Pointer Chitosan was used as carbon and nitrogen resource to modify TiO{sub 2} nanostructure. Black-Right-Pointing-Pointer Nanocomposites with mesostructure were obtained by one-step solvothermal method. Black-Right-Pointing-Pointer Carbon species were modified on the surface of TiO{sub 2}. Black-Right-Pointing-Pointer Nitrogen was doped into the anatase titania lattice. Black-Right-Pointing-Pointer CTS-TiO{sub 2} nanocomposites show superior visible light photocatalytic activity. - Abstract: Visible light-active carbon coated N-doped TiO{sub 2} nanostructures(CTS-TiO{sub 2}) were prepared by a facile one-step solvothermal method with chitosan as carbon and nitrogen resource at 180 Degree-Sign C. The as-prepared samples were characterized by transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), N{sub 2} adsorption-desorption analysis, X-ray photoelectron spectroscopy (XPS), and ultraviolet-visible (UV-vis) diffuse reflectance spectroscopy. The CTS-TiO{sub 2} nanocomposites possess anatase phase of nanocrystalline structure with average particle size of about 5-7 nm. A wormhole mesostructure can be observed in the CTS-TiO{sub 2} nanocomposites due to the constituent agglomerated of nanoparticles. It has been evidenced that the nitrogen was doped into the anatase titania lattice and the carbon species were modified on the surface of TiO{sub 2}. The photocatalytic activities of the as-prepared photocatalysts were measured by the degradation of methylene blue (MB) under visible light irradiation at {lambda} {>=} 400 nm. The results show that CTS-TiO{sub 2} nanostructures display a higher visible light photocatalytic activity than pure TiO{sub 2}, commercial P25 and C-coated TiO{sub 2} (C-TiO{sub 2}) photocatalysts. The higher photocatalytic activity could be attributed to the band-gap narrowed by N-doping and the accelerated separation of the photo-generated electrons

  3. 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.

  4. 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%.

  5. Solvothermal synthesis of Zn1−xMnxO nanoparticles using oxalate precursor route: Optical and magnetic properties

    Directory of Open Access Journals (Sweden)

    Tokeer Ahmad

    2017-05-01

    Full Text Available Nanoparticles of Zn1−xMnxO (x = 0.022, 0.061 and 0.098 were synthesized by a modified solvothermal method through the oxalate precursor route. The precursors were characterized by TG/DTA analysis. Their kinetics has also been studied using the Freeman and Carroll method. The prepared oxide nanoparticles were investigated by powder X-ray diffraction (PXRD, transmission electron microscopy (TEM, optical and BET surface area studies. PXRD patterns were matched with hexagonal ZnO structure, however few impurity peaks of ZnMnO3 appeared. Reflectance measurements showed that Mn2+ is incorporated in the Zn matrix. The band gap decreases on increasing Mn concentration. The particle size decreases from 18 to 9 nm and the surface area increases (255.4–582.9 m2g−1 on increasing Mn concentration. All these solid solutions show paramagnetic behaviour with very weak antiferromagnetic interactions. The effective magnetic moment of these nanoparticles comes out to be 4.91, 4.77 and 4.18 μB/Mn2+.

  6. Solvothermal Synthesis of Hierarchical Colloidal Nanocrystal Assemblies of ZnFe2O4 and Their Application in Water Treatment

    Directory of Open Access Journals (Sweden)

    Peizhi Guo

    2016-09-01

    Full Text Available Hierarchical colloidal nanocrystal assemblies (CNAs of ZnFe2O4 have been synthesized controllably by a solvothermal method. Hollow ZnFe2O4 spheres can be formed with the volume ratios of ethylene glycol to ethanol of 1:4 in the starting systems, while solid ZnFe2O4 CNAs are obtained by adjusting the volume proportion of ethylene glycol to ethanol from 1:2 to 2:1. Magnetometric measurement data showed that the ZnFe2O4 CNAs obtained with the volume ratios of 1:2 and 1:1 exhibited weak ferromagnetic behavior with high saturation magnetization values of 60.4 and 60.3 emu·g−1, respectively. However, hollow spheres showed a saturation magnetization value of 52.0 emu·g−1, but the highest coercivity among all the samples. It was found that hollow spheres displayed the best ability to adsorb Congo red dye among all the CNAs. The formation mechanisms of ZnFe2O4 CNAs, as well as the relationship between their structure, crystallite size, and properties were discussed based on the experimental results.

  7. Solvothermal Synthesis of Hierarchical Colloidal Nanocrystal Assemblies of ZnFe₂O₄ and Their Application in Water Treatment.

    Science.gov (United States)

    Guo, Peizhi; Lv, Meng; Han, Guangting; Wen, Changna; Wang, Qianbin; Li, Hongliang; Zhao, Xiusong

    2016-09-29

    Hierarchical colloidal nanocrystal assemblies (CNAs) of ZnFe₂O₄ have been synthesized controllably by a solvothermal method. Hollow ZnFe₂O₄ spheres can be formed with the volume ratios of ethylene glycol to ethanol of 1:4 in the starting systems, while solid ZnFe₂O₄ CNAs are obtained by adjusting the volume proportion of ethylene glycol to ethanol from 1:2 to 2:1. Magnetometric measurement data showed that the ZnFe₂O₄ CNAs obtained with the volume ratios of 1:2 and 1:1 exhibited weak ferromagnetic behavior with high saturation magnetization values of 60.4 and 60.3 emu·g -1 , respectively. However, hollow spheres showed a saturation magnetization value of 52.0 emu·g -1 , but the highest coercivity among all the samples. It was found that hollow spheres displayed the best ability to adsorb Congo red dye among all the CNAs. The formation mechanisms of ZnFe₂O₄ CNAs, as well as the relationship between their structure, crystallite size, and properties were discussed based on the experimental results.

  8. Solvothermal synthesis of TiO2 nanocrystals with {001} facets using titanic acid nanobelts for superior photocatalytic activity

    Science.gov (United States)

    Cao, Yuhui; Zong, Lanlan; Li, Qiuye; Li, Chen; Li, Junli; Yang, Jianjun

    2017-01-01

    Anatase TiO2 nanocrystals exposed with {001} facets were fabricated by solvothermal strategy in HF-C4H9OH 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- is easily adsorbed on the surface of the nanobelts, inducing a higher exposure of {001} facet of TiO2 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, N2 adsorption-desorption isotherms, X-ray diffraction, Raman spectroscopy, and X-ray photoelectron spectroscope. The photocatalytic measurement showed that TiO2 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.

  9. Synthesis and Piezoelectric Properties of Li, Ca and Mn-codoped BaTiO3 by a Solvothermal Approach

    International Nuclear Information System (INIS)

    Kimura, T; Dong, Q; Yin, S; Sato, T; Hashimoto, T; Sasaki, A; Aisawa, S

    2013-01-01

    3 at.% Li-doped (Ba 1-x Ca x )(Ti 1-y Mn y )O 3 particles with the Ca 2+ mole fraction, x, of 0–0.09 and Mn mole fraction, y, of 0 and 0.0005 were synthesized by a solvothermal approach at 200°C. The products consisted of nanoparticles of 50–100 nm in diameter, and did not change very much depending on the amount of Li, Ca and Mn-codoping. The change in relative dielectric constant, Δε r , in around room temperature decreased by doping Ca 2+ , and the lowest Δε r (4.51%) could be realized at x value of 0.03. The mechanical quality factor, Q m , of 3 at.% Li-doped (Ba 0.97 Ca 0.03 )(Ti 0.9995 Mn 0.0005 )O 3 increased to 521, and Δε r decreased to 1.72%, while the piezoelectric constant, d 33 (234pC/N), and electromechanical coupling factor, k p (40.0%), did not change very much compared with 3 at.% Li-doped BaTiO 3

  10. 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

  11. Solvothermal synthesis of InP quantum dots and their enhanced luminescent efficiency by post-synthetic treatments.

    Science.gov (United States)

    Byun, Ho-June; Lee, Ju Chul; Yang, Heesun

    2011-03-01

    InP quantum dots (QDs) were solvothermally synthesized by using a greener phosphorus source of P(N(CH(3))(2))(3) instead of highly toxic P(TMS)(3) widely used, and subsequently subjected to a size-sorting processing. While as-grown QDs showed an undetectably low emission intensity, post-synthetic treatments such as photo-etching, photo-radiation, and photo-assisted ZnS shell coating gave rise to a substantial increase in emission efficiency due to the effective removal and passivation of surface states. The emission efficiency of the photo-etched QDs was further enhanced by a consecutive UV photo-radiation, attributable to the photo-oxidation at QD surface. Furthermore, a relatively thick ZnS shell on the surface of InP QDs that were surface-modified with hydrophilic ligands beforehand was photochemically generated in an aqueous solution at room temperature. The resulting InP/ZnS core/shell QDs, emitting from blue to red wavelengths, were more efficient than the above photo-treated InP QDs, and their luminescent properties (emission bandwidth and quantum yield) were comparable to those of InP QDs synthesized with P(TMS)(3). Structural, size, and compositional analyses on InP/ZnS QDs were also conducted to elucidate their core/shell structure. Copyright © 2010 Elsevier Inc. All rights reserved.

  12. 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.

  13. 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

  14. 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 The preparation of metal nanoparticles (Pd, Ni, Sn) supported on sulfonated multi-walled carbon nanotubes (SF-MWCNTs) using a very rapid microwave-assisted solvothermal strategy has been described. Electrocatalytic behaviour of the SF...

  15. Template-free electrochemical nanofabrication of polyaniline nanobrush and hybrid polyaniline with carbon nanohorns for supercapacitors

    Energy Technology Data Exchange (ETDEWEB)

    Wei Di; Andrew, Piers; Ryhaenen, Tapani [Nokia Research Centre Cambridge, Broers Building, 21 J J Thomson Avenue, Cambridge CB3 0FA (United Kingdom); Wang, Haolan; Hiralal, Pritesh; Amaratunga, Gehan A J [Electrical Engineering Division, Department of Engineering, University of Cambridge, 9 J J Thomson Avenue, Cambridge CB3 0FA (United Kingdom); Hayashi, Yasuhiko, E-mail: di.wei@nokia.com, E-mail: gaja1@cam.ac.uk [Department of Materials Science, Nagoya Institute of Technology, Nagoya 466-8555 (Japan)

    2010-10-29

    Polyaniline (PANI) nanobrushes were synthesized by template-free electrochemical galvanostatic methods. When the same method was applied to the carbon nanohorn (CNH) solution containing aniline monomers, a hybrid nanostructure containing PANI and CNHs was enabled after electropolymerization. This is the first report on the template-free method to make PANI nanobrushes and homogeneous hybrid soft matter (PANI) with carbon nanoparticles. Raman spectroscopy was used to analyze the interaction between CNH and PANI. Electrochemical nanofabrication offers simplicity and good control when used to make electronic devices. Both of these materials were applied in supercapacitors and an improvement capacitive current by using the hybrid material was observed.

  16. Template-free electrochemical nanofabrication of polyaniline nanobrush and hybrid polyaniline with carbon nanohorns for supercapacitors

    Science.gov (United States)

    Wei, Di; Wang, Haolan; Hiralal, Pritesh; Andrew, Piers; Ryhänen, Tapani; Hayashi, Yasuhiko; Amaratunga, Gehan A. J.

    2010-10-01

    Polyaniline (PANI) nanobrushes were synthesized by template-free electrochemical galvanostatic methods. When the same method was applied to the carbon nanohorn (CNH) solution containing aniline monomers, a hybrid nanostructure containing PANI and CNHs was enabled after electropolymerization. This is the first report on the template-free method to make PANI nanobrushes and homogeneous hybrid soft matter (PANI) with carbon nanoparticles. Raman spectroscopy was used to analyze the interaction between CNH and PANI. Electrochemical nanofabrication offers simplicity and good control when used to make electronic devices. Both of these materials were applied in supercapacitors and an improvement capacitive current by using the hybrid material was observed.

  17. 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.

  18. 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.

  19. 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

  20. Phase controlled solvothermal synthesis of Cu_2ZnSnS_4, Cu_2ZnSn(S,Se)_4 and Cu_2ZnSnSe_4 Nanocrystals: The effect of Se and S sources on phase purity

    International Nuclear Information System (INIS)

    Pal, Mou; Mathews, N.R.; Paraguay-Delgado, F.; Mathew, X.

    2015-01-01

    In this study, we have reported the synthesis of Cu_2ZnSnSe_4 (CZTSe), Cu_2ZnSnS_4 (CZTS) and Cu_2ZnSn(S,Se)_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_3(CH_2)_1_1SH)/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.

  1. Key insights on the structural characterization of textured Er2O3–ZrO2 nano-oxides prepared by a surfactant-free solvothermal route

    International Nuclear Information System (INIS)

    Julián-López, Beatriz; Luz, Verónica de la; Gonell, Francisco; Cordoncillo, Eloisa; López-Haro, Miguel; Calvino, Jose J.; Escribano, Purificación

    2012-01-01

    Highlights: ► Structural resolution of fluorite vs. pyrochlore in small nanocrystals. ► Simple template-free solvothermal synthesis of Er 2 O 3 –ZrO 2 nanooxides. ► Good control over size, morphology and surface properties (280 m 2 g −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 2 O 3 –ZrO 2 oxide. The material was prepared by a simple template-free solvothermal route that provided nanocrystalline powders at low temperature (170 °C) with spherical morphology, and high surface area (∼280 m 2 g −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 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 that the material is constituted, irrespective of the temperature of the final calcination step, by an ensemble of randomly

  2. Tin phosphide-based anodes for sodium-ion batteries: synthesis via solvothermal transformation of Sn metal and phase-dependent Na storage performance

    Science.gov (United States)

    Shin, Hyun-Seop; Jung, Kyu-Nam; Jo, Yong Nam; Park, Min-Sik; Kim, Hansung; Lee, Jong-Won

    2016-01-01

    There is a great deal of current interest in the development of rechargeable sodium (Na)-ion batteries (SIBs) for low-cost, large-scale stationary energy storage systems. For the commercial success of this technology, significant progress should be made in developing robust anode (negative electrode) materials with high capacity and long cycle life. Sn-P compounds are considered promising anode materials that have considerable potential to meet the required performance of SIBs, and they have been typically prepared by high-energy mechanical milling. Here, we report Sn-P-based anodes synthesised through solvothermal transformation of Sn metal and their electrochemical Na storage properties. The temperature and time period used for solvothermal treatment play a crucial role in determining the phase, microstructure, and composition of the Sn-P compound and thus its electrochemical performance. The Sn-P compound prepared under an optimised solvothermal condition shows excellent electrochemical performance as an SIB anode, as evidenced by a high reversible capacity of ~560 mAh g−1 at a current density of 100 mA g−1 and cycling stability for 100 cycles. The solvothermal route provides an effective approach to synthesising Sn-P anodes with controlled phases and compositions, thus tailoring their Na storage behaviour. PMID:27189834

  3. 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

  4. 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.

  5. 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.

  6. 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.

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

    OpenAIRE

    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 increas...

  8. One-pot solvothermal synthesis of highly efficient, daylight active and recyclable Ag/AgBr coupled photocatalysts with synergistic dual photoexcitation

    International Nuclear Information System (INIS)

    Zhang, Caihong; Ai, Lunhong; Li, Lili; Jiang, Jing

    2014-01-01

    Highlights: • Ag/AgBr photocatalysts were controllably synthesized by solvothermal process. • Ag/AgBr composites showed excellent daylight driven photocatalytic activity. • The remarkable activity is attributed to the synergistic dual photoexcitation. -- Abstract: Efficient light harvesting has been considered to be critical for manipulating the photocatalytic behavior of photocatalysts, because it directly determines the generation of reactive redox charge carriers involved in photoreaction process. In this study, we present a successful example on efficient conversion of solar energy by Ag/AgBr coupled photocatalysts that hold unique synergistic dual photoexcitation. A series of Ag/AgBr coupled photocatalysts were controllably synthesized by an easily manipulated mild solvothermal process. The physicochemical properties of the as-prepared Ag/AgBr coupled photocatalysts were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray energy dispersive spectroscopy (EDS) and UV–vis diffuse reflectance spectroscopy (DRS). The results showed the solvothermal reaction time played key role for control of crystalline structure, morphology, composition, and visible light absorption ability of the resulting photocatalysts. The as-prepared Ag/AgBr coupled photocatalysts exhibited remarkable photocatalytic performance and good reusability for decomposing organic dyes in aqueous solution under the irradiation of commercial 20 W cool daylight fluorescent lamp, owing to the synergistic dual photoexcitation cooperating between plasmonic Ag nanoparticles and narrow-band-gap AgBr

  9. Scaled-up solvothermal synthesis of nanosized metastable indium oxyhydroxide (InOOH) and corundum-type rhombohedral indium oxide (rh-In{sub 2}O{sub 3})

    Energy Technology Data Exchange (ETDEWEB)

    Schlicker, Lukas; Bekheet, Maged F.; Gurlo, Aleksander [Technische Univ. Berlin (Germany). Fachgebiet Keramische Werkstoffe

    2017-03-01

    Phase pure metastable indium oxyhydroxide (InOOH) with crystallite size in the range ca. 2-7 nm is synthesized by a nonaqueous solvothermal synthesis route in ethanol. The influence of synthesis parameters such as temperature, basicity (pH), synthesis time, and water content is carefully addressed. T-pH maps summarize the impact of synthesis temperature and pH and reveal that phase pure InOOH is obtained in water-free solutions at mild temperatures (150-180 C) in highly basic conditions (pH>12). Subsequent calcination of InOOH at 375-700 C in ambient air atmosphere results in metastable nanoscaled rhombohedral indium oxide (rh-In{sub 2}O{sub 3}). The synthesis protocol for phase pure nanocrystalline InOOH material was successfully upscaled allowing for obtaining ca. 3 g of phase-pure InOOH with a yield of ca. 78%. The upscaled InOOH and rh-In{sub 2}O{sub 3} batches are now available for a detailed in-situ characterization of the mechanism of decomposition of InOOH to rh-In{sub 2}O{sub 3} to c-In{sub 2}O{sub 3} as well as for the characterization of the functional properties of InOOH and rh-In{sub 2}O{sub 3} materials.

  10. 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.

  11. Annealing-free synthesis of C-N co-doped TiO{sub 2} hierarchical spheres by using amine agents via microwave-assisted solvothermal method and their photocatalytic activities

    Energy Technology Data Exchange (ETDEWEB)

    Wu, Yu-Chun, E-mail: yuchunwu@mail.ncku.edu.tw; Ju, Lung-Shen

    2014-08-01

    Highlights: • The synthesis method for C-N co-doped TiO{sub 2} hierarchical spheres is proposed. • Microwave-assisted solvothermal method is applied. • C and N are doped into TiO{sub 2} via a direct chelating reaction of amine compounds. • The photodegradation rate is eightfold higher than the commercial P25 powders. - Abstract: The annealing-free synthesis of C-N co-doped TiO{sub 2} hierarchical spheres is proposed in this study. C and N were doped into the TiO{sub 2} structure via a direct chelating process to the Ti-precursor by using different amine agents, including hexadecylamine (HDA), diethylamine (DEA), trimethylamine (TMA), and diethylenetriamine (DETA). C-N co-doped TiO{sub 2} spheres (300 nm to 500 nm) composed of nanoparticles approximately 11 nm to 13 nm in size were obtained via an efficient microwave-assisted solvothermal reaction at 190 °C for 60 min. The effects of C and N doping by using different amine compounds on the bandgap energy and photocatalytic performance of TiO{sub 2} were investigated. Among the amine compounds, DETA provided the highest chelating efficiency because it provides two primary amine groups, which resulted in the highest C and N doping concentrations and the largest degree of bandgap narrowing (2.77 eV); nevertheless, the high chelating ratio of C and N restrained the crystallization of TiO{sub 2} and considerably decreased its photocatalytic activity. The use of TMA produced optimal C and N doping concentrations, which effectively reduced the bandgap of TiO{sub 2} to 2.85 eV without affecting its crystallization. Its photodecomposition activity to rhodamine B was eightfold of that of commercial Degussa P25 powders under visible light irradiation.

  12. 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

  13. 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

  14. Heterometallic clusters arising from cubic Ni3M'O4 (M'=K and Na) entity: Solvothermal synthesis with/without the assistance of microwave

    International Nuclear Information System (INIS)

    Zhang Shuhua; Zhou Yanling; Sun Xiaojun; Wei, Lian-Qiang; Zeng Minghua; Liang Hong

    2009-01-01

    Solvothermal reaction assisted with microwave leads to the formation of two unique heterometallic cubic clusters [Ni 3 M'(L) 3 (OH)(CH 3 CN) 3 ] 2 .CH 3 CN (M'=K for 1 and M'=Na for 2, where L is an anion of 2-[(2-hydroxy-3-methoxy-benzylidene)-amino]-ethanesulfonate) with higher efficiency, yields and purity than those without it. The 6-metallacrown-3 [Ni 3 (OH)(L) 3 ] - groups exhibit interesting ion trapping and self-assembly of size-different Na + and K + through form recognition and coordination activity in 1 and 2. The magnetic studies for 1 and 2 suggest that the {Ni 3 M'O 4 } (M'=K and Na) cores both display dominant ferromagnetic interactions from the nature of the binding modes of μ 3 -O (oxidophenyl) and μ 3 -OH. - Graphical abstract: Solvothermal reaction assisted with microwave leads to two heterometallic cubic clusters with 6-metallacrown-3 structure [Ni 3 O 3 (OH)] - acting as a host for a K + or Na + ion. The {Ni 3 M'O 4 } (M'=K, Na) cores display dominant ferromagnetic interactions.

  15. 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.

  16. Solvothermal synthesis, characterization and optical properties of ZnO, ZnO-MgO and ZnO-NiO, mixed oxide nanoparticles

    International Nuclear Information System (INIS)

    Aslani, Alireza; Arefi, Mohammad Reza; Babapoor, Aziz; Amiri, Asghar; Beyki-Shuraki, Khalil

    2011-01-01

    ZnO-MgO and ZnO-NiO mixed oxides nanoparticles were produced from a solution containing Zinc acetate, Mg and Ni nitrate by Solvothermal method. The calcination process of the ZnO-MgO and ZnO-NiO composites nanoparticles brought forth polycrystalline two-phase ZnO-MgO and ZnO-NiO nanoparticles of 40-80 nm in diameters. ZnO, MgO and NiO were crystallized into wuertzite and rock salt structures, respectively. The optical properties of ZnO-MgO and ZnO-NiO nanoparticles were obtained by solid state UV and solid state florescent. The XRD, SEM and Raman spectroscopies of these nanoparticles were analyzed.

  17. Solvothermal synthesis, characterization and optical properties of ZnO, ZnO-MgO and ZnO-NiO, mixed oxide nanoparticles

    Science.gov (United States)

    Aslani, Alireza; Arefi, Mohammad Reza; Babapoor, Aziz; Amiri, Asghar; Beyki-Shuraki, Khalil

    2011-03-01

    ZnO-MgO and ZnO-NiO mixed oxides nanoparticles were produced from a solution containing Zinc acetate, Mg and Ni nitrate by Solvothermal method. The calcination process of the ZnO-MgO and ZnO-NiO composites nanoparticles brought forth polycrystalline two-phase ZnO-MgO and ZnO-NiO nanoparticles of 40-80 nm in diameters. ZnO, MgO and NiO were crystallized into würtzite and rock salt structures, respectively. The optical properties of ZnO-MgO and ZnO-NiO nanoparticles were obtained by solid state UV and solid state florescent. The XRD, SEM and Raman spectroscopies of these nanoparticles were analyzed.

  18. Solvothermal synthesis, characterization and optical properties of ZnO, ZnO-MgO and ZnO-NiO, mixed oxide nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Aslani, Alireza, E-mail: a.aslani@vru.ac.ir [Department of Chemistry, Faculty of Science, Vali-E-Asr University of Rafsanjan, Rafsanjan, PO Box: 77176 (Iran, Islamic Republic of); Arefi, Mohammad Reza [Islamic Azad University, Yazd Brunch, Young researchers Club, Yazd (Iran, Islamic Republic of); Babapoor, Aziz [Department of Chemical Engineering, Ahar Branch, Islamic Azad University, Ahar, PO Box: 54516 (Iran, Islamic Republic of); Amiri, Asghar; Beyki-Shuraki, Khalil [Department of Chemistry, Faculty of Science, Vali-E-Asr University of Rafsanjan, Rafsanjan, PO Box: 77176 (Iran, Islamic Republic of)

    2011-03-15

    ZnO-MgO and ZnO-NiO mixed oxides nanoparticles were produced from a solution containing Zinc acetate, Mg and Ni nitrate by Solvothermal method. The calcination process of the ZnO-MgO and ZnO-NiO composites nanoparticles brought forth polycrystalline two-phase ZnO-MgO and ZnO-NiO nanoparticles of 40-80 nm in diameters. ZnO, MgO and NiO were crystallized into wuertzite and rock salt structures, respectively. The optical properties of ZnO-MgO and ZnO-NiO nanoparticles were obtained by solid state UV and solid state florescent. The XRD, SEM and Raman spectroscopies of these nanoparticles were analyzed.

  19. Large scale solvothermal synthesis and a strategy to obtain stable Langmuir–Blodgett film of CoFe{sub 2}O{sub 4} nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Thampi, Arya; Babu, Keerthi; Verma, Seema, E-mail: sa.verma@iiserpune.ac.in

    2013-07-05

    Highlights: • Large scale, monodisperse CoFe{sub 2}O{sub 4} nanoparticles by solvothermal route. • LB technique to obtain stable film of CoFe{sub 2}O{sub 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{sub 2}O{sub 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{sub 2}O{sub 4} nanoparticles is reported for a surface pressure more than 15 mN/m.

  20. 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.

  1. Solvothermal synthesis of size-tunable ZnFe{sub 2}O{sub 4} colloidal nanocrystal assemblies and their electrocatalytic activity towards hydrogen peroxide

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Ruirui, E-mail: liurui1114@outlook.com; Lv, Meng, E-mail: lm199133@126.com; Wang, Qianbin, E-mail: material_wqb@163.com; Li, Hongliang, E-mail: lhl@qdu.edu.cn; Guo, Peizhi, E-mail: pzguo@qdu.edu.cn; Zhao, X.S., E-mail: chezxs@qdu.edu.cn

    2017-02-15

    Three ZnFe{sub 2}O{sub 4} colloidal nanocrystal assemblies (CNAs), namely CNA1, CNA2 and CNA3, have been synthesized solvothermally with the size of 560 nm, 460 nm and 330 nm and are formed by the self-assembly of primary nanocrystals with the crystallite sizes of 19.2 nm, 15.5 nm and 21.8 nm, respectively. It was found that CNA2 performed superparamagnetic behavior with a saturation magnetization value of 36.9 emu g{sup −1} while either CNA1 or CNA3 exhibited weak ferromagnetic with a small hysteresis loop and large saturation magnetization. Electrochemical sensing measurements toward the reduction of hydrogen peroxide showed that the peak currents of the CNAs in cyclic voltammograms showed a linear relationship with the concentration of hydrogen peroxide in the experimental conditions and the peak potentials were increased with the order of CNA3, CNA2 and CNA1. The formation mechanism of ZnFe{sub 2}O{sub 4} CNAs had been discussed based on the experimental data. The magnetism and electrocatalysis of the ZnFe{sub 2}O{sub 4} CNAs were supposed to be dependent on the size of primary nanoparticles and the structure of the CNAs. - Highlights: • Size-tunable ZnFe{sub 2}O{sub 4} colloidal nanocrystal assemblies were synthesized solvothermally. • Magnetic properties of ZnFe{sub 2}O{sub 4} assemblies are depended on the size and self-assembly of primary nanoparticles. • Electrocatalytic activity of ZnFe{sub 2}O{sub 4} assemblies is determined by their structure.

  2. Solvothermal synthesis of Ni(HCO{sub 3}){sub 2}/graphene composites toward supercapacitors and the faradiac redox mechanism in KOH solution

    Energy Technology Data Exchange (ETDEWEB)

    Sun, Jinfeng [State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000 (China); University of Chinese Academy of Sciences, Beijing 100080 (China); Li, Zhangpeng [State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000 (China); Wang, Jinqing, E-mail: jqwang@licp.cas.cn [State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000 (China); Wang, Zhaofeng [State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000 (China); Niu, Lengyuan; Gong, Peiwei [State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000 (China); University of Chinese Academy of Sciences, Beijing 100080 (China); Liu, Xiaohong; Wang, Honggang [State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000 (China); Yang, Shengrong, E-mail: sryang@licp.cas.cn [State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000 (China)

    2013-12-25

    Highlights: •Ni(HCO{sub 3}){sub 2}/GS composites were prepared by a simple solvothermal method. •Ni(HCO{sub 3}){sub 2}/GS composites exhibited good supercapacitive performance. •Ni(HCO{sub 3}){sub 2}/GS2 presented the highest capacitance of 1200 F g{sup −1} at 4 A g{sup −1}. -- Abstract: In this work, a series of composites consisting of Ni(HCO{sub 3}){sub 2} and graphene nanosheets (GS) have been prepared by a facile solvothermal method, and then their application as electrode materials for supercapacitors has been investigated by cyclic voltammetry (CV) and galvanostatic charge–discharge tests. Morphological and structural analyses by field-emission scanning electron microscopy, high resolution transmission electron microscopy, X-ray diffraction and X-ray photoelectron spectroscopy indicated that Ni(HCO{sub 3}){sub 2} particles deposited on the GS and formed a loosely packed microstructure, actualizing the successful combination of Ni(HCO{sub 3}){sub 2} particles with GS. Among the prepared composites, the sample of Ni(HCO{sub 3}){sub 2}/GS2 exhibited the highest capacitance of 1200 F g{sup −1} at a current density of 4 A g{sup −1}, illustrating that such composite is a promising candidate as electrode material for supercapacitors. Moreover, the Faradic redox mechanism of the Ni(HCO{sub 3}){sub 2}/GS composite was further studied in virtue of XRD analysis, which revealed that the Ni(HCO{sub 3}){sub 2} phase could be quickly transformed into Ni(OH){sub 2} phase by an electrochemically induced phase transformation process during the galvanostatic charge–discharge tests.

  3. 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

  4. 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.

  5. Synthesis of monodisperse MFe{sub 2}O{sub 4} (M = Fe and Zn) nanoparticles for polydiethylsiloxane-based ferrofluid with a solvothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Wei [State Key Laboratory of Optoelectronic Materials and Technologies, Guangdong Provincial Key Laboratory of Photovoltaics Technologies, School of Physics and Engineering, Sun Yat-Sen University, Guangzhou 510275 (China); Laboratory of Nanophotonic Functional Materials and Devices, Institute of Optoelectronic Materials and Technology, South China Normal University, Guangzhou 510631 (China); Zhuang, Lin, E-mail: stszhl@mail.sysu.edu.cn [State Key Laboratory of Optoelectronic Materials and Technologies, Guangdong Provincial Key Laboratory of Photovoltaics Technologies, School of Physics and Engineering, Sun Yat-Sen University, Guangzhou 510275 (China); Zhang, Yong [Laboratory of Nanophotonic Functional Materials and Devices, Institute of Optoelectronic Materials and Technology, South China Normal University, Guangzhou 510631 (China); Shen, Hui [State Key Laboratory of Optoelectronic Materials and Technologies, Guangdong Provincial Key Laboratory of Photovoltaics Technologies, School of Physics and Engineering, Sun Yat-Sen University, Guangzhou 510275 (China)

    2015-09-15

    Highlights: • MFe{sub 2}O{sub 4} nanoparticles were synthesized through a facile solvothermal method. • The relationship between viscosity and temperature of the polydiethylsiloxane-based ferrofluid is discussed. • Fe{sub 3}O{sub 4} nanoparticles have a saturation magnetization of 73.06 emu/g at room temperature. - Abstract: Monodisperse MFe{sub 2}O{sub 4} (M = Fe, Zn) nanoparticles were successfully synthesized for the application of polydiethylsiloxane-based (PDES) ferrofluids (FFs) via a novel solvothermal method, with which 1-octanol and 1-octanamine act as binary solvent, oleic acid (OA) as the surfactant and metal acetylacetonate [M(acac){sub 3}](M = Fe and Zn) as the metal source. X-ray diffractometer confirms that the resultant nanoparticles are pure MFe{sub 2}O{sub 4} with a spinel structure. Infrared spectroscopy indicates that oleic acid is bound to the surface of MFe{sub 2}O{sub 4} through a covalent bond between carboxylate (COO{sup −}) and metal cations. The ratio of 1-octanol and 1-octanamine plays a key role in the formation of the sphere-shaped morphology. Transmission electron microscopy (TEM) images confirm that the Fe{sub 3}O{sub 4} particles are of 4–11 nm with good monodispersity and a narrow size distribution. The saturation magnetization of Fe{sub 3}O{sub 4} nanoparticles with sizes of 7 nm can reach up to 73.06 emu/g. Polydiethylsiloxane-based (PDES) FFs show relatively smaller changes of the viscosity with low temperatures (from −7 to 20 °C) than the polydimethylsiloxane-based (PDMS) FFs. For FFs applications, the relationship between viscosity and temperature is also discussed.

  6. 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.

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

    African Journals Online (AJOL)

    They were both subjected to beneficiation, calcinations, dealumination and the gels formed, had molar composition of 9Na2OX30SiO2XAl2O3X225H2O. The raw, intermediate and final products were fully characterized using XRD, XRF, BET and SEM/EDX. The prominent XRD peaks for ZSM11 were noticed for Kankara ...

  8. One-pot template-free synthesis of monodisperse hollow hydrogel microspheres and their resulting properties.

    Science.gov (United States)

    Lim, Hyung-Seok; Kwon, Eunji; Lee, Moonjoo; Moo Lee, Young; Suh, Kyung-Do

    2013-08-01

    Monodisperse poly(methacrylic acid/ethyleneglycoldimethacrylate) (MAA/EGDMA) hollow microcapsules, which exhibit pH-responsive behavior, are prepared by diffusion of cationic surfactants and hydrophobic interaction. During the association of the negatively charged hydrogel microspheres and an oppositely charged surfactant (cetyltrimethylammonium bromide, CTA(+)B), the hydrophobic polymer-surfactant complexes that form are separated from the internal water; consequently, a hollow structure can be formed. Confocal laser scanning microscopy, UV spectro-scopy and zeta potential are employed to study the formation of the hollow structure during the diffusion of the cationic surfactant. The controlled release behavior of methylene blue as a model drug from the as-prepared poly(MAA/EGDMA) microcapsules with a hollow structure is investigated under different pH conditions. The hollow structure can be retained, even during repetitive pH changes. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. BULK AND TEMPLATE-FREE SYNTHESIS OF SILVER NANOWIRES USING CAFFEINE AT ROOM TEMPERATURE

    Science.gov (United States)

    A simple eco-friendly one-pot method is described to synthesize bulk quantities of nanowires of silver (Ag) using caffeine without the need of reducing agent, surfactants, and/or large amounts of insoluble templates. Chemical reduction of silver salts with caffeine dramatically c...

  10. Facile synthesis of morphology-controlled Co3O4 nanostructures through solvothermal method with enhanced catalytic activity for H2O2 electroreduction

    Science.gov (United States)

    Cheng, Kui; Cao, Dianxue; Yang, Fan; Xu, Yang; Sun, Gaohui; Ye, Ke; Yin, Jinling; Wang, Guiling

    2014-05-01

    Hydrogen peroxide (H2O2) replaced oxygen (O2) as oxidant has been widely investigated due to its faster reduction kinetics, easier storage and handling than gaseous oxygen. The main challenge of using H2O2 as oxidant is the chemical decomposition. In this article, by using different C2H5OH/H2O volume ratio as the solvent, Co3O4 with different morphologies (nanosheet, nanowire, ultrafine nanowire net, nanobelts, and honeycomb-like) direct growth on Ni foam are synthesized via a simple solvothermal method for the first time. Results show that the introduction of ethanol could obviously improve the catalytic performance toward H2O2 electroreduction. The sample prepared in the solution with the C2H5OH/H2O volume ratio of 1:2 shows the best catalytic performance among the five samples and a current density of 0.214 A cm-2 is observed in 3.0 mol L-1 KOH + 0.5 mol L-1 H2O2 at -0.4 V (vs. Ag/AgCl KCl), which is much larger than that on the other metal oxides reported previously, almost comparable with the precious metals. This electrode of Co3O4 directly grown on Ni foam has superior mass transport property, which combining with its low-cost and facile preparation, make it a promising electrode for fuel cell using H2O2 as the oxidant.

  11. Solvothermal one-step synthesis of Ni-Al layered double hydroxide/carbon nanotube/reduced graphene oxide sheet ternary nanocomposite with ultrahigh capacitance for supercapacitors.

    Science.gov (United States)

    Yang, Wanlu; Gao, Zan; Wang, Jun; Ma, Jing; Zhang, Milin; Liu, Lianhe

    2013-06-26

    A Ni-Al layered double hydroxide (LDH), mutil-wall carbon nanotube (CNT), and reduced graphene oxide sheet (GNS) ternary nanocomposite electrode material has been developed by a facile one-step ethanol solvothermal method. The obtained LDH/CNT/GNS composite displayed a three-dimensional (3D) architecture with flowerlike Ni-Al LDH/CNT nanocrystallites gradually self-assembled on GNS nanosheets. GNS was used as building blocks to construct 3D nanostructure, and the LDH/CNT nanoflowers in turn separated the two-dimensional (2D) GNS sheets, which preserved the high surface area of GNSs. Furthermore, the generated porous networks with a narrow pore size distribution in the LDH/CNT/GNS composite were also demonstrated by the N2 adsorption/desorption experiment. Such morphology would be favorable to improve the mass transfer and electrochemical action of the electrode. As supercapacitor electrode material, the LDH/CNT/GNS hybrid exhibited excellent electrochemical performance, including ultrahigh specific capacitance (1562 F/g at 5 mA/cm(2)), excellent rate capability, and long-term cycling performance, which could be a promising energy storage/conversion material for supercapacitor application.

  12. Solvothermal synthesis of Mg-doped Li2FeSiO4/C nanocomposite cathode materials for lithium-ion batteries

    Science.gov (United States)

    Kumar, Ajay; Jayakumar, O. D.; Naik, V. M.; Nazri, G. A.; Naik, R.

    Lithium transition metal orthosilicates, such as Li2FeSiO4 and Li2MnSiO4, as cathode material have attracted much attention lately due to their high theoretical capacity ( 330 mAh/g), low cost, and environmental friendliness. However, they suffer from poor electronic conductivity and slow lithium ion diffusion in the solid phase. Several cation-doped orthosilicates have been studied to improve their electrochemical performance. We have synthesized partially Mg-substituted Li2Mgx Fe1-x SiO4-C, (x = 0.0, 0.01, 0.02, and 0.04) nano-composites by solvothermal method followed by annealing at 600oC in argon flow. The structure and morphology of the composites were characterized by XRD, SEM and TEM. The surface area and pore size distribution were measured by using N2 adsorption/desorption curves. The electrochemical performance of the Li2MgxFe1-x SiO4-C composites was evaluated by Galvanostatic cycling against metallic lithium anode, electrochemical impedance spectroscopy, and cyclic voltammetry. Li2Mg0.01Fe0.99SiO4-C sample shows a capacity of 278 mAh/g (at C/30 rate in the 1.5-4.6 V voltage window) with an excellent rate capability and stability, compared to the other samples. We attribute this observation to its higher surface area, enhanced electronic conductivity and higher lithium ion diffusion coefficient.

  13. Solvothermal synthesis of mesoporous slabstone-like TiO{sub 2} and its photodegradation preference in a methyl orange-rhodamine B mixture solution

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Kun; Zhu, Lianjie; Li, Naixuan; Sun, Youguang; Li, Hongbin; Zhu, Xuchen [School of Chemistry and Chemical Engineering, Tianjin University of Technology, Tianjin 300384 (China)

    2012-10-15

    Mesoporous slabstone-like anatase TiO{sub 2} micro-nanometer composite structure has been successfully synthesized by a facile solvothermal method at 180 C using polyethylene glycol (PEG) as a structure-directing agent, followed by calcination at 400 C for 2 h. The crystal structure and morphology of the product were characterized by XRD, SEM, TEM and HRTEM. Its BET specific surface area was obtained from N{sub 2} adsorption-desorption isotherm measurement. Rhodamine B (RB) aqueous solution was used to evaluate the photocatalytic activity of the as-prepared TiO{sub 2} under simulated sunlight irradiation and compared with that of commercial TiO{sub 2} (P25). A RB and methyl orange (MO) coexisting solution was chosen to investigate the photodegradation preference of the slabstone-like TiO{sub 2} on these two dyes. The results show that the photocatalytic activity of the as-prepared TiO{sub 2} is much higher than that of P25, and MO is the preferential degradation species in the MO-RB mixture solution. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  14. One-pot solvothermal synthesis of graphene wrapped rice-like ferrous carbonate nanoparticles as anode materials for high energy lithium-ion batteries

    Science.gov (United States)

    Zhang, Fan; Zhang, Ruihan; Feng, Jinkui; Ci, Lijie; Xiong, Shenglin; Yang, Jian; Qian, Yitai; Li, Lifei

    2014-11-01

    Well dispersed rice-like FeCO3 nanoparticles were produced and combined with reduced graphene oxide (RGO) via a one-pot solvothermal route. SEM characterization shows that rice-like FeCO3 nanoparticles are homogeneously anchored on the surface of the graphene nanosheets; the addition of RGO is helpful to form a uniform morphology and reduce the particle size of FeCO3 to nano-grade. As anode materials for lithium-ion batteries, the FeCO3/RGO nanocomposites exhibit significantly improved lithium storage properties with a large reversible capacity of 1345 mA h g-1 for the first cycle and a capacity retention of 1224 mA h g-1 after 50 cycles with a good rate capability compared with pure FeCO3 particles. The superior electrochemical performance of the FeCO3/RGO nanocomposite electrode compared to the pure FeCO3 electrode can be attributed to the well dispersed RGO which enhances the electronic conductivity and accommodates the volume change during the conversion reactions. Our study shows that the FeCO3/RGO nanocomposite could be a suitable candidate for high capacity lithium-ion batteries.

  15. 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.

  16. Solvothermal synthesis of NiAl double hydroxide microspheres on a nickel foam-graphene as an electrode material for pseudo-capacitors

    International Nuclear Information System (INIS)

    Momodu, Damilola; Bello, Abdulhakeem; Dangbegnon, Julien; Barzeger, Farshad; Taghizadeh, Fatimeh; Fabiane, Mopeli; Manyala, Ncholu; Johnson, A. T. Charlie

    2014-01-01

    In this paper, we demonstrate excellent pseudo-capacitance behavior of nickel-aluminum double hydroxide microspheres (NiAl DHM) synthesized by a facile solvothermal technique using tertbutanol as a structure-directing agent on nickel foam-graphene (NF-G) current collector as compared to use of nickel foam current collector alone. The structure and surface morphology were studied by X-ray diffraction analysis, Raman spectroscopy and scanning and transmission electron microscopies respectively. NF-G current collector was fabricated by chemical vapor deposition followed by an ex situ coating method of NiAl DHM active material which forms a composite electrode. The pseudocapacitive performance of the composite electrode was investigated by cyclic voltammetry, constant charge–discharge and electrochemical impedance spectroscopy measurements. The composite electrode with the NF-G current collector exhibits an enhanced electrochemical performance due to the presence of the conductive graphene layer on the nickel foam and gives a specific capacitance of 1252 F g −1 at a current density of 1 A g −1 and a capacitive retention of about 97% after 1000 charge–discharge cycles. This shows that these composites are promising electrode materials for energy storage devices

  17. 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

    2017-01-01

    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. PMID:29099814

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

    Directory of Open Access Journals (Sweden)

    Yang Liu

    2017-11-01

    Full Text Available 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.

  19. Solvothermal synthesis of monodisperse LiFePO4 micro hollow spheres as high performance cathode material for lithium ion batteries.

    Science.gov (United States)

    Yang, Shiliu; Hu, Mingjun; Xi, Liujiang; Ma, Ruguang; Dong, Yucheng; Chung, C Y

    2013-09-25

    A microspherical, hollow LiFePO4 (LFP) cathode material with polycrystal structure was simply synthesized by a solvothermal method using spherical Li3PO4 as the self-sacrificed template and FeCl2·4H2O as the Fe(2+) source. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) show that the LFP micro hollow spheres have a quite uniform size of ~1 μm consisting of aggregated nanoparticles. The influences of solvent and Fe(2+) source on the phase and morphology of the final product were chiefly investigated, and a direct ion exchange reaction between spherical Li3PO4 templates and Fe(2+) ions was firstly proposed on the basis of the X-ray powder diffraction (XRD) transformation of the products. The LFP nanoparticles in the micro hollow spheres could finely coat a uniform carbon layer ~3.5 nm by a glucose solution impregnating-drying-sintering process. The electrochemical measurements show that the carbon coated LFP materials could exhibit high charge-discharge capacities of 158, 144, 125, 101, and even 72 mAh g(-1) at 0.1, 1, 5, 20, and 50 C, respectively. It could also maintain 80% of the initial discharge capacity after cycling for 2000 times at 20 C.

  20. Single-step solvothermal synthesis of mesoporous Ag-TiO2-reduced graphene oxide ternary composites with enhanced photocatalytic activity

    Science.gov (United States)

    Arif Sher Shah, Md. Selim; Zhang, Kan; Park, A. Reum; Kim, Kwang Su; Park, Nam-Gyu; Park, Jong Hyeok; Yoo, Pil J.

    2013-05-01

    With growing interest in the photocatalytic performance of TiO2-graphene composite systems, the ternary phase of TiO2, graphene, and Ag is expected to exhibit improved photocatalytic characteristics because of the improved recombination rate of photogenerated charge carriers and potential contribution of the generation of localized surface plasmon resonance at Ag sites on a surface of the TiO2-graphene binary matrix. In this work, Ag-TiO2-reduced graphene oxide ternary nanocomposites were successfully synthesized by a simple solvothermal process. In a single-step synthetic procedure, the reduction of AgNO3 and graphene oxide and the hydrolysis of titanium tetraisopropoxide were spontaneously performed in a mixed solvent system of ethylene glycol, N,N-dimethylformamide and a stoichiometric amount of water without resorting to the use of typical reducing agents. The nanocomposites were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, along with different microscopic and spectroscopic techniques, enabling us to confirm the successful reduction of AgNO3 and graphite oxide to metallic Ag and reduced graphene oxide, respectively. Due to the highly facilitated electron transport of well distributed Ag nanoparticles, the synthesized ternary nanocomposite showed enhanced photocatalytic activity for degradation of rhodamine B dye under visible light irradiation.With growing interest in the photocatalytic performance of TiO2-graphene composite systems, the ternary phase of TiO2, graphene, and Ag is expected to exhibit improved photocatalytic characteristics because of the improved recombination rate of photogenerated charge carriers and potential contribution of the generation of localized surface plasmon resonance at Ag sites on a surface of the TiO2-graphene binary matrix. In this work, Ag-TiO2-reduced graphene oxide ternary nanocomposites were successfully synthesized by a simple solvothermal process. In a single-step synthetic procedure, the reduction

  1. 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.

  2. Solvothermal Synthesis of Three-Dimensional Hierarchical CuS Microspheres from a Cu-Based Ionic Liquid Precursor for High-Performance Asymmetric Supercapacitors.

    Science.gov (United States)

    Zhang, Jing; Feng, Huijie; Yang, Jiaqin; Qin, Qing; Fan, Hongmin; Wei, Caiying; Zheng, Wenjun

    2015-10-07

    It is meaningful to exploit copper sulfide materials with desired structure as well as potential application due to their cheapness and low toxicity. A low-temperature and facile solvothermal method for preparing three-dimensional (3D) hierarchical covellite (CuS) microspheres from an ionic liquid precursor [Bmim]2Cu2Cl6 (Bmim = 1-butyl-3-methylimidazolium) is reported. The formation of CuS nanostructures was achieved by decomposition of intermediate complex Cu(Tu)3Cl (thiourea = Tu), which produced CuS microspheres with diameters of 2.5-4 μm assembled by nanosheets with thicknesses of 10-15 nm. The ionic liquid, as an "all-in-one" medium, played a key role for the fabrication and self-assembly of CuS nanosheets. The alkylimidazolium rings ([Bmim](+)) were found to adsorb onto the (001) facets of CuS crystals, which inhibited the crystal growth along the [001] direction, while the alkyl chain had influence on the assembly of CuS nanosheets. The CuS microspheres showed enhanced electrochemical performance and high stability for the application in supercapacitors due to intriguing structural design and large specific surface area. When this well-defined CuS electrode was assembled into an asymmetric supercapacitor (ASC) with an activated carbon (AC) electrode, the CuS//AC-ASC demonstrated good cycle performance (∼88% capacitance after 4000 cycles) and high energy density (15.06 W h kg(-1) at a power density of 392.9 W kg(-1)). This work provides new insights into the use of copper sulfide electrode materials for asymmetric supercapacitors and other electrochemical devices.

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

    Directory of Open Access Journals (Sweden)

    Abul Kalam

    2018-03-01

    Full Text Available 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. Keywords: Cobalt ferrite, Photocatalysis, Kinetics, Optical properties, Surface area studies

  4. Solvothermal synthesis of stable nanoporous polymeric bases-crystalline TiO2 nanocomposites: visible light active and efficient photocatalysts for water treatment.

    Science.gov (United States)

    Liu, Fujian; Kong, Weiping; Wang, Liang; Noshadi, Iman; Zhang, Zhonghua; Qi, Chenze

    2015-02-27

    Visible light active and stable nanoporous polymeric base-crystalline TiO2 nanocomposites were solvothermally synthesized from in situ copolymerization of divinylbenzene (DVB) with 1-vinylimidazolate (VI) or 4-vinylpyridine (Py) in the presence of tetrabutyl titanate without the use of any other additives (PDVB-VI-TiO2-x, PDVB-Py-TiO2-x, where x stands for the molar ratio of TiO2 to VI or Py), which showed excellent activity with respect to catalyzing the degradation of organic pollutants of p-nitrophenol (PNP) and rhodamine-B (RhB). TEM and SEM images show that PDVB-VI-TiO2-x and PDVB-Py-TiO2-x have abundant nanopores, and TiO2 nanocrystals with a high degree of crystallinity were homogeneously embedded in the PDVB-VI-TiO2-x and PDVB-Py-TiO2-x, forming a stable 'brick-and-mortar' nanostructure. PDVB-VI and PDVB-Py supports act as the glue linking TiO2 nanocrystals to form nanopores and constraining the agglomeration of TiO2 nanocrystals. XPS spectra show evidence of unique interactions between TiO2 and basic sites in these samples. UV diffuse reflectance shows that PDVB-VI-TiO2-x and PDVB-Py-TiO2-x exhibit a unique response to visible light. Catalytic tests show that the PDVB-VI-TiO2-x and PDVB-Py-TiO2-x were active in catalyzing the degradation of PNP and RhB organic pollutants under visible light irradiation. The enhanced activities of the PDVB-VI-TiO2-x and PDVB-Py-TiO2-x were ascribed to synergistic effects between abundant nanopores and the unique optical adsorption of visible light in the samples.

  5. Solvothermal synthesis of stable nanoporous polymeric bases-crystalline TiO2 nanocomposites: visible light active and efficient photocatalysts for water treatment

    Science.gov (United States)

    Liu, Fujian; Kong, Weiping; Wang, Liang; Noshadi, Iman; Zhang, Zhonghua; Qi, Chenze

    2015-02-01

    Visible light active and stable nanoporous polymeric base-crystalline TiO2 nanocomposites were solvothermally synthesized from in situ copolymerization of divinylbenzene (DVB) with 1-vinylimidazolate (VI) or 4-vinylpyridine (Py) in the presence of tetrabutyl titanate without the use of any other additives (PDVB-VI-TiO2-x, PDVB-Py-TiO2-x, where x stands for the molar ratio of TiO2 to VI or Py), which showed excellent activity with respect to catalyzing the degradation of organic pollutants of p-nitrophenol (PNP) and rhodamine-B (RhB). TEM and SEM images show that PDVB-VI-TiO2-x and PDVB-Py-TiO2-x have abundant nanopores, and TiO2 nanocrystals with a high degree of crystallinity were homogeneously embedded in the PDVB-VI-TiO2-x and PDVB-Py-TiO2-x, forming a stable ‘brick-and-mortar’ nanostructure. PDVB-VI and PDVB-Py supports act as the glue linking TiO2 nanocrystals to form nanopores and constraining the agglomeration of TiO2 nanocrystals. XPS spectra show evidence of unique interactions between TiO2 and basic sites in these samples. UV diffuse reflectance shows that PDVB-VI-TiO2-x and PDVB-Py-TiO2-x exhibit a unique response to visible light. Catalytic tests show that the PDVB-VI-TiO2-x and PDVB-Py-TiO2-x were active in catalyzing the degradation of PNP and RhB organic pollutants under visible light irradiation. The enhanced activities of the PDVB-VI-TiO2-x and PDVB-Py-TiO2-x were ascribed to synergistic effects between abundant nanopores and the unique optical adsorption of visible light in the samples.

  6. Template-free approach to synthesize hierarchical porous nickel cobalt oxides for supercapacitors

    Science.gov (United States)

    Chang, Jie; Sun, Jing; Xu, Chaohe; Xu, Huan; Gao, Lian

    2012-10-01

    Nickel cobalt oxides with various Ni/Co ratios were synthesized using a facile template-free approach for electrochemical supercapacitors. The texture and morphology of the nanocomposites were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Brunauer-Emmett-Teller analysis (BET). The results show that a hierarchical porous structure assembled from nanoflakes with a thickness of ~10 nm was obtained, and the ratio of nickel to cobalt in the nanocomposites was very close to the precursors. Cyclic voltammetry (CV) and galvanostatic charge and discharge tests were carried out to study the electrochemical performance. Both nickel cobalt oxides (Ni-Co-O-1 with Ni : Co = 1, Ni-Co-O-2 with Ni : Co = 2) outperform pure NiO and Co3O4. The Ni-Co-O-1 and Ni-Co-O-2 possess high specific capacities of 778.2 and 867.3 F g-1 at 1 A g-1 and capacitance retentions of 84.1% and 92.3% at 10 A g-1, respectively. After full activation, the Ni-Co-O-1 and Ni-Co-O-2 could achieve a maximum value of 971 and 1550 F g-1 and remain at ~907 and ~1450 F g-1 at 4 A g-1, respectively. Also, the nickel cobalt oxides show high capacity retention when fast charging.Nickel cobalt oxides with various Ni/Co ratios were synthesized using a facile template-free approach for electrochemical supercapacitors. The texture and morphology of the nanocomposites were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Brunauer-Emmett-Teller analysis (BET). The results show that a hierarchical porous structure assembled from nanoflakes with a thickness of ~10 nm was obtained, and the ratio of nickel to cobalt in the nanocomposites was very close to the precursors. Cyclic voltammetry (CV) and galvanostatic charge and discharge tests were carried out to study the electrochemical performance. Both nickel cobalt oxides (Ni-Co-O-1 with Ni : Co = 1, Ni-Co-O-2 with Ni

  7. A template-free method for stable CuO hollow microspheres fabricated from a metal organic framework (HKUST-1).

    Science.gov (United States)

    Zhang, Suoying; Liu, Hong; Liu, Pengfei; Yang, Zhuhong; Feng, Xin; Huo, Fengwei; Lu, Xiaohua

    2015-06-07

    Uniform CuO hollow microspheres were successfully achieved from a non-uniform metal organic framework by using a template-free method. The process mechanism has been revealed to be spherical aggregation and Ostwald ripening. When tested in CO oxidation and heat treatment, these assembled microspheres exhibited an excellent catalytic performance and show a much better stability than the inherited hollow structure from MOFs.

  8. 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.

  9. 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.

  10. Solvothermal crystallization of nanocrystals of metal oxides

    International Nuclear Information System (INIS)

    Furukawa, S; Amino, H; Iwamoto, S; Inoue, M

    2008-01-01

    Solvothermal crystallization of the hydroxide gels obtained by hydrolysis of alkoxides (Zr, Ta, Nb, ln, Sn, Ti and Al) was examined. Nanocrystals having high surface areas (S BET > 170 m 2 g -1 ) were obtained except for the product derived from indium isopropoxide. The effect of water in organic solvent upon the crystallinity of the product was investigated. The increase in the activity of water by using high concentration of alkoxide or intentional addition of water to the solvothermal medium led to crystal growth of the products. In contrast, decrease in activity of water by adding ethylene glycol before solvothermal treatment caused a decrease in crystallinity of the product

  11. Solvothermal crystallization of nanocrystals of metal oxides

    Science.gov (United States)

    Furukawa, S.; Amino, H.; Iwamoto, S.; Inoue, M.

    2008-07-01

    Solvothermal crystallization of the hydroxide gels obtained by hydrolysis of alkoxides (Zr, Ta, Nb, ln, Sn, Ti and Al) was examined. Nanocrystals having high surface areas (SBET > 170 m2 g-1) were obtained except for the product derived from indium isopropoxide. The effect of water in organic solvent upon the crystallinity of the product was investigated. The increase in the activity of water by using high concentration of alkoxide or intentional addition of water to the solvothermal medium led to crystal growth of the products. In contrast, decrease in activity of water by adding ethylene glycol before solvothermal treatment caused a decrease in crystallinity of the product.

  12. Hierarchical structures of ZnO spherical particles synthesized solvothermally

    Science.gov (United States)

    Saito, Noriko; Haneda, Hajime

    2011-12-01

    We review the solvothermal synthesis, using a mixture of ethylene glycol (EG) and water as the solvent, of zinc oxide (ZnO) particles having spherical and flower-like shapes and hierarchical nanostructures. The preparation conditions of the ZnO particles and the microscopic characterization of the morphology are summarized. We found the following three effects of the ratio of EG to water on the formation of hierarchical structures: (i) EG restricts the growth of ZnO microcrystals, (ii) EG promotes the self-assembly of small crystallites into spheroidal particles and (iii) the high water content of EG results in hollow spheres.

  13. 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

  14. 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.

  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. 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.

  17. 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.

  18. Solvothermal synthesis and characterisation of new one-dimensional indium and gallium sulphides: [C1N4H26]0.5[InS2] and [C1N4H26]0.5[GaS2

    International Nuclear Information System (INIS)

    Vaqueiro, Paz

    2006-01-01

    Two new main group metal sulphides, [C 1 N 4 H 26 ] 0.5 [InS 2 ] (1) and [C 1 N 4 H 26 ] 0.5 [GaS 2 ] (2) have been prepared solvothermally in the presence of 1,4-bis(3-aminopropyl)piperazine and their crystal structures determined by single-crystal X-ray diffraction. Both compounds are isostructural and crystallise in the monoclinic space group P2 1 /n (Z=4), with a=6.5628(5), b=11.2008(9), c=12.6611(9) A and β=94.410(4) o (wR=0.035) for compound (1) and a=6.1094(5), b=11.2469(9), c=12.7064(10) A and β=94.313(4) o (wR=0.021) for compound (2). The structure of [C 1 N 4 H 26 ] 0.5 [MS 2 ] (M=In,Ga) consists of one-dimensional [MS 2 ] - chains which run parallel to the crystallographic a axis and are separated by diprotonated amine molecules. These materials represent the first example of solvothermally prepared one-dimensional gallium and indium sulphides. -- Graphical abstract: [C 1 N 4 H 26 ] 0.5 [InS 2 ] and [C 1 N 4 H 26 ] 0.5 [GaS 2 ], prepared under solvothermal conditions, consist of one-dimensional [MS 2 ] - chains separated by diprotonated 1,4-bis(3-aminopropyl)piperazine molecules

  19. 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.

  20. 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....

  1. Room temperature synthesis and characterization of ultralong Cd(OH)2 nanowires: a simple and template-free chemical route

    International Nuclear Information System (INIS)

    Sahraei, R.; Daneshfar, A.; Roushani, M.; Mihandoost, A.; Nabiyouni, G.; Majles Ara, M.H.

    2012-01-01

    Ultralong Cd(OH) 2 nanowires were fabricated in high yield by a convenient chemical method using alkali medium at room temperature without using any templates. The preparation conditions induce a unilateral growth of nanowires, despite the absence of any template. The length of the nanowires reached several hundreds of micrometers, giving an aspect ratio of a few thousands. The X-ray diffraction shows that the Cd(OH) 2 nanostructures crystallized in the wurtzite structure without any special orientation. The photoluminescence spectrum of Cd(OH) 2 nanostructures appears as two emission bands: one related to green emission at 475-510 nm, and the other related to deep level emission at 510-540 nm. Also the formation mechanisms of the nanowires are presented. The growth mechanism involves the irreversible and specifically oriented self-assembly of primary nanocrystals and results in the formation of the nanowires. (orig.)

  2. 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.

  3. 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.

  4. 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.

  5. Hexagonal-layered Na{sub 0.7}MnO{sub 2.05} via solvothermal synthesis as an electrode material for aqueous Na-ion supercapacitors

    Energy Technology Data Exchange (ETDEWEB)

    Hou, Yan; Tang, Hongwei; Li, Bao; Chang, Kun [Collaborative Innovation Center of Henan Province for Green Manufacturing of Fine Chemicals, Key Laboratory of Green Chemical Media and Reactions, Ministry of Education, School of Chemistry and Chemical Engineering, Henan Normal University, Xinxiang, Henan, 453007 (China); Chang, Zhaorong, E-mail: czr_56@163.com [Collaborative Innovation Center of Henan Province for Green Manufacturing of Fine Chemicals, Key Laboratory of Green Chemical Media and Reactions, Ministry of Education, School of Chemistry and Chemical Engineering, Henan Normal University, Xinxiang, Henan, 453007 (China); Yuan, Xiao-Zi; Wang, Haijiang [National Research Council of Canada, V6T 1W5, Vancouver, BC (Canada)

    2016-03-01

    The layered sodium manganese oxides Na{sub 0.7}MnO{sub 2.05} material was synthesized using Na{sub 2}CO{sub 3} and Mn{sub 3}O{sub 4} precursors via a solvothermal method at different temperatures. The X-ray diffraction (XRD) shows that the Na{sub 0.7}MnO{sub 2.05} sample has a high crystallinity with hexagonal crystal system. The electrochemical performance was characterized by cyclic voltammetry (CV), impedance measurements and galvanostatic charge–discharge tests in symmetric Na-ion supercapacitors with 1 mol L{sup −1} Na{sub 2}SO{sub 4} solution as electrolyte. The Na{sub 0.7}MnO{sub 2.05} material shows a high specific capacity of about 162.5 F g{sup −1} at a current density of 50 mA g{sup −1} and a high coulombic efficiency approaching 100%. Even at a current density of 200 mA g{sup −1}, the discharge capacity of the material can reach to 146 F g{sup −1}. This electrode material holds great promise for practical applications. - Highlights: • Novel electrode material for supercapacitor: hexagonal-layered Na{sub 0.7}MnO{sub 2.05}. • Na{sub 0.7}MnO{sub 2.05} is synthesized using Mn{sub 3}O{sub 4} precursors via solvothermal method. • Obtained Na{sub 0.7}MnO{sub 2.05} exhibits superior electrochemical performance.

  6. Solvothermal preparation of micro/nanostructured TiO_2 with enhanced lithium storage capability

    International Nuclear Information System (INIS)

    Li, Jie; Wang, Chao; Zheng, Ping; Zhang, Lei; Chen, Gongxuan; Tang, Chengchun; Wu, Tian

    2017-01-01

    Facile and controllable preparation of TiO_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_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_2 shows higher specific capacity and enhanced cycle stability as anode material for lithium ion batteries. - Highlights: • Controllable preparation of nano-TiO_2 is achieved by a solvothermal method. • TiO_2 morphology is tailored by tuning reactant ratio, temperature and duration. • Needle structured TiO_2 shows enhanced lithium storage capability.

  7. 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.

  8. 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).

  9. Crystal structure, solvothermal synthesis, thermogravimetric studies and DFT calculations of a five-coordinate cobalt(II) compound based on the N,N-bis-(2-hy-droxy-eth-yl)glycine anion.

    Science.gov (United States)

    Zhou, Yanling; Liu, Xianrong; Wang, Qijun; Wang, Lisheng; Song, Baoling

    2016-10-01

    The reaction of CoCl 2 ·6H 2 O, N , N -bis-(2-hy-droxy-eth-yl)glycine and tri-ethyl-amine (Et 3 N) in ethanol solution under solvothermal conditions produced crystals of [ N , N -bis-(2-hy-droxy-eth-yl)glycinato]chloridocobalt(II), [Co(C 6 H 12 NO 4 )Cl]. The Co II ion is coordinated in a slightly distorted trigonal-bipyramidal environment which is defined by three O atoms occupying the equatorial plane and the N and Cl atoms in the apical sites. In the crystal, two types of O-H⋯O hydrogen bonds connect the mol-ecules, forming a two-dimensional network parallel to (001). The mol-ecular structure of the title compound confirms the findings of FTIR, elemental analysis, ESI-MS analysis and TG analysis. By using the density functional theory (DFT) (B3LYP) method with 6-31G(d) basis set, the molecular structure has been calculated and optimized.

  10. Novel Evaporation Process for Deposition of Kesterite Thin Films Synthesized by Solvothermal Method

    Directory of Open Access Journals (Sweden)

    J. A. Estrada-Ayub

    2017-01-01

    Full Text Available Kesterite, a quaternary compound of Cu2ZnSnS4, is a promising option as a material absorber to reduce the cost of photovoltaic solar cells. The solvothermal method is a way to synthesize nanoparticles of this material. In this work, once synthesized, particles were deposited on a substrate through evaporation, and their morphological, structural, and optical properties were studied. Results show that changes of precursor ratios during solvothermal synthesis result in a modification of particle morphology but not on its size. The deposition of already synthesized kesterite through evaporation preserves kesterite structure and permits the formation of a homogenous film on a substrate. Optical reflectance and transmittance measurements allowed estimating the band-gap energy between 1.41 and 1.46 eV for representative samples, which is near the optimum for the absorber material.

  11. One-pot solvothermal synthesis of Co{sub 1−x}Mn{sub x}C{sub 2}O{sub 4} and their application as anode materials for lithium-ion batteries

    Energy Technology Data Exchange (ETDEWEB)

    Ang, Wei An Elijah [School of Materials Science and Engineering, Nanyang Technological University, 50 Nanyang Avenue, Singapore 639798 (Singapore); Energy Research Institute @ NTU (ERI-N), Nanyang Technological University, 50 Nanyang Drive, Singapore 637553 (Singapore); Cheah, Yan Ling; Wong, Chui Ling [Energy Research Institute @ NTU (ERI-N), Nanyang Technological University, 50 Nanyang Drive, Singapore 637553 (Singapore); Hng, Huey Hoon [School of Materials Science and Engineering, Nanyang Technological University, 50 Nanyang Avenue, Singapore 639798 (Singapore); Madhavi, Srinivasan, E-mail: madhavi@ntu.edu.sg [School of Materials Science and Engineering, Nanyang Technological University, 50 Nanyang Avenue, Singapore 639798 (Singapore); Energy Research Institute @ NTU (ERI-N), Nanyang Technological University, 50 Nanyang Drive, Singapore 637553 (Singapore); TUM CREATE Center for Electromobility, 1 CREATE Way, #10-02 CREATE Tower, Singapore 138602 (Singapore)

    2015-07-25

    Graphical abstract: MnC{sub 2}O{sub 4} exhibited good cycling stability while CoC{sub 2}O{sub 4} showed severe capacity fading phenomenon after 40 cycles. Notably, mixed solid solution having Co{sub 0.52}Mn{sub 0.48}C{sub 2}O{sub 4} composition improved the specific reversible discharge capacity to a stable value of ∼1000 mA h g{sup −1} (1 C-rate). - Highlights: • Mixed metal oxalates are synthesized by solvothermal method for the first time. • We control morphologies by varying solvent mixtures and transition metal types. • Li/Co{sub 0.52}Mn{sub 0.48}C{sub 2}O{sub 4} is the best capacity and rate-performing cell in this study. • The positive synergistic effect is attributed to optimal Co:Mn mole ratio. • Properties of Co give high capacity values while Mn give good cycling stability. - Abstract: A facile one-pot solvothermal route has been developed to synthesize phase pure M{sub x}C{sub 2}O{sub 4}⋅2H{sub 2}O (M = Mn, Co; 0 < x ⩽ 1) microstructures without employing any hard/soft template and their electrochemical performance in lithium-ion batteries has been systematically investigated. Morphology, microstructure and composition of the synthesized materials are characterized by field emission-scanning electron microscopy, X-ray diffraction and energy-dispersive X-ray spectroscopy. Anhydrous micron-sized MnC{sub 2}O{sub 4} and CoC{sub 2}O{sub 4} exhibits specific reversible discharge capacity of ∼800 and 950 mA h g{sup −1} respectively, at 1 C-rate. MnC{sub 2}O{sub 4} exhibited good cycling stability while CoC{sub 2}O{sub 4} showed severe capacity fading phenomenon after 40 cycles, thereafter attaining 400–600 mA h g{sup −1} for all C-rates. Interestingly, mixed solid solution having Co{sub 0.52}Mn{sub 0.48}C{sub 2}O{sub 4} composition improved the specific reversible discharge capacity to a stable value of ∼1000 mA h g{sup −1} (1 C-rate), which is one of the highest reported values for such oxalates. The cycling stability of this

  12. Solvothermal synthesis of a new 3-D mixed-metal sulfide framework, (H{sub 1.33}tren)[In{sub 2.67}Sb{sub 1.33}S{sub 8}]·tren

    Energy Technology Data Exchange (ETDEWEB)

    Lampkin, John D., E-mail: j.lampkin@pgr.rdg.ac.uk; Powell, Anthony V., E-mail: a.v.powell@rdg.ac.uk; Chippindale, Ann M., E-mail: a.m.chippindale@rdg.ac.uk

    2016-11-15

    A new indium(III) antimony(V) sulfide, (H{sub 1.33}tren)[In{sub 2.67}Sb{sub 1.33}S{sub 8}]·tren, has been prepared solvothermally at 433 K. The compound crystallises in the tetragonal space group I-42d (lattice parameters, a=12.6248(5) and c=19.4387(18) Å at 150 K) and contains adamantane-like T2 supertetrahedral units comprised of corner-sharing InS{sub 4}{sup 5−} and SbS{sub 4}{sup 3−} tetrahedra. The adamantane-like units are then linked through sulfur vertices to generate an open, 3-D framework structure containing large pores in which neutral, protonated tren (tris(2-aminoethylene)amine) molecules reside. The presence of the organic components was confirmed by solid-state {sup 13}C NMR (10 kHz), combustion and thermogravimetric analysis. The band gap, obtained from UV–vis diffuse reflectance measurements, is 2.7(2) eV. Stirring with either water or alkali-metal salt solution leads to removal of the neutral tren molecules and an ~9% reduction in unit-cell volume on formation of (H{sub 1.33}tren)[In{sub 2.67}Sb{sub 1.33}S{sub 8}]·(H{sub 2}O){sub 4}. - Graphical abstract: Linking of In(III)-Sb(V)-S adamantane units to form a 3-D open framework. - Highlights: • Preparation and structural characterisation of a new mixed-metal thiometallate. • The first mixed In(III)/Sb(V) supertetrahedron. • Optical band gap of 2.7(2) eV. • Soaking in aqueous alkali-metal solutions leads to removal of ca. 50% of the organic content.

  13. Ag-doped TiO2 hollow microspheres with visible light response by template-free route for removal of tetracycline hydrochloride from aqueous solution

    Science.gov (United States)

    Zhang, Jian; Li, Xuanhua; Peng, Meiling; Tang, Yuanyuan; Ke, Anqi; Gan, Wei; Fu, Xucheng; Hao, Hequn

    2018-06-01

    In this study, Ag-doped TiO2 hollow microspheres were synthesized by a template-free route, and their photocatalytic performance and catalytic mechanism were investigated. The hollow microspheres were characterized by x-ray diffraction, scanning electron microscopy, transmission electron microscopy, x-ray photoelectron spectroscopy and UV–vis spectroscopy. Ag-doped hollow TiO2 microspheres exhibited excellent photocatalytic performance for tetracycline hydrochloride (TC) in water. TC degradation follows pseudo first-order kinetics, and hydroxyl radical (OH·) and holes (h+) were active substances in the photocatalytic reaction.

  14. 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

  15. Solvothermal tuning of photoluminescent graphene quantum dots: from preparation to photoluminescence mechanism

    Science.gov (United States)

    Qi, Bao-Ping; Zhang, Xiaoru; Shang, Bing-Bing; Xiang, Dongshan; Zhang, Shenghui

    2018-02-01

    Solvothermal synthesis was employed to tune the surface states of graphene quantum dots (GQDs). Two series of GQDs with the particle sizes from 2.6 to 4.5 nm were prepared as follows: (I) GQDs with the same size but different oxygen degrees; (II) GQDs with different core sizes but the similar surface chemistry. Both the large sizes and the high surface oxidation degrees led to the redshift photoluminescence (PL) of GQDs. Electrochemiluminescence (ECL) spectra from two series of GQDs were all in accordance with their PL spectra, respectively, which provided good evidence for the conjugated structures in GQDs responsible for PL. [Figure not available: see fulltext.

  16. Preparation and thermoelectric properties of sulfur doped Ag2Te nanoparticles via solvothermal methods.

    Science.gov (United States)

    Zhou, Wenwen; Zhao, Weiyun; Lu, Ziyang; Zhu, Jixin; Fan, Shufen; Ma, Jan; Hng, Huey Hoon; Yan, Qingyu

    2012-07-07

    In this work, n-type Ag(2)Te nanoparticles are prepared by a solvothermal approach with uniform and controllable sizes, e.g. 5-15 nm. The usage of dodecanethiol during the synthesis effectively introduces sulfur doping into the sample, which optimizes the charge carrier concentration of the nanoparticles to >1 × 10(20) cm(-3). This allows us to achieve the desired electrical resistivities of nanoparticles with effective sulphur doping show a maximum ZT value of ~0.62 at 550 K.

  17. Precursor directed synthesis - ``molecular'' mechanisms in the Soft Chemistry approaches and their use for template-free synthesis of metal, metal oxide and metal chalcogenide nanoparticles and nanostructures

    Science.gov (United States)

    Seisenbaeva, Gulaim A.; Kessler, Vadim G.

    2014-05-01

    This review provides an insight into the common reaction mechanisms in Soft Chemistry processes involved in nucleation, growth and aggregation of metal, metal oxide and chalcogenide nanoparticles starting from metal-organic precursors such as metal alkoxides, beta-diketonates, carboxylates and their chalcogene analogues and demonstrates how mastering the precursor chemistry permits us to control the chemical and phase composition, crystallinity, morphology, porosity and surface characteristics of produced nanomaterials.This review provides an insight into the common reaction mechanisms in Soft Chemistry processes involved in nucleation, growth and aggregation of metal, metal oxide and chalcogenide nanoparticles starting from metal-organic precursors such as metal alkoxides, beta-diketonates, carboxylates and their chalcogene analogues and demonstrates how mastering the precursor chemistry permits us to control the chemical and phase composition, crystallinity, morphology, porosity and surface characteristics of produced nanomaterials. To Professor David Avnir on his 65th birthday.

  18. 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

  19. C-oriented and {010} facets exposed BiVO4 nanowall films: template-free fabrication and their enhanced photoelectrochemical properties.

    Science.gov (United States)

    Zhou, Min; Zhang, Shudong; Sun, Yongfu; Wu, Changzheng; Wang, Mingtai; Xie, Yi

    2010-12-03

    Vertically aligned BiVO(4) nanowall films on indium tin oxide (ITO) glass have been fabricated through a template-free hydrothermal method for the first time. Based on the structural understanding of both BiVO(4) and ITO, the lattice matches ({020}(BiVO4) and {040}(ITO), {200}(BiVO4) and {004}(ITO), respectively) and the similarity of metal atomic arrangement parallel to {001} planes turn out to be crucial for the fabrication of the nanowalls. Consequently, the growth of a BiVO(4) film begins from heteroepitaxy and undergoes an Ostwald ripening process to form an extended network, resulting in a c-orientation and exposing {010} facets. Through this process, it is much easier to obtain a range of nanowall films with different packing densities, as the surface state of ITO glass is alterable by adjusting the concentration of acid. The films can be directly used as an electrode, which exhibits an excellent response to visible light, especially light with low intensity, allowing for the electrical interconnection, highly active surface, appropriate orientation, and a good contact with the substrate. There are great benefits in improving the technique for detecting the weak light source signals.

  20. 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.

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

    Indian Academy of Sciences (India)

    life sciences, clinical medicine, and material chem- istry.11–14 Many .... environment and charge balance, the H3BTC should be fully deprotonated, but the ..... ous work, we now attempt to combine rare earth metal ions with adduct 1 to ...

  2. 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.

  3. 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.

  4. In situ XAS of the solvothermal decomposition of dithiocarbamate complexes

    NARCIS (Netherlands)

    Islam, H.-U.; Roffey, A.; Hollingsworth, N.; Catlow, R.; Wolthers, M.; de Leeuw, N.H.; Bras, W.; Sankar, G.; Hogarth, G.

    2012-01-01

    An in situ XAS study of the solvothermal decomposition of iron and nickel dithiocarbamate complexes was performed in order to gain understanding of the decomposition mechanisms. This work has given insight into the steps involved in the decomposition, showing variation in reaction pathways between

  5. Utilization of solvothermally grown InP/ZnS quantum dots as wavelength converters for fabrication of white light-emitting diodes.

    Science.gov (United States)

    Jang, Eun-Pyo; Yang, Heesun

    2013-09-01

    This work reports on a simple solvothermal synthesis of InP/ZnS core/shell quantum dots (QDs) using a much safer and cheaper phosphorus precursor of tris(dimethylamino)phosphine than the most popularly chosen tris(trimethylsilyl)phosphine. The band gap of InP QDs is facilely controlled by varying the solvothermal core growth time (4 vs. 6 h) with a fixed temperature of 150 degrees C, and the successive solvothermal ZnS shelling at 220 degrees C for 6 h results in green- and yellow-emtting InP/ZnS QD with emission quantum yield of 41-42%. The broad size distribution of as-synthesized InP/ZnS QDs, which appears to be inherent in the current solvothermal approach, is improved by a size-selective sorting procedure, and the emission properties of the resulting size-sorted QD fractions are investigated. To produce white emission for general lighting source, a blue light-emitting diode (LED) is combined with non-size-soroted green or yellow QDs as wavelength converters. Furthermore, the QD-LED that includes a blend of green and yellow QDs is fabricated to generate a white lighting source with an enhanced color rendering performance, and its electroluminescent properties are characterized in detail.

  6. 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.

  7. 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

  8. 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.

  9. 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

  10. Solvothermally synthesized europium-doped CdS nanorods: applications as phosphors

    International Nuclear Information System (INIS)

    Kumar, Sunil; Jindal, Zinki; Kumari, Nitu; Verma, Narendra Kumar

    2011-01-01

    To exploit the photoluminescent behavior of CdS at nanoscale with different doping concentration of europium—a rare earth element, we report the synthesis of Eu-doped CdS nanorods by using low temperature solvothermal process by using ethylenediamine. The outcomes can have future applications as phosphors, photovoltaic cells, lasers, light emitting diodes, bio-imaging, and sensors. The doping was confirmed by electron dispersive spectroscopy supported by X-ray diffraction. From scanning electron microscopy and transmission electron microscopy analysis it was observed that the average diameter of the Cd 1−x Eu x S nanorods is about 10–12 nm having lengths in the range of 50–100 nm. UV–Visible spectroscopy study was carried out to determine the band gap of the nanorods and the absorbance peaks showed blue shift with respect to the bulk CdS. The blue shift was also observed as the doping concentration of Eu increases. From photoluminescence (PL) studies at λ ex = 450 nm, peaks at 528 and 540 nm were observed due to CdS, peak at 570 nm is due to defects related transitions, while the peak at 613 nm is due to Eu. As the doping concentration of Eu is increased the intensity of the luminescent peak at 613 nm is increased. Thermogravimetric analysis showed the nanorods are thermally stable up to 300 °C. The traces of impurities adsorbed on the nanorods were confirmed by Fourier transform infrared spectroscopy.

  11. 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.

  12. Positron annihilation spectroscopic studies of solvothermally synthesized ZnO nanobipyramids and nanoparticles

    Science.gov (United States)

    Ghoshal, Tandra; Biswas, Subhajit; Kar, Soumitra; Chaudhuri, Subhadra; Nambissan, P. M. G.

    2008-02-01

    Zinc oxide (ZnO) samples in the form of hexagonal-based bipyramids and particles of nanometer dimensions were synthesized through solvothermal route and characterized by x-ray diffraction and transmission electron microscopy. Positron annihilation experiments were performed to study the structural defects such as vacancies and surfaces in these nanosystems. From coincidence Doppler broadening measurements, the positron trapping sites were identified as Zn vacancies or Zn-O-Zn trivacancy clusters. The positron lifetimes, their relative intensities, and the Doppler broadened lineshape parameter S all showed characteristic changes across the nanobipyramid size corresponding to the thermal diffusion length of positrons. In large nanobipyramids, vacancies within the crystallites also trapped positrons and the effects of agglomeration of such vacancies due to increased temperatures of synthesis were reflected in the variation of the annihilation parameters with their base diameters. The sizes of the nanoparticles used were all in the limit of thermal diffusion length of positrons and the annihilation characteristics were in accordance with the decreasing contribution from surfaces with increasing particle size.

  13. 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.

  14. 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.

  15. Controllable solvothermal synthesis and photocatalytic properties of complex (oxy)fluorides K{sub 2}TiOF{sub 4}, K{sub 3}TiOF{sub 5}, K{sub 7}Ti{sub 4}O{sub 4}F{sub 7} and K{sub 2}TiF{sub 6}

    Energy Technology Data Exchange (ETDEWEB)

    Sheng Jie [Division of Nanomaterials and Nanochemistry, Hefei National Laboratory for Physical Sciences at Microscale, Hefei, Anhui 230026 (China); Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026 (China); Tang Kaibin, E-mail: kbtang@ustc.edu.cn [Division of Nanomaterials and Nanochemistry, Hefei National Laboratory for Physical Sciences at Microscale, Hefei, Anhui 230026 (China); Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026 (China); Cheng Wei; Wang Junli; Nie Yanxiang; Yang Qing [Division of Nanomaterials and Nanochemistry, Hefei National Laboratory for Physical Sciences at Microscale, Hefei, Anhui 230026 (China); Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026 (China)

    2009-11-15

    Complex (oxy)fluorides K{sub 2}TiF{sub 6}, K{sub 2}TiOF{sub 4}, K{sub 3}TiOF{sub 5} and K{sub 7}Ti{sub 4}O{sub 4}F{sub 7} have been successfully synthesized for the first time through a controllable solvothermal route involving different solvents, for example, methanol, methanol-H{sub 2}O and methanol-H{sub 2}O{sub 2}. The as-prepared products were characterized by X-ray powder diffraction, N{sub 2} surface area adsorption, scanning electron microscope, Fourier transform infrared spectroscopy, UV-vis absorption spectra and X-ray fluorescence. The influences of reaction conditions such as the ratio of methanol to H{sub 2}O{sub 2} or methanol to H{sub 2}O, reaction temperature on the phase, crystallizability and purity of the (oxy)fluorides products were discussed in detail. Meanwhile, the photocatalytic behaviors of the as-prepared K{sub 2}TiF{sub 6}, K{sub 2}TiOF{sub 4}, K{sub 3}TiOF{sub 5} and K{sub 7}Ti{sub 4}O{sub 4}F{sub 7} were evaluated by degradation of rhodamine B molecules, and the results showed that all of the products possessed photocatalytic activities in the order of K{sub 2}TiOF{sub 4} > K{sub 2}TiF{sub 6} > K{sub 7}Ti{sub 4}O{sub 4}F{sub 7} > K{sub 3}TiOF{sub 5} at room temperature under the UV light.

  16. Solvothermal indium fluoride chemistry: Syntheses and crystal structures of K5In3F14, β-(NH4)3InF6 and [NH4]3[C6H21N4]2[In4F21

    International Nuclear Information System (INIS)

    Jayasundera, Anil C.A.; Goff, Richard J.; Li Yang; Finch, Adrian A.; Lightfoot, Philip

    2010-01-01

    The solvothermal syntheses and crystal structures of three indium fluorides are presented. K 5 In 3 F 14 (1) and β-(NH 4 ) 3 InF 6 (2) are variants on known inorganic structure types chiolite and cryolite, respectively, with the latter exhibiting a complex and apparently novel structural distortion. [NH 4 ] 3 [C 6 H 21 N 4 ] 2 [In 4 F 21 ] (3) represents a new hybrid composition displaying a unique trimeric metal fluoride building unit. - Graphical abstract: Solvothermal synthesis has been used to prepare three indium fluorides, including a novel hybrid material containing a unique [In 3 F 15 ] trimer templated by tren.

  17. Enhanced photocatalytic CO₂-reduction activity of electrospun mesoporous TiO₂ nanofibers by solvothermal treatment.

    Science.gov (United States)

    Fu, Junwei; Cao, Shaowen; Yu, Jiaguo; Low, Jingxiang; Lei, Yongpeng

    2014-06-28

    Photocatalytic reduction of CO2 into renewable hydrocarbon fuels using semiconductor photocatalysts is considered as a potential solution to the energy deficiency and greenhouse effect. In this work, mesoporous TiO2 nanofibers with high specific surface areas and abundant surface hydroxyl groups are prepared using an electrospinning strategy combined with a subsequent calcination process, followed by a solvothermal treatment. The solvothermally treated mesoporous TiO2 nanofibers exhibit excellent photocatalytic performance on CO2 reduction into hydrocarbon fuels. The significantly improved photocatalytic activity can be attributed to the enhanced CO2 adsorption capacity and the improved charge separation after solvothermal treatment. The highest activity is achieved for the sample with a 2-h solvothermal treatment, showing 6- and 25-fold higher CH4 production rate than those of TiO2 nanofibers without solvothermal treatment and P25, respectively. This work may also provide a prototype for studying the effect of solvothermal treatment on the structure and photocatalytic activity of semiconductor photocatalysts.

  18. 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.

  19. 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.

  20. 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.

  1. Precursor directed synthesis--"molecular" mechanisms in the Soft Chemistry approaches and their use for template-free synthesis of metal, metal oxide and metal chalcogenide nanoparticles and nanostructures.

    Science.gov (United States)

    Seisenbaeva, Gulaim A; Kessler, Vadim G

    2014-06-21

    This review provides an insight into the common reaction mechanisms in Soft Chemistry processes involved in nucleation, growth and aggregation of metal, metal oxide and chalcogenide nanoparticles starting from metal-organic precursors such as metal alkoxides, beta-diketonates, carboxylates and their chalcogene analogues and demonstrates how mastering the precursor chemistry permits us to control the chemical and phase composition, crystallinity, morphology, porosity and surface characteristics of produced nanomaterials.

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

    International Nuclear Information System (INIS)

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

    2012-01-01

    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 S2p 3/2 and S2p 1/2 electrons and the S2s 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 HgS 4 coordination environment, with a distinct Hg–S bond asymmetry.

  3. 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.

  4. Highly biocompatible, nanocrystalline hydroxyapatite synthesized in a solvothermal process driven by high energy density microwave radiation

    Science.gov (United States)

    Smolen, Dariusz; Chudoba, Tadeusz; Malka, Iwona; Kedzierska, Aleksandra; Lojkowski, Witold; Swieszkowski, Wojciech; Kurzydlowski, Krzysztof Jan; Kolodziejczyk-Mierzynska, Małgorzata; Lewandowska-Szumiel, Małgorzata

    2013-01-01

    A microwave, solvothermal synthesis of highly biocompatible hydroxyapatite (HAp) nanopowder was developed. The process was conducted in a microwave radiation field having a high energy density of 5 W/mL and over a time less than 2 minutes. The sample measurements included: powder X-ray diffraction, density, specific surface area, and chemical composition. The morphology and structure were investigated by scanning electron microscopy as well as transmission electron microscopy (TEM). The thermal behavior analysis was conducted using a simultaneous thermal analysis technique coupled with quadruple mass spectrometry. Additionally, Fourier transform infrared spectroscopy tests of heated samples were performed. A degradation test and a biocompatibility study in vitro using human osteoblast cells were also conducted. The developed method enables the synthesis of pure, fully crystalline hexagonal HAp nanopowder with a specific surface area close to 240 m2/g and a Ca/P molar ratio equal to 1.57. TEM measurements showed that this method results in particles with an average grain size below 6 nm. A 28-day degradation test conducted according to the ISO standard indicated a 22% loss of initial weight and a calcium ion concentration at 200 μmol/dm3 in the tris(hydroxymethyl)aminomethane hydrochloride test solution. The cytocompatibility of the obtained material was confirmed in a culture of human bone derived cells, both in an indirect test using the material extract, and in direct contact. A quantitative analysis was based on the 2,3-bis-(2-methoxy-4-nitro-5-sulfophenyl)-2H-tetrazolium-5-carboxanilide. Viability assay as well as on DNA content measurements in the PicoGreen test. Indirect observations were performed at one point in time according to the ISO standard for in vitro cytotoxicity (ie, after 24 hours of cell exposure to the extracts). The direct contact tests were completed at three time points: after 24 hours, on day 7, and on day 14 of a culture in an osteogenic

  5. 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.

  6. 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

  7. 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.

  8. Rose-like monodisperse bismuth subcarbonate hierarchical hollow microspheres: One-pot template-free fabrication and excellent visible light photocatalytic activity and photochemical stability for NO removal in indoor air

    International Nuclear Information System (INIS)

    Dong, Fan; Lee, S.C.; Wu, Zhongbiao; Huang, Yu; Fu, Min; Ho, Wing-Kei; Zou, Shichun; Wang, Bo

    2011-01-01

    Graphical abstract: Rose-like monodisperse hierarchical nitrogen doped (BiO) 2 CO 3 hollow microspheres fabricated by a one-pot template-free method exhibit excellent visible light photocatalytic activity and photochemical stability in the removal of NO in indoor air. The special hierarchical microstructure, the high charge separation efficiency and two-band-gap structure in all contribute to the outstanding photocatalytic performance. Highlights: → Rose-like monodisperse hierarchical (BiO) 2 CO 3 hollow microspheres are fabricated. → The (BiO) 2 CO 3 microspheres are self-assembled of single-crystalline nanosheets. → Nitrogen is in situ doped into the lattice of hierarchical (BiO) 2 CO 3 microspheres. → The (BiO) 2 CO 3 microspheres exhibit outstanding visible light activity for NO removal. → The (BiO) 2 CO 3 microspheres also exhibit high photochemical stability. - Abstract: Rose-like monodisperse hierarchical (BiO) 2 CO 3 hollow microspheres are fabricated by a one-pot template-free method for the first time based on hydrothermal treatment of ammonia bismuth citrate and urea in water. The microstructure and band structure of the as-prepared (BiO) 2 CO 3 superstructure are characterized in detail by X-ray diffraction, Raman spectroscopy, Fourier transform-infrared spectroscopy, transmission electron microscopy, scanning electron microscopy, N 2 adsorption-desorption isotherms, X-ray photoelectron spectroscopy and UV-vis diffuse reflectance spectroscopy. The monodisperse hierarchical (BiO) 2 CO 3 microspheres are constructed by the self-assembly of single-crystalline nanosheets. The aggregation of nanosheets result in the formation of three dimensional hierarchical framework containing mesopores and macropores, which is favorable for efficient transport of reaction molecules and harvesting of photo-energy. The result reveals the existence of special two-band-gap structure (3.25 and 2.0 eV) for (BiO) 2 CO 3 . The band gap of 3.25 eV is intrinsic and the

  9. 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.

  10. 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.

  11. Removal of brominated flame retardant from electrical and electronic waste plastic by solvothermal technique

    International Nuclear Information System (INIS)

    Zhang, Cong-Cong; Zhang, Fu-Shen

    2012-01-01

    Highlights: ► A process for brominated flame retardants (BFRs) removal in plastic was established. ► The plastic became bromine-free with the structure maintained after this treatment. ► BFRs transferred into alcohol solvent were easily debrominated by metallic copper. - Abstract: Brominated flame retardants (BFRs) in electrical and electronic (E and E) waste plastic are toxic, bioaccumulative and recalcitrant. In the present study, tetrabromobisphenol A (TBBPA) contained in this type of plastic was tentatively subjected to solvothermal treatment so as to obtain bromine-free plastic. Methanol, ethanol and isopropanol were examined as solvents for solvothermal treatment and it was found that methanol was the optimal solvent for TBBPA removal. The optimum temperature, time and liquid to solid ratio for solvothermal treatment to remove TBBPA were 90 °C, 2 h and 15:1, respectively. After the treatment with various alcohol solvents, it was found that TBBPA was finally transferred into the solvents and bromine in the extract was debrominated catalyzed by metallic copper. Bisphenol A and cuprous bromide were the main products after debromination. The morphology and FTIR properties of the plastic were generally unchanged after the solvothermal treatment indicating that the structure of the plastic maintained after the process. This work provides a clean and applicable process for BFRs-containing plastic disposal.

  12. Removal of brominated flame retardant from electrical and electronic waste plastic by solvothermal technique

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Cong-Cong [Research Center For Eco-Environmental Sciences, Chinese Academy of Sciences, 18 Shuangqing Road, Beijing 100085 (China); Zhang, Fu-Shen, E-mail: fszhang@rcees.ac.cn [Research Center For Eco-Environmental Sciences, Chinese Academy of Sciences, 18 Shuangqing Road, Beijing 100085 (China)

    2012-06-30

    Highlights: Black-Right-Pointing-Pointer A process for brominated flame retardants (BFRs) removal in plastic was established. Black-Right-Pointing-Pointer The plastic became bromine-free with the structure maintained after this treatment. Black-Right-Pointing-Pointer BFRs transferred into alcohol solvent were easily debrominated by metallic copper. - Abstract: Brominated flame retardants (BFRs) in electrical and electronic (E and E) waste plastic are toxic, bioaccumulative and recalcitrant. In the present study, tetrabromobisphenol A (TBBPA) contained in this type of plastic was tentatively subjected to solvothermal treatment so as to obtain bromine-free plastic. Methanol, ethanol and isopropanol were examined as solvents for solvothermal treatment and it was found that methanol was the optimal solvent for TBBPA removal. The optimum temperature, time and liquid to solid ratio for solvothermal treatment to remove TBBPA were 90 Degree-Sign C, 2 h and 15:1, respectively. After the treatment with various alcohol solvents, it was found that TBBPA was finally transferred into the solvents and bromine in the extract was debrominated catalyzed by metallic copper. Bisphenol A and cuprous bromide were the main products after debromination. The morphology and FTIR properties of the plastic were generally unchanged after the solvothermal treatment indicating that the structure of the plastic maintained after the process. This work provides a clean and applicable process for BFRs-containing plastic disposal.

  13. Preparation of low valent technetium metal-metal bonded species via solvothermal reduction of pertechnetate salts

    International Nuclear Information System (INIS)

    Kerlin, W.M.; Poineau, F.; Forster, P.M.; Czerwinski, K.R.; Sattelberger, A.P.

    2013-01-01

    A new one-step solvothermal synthesis route for reduction of pertechnetate salts to low valent technetium metal-metal bonded dimers will be presented. The reaction of potassium pertechnetate with glacial acetic acid plus either halo acids or halo salts under in-situ hydrogen production by sodium borohydride at various temperatures yields multiple products consisting of tetraacetate Tc-Tc (II,III) and Tc-Tc (III,III) paddle wheel dimers. Solid products isolated and analyzed via Single Crystal X-ray Diffraction (SC-XRD) in these reactions consist of polymeric chains Tc 2 +5 core: Tc 2 (μ-O 2 CCH 3 ) 4 (O 2 CCH 3 ), Tc 2 (μ-O 2 CCH 3 ) 4 Cl, Tc 2 (μ-O 2 CCH 3 ) 4 Br, Tc 2 (μ-O 2 CCH 3 ) 4 I, molecular Tc 2 +5 core: Tc 2 (μ-O 2 CCH 3 ) 3 Cl 2 (H 2 O) 2 ·H 2 O, K[Tc 2 (μ-O 2 CCH 3 ) 4 Br 2 ], and molecular Tc 2 +6 core: Tc 2 (μ-O 2 CCH 3 ) 4 Cl 2 , Tc 2 (μ-O 2 CCH 3 ) 4 Br 2 . Of the compounds listed, four are newly discovered using the one-step technique and two more additions to crystal database. Additional spectroscopic (X-ray Absorbance Fine Structure, UV-Vis, and FT-IR) characterization of the new compounds will be shown and used to propose a mechanism. Analysis of the mother liquor of each reaction by UV-Vis and formation of crystals over time due to oxidation of solutions affords a possible insight into mechanism of the Tc 2 +5 to Tc 2 +6 core formation. The oxidation states of Tc-Tc dimers formed is also dependent on temperature and pH of the starting solutions and will be explained in extensive detail. These one step reactions of reducing Tc(VII) to low valent technetium provides high yield intermediates for potential waste forms, use in nuclear fuel cycle separations, and radiopharmaceuticals. (author)

  14. Solvothermal preparation and fluorescent properties of color-tunable InP/ZnS quantum dots

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Ju Chul; Jang, Eun-Pyo [Department of Materials Science and Engineering, Hongik University, Seoul 121-791 (Korea, Republic of); Jang, Dong Seon; Choi, Yoonyoung; Choi, Moongoo [Materials and Devices Laboratory, LGE Advanced Research Institute, LG Electronics, Seoul 137-724 (Korea, Republic of); Yang, Heesun, E-mail: hyang@hongik.ac.kr [Department of Materials Science and Engineering, Hongik University, Seoul 121-791 (Korea, Republic of)

    2013-02-15

    This work reports on the solvothermal preparation and optical properties of InP core and InP/ZnS core/shell quantum dots (QDs). InP QDs are synthesized using a phosphorus (P) source of tris(dimethylamino)phosphine (P(N(CH{sub 3}){sub 2}){sub 3}) under the solvothermal conditions in the range of reaction temperature of 120-180 Degree-Sign C and reaction time of 12 h-1 week to tune their size. ZnS shelling is also solvothermally performed by varying the shell growth temperature from 180 to 220 Degree-Sign C for 6 h, and then respective InP and InP/ZnS QDs are subjected to the size-sorting procedure. Effects of the shelling temperature on the fluorescent attributes (emission peak wavelength, bandwidth, and quantum yield) of the resulting size-sorted InP/ZnS QD fractions are investigated. The qualitative information on the shell thickness as a function of shelling temperature is furthermore provided by x-ray diffraction and x-ray photoelectron spectroscopy. - Highlights: Black-Right-Pointing-Pointer InP/ZnS core/shell QDs are prepared using a P source of P(N(CH{sub 3}){sub 2}){sub 3} by a stepwise solvothermal approach. Black-Right-Pointing-Pointer Widely emission-tuable InP/ZnS QDs are realized by varying the solvothermal condition for core QD growth. Black-Right-Pointing-Pointer Effects of ZnS shelling temperature on fluorescent properties of InP/ZnS QDs are investigated.

  15. Solvothermal preparation and fluorescent properties of color-tunable InP/ZnS quantum dots

    International Nuclear Information System (INIS)

    Lee, Ju Chul; Jang, Eun-Pyo; Jang, Dong Seon; Choi, Yoonyoung; Choi, Moongoo; Yang, Heesun

    2013-01-01

    This work reports on the solvothermal preparation and optical properties of InP core and InP/ZnS core/shell quantum dots (QDs). InP QDs are synthesized using a phosphorus (P) source of tris(dimethylamino)phosphine (P(N(CH 3 ) 2 ) 3 ) under the solvothermal conditions in the range of reaction temperature of 120–180 °C and reaction time of 12 h−1 week to tune their size. ZnS shelling is also solvothermally performed by varying the shell growth temperature from 180 to 220 °C for 6 h, and then respective InP and InP/ZnS QDs are subjected to the size-sorting procedure. Effects of the shelling temperature on the fluorescent attributes (emission peak wavelength, bandwidth, and quantum yield) of the resulting size-sorted InP/ZnS QD fractions are investigated. The qualitative information on the shell thickness as a function of shelling temperature is furthermore provided by x-ray diffraction and x-ray photoelectron spectroscopy. - Highlights: ► InP/ZnS core/shell QDs are prepared using a P source of P(N(CH 3 ) 2 ) 3 by a stepwise solvothermal approach. ► Widely emission-tuable InP/ZnS QDs are realized by varying the solvothermal condition for core QD growth. ► Effects of ZnS shelling temperature on fluorescent properties of InP/ZnS QDs are investigated.

  16. 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

  17. 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.

  18. Highly biocompatible, nanocrystalline hydroxyapatite synthesized in a solvothermal process driven by high energy density microwave radiation

    Directory of Open Access Journals (Sweden)

    Smolen D

    2013-02-01

    Full Text Available Dariusz Smolen1, Tadeusz Chudoba1, Iwona Malka1, Aleksandra Kedzierska1, Witold Lojkowski1, Wojciech Swieszkowski2, Krzysztof Jan Kurzydlowski2, Malgorzata Kolodziejczyk-Mierzynska3, Malgorzata Lewandowska-Szumiel31Polish Academy of Science, Institute of High Pressure Physics, Warsaw, Poland; 2Faculty of Materials Engineering, Warsaw University of Technology, Warsaw, Poland; 3Department of Histology and Embryology, Center of Biostructure Research, Medical University of Warsaw, Warsaw, PolandAbstract: A microwave, solvothermal synthesis of highly biocompatible hydroxyapatite (HAp nanopowder was developed. The process was conducted in a microwave radiation field having a high energy density of 5 W/mL and over a time less than 2 minutes. The sample measurements included: powder X-ray diffraction, density, specific surface area, and chemical composition. The morphology and structure were investigated by scanning electron microscopy as well as transmission electron microscopy (TEM. The thermal behavior analysis was conducted using a simultaneous thermal analysis technique coupled with quadruple mass spectrometry. Additionally, Fourier transform infrared spectroscopy tests of heated samples were performed. A degradation test and a biocompatibility study in vitro using human osteoblast cells were also conducted. The developed method enables the synthesis of pure, fully crystalline hexagonal HAp nanopowder with a specific surface area close to 240 m2/g and a Ca/P molar ratio equal to 1.57. TEM measurements showed that this method results in particles with an average grain size below 6 nm. A 28-day degradation test conducted according to the ISO standard indicated a 22% loss of initial weight and a calcium ion concentration at 200 µmol/dm3 in the tris(hydroxymethylaminomethane hydrochloride test solution. The cytocompatibility of the obtained material was confirmed in a culture of human bone derived cells, both in an indirect test using the material

  19. A Comparative Study of Solvothermal and Sol-Gel-Derived Nanocrystalline Alumina Catalysts for Ethanol Dehydration

    Directory of Open Access Journals (Sweden)

    Mingkwan Wannaborworn

    2015-01-01

    Full Text Available The ethanol dehydration to ethylene over alumina catalysts prepared by solvothermal and sol-gel methods was investigated. Also, a commercial alumina was used for comparison purposes. The results showed that the catalytic activity depends on the properties of catalyst derived from different preparation methods and reaction temperature. The alumina synthesized by solvothermal method exhibited the highest activity. This can be attributed to the higher surface area and larger amount of acid site, especially the ratio of weak/strong acid strength as determined by N2 physisorption and NH3-TPD studies. The solvothermal-derived catalyst exhibited an excellent performance with complete ethanol conversion and 100% selectivity to ethylene at 350°C in comparison with other ones. In addition, we further studied the catalytic dehydration of alumina catalyst modified with Fe. The presence of 10 wt.% Fe decreased both conversion and ethylene selectivity. However, the acetaldehyde selectivity apparently increased. It was related to the dehydrogenation pathway that takes place on Fe species.

  20. Solvothermal and electrochemical synthetic method of HKUST-1 and its methane storage capacity

    Science.gov (United States)

    Wahyu Lestari, Witri; Adreane, Marisa; Purnawan, Candra; Fansuri, Hamzah; Widiastuti, Nurul; Budi Rahardjo, Sentot

    2016-02-01

    A comparison synthetic strategy of Metal-Organic Frameworks, namely, Hongkong University of Techhnology-1 {HKUST-1[Cu3(BTC)]2} (BTC = 1,3,5-benzene-tri-carboxylate) through solvothermal and electrochemical method in ethanol:water (1:1) has been conducted. The obtained material was analyzed using powder X-ray diffraction, Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FTIR), Thermo-Gravimetric Analysis (TGA) and Surface Area Analysis (SAA). While the voltage in the electrochemical method are varied, ranging from 12 to 15 Volt. The results show that at 15 V the texture of the material has the best degree of crystallinity and comparable with solvothermal product. This indicated from XRD data and supported by the SEM image to view the morphology. The thermal stability of the synthesized compounds is up to 320 °C. The shape of the nitrogen sorption isotherm of the compound corresponds to type I of the IUPAC adsorption isotherm classification for microporous materials with BET surface area of 629.2 and 324.3 m2/g (for solvothermal and electrochemical product respectively) and promising for gas storage application. Herein, the methane storage capacities of these compounds are also tested.

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

    Indian Academy of Sciences (India)

    Administrator

    dispersive X-ray microanalysis (EDAX), X-ray photoelectron spectroscopy (XPS), scanning electron micro- ... acicular shaped nanoparticles are seen in TEM images with an aspect ratio ~ 12; typically 8–12 nm wide and .... no impurity signal.

  2. 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.

  3. 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)

  4. MIL-125-NH2@TiO2 Core-Shell Particles Produced by a Post-Solvothermal Route for High-Performance Photocatalytic H2 Production.

    Science.gov (United States)

    Zhang, Bingxing; Zhang, Jianling; Tan, Xiuniang; Shao, Dan; Shi, Jinbiao; Zheng, Lirong; Zhang, Jing; Yang, Guanying; Han, Buxing

    2018-05-02

    Metal-organic frameworks (MOFs) have proven to be an interesting class of sacrificial precursors of functional inorganic materials for catalysis, energy storage, and conversion applications. However, the controlled synthesis of MOF-derived materials with desirable compositions, structures, and properties still remains a big challenge. Herein, we propose a post-solvothermal route for the outer-to-inner loss of organic linkers from MOF, which is simple, rapid, and controllable and can be operated at temperature much lower than that of the commonly adopted pyrolysis method. By such a strategy, the MIL-125-NH 2 particles coated by TiO 2 nanosheets were produced, and the thickness of TiO 2 shell can be easily tuned. The MIL-125-NH 2 @TiO 2 core-shell particles combine the advantages of highly active TiO 2 nanosheets, MIL-125-NH 2 photosensitizer, plenty of linker defects and oxygen vacancies, and mesoporous structure, which allows them to be utilized as photocatalysts for the visible-light-driven hydrogen production reaction. It is remarkable that the hydrogen evolution rate by MIL-125-NH 2 @TiO 2 can be enhanced 70 times compared with the pristine MIL-125-NH 2 . Such a route can be easily applied to the synthesis of different kinds of MOF-derived functional materials.

  5. The iron member of the CPO-27 coordination polymer series: Synthesis, characterization, and intriguing redox properties

    DEFF Research Database (Denmark)

    Märcz, Matthias; Johnsen, Rune; Dietzel, Pascal D.C.

    2012-01-01

    The microporous coordination polymer CPO-27-Fe was synthesized from iron salts and 2,5-dihydroxyterephthalic acid by microwave assisted solvothermal synthesis. The crystal structures of the as-synthesized compounds were determined by Rietveld refinement from powder X-ray diffraction data using...

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

    KAUST Repository

    Pan, Yichang; Liu, Yunyang; Zeng, Gaofeng; Zhao, Lan; Lai, Zhiping

    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.

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

    KAUST Repository

    Davaasuren, Bambar; Dashjav, Enkhtsetseg; Rothenberger, Alexander

    2014-01-01

    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

  8. 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

  9. 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.

  10. Capacitive and photocatalytic performance of Bi_2S_3 nanostructures synthesized by solvothermal method

    International Nuclear Information System (INIS)

    Liang, Kangqiang; Wang, Chenggang; Xu, Xijin; Leng, Jiancai; Ma, Hong

    2017-01-01

    Different Bi_2S_3 nanoarchitectures (nanorods and nanobelts) were successfully synthesized with a facile solvothermal method at different temperature. The nanobelts transformed into nanorods when the temperature was 200 °C increased from 150 °C. The nanorod-morphology was kept even the temperature was further increased. The galvanostatic charge/discharge performance showed that the prepared Bi_2S_3 nanorods had good performance of discharge efficiency at current density from 1 A g"−"1 to 4 A g"−"1. The specific capacitance was 270 F g"−"1 at a current density of 1 A g"−"1. Furthermore, the nanorods were also used as the efficient UV-light photocatalysts for the degradation of Rhodamine B (RhB), which showed almost complete degradation (∼87%) of RhB dye at 100 min. - Highlights: • Bi_2S_3 nanorods were successfully synthesized with a facile solvothermal method. • The specific capacitance can be 270 F g"−"1 at a current density of 1 A g"−"1. • 87% of RhB dye can be degraded at 100 min.

  11. 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.

  12. [Cu(I)(bpp)]BF4: the first extended coordination network prepared solvothermally in an ionic liquid solvent.

    Science.gov (United States)

    Jin, Kun; Huang, Xiaoying; Pan, Long; Li, Jing; Appel, Aaron; Wherland, Scot; Pang, Long

    2002-12-07

    Use of an ionic liquid [bmim][BF4] (bmim = 1-butyl-3-methylimidazolium) as solvent has resulted in the first extended coordination structure, the two-dimensional network [Cu(bpp)]BF4 [bpp = 1,3-bis(4-pyridyl)propane], produced via a solvothermal route.

  13. 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.

  14. Effect of Cu/In molar ratio on the microstructural and optical properties of microcrystalline CuInS2 prepared by solvothermal route

    International Nuclear Information System (INIS)

    Das, Kajari; Panda, Subhendu K.; Gorai, Soma; Mishra, Pratima; Chaudhuri, Subhadra

    2008-01-01

    Synthesis and characterization of CuInS 2 powder sample prepared by a simple and convenient solvothermal method is reported. The influence of the variation of Cu/In molar ratio from 0.69 to 1.25 on the particle morphology, crystal structure and optical properties of CuInS 2 samples was studied. The X-ray diffraction studies indicated that the samples were polycrystalline in nature. SEM images of the samples revealed that the copper-rich products were uniform microspheres with smooth surfaces, whereas microspheres formed by network of interconnected flakes were obtained for indium-rich products. The optical band gaps (E g ) of the products decreased from 1.60 to 1.43 eV with variation of Cu/In molar ratio. The variation of the Urbach tail width with Cu/In molar ratio indicated that the density of the defects is much higher for the indium-rich CuInS 2 , which was clearly revealed from Raman measurements

  15. 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.

  16. p-type ZnS:N nanowires: Low-temperature solvothermal doping and optoelectronic properties

    International Nuclear Information System (INIS)

    Wang, Ming-Zheng; Xie, Wei-Jie; Hu, Han; Yu, Yong-Qiang; Wu, Chun-Yan; Wang, Li; Luo, Lin-Bao

    2013-01-01

    Nitrogen doped p-type ZnS nanowires (NWs) were realized using thermal decomposition of triethylamine at a mild temperature. Field-effect transistors made from individual ZnS:N NWs revealed typical p-type conductivity behavior, with a hole mobility of 3.41 cm 2 V −1 s −1 and a hole concentration of 1.67 × 10 17  cm −3 , respectively. Further analysis found that the ZnS:N NW is sensitive to UV light irradiation with high responsivity, photoconductive gain, and good spectral selectivity. The totality of this study suggests that the solvothermal doping method is highly feasible to dope one dimensional semiconductor nanostructures for optoelectronic devices application

  17. 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

  18. Surfactant-assisted solvothermal preparation of submicrometer-sized hollow hematite particles and their photocatalytic activity

    International Nuclear Information System (INIS)

    Lian Suoyuan; Wang Enbo; Gao Lei; Wu Di; Song Yanli; Xu Lin

    2006-01-01

    Submicrometer-sized hollow hematite particles were prepared through a surfactant-assisted solvothermal process. The amount of FeCl 3 .H 2 O and cetyltrimethylammonium bromide, and the acidity of the solution were systematically altered to study their effects on the final results. Hollow hematite particles with shapes from sphere, ellipsoid to peanut were obtained. Their sizes range from 500 nm to 2 μm with shell thickness from 100 to 500 nm. Powder X-ray diffraction, scanning electron microscopy, transmission electron microscopy and selected area electron diffraction were applied to investigate the products' crystallinity, purity, morphology, size and structural features. Finally, the study on the photocatalysis of Fe 2 O 3 for the destruction of diethyl phthalate in water was carried out. The result proved that Fe 2 O 3 hollow particles were effective photocatalysts for the degradation of DEP, with 96.8% destruction ratio being obtained within 60 min

  19. 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

  20. 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...

  1. 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.

  2. 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%.

  3. Surface-roughness-assisted formation of large-scale vertically aligned CdS nanorod arrays via solvothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Minmin [National Laboratory of Solid State Microstructures, School of Electronic Science and Engineering, Nanjing University, Nanjing 210093 (China); Yan, Shancheng, E-mail: yansc@njupt.edu.cn [National Laboratory of Solid State Microstructures, School of Electronic Science and Engineering, Nanjing University, Nanjing 210093 (China); School of Geography and Biological Information, Nanjing University of Posts and Telecommunications, Nanjing 210046 (China); Shi, Yi, E-mail: yshi@nju.edu.cn [National Laboratory of Solid State Microstructures, School of Electronic Science and Engineering, Nanjing University, Nanjing 210093 (China); Yang, Meng; Sun, Huabin; Wang, Jianyu; Yin, Yao; Gao, Fan [National Laboratory of Solid State Microstructures, School of Electronic Science and Engineering, Nanjing University, Nanjing 210093 (China)

    2013-05-15

    Large-scale cadmium sulfide (CdS) nanorod arrays were successfully synthesized on several different substrates through solvothermal reaction. During the growth experiments, we observed that the adhesion strength of the CdS nanorod arrays to different substrates differed dramatically, causing some of the CdS coating being easily flushed away by deionized water (DI water). With doubts and suspicions, we seriously investigate the original morphology of all the substrates by using atomic force microscopy (AFM). The phase, morphology, crystal structure and photoelectric property of all the products were characterized by X-ray diffractometer (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy and current–voltage (I–V) probe station. The growth mechanism of solvothermal reaction was proposed on the basis of all the characterizations. Our approach presents a universal method of liquid phase epitaxy of 1D material on a wide range of substrates of any shape.

  4. Solvothermal growth of a ruthenium metal-organic framework featuring HKUST-1 structure type as thin films on oxide surfaces.

    Science.gov (United States)

    Kozachuk, Olesia; Yusenko, Kirill; Noei, Heshmat; Wang, Yuemin; Walleck, Stephan; Glaser, Thorsten; Fischer, Roland A

    2011-08-14

    Phase-pure crystalline thin films of a mixed-valence Ru(2)(II,III) metal-organic framework with 1,3,5-benzenetricarboxylate (btc) as a linker were solvothermally grown on amorphous alumina and silica surfaces. Based on the Rietveld refinement, the structure of Ru-MOF was assigned to be analogous to [Cu(3)(btc)(2)] (HKUST-1). This journal is © The Royal Society of Chemistry 2011

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

    International Nuclear Information System (INIS)

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

    2015-01-01

    Graphical abstract: - Highlights: • In 2 S 3 sensitized TiO 2 anode is prepared by combining SILAR with solvothermal process. • The deposition cycle in SILAR process has an impact on cell performances. • A promising conversion efficiency of 1.39% is obtained for the optimal device. • The cell performances are markedly increased compared with SILAR technique. - Abstract: 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 (In 2 S 3 ) quantum dot-sensitized titanium dioxide (TiO 2 ) photoanode by combining successive ionic layer adsorption and reaction (SILAR) with solvothermal processes. The resultant QDSC consists of an In 2 S 3 sensitized TiO 2 photoanode, a liquid polysulfide electrolyte, and a Co 0.85 Se 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%.

  6. 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.

  7. 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

  8. 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).

  9. Preparation of CuIn1-xGaxS2 (x = 0.5) flowers consisting of nanoflakes via a solvothermal method

    International Nuclear Information System (INIS)

    Liang Xiaojuan; Zhong Jiasong; Yang Fan; Hua Wei; Jin Huaidong; Liu Haitao; Sun Juncai; Xiang Weidong

    2011-01-01

    Highlights: → We report for the first time a small biomolecule-assisted route using L-cysteine as sulfur source and complexing agent to synthesis CuIn 0.5 Ga 0.5 S 2 crystals. → The possible mechanisms leading to CuIn 0.5 Ga 0.5 S 2 flowers consisting of nanoflakes were proposed. → In addition, the morphology, structure, and phase composition of the as-prepared CuIn 0.5 Ga 0.5 S 2 products were investigated in detail by XRD, FESEM, EDS, XPS, TEM (HRTEM) and SAED. - Abstract: CuIn 1-x Ga x S 2 (x = 0.5) flowers consisting of nanoflakes were successfully prepared by a biomolecule-assisted solvothermal route at 220 deg. C for 10 h, employing copper chloride, gallium chloride, indium chloride and L-cysteine as precursors. The biomolecule L-cysteine acting as sulfur source was found to play a very important role in the formation of the final product. The diameter of the CuIn 0.5 Ga 0.5 S 2 flowers was 1-2 μm, and the thickness of the flakes was about 15 nm. The obtained products were characterized by X-ray diffraction (XRD), energy dispersion spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction spectroscopy (SAED), and UV-vis absorption spectroscopy. The influences of the reaction temperature, reaction time, sulfur source and the molar ratio of Cu-to-L-cysteine (reactants) on the formation of the target compound were investigated. The formation mechanism of the CuIn 0.5 Ga 0.5 S 2 flowers consisting of flakes was discussed.

  10. 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.

  11. Study of structural and optical properties of CaMoO{sub 4} nanoparticles synthesized by the microwave-assisted solvothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Botelho, G., E-mail: gleice.lorena@gmail.com [INCTMN-UFSCar, Universidade Federal de São Carlos, P.O. Box 676, 13565-905, São Carlos, SP (Brazil); Nogueira, I.C. [Instituto Federal do Maranhão, PPG em Engenharia de Materiais, 65030-005, São Luís, MA (Brazil); Moraes, E. [INCTMN-UFSCar, Universidade Federal de São Carlos, P.O. Box 676, 13565-905, São Carlos, SP (Brazil); Longo, E. [INCTMN-UNESP, Universidade Estadual Paulista, P.O. Box 355, CEP, 14801-907, Araraquara, SP (Brazil)

    2016-11-01

    Calcium molybdate (CaMoO{sub 4}) nanoparticles were synthesized by using a rapid assisted-microwave solvothermal method. X-ray diffraction measurements, Fourier transform Raman and Fourier transform infrared spectroscopies, revealed that the samples all have a scheelite-type tetragonal structure. In addition, the data obtained from the Rietveld refinements revealed distortions of the [Ca−O] and [Mo−O] bonds that led, in turn, to distortions of the [CaO{sub 8}] and [MoO{sub 4}] clusters. The presence of irregular spherical-like CaMoO{sub 4} nanoparticles and the corresponding crystallographic arrangement were confirmed and determined via transmission electron microscopy and high resolution transmission electron microscopy, respectively. First-principles quantum mechanical calculations based on the density functional theory at the B3LYP level were employed in order to understand the band structure and density of states of CaMoO{sub 4} in the excited singlet and triplet states. Furthermore, the optical properties were investigated by performing ultraviolet–visible spectroscopy and photoluminescence (PL) measurements. Maximum PL emission of CaMoO{sub 4} powders was detected in the green-region wavelength of the electromagnetic spectrum; this emission was attributed to the distorted [MoO{sub 4}] clusters. - Highlights: • Effect of propane-1,3-diol in the synthesis of nanoparticles by a rapid method. • Utilization of first-principles quantum mechanical calculations. • Investigation of photoluminescent properties of CaMoO{sub 4} nanoparticles.

  12. Room temperature chemical synthesis of highly oriented PbSe nanotubes based on negative free energy of formation

    Energy Technology Data Exchange (ETDEWEB)

    Sankapal, B.R., E-mail: brsankapal@rediffmail.com [Thin Film and Nano Science Laboratory, Department of Physics, School of Physical Sciences, North Maharashtra University, Jalgaon 425 001 (MS) (India); Ladhe, R.D.; Salunkhe, D.B.; Baviskar, P.K. [Thin Film and Nano Science Laboratory, Department of Physics, School of Physical Sciences, North Maharashtra University, Jalgaon 425 001 (MS) (India); Gupta, V.; Chand, S. [Organic and Hybrid Solar Cell, Physics of Energy Harvesting Division, Dr. K.S. Krishnan Marg, National Physical Laboratory, New Delhi 110012 (India)

    2011-10-13

    Highlights: > Simple, inexpensive and room temperature chemical synthesis route. > Highly oriented PbSe nanotubes from Cd(OH){sub 2} nanowires through lead hydroxination. > The process was template free without the use of any capping agent. > Reaction kinetics was accomplished due to more negative free energy of formation. > The ion exchange mechanism due to difference in the solubility products. - Abstract: The sacrificial template free chemical synthesis of PbSe nanotubes at room temperature has been performed by lead hydroxination from cadmium hydroxide nanowires. This process was based on the ion exchange reaction to replace Cd{sup 2+} with Pb{sup 2+} ions from hydroxyl group followed by replacement of hydroxyl group with selenium ions. The reaction kinetics was accomplished due to more negative free energy of formation and thus the difference in the solubility products. The formed nanotubes were inclusive of Pb and Se with proper inter-chemical bonds with preferred orientations having diameter in tens of nanometer. These nanotubes can have future applications in electronic, optoelectronics and photovoltaic's as well.

  13. Room temperature chemical synthesis of highly oriented PbSe nanotubes based on negative free energy of formation

    International Nuclear Information System (INIS)

    Sankapal, B.R.; Ladhe, R.D.; Salunkhe, D.B.; Baviskar, P.K.; Gupta, V.; Chand, S.

    2011-01-01

    Highlights: → Simple, inexpensive and room temperature chemical synthesis route. → Highly oriented PbSe nanotubes from Cd(OH) 2 nanowires through lead hydroxination. → The process was template free without the use of any capping agent. → Reaction kinetics was accomplished due to more negative free energy of formation. → The ion exchange mechanism due to difference in the solubility products. - Abstract: The sacrificial template free chemical synthesis of PbSe nanotubes at room temperature has been performed by lead hydroxination from cadmium hydroxide nanowires. This process was based on the ion exchange reaction to replace Cd 2+ with Pb 2+ ions from hydroxyl group followed by replacement of hydroxyl group with selenium ions. The reaction kinetics was accomplished due to more negative free energy of formation and thus the difference in the solubility products. The formed nanotubes were inclusive of Pb and Se with proper inter-chemical bonds with preferred orientations having diameter in tens of nanometer. These nanotubes can have future applications in electronic, optoelectronics and photovoltaic's as well.

  14. Research Update: Facile synthesis of CoFe2O4 nano-hollow spheres for efficient bilirubin adsorption

    Science.gov (United States)

    Rakshit, Rupali; Pal, Monalisa; Chaudhuri, Arka; Mandal, Madhuri; Mandal, Kalyan

    2015-11-01

    Herein, we report an unprecedented bilirubin (BR) adsorption efficiency of CoFe2O4 (CFO) nanostructures in contrast to the commercially available activated carbon and resin which are generally used for haemoperfusion and haemodialysis. We have synthesized CFO nanoparticles of diameter 100 nm and a series of nano-hollow spheres of diameter 100, 160, 250, and 350 nm using a simple template free solvothermal technique through proper variation of reaction time and capping agent, oleylamine (OLA), respectively, and carried out SiO2 coating by employing Stöber method. The comparative BR adsorption study of CFO and SiO2 coated CFO nanostructures indicates that apart from porosity and hollow configuration of nanostructures, the electrostatic affinity between anionic carboxyl group of BR and cationic amine group of OLA plays a significant role in adsorbing BR. Finally, we demonstrate that the BR adsorption capacity of the nanostructures can be tailored by varying the morphology as well as size of the nanostructures. We believe that our developed magnetic nanostructures could be considered as a potential material towards therapeutic applications against hyperbilirubinemia.

  15. 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

  16. 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.

  17. 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.

  18. 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.

  19. 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,.

  20. 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.

  1. 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

  2. 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

    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...... 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 CO2...... 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....

  3. 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

    interface coatings for SiC/SiC composites. This approach was found to be promising and deserves further evaluation in a systematic mode. 15. SUBJECT TERMS...approximately 200 words ) factual summary of the most significant information. 1 S. SUBJECT TERMS. Key words or phrases identifying major concepts in the...improved adhesion, wettability, electroactivity, and water -repellant qualities, among others. In these cases, the reactive bonding sites are already

  4. A shortcut hydrothermal strategy for the synthesis of zinc nanowires

    International Nuclear Information System (INIS)

    Hu Jianqiang; Chen Zhiwu; Xie Jingsi; Yu Ying

    2008-01-01

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

  5. Capacitive and photocatalytic performance of Bi{sub 2}S{sub 3} nanostructures synthesized by solvothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Liang, Kangqiang, E-mail: liang_kangqiang@126.com [School of Physics and Electronics, Shandong Normal University, Jinan 250014 (China); Wang, Chenggang, E-mail: ujnsps_wangchg@163.com [School of Physics and Technology, University of Jinan, 336 West Road of Nan Xinzhuang, Jinan, 250022, Shandong Province (China); Xu, Xijin, E-mail: sps_xuxj@ujn.edu.cn [School of Physics and Technology, University of Jinan, 336 West Road of Nan Xinzhuang, Jinan, 250022, Shandong Province (China); Key Laboratory for Photonic and Electric Bandgap Materials, Ministry of Education, Harbin Normal University, Harbin, 150025 (China); Leng, Jiancai, E-mail: jiancaileng@qlu.edu.cn [School of Science, Qilu University of Technology, Jinan 250353 (China); Ma, Hong, E-mail: mahong@sdnu.edu.cn [School of Physics and Electronics, Shandong Normal University, Jinan 250014 (China)

    2017-02-12

    Different Bi{sub 2}S{sub 3} nanoarchitectures (nanorods and nanobelts) were successfully synthesized with a facile solvothermal method at different temperature. The nanobelts transformed into nanorods when the temperature was 200 °C increased from 150 °C. The nanorod-morphology was kept even the temperature was further increased. The galvanostatic charge/discharge performance showed that the prepared Bi{sub 2}S{sub 3} nanorods had good performance of discharge efficiency at current density from 1 A g{sup −1} to 4 A g{sup −1}. The specific capacitance was 270 F g{sup −1} at a current density of 1 A g{sup −1}. Furthermore, the nanorods were also used as the efficient UV-light photocatalysts for the degradation of Rhodamine B (RhB), which showed almost complete degradation (∼87%) of RhB dye at 100 min. - Highlights: • Bi{sub 2}S{sub 3} nanorods were successfully synthesized with a facile solvothermal method. • The specific capacitance can be 270 F g{sup −1} at a current density of 1 A g{sup −1}. • 87% of RhB dye can be degraded at 100 min.

  6. Microstructure and electrical-optical properties of cesium tungsten oxides synthesized by solvothermal reaction followed by ammonia annealing

    International Nuclear Information System (INIS)

    Liu Jingxiao; Ando, Yoshihiko; Dong Xiaoli; Shi Fei; Yin Shu; Adachi, Kenji; Chonan, Takeshi; Tanaka, Akikazu; Sato, Tsugio

    2010-01-01

    Cesium tungsten oxides (Cs x WO 3 ) were synthesized by solvothermal reactions using ethanol and 57.1 vol% ethanol aqueous solution at 200 o C for 12 h, and the effects of post annealing in ammonia atmosphere on the microstructure and electrical-optical properties were investigated. Agglomerated particles consisting of disk-like nanoparticles and nanorods of Cs x WO 3 were formed in the pure ethanol and ethanol aqueous solutions, respectively. The samples retained the original morphology and crystallinity after annealing in ammonia atmosphere up to 500 o C, while a small amount of nitrogen ion were incorporated in the lattice. The as-prepared Cs x WO 3 sample showed excellent near infrared (NIR) light shielding ability as well as high transparency in the visible light region. The electrical resistivity of the pressed pellets of the powders prepared in pure ethanol and 57.1 vol% ethanol aqueous solution greatly decreased after ammonia annealing at 500 o C, i.e., from 734 to 31.5 and 231 to 3.58 Ω cm, respectively. - Graphical abstract: Cesium tungsten oxides (Cs x WO 3 ) with different morphology were synthesized by solvothermal reaction, and the effects of post-ammonia annealing on the microstructure and electrical-optical properties were investigated.

  7. 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.

  8. Highly effective synthesis of a cobalt(ii) metal-organic coordination polymer by using continuous flow chemistry.

    Science.gov (United States)

    Gong, Chunhua; Zhang, Junyong; Zeng, Xianghua; Xie, Jingli

    2016-12-20

    The coordination polymer [Co 2 L 4 (H 2 O) 2 ]·CH 3 CN·H 2 O (HL = (E)-2-[2-(4-chlorophenyl)vinyl]-8-hydroxyquinoline) has been achieved with 95% yield by using an Asia flow synthesis system (chip reactor). Compared with the conventional batch-type methods such as diffusion, reflux and solvothermal reactions, higher yielding reactions carried out in a flow reactor have demonstrated that this technique is a powerful strategy to obtain coordination compounds.

  9. Preparation of CuIn{sub 1-x}Ga{sub x}S{sub 2} (x = 0.5) flowers consisting of nanoflakes via a solvothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Liang Xiaojuan [College of Chemistry and Materials Engineering, Wenzhou University, Wenzhou, Zhejiang Province 325035 (China); Institute of Materials and Technology, Dalian Maritime University, Dalian 116026 (China); Zhong Jiasong; Yang Fan; Hua Wei; Jin Huaidong [College of Chemistry and Materials Engineering, Wenzhou University, Wenzhou, Zhejiang Province 325035 (China); Liu Haitao, E-mail: lht@wzu.edu.cn [College of Chemistry and Materials Engineering, Wenzhou University, Wenzhou, Zhejiang Province 325035 (China); Sun Juncai [Institute of Materials and Technology, Dalian Maritime University, Dalian 116026 (China); Xiang Weidong, E-mail: weidongxiang@yahoo.com.cn [College of Chemistry and Materials Engineering, Wenzhou University, Wenzhou, Zhejiang Province 325035 (China)

    2011-05-26

    Highlights: > We report for the first time a small biomolecule-assisted route using L-cysteine as sulfur source and complexing agent to synthesis CuIn{sub 0.5}Ga{sub 0.5}S{sub 2} crystals. > The possible mechanisms leading to CuIn{sub 0.5}Ga{sub 0.5}S{sub 2} flowers consisting of nanoflakes were proposed. > In addition, the morphology, structure, and phase composition of the as-prepared CuIn{sub 0.5}Ga{sub 0.5}S{sub 2} products were investigated in detail by XRD, FESEM, EDS, XPS, TEM (HRTEM) and SAED. - Abstract: CuIn{sub 1-x}Ga{sub x}S{sub 2} (x = 0.5) flowers consisting of nanoflakes were successfully prepared by a biomolecule-assisted solvothermal route at 220 deg. C for 10 h, employing copper chloride, gallium chloride, indium chloride and L-cysteine as precursors. The biomolecule L-cysteine acting as sulfur source was found to play a very important role in the formation of the final product. The diameter of the CuIn{sub 0.5}Ga{sub 0.5}S{sub 2} flowers was 1-2 {mu}m, and the thickness of the flakes was about 15 nm. The obtained products were characterized by X-ray diffraction (XRD), energy dispersion spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction spectroscopy (SAED), and UV-vis absorption spectroscopy. The influences of the reaction temperature, reaction time, sulfur source and the molar ratio of Cu-to-L-cysteine (reactants) on the formation of the target compound were investigated. The formation mechanism of the CuIn{sub 0.5}Ga{sub 0.5}S{sub 2} flowers consisting of flakes was discussed.

  10. Review on the progress in synthesis and application of magnetic carbon nanocomposites

    Science.gov (United States)

    Zhu, Maiyong; Diao, Guowang

    2011-07-01

    This review focuses on the synthesis and application of nanostructured composites containing magnetic nanostructures and carbon-based materials. Great progress in fabrication of magnetic carbon nanocomposites has been made by developing methods including filling process, template-based synthesis, chemical vapor deposition, hydrothermal/solvothermal method, pyrolysis procedure, sol-gel process, detonation induced reaction, self-assembly method, etc. The applications of magnetic carbon nanocomposites expanded to a wide range of fields such as environmental treatment, microwave absorption, magnetic recording media, electrochemical sensor, catalysis, separation/recognization of biomolecules and drug delivery are discussed. Finally, some future trends and perspectives in this research area are outlined.

  11. Surfactant assisted synthesis of lamellar nanostructured LiFePO4 at 388 K

    International Nuclear Information System (INIS)

    Liu Chao; Ma Dongxia; Ji Xiujie; Zhao Shanshan; Li Song

    2011-01-01

    Lamellar nanostructured lithium iron phosphate (Lα-LFP) was synthesized using anion surfactant sodium dodecyl sulphonate (SDS) as supermolecular template in water-ethanol media at 388 K under self-generated pressure. FeSO 4 , (NH 4 ) 2 HPO 4 and LiOH were used as Fe, P and Li sources, respectively. The inorganic phase was analyzed by X-ray diffraction (XRD). The morphology and the lamellar nanostructure were observed by field emitting scanning electron microscopy (FESEM). The results showed that the synthesized Lα-LFP presents not only the ordered lamellar microstructure accumulated by 20-40-nm thick LFP layers, but also the consequent self-assembled blocky particles of 0.5-1 μm. In contrast, template free LFP (TF-LFP) show a flake-shaped and mess-orientated microstructure. As a soft template, SDS played the roles of inducing the lamellar nanostructure, purifying the inorganic phase and decreasing the synthesis temperature.

  12. 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

  13. 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.

  14. 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.

  15. One-pot solvothermal route to self-assembly of cauliflower-shaped CdS microspheres

    Energy Technology Data Exchange (ETDEWEB)

    Ge Ming [Tianjin Key Laboratory of Environmental Remediation and Pollution Control, Nankai University, Tianjin 300071 (China); Cui Yao [Institute of New Energy Material Chemistry, and Key Laboratory of Advanced Energy Materials Chemistry (Ministry of Education), Nankai University, Tianjin 300071 (China); Liu Lu, E-mail: liul@nankai.edu.cn [Tianjin Key Laboratory of Environmental Remediation and Pollution Control, Nankai University, Tianjin 300071 (China); Zhou Zhen, E-mail: zhouzhen@nankai.edu.cn [Institute of New Energy Material Chemistry, and Key Laboratory of Advanced Energy Materials Chemistry (Ministry of Education), Nankai University, Tianjin 300071 (China)

    2011-05-15

    Nearly monodispersed cauliflower-shaped CdS microspheres were prepared through a simple one-step solvothermal route on a large scale by employing sodium dodecyl sulfate (SDS) as the surfactant. Images by field emission scanning electron microscope (FESEM) and transmission electron microscope (TEM) indicate that cauliflower-shaped CdS microspheres with diameters in the range from 1.3 to 4.5 {mu}m are assembled by nanoparticles with an average diameter of approximately 30 nm. The possible formation mechanism of the cauliflower-shaped CdS microspheres was also proposed. The photovoltaic activity of cauliflower-shaped CdS architectures has been investigated, indicating that the as-obtained CdS microspheres exhibited higher photovoltaic performance in comparison with CdS nanoparticles.

  16. 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.

  17. 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

  18. 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.

  19. 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.

  20. A strategy of combining SILAR with solvothermal process for In{sub 2}S{sub 3} sensitized quantum dot-sensitized solar cells

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Peizhi, E-mail: pzhyang@hotmail.com [Key Laboratory of Advanced Technique & Preparation for Renewable Energy Materials, Ministry of Education, Yunnan Normal University, Kunming 650500 (China); Tang, Qunwei, E-mail: tangqunwei@ouc.edu.cn [Institute of Materials Science and Engineering, Ocean University of China, Qingdao 266100 (China); Ji, Chenming; Wang, Haobo [Institute of Materials Science and Engineering, Ocean University of China, Qingdao 266100 (China)

    2015-12-01

    Graphical abstract: - Highlights: • In{sub 2}S{sub 3} sensitized TiO{sub 2} anode is prepared by combining SILAR with solvothermal process. • The deposition cycle in SILAR process has an impact on cell performances. • A promising conversion efficiency of 1.39% is obtained for the optimal device. • The cell performances are markedly increased compared with SILAR technique. - Abstract: 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 (In{sub 2}S{sub 3}) quantum dot-sensitized titanium dioxide (TiO{sub 2}) photoanode by combining successive ionic layer adsorption and reaction (SILAR) with solvothermal processes. The resultant QDSC consists of an In{sub 2}S{sub 3} sensitized TiO{sub 2} photoanode, a liquid polysulfide electrolyte, and a Co{sub 0.85}Se 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%.

  1. Facile consecutive solvothermal growth of highly fluorescent InP/ZnS core/shell quantum dots using a safer phosphorus source.

    Science.gov (United States)

    Byun, Ho-June; Song, Woo-Seuk; Yang, Heesun

    2011-06-10

    The work presents a facile, stepwise synthetic approach for the production of highly fluorescent InP/ZnS core/shell quantum dots (QDs) by using a safer phosphorus (P) precursor. First, InP quantum dots (QDs) were solvothermally prepared at 180 °C for 24 h by using a P source of P(N(CH(3))(2))(3). The as-grown InP QDs were consecutively placed in another solvothermal condition for ZnS shell overcoating. In contrast to the almost non-fluorescent InP QDs, due to their highly defective surface states, the ZnS-coated InP QDs were highly fluorescent as a result of effective surface passivation. After the shell growth, the resulting InP/ZnS core/shell QDs were subjected to a size-sorting processing, by which red- to green-emitting QDs with quantum yields (QYs) of 24-60% were produced. Solvothermal shell growth parameters such as the reaction time and Zn/In solution concentration ratio were varied and optimized toward the highest QYs of core/shell QDs.

  2. Facile consecutive solvothermal growth of highly fluorescent InP/ZnS core/shell quantum dots using a safer phosphorus source

    International Nuclear Information System (INIS)

    Byun, Ho-June; Song, Woo-Seuk; Yang, Heesun

    2011-01-01

    The work presents a facile, stepwise synthetic approach for the production of highly fluorescent InP/ZnS core/shell quantum dots (QDs) by using a safer phosphorus (P) precursor. First, InP quantum dots (QDs) were solvothermally prepared at 180 deg. C for 24 h by using a P source of P(N(CH 3 ) 2 ) 3 . The as-grown InP QDs were consecutively placed in another solvothermal condition for ZnS shell overcoating. In contrast to the almost non-fluorescent InP QDs, due to their highly defective surface states, the ZnS-coated InP QDs were highly fluorescent as a result of effective surface passivation. After the shell growth, the resulting InP/ZnS core/shell QDs were subjected to a size-sorting processing, by which red- to green-emitting QDs with quantum yields (QYs) of 24-60% were produced. Solvothermal shell growth parameters such as the reaction time and Zn/In solution concentration ratio were varied and optimized toward the highest QYs of core/shell QDs.

  3. Facile consecutive solvothermal growth of highly fluorescent InP/ZnS core/shell quantum dots using a safer phosphorus source

    Science.gov (United States)

    Byun, Ho-June; Song, Woo-Seuk; Yang, Heesun

    2011-06-01

    The work presents a facile, stepwise synthetic approach for the production of highly fluorescent InP/ZnS core/shell quantum dots (QDs) by using a safer phosphorus (P) precursor. First, InP quantum dots (QDs) were solvothermally prepared at 180 °C for 24 h by using a P source of P(N(CH3)2)3. The as-grown InP QDs were consecutively placed in another solvothermal condition for ZnS shell overcoating. In contrast to the almost non-fluorescent InP QDs, due to their highly defective surface states, the ZnS-coated InP QDs were highly fluorescent as a result of effective surface passivation. After the shell growth, the resulting InP/ZnS core/shell QDs were subjected to a size-sorting processing, by which red- to green-emitting QDs with quantum yields (QYs) of 24-60% were produced. Solvothermal shell growth parameters such as the reaction time and Zn/In solution concentration ratio were varied and optimized toward the highest QYs of core/shell QDs.

  4. Facile consecutive solvothermal growth of highly fluorescent InP/ZnS core/shell quantum dots using a safer phosphorus source

    Energy Technology Data Exchange (ETDEWEB)

    Byun, Ho-June; Song, Woo-Seuk; Yang, Heesun, E-mail: hyang@hongik.ac.kr [Department of Materials Science and Engineering, Hongik University, Seoul 121-791 (Korea, Republic of)

    2011-06-10

    The work presents a facile, stepwise synthetic approach for the production of highly fluorescent InP/ZnS core/shell quantum dots (QDs) by using a safer phosphorus (P) precursor. First, InP quantum dots (QDs) were solvothermally prepared at 180 deg. C for 24 h by using a P source of P(N(CH{sub 3}){sub 2}){sub 3}. The as-grown InP QDs were consecutively placed in another solvothermal condition for ZnS shell overcoating. In contrast to the almost non-fluorescent InP QDs, due to their highly defective surface states, the ZnS-coated InP QDs were highly fluorescent as a result of effective surface passivation. After the shell growth, the resulting InP/ZnS core/shell QDs were subjected to a size-sorting processing, by which red- to green-emitting QDs with quantum yields (QYs) of 24-60% were produced. Solvothermal shell growth parameters such as the reaction time and Zn/In solution concentration ratio were varied and optimized toward the highest QYs of core/shell QDs.

  5. One-step synthesis of hierarchically porous hybrid TiO2 hollow spheres with high photocatalytic activity

    Science.gov (United States)

    Liu, Ruiping; Ren, Feng; Yang, Jinlin; Su, Weiming; Sun, Zhiming; Zhang, Lei; Wang, Chang-an

    2016-03-01

    Hierarchically porous hybrid TiO2 hollow spheres were solvothermally synthesized successfully by using tetrabutyl titanate as titanium precursor and hydrated metal sulfates as soft templates. The as-prepared TiO2 spheres with hierarchically pore structures and high specific surface area and pore volume consisted of highly crystallized anatase TiO2 nanocrystals hybridized with a small amount of metal oxide from the hydrated sulfate. The proposed hydrated-sulfate assisted solvothermal (HAS) synthesis strategy was demonstrated to be widely applicable to various systems. Evaluation of the hybrid TiO2 hollow spheres for the photo-decomposition of methyl orange (MO) under visible-light irradiation revealed that they exhibited excellent photocatalytic activity and durability.

  6. Synthesis and characterization of ester and amide derivatives of titanium(IV) carboxymethylphosphonate

    International Nuclear Information System (INIS)

    Melánová, Klára; Beneš, Ludvík; Trchová, Miroslava; Svoboda, Jan; Zima, Vítězslav

    2013-01-01

    A set of layered ester and amide derivatives of titanium(IV) carboxymethylphosphonate was prepared by solvothermal treatment of amorphous titanium(IV) carboxymethylphosphonate with corresponding 1-alkanols, 1,ω-alkanediols, 1-aminoalkanes, 1,ω-diaminoalkanes and 1,ω-amino alcohols and characterized by powder X-ray diffraction, IR spectroscopy and thermogravimetric analysis. Whereas alkyl chains with one functional group form bilayers tilted to the layers, 1,ω-diaminoalkanes and most of 1,ω-alkanediols form bridges connecting the adjacent layers. In the case of amino alcohols, the alkyl chains form bilayer and either hydroxyl or amino group is used for bonding. This simple method for the synthesis of ester and amide derivatives does not require preparation of acid chloride derivative as a precursor or pre-intercalation with alkylamines and can be used also for the preparation of ester and amide derivatives of titanium carboxyethylphosphonate and zirconium carboxymethylphosphonate. - Graphical abstract: Ester and amide derivatives of layered titanium carboxymethylphosphonate were prepared by solvothermal treatment of amorphous solid with alkanol or alkylamine. - Highlights: • Ester and amide derivatives of titanium carboxymethylphosphonate. • Solvothermal treatment of amorphous solid with alkanol or alkylamine. • Ester and amide formation confirmed by IR spectroscopy

  7. Template-Independent Enzymatic Oligonucleotide Synthesis (TiEOS): Its History, Prospects, and Challenges.

    Science.gov (United States)

    Jensen, Michael A; Davis, Ronald W

    2018-03-27

    There is a growing demand for sustainable methods in research and development, where instead of hazardous chemicals, an aqueous medium is chosen to perform biological reactions. In this Perspective, we examine the history and current methodology of using enzymes to generate artificial single-stranded DNA. By using traditional solid-phase phosphoramidite chemistry as a metric, we also explore criteria for the method of template-independent enzymatic oligonucleotide synthesis (TiEOS). As its key component, we delve into the biology of one of the most enigmatic enzymes, terminal deoxynucleotidyl transferase (TdT). As TdT is found to exponentially increase antigen receptor diversity in the vertebrate immune system by adding nucleotides in a template-free manner, researchers have exploited this function as an alternative to the phosphoramidite synthesis method. Though TdT is currently the preferred enzyme for TiEOS, its random nucleotide incorporation presents a barrier in synthesis automation. Taking a closer look at the TiEOS cycle, particularly the coupling step, we find it is comprised of additions > n+1 and deletions. By tapping into the physical and biochemical properties of TdT, we strive to further elucidate its mercurial behavior and offer ways to better optimize TiEOS for production-grade oligonucleotide synthesis.

  8. Mg doped Li2FeSiO4/C nanocomposites synthesized by the solvothermal method for lithium ion batteries.

    Science.gov (United States)

    Kumar, Ajay; Jayakumar, O D; Jagannath; Bashiri, Parisa; Nazri, G A; Naik, Vaman M; Naik, Ratna

    2017-10-14

    A series of porous Li 2 Fe 1-x Mg x SiO 4 /C (x = 0, 0.01, 0.02, 0.04) nanocomposites (LFS/C, 1Mg-LFS/C, 2Mg-LFS and 4Mg-LFS/C) have been synthesized via a solvo-thermal method using the Pluronic P123 polymer as an in situ carbon source. Rietveld refinement of the X-ray diffraction data of Li 2 Fe 1-x Mg x SiO 4 /C composites confirms the formation of the monoclinic P2 1 structure of Li 2 FeSiO 4 . The addition of Mg facilitates the growth of impurity-free Li 2 FeSiO 4 with increased crystallinity and particle size. Despite having the same percentage of carbon content (∼15 wt%) in all the samples, the 1Mg-LFS/C nanocomposite delivered the highest initial discharge capacity of 278 mA h g -1 (∼84% of the theoretical capacity) at the C/30 rate and also exhibited the best rate capability and cycle stability (94% retention after 100 charge-discharge cycles at 1C). This is attributed to its large surface area with a narrow pore size distribution and a lower charge transfer resistance with enhanced Li-ion diffusion coefficient compared to other nanocomposites.

  9. 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.

  10. 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%).

  11. Oriented growth of magnetite along the carbon nanotubes via covalently bonded method in a simple solvothermal system

    Energy Technology Data Exchange (ETDEWEB)

    Zhan Yingqing; Zhao Rui; Meng Fanbing; Lei Yajie; Zhong Jiachun; Yang Xulin [Research Branch of Functional Materials, Institute of Microelectronic and Solid State Electronic, University of Electronic Science and Technology of China, Chengdu 610054 (China); Liu Xiaobo, E-mail: liuxb@uestc.edu.cn [Research Branch of Functional Materials, Institute of Microelectronic and Solid State Electronic, University of Electronic Science and Technology of China, Chengdu 610054 (China)

    2011-06-15

    Highlights: > Novel CNTs/magnetite hybrid materials were prepared via covalently bonded method. > Stable interaction between nitriles and iron ion promoted the oriented growth of magnetite. > The hybrid material exhibited higher magnetism and electromagnetic properties - Abstract: A new type of CNTs/magnetite hybrid material was prepared via covalently bonded method in a simple solvothermal system using FeCl{sub 3} as iron source, ethylene glycol as the reducing agent, and 4-aminophenoxyphthalonitrile-grafted CNTs as templates. The magnetite nanoparticles, with the diameters of 70-80 nm, were self-assembled along the CNTs. The FTIR, UV-vis and DSC revealed that a stable covalent bond between nitriles group and iron ion promoted the oriented growth of magnetite nanoparticles along the CNTs, resulting in good dispersibility and solution storage stability. The magnetic properties measurements indicated that a higher saturated magnetization (70.7 emu g{sup -1}) existed in the CNTs/magnetite hybrid material, which further enhanced the electromagnetic properties. The magnetic loss was caused mainly by natural resonance, which is in good agreement with the Kittel equation results. The novel electromagnetic hybrid material is believed to have potential applications in the microwave absorbing performances.

  12. Oriented growth of magnetite along the carbon nanotubes via covalently bonded method in a simple solvothermal system

    International Nuclear Information System (INIS)

    Zhan Yingqing; Zhao Rui; Meng Fanbing; Lei Yajie; Zhong Jiachun; Yang Xulin; Liu Xiaobo

    2011-01-01

    Highlights: → Novel CNTs/magnetite hybrid materials were prepared via covalently bonded method. → Stable interaction between nitriles and iron ion promoted the oriented growth of magnetite. → The hybrid material exhibited higher magnetism and electromagnetic properties - Abstract: A new type of CNTs/magnetite hybrid material was prepared via covalently bonded method in a simple solvothermal system using FeCl 3 as iron source, ethylene glycol as the reducing agent, and 4-aminophenoxyphthalonitrile-grafted CNTs as templates. The magnetite nanoparticles, with the diameters of 70-80 nm, were self-assembled along the CNTs. The FTIR, UV-vis and DSC revealed that a stable covalent bond between nitriles group and iron ion promoted the oriented growth of magnetite nanoparticles along the CNTs, resulting in good dispersibility and solution storage stability. The magnetic properties measurements indicated that a higher saturated magnetization (70.7 emu g -1 ) existed in the CNTs/magnetite hybrid material, which further enhanced the electromagnetic properties. The magnetic loss was caused mainly by natural resonance, which is in good agreement with the Kittel equation results. The novel electromagnetic hybrid material is believed to have potential applications in the microwave absorbing performances.

  13. 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.

  14. Magnetic and photocatalytic studies on Zn1-xMgxFe2O4 nanocolloids synthesized by solvothermal reflux method.

    Science.gov (United States)

    Manohar, A; Krishnamoorthi, C

    2017-12-01

    Biocompatible magnetic semiconductor Zn 1-x Mg x Fe 2 O 4 (x=0, 0.1, 0.3, 0.5 & 0.7) nanoparticles of around 10nm diameter were synthesized by solvothermal reflux method. The method produces well separated and narrow size distributed nanoparticles. Crystal structure, morphology, particles surface properties, surfactant quantity, colloidal stability, magnetic properties and photocatalytic properties of the synthesized nanoparticles were studied. Different characterizations confirmed that all compounds were single crystals and superparamagnetic at room temperature. Saturation mass magnetization (M s =57.5emu/g) enhances with substituent Mg 2+ concentration due to promotion of mixed spinel (normal and inverse) structure. Photocatalytic activity of all synthesized magnetic semiconductor nanoparticles were studied through methylene blue degradation. The degradation of 98% methylene blue was observed on 60 min irradiation of light. It is observed that photocatalytic activity slightly enhances with substituent Mg 2+ concentration. The synthesized biocompatible magnetic semiconductor nanoparticles can be utilized as photocatalysts and could also be recycled and separated by applying an external magnetic field. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. 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.

  16. Rapid adsorption properties of flower-like BiOI nanoplates synthesized via a simple EG-assisted solvothermal process

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Bin; Ji, Guangbin, E-mail: gbji@nuaa.edu.cn [Nanjing University of Aeronautics and Astronautics, College of Materials Science and Technology (China); Gondal, M. A. [King Fahd University of Petroleum and Minerals, Physics Department (Saudi Arabia); Liu, Yousong; Zhang, Xingmiao; Chang, Xiaofeng; Li, Nianwu [Nanjing University of Aeronautics and Astronautics, College of Materials Science and Technology (China)

    2013-07-15

    Uniform well-crystallized flower-like BiOI nanoplates contained 3.7 nm mesopores, which may be attributed to the internanosheet spaces of BiOI with maximum pore diameters of about 30 nm, were successfully synthesized via a simple ethylene glycol-assisted solvothermal method. The as-prepared porous BiOI nanoplates exhibited excellent adsorption ability, and the saturated extent of adsorption of BiOI over an RhB solution was as high as 197 mg/g, which is much higher than those for BiOCl and BiOBr prepared via the same method and with a similar surface area. The probable adsorption mechanism could have originated from the interaction between the I atom in BiOI and a proton in RhB at different pH values and temperatures. With visible light irradiation ({lambda} > 420 nm), 80 % of the RhB was degraded in 4 h, while BiOI still demonstrated reasonably outstanding photocatalytic ability under green light ({lambda} = 550 {+-} 15 nm) because of its low-energy gap (1.72 eV). The degradation test for BiOI under irradiation at {lambda} = 550 {+-} 15 nm is an excellent achievement for field applications because the catalyst can be applied in solar irradiation to remove organic pollutants, which may be of great value BiOI complex.

  17. 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.

  18. 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.

  19. Solution-phase synthesis of nanomaterials at low temperature

    Science.gov (United States)

    Zhu, Yongchun; Qian, Yitai

    2009-01-01

    This paper reviews the solution-phase synthesis of nanoparticles via some routes at low temperatures, such as room temperature route, wave-assisted synthesis (γ-irradiation route and sonochemical route), directly heating at low temperatures, and hydrothermal/solvothermal methods. A number of strategies were developed to control the shape, the size, as well as the dispersion of nanostructures. Using diethylamine or n-butylamine as solvent, semiconductor nanorods were yielded. By the hydrothermal treatment of amorphous colloids, Bi2S3 nanorods and Se nanowires were obtained. CdS nanowires were prepared in the presence of polyacrylamide. ZnS nanowires were obtained using liquid crystal. The polymer poly (vinyl acetate) tubule acted as both nanoreactor and template for the CdSe nanowire growth. Assisted by the surfactant of sodium dodecyl benzenesulfonate (SDBS), nickel nanobelts were synthesized. In addition, Ag nanowires, Te nanotubes and ZnO nanorod arrays could be prepared without adding any additives or templates.

  20. Graphene-spindle shaped TiO2 mesocrystal composites: Facile synthesis and enhanced visible light photocatalytic performance

    International Nuclear Information System (INIS)

    Yang, Xiaofei; Qin, Jieling; Li, Yang; Zhang, Rongxian; Tang, Hua

    2013-01-01

    Highlights: • Graphene-TiO 2 mesocrystal composites were fabricated via a facile approach. • Graphene sheets were decorated with spindle-like TiO 2 mesocrystals. • Graphene causes enhanced light absorbance and visible light photocatalytic activity. • Oxygen-containing radicals are believed to responsible for its improved activity. -- Abstract: Graphene (GR)-TiO 2 mesocrystal composites were prepared by a facile template-free process based on the combination of sol–gel and solvothermal methods, and were characterized using field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), Raman spectroscopy, UV–vis diffuse reflectance spectroscopy (UV–vis DRS), nitrogen absorption and electron spin resonance (ESR). Visible light photocatalytic performance of GR-TiO 2 composites was evaluated for photocatalytic degradation of organic dye Rhodamine B. It was found that the amount of graphene oxide (GO) added obviously affects morphologies of TiO 2 mesocrystals and photocatalytic activities of as-prepared nanocomposites. Composites prepared in the presence of different amounts of GO all exhibit higher photocatalytic activity than pure TiO 2 mesocrystals and P25, the composite obtained by using 20 mg GO presents the most uniform TiO 2 mesocrystals in the composite and shows the highest photocatalytic efficiency. The mechanism for the generation of TiO 2 mesocrystals in the GR-TiO 2 composite is proposed and possible reasons for the enhancement in visible light photocatalytic efficiency are also discussed

  1. 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.

  2. 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.

  3. Facile synthesis of hierarchically porous Li{sub 4}Ti{sub 5}O{sub 12} microspheres for high rate lithium ion batteries

    Energy Technology Data Exchange (ETDEWEB)

    Shen, L.F.; Luo, H.J.; Yuan, C.Z.; Su, X.F.; Xu, K.; Zhang, X.G. [Nanjing Univ. of Aeronautics and Astronautics (China). College of Material Science and Engineering

    2010-07-01

    Lithium-ion (Li-ion) batteries are used in electric vehicles (EVs) and hybrid electric vehicles (HEVs) due to their excellent energy storage capacity. Graphite is widely used as an anode material in EV and HEV applications. This study investigated the use of a lithium-titanium alloy (Li{sub 4}Ti{sub 5}O{sub 12}) designed to avoid reductions of the electrolyte on the surface of the electrode. The study showed that the composite material shows excellent cycling performance, excellent reversibility, structural stability, and Li-ion mobility in the charge-discharge process. A simple template-free hydrothermal method for fabricating Li{sub 4}Ti{sub 5}O{sub 12} hierarchical microspheres assembled by uniform nanoparticles was presented. The 1-step process produced microspheres with a high yield and uniform diameter. Details of the synthesis process, and the electrochemical and structural properties of the resulting materials were presented. 5 refs.

  4. Graphene-supported SnO2 nanoparticles prepared by a solvothermal approach for an enhanced electrochemical performance in lithium-ion batteries

    OpenAIRE

    Wang, Bei; Su, Dawei; Park, Jinsoo; Ahn, Hyojun; Wang, Guoxiu

    2012-01-01

    SnO2 nanoparticles were dispersed on graphene nanosheets through a solvothermal approach using ethylene glycol as the solvent. The uniform distribution of SnO2 nanoparticles on graphene nanosheets has been confirmed by scanning electron microscopy and transmission electron microscopy. The particle size of SnO2 was determined to be around 5 nm. The as-synthesized SnO2/graphene nanocomposite exhibited an enhanced electrochemical performance in lithium-ion batteries, compared with bare graphene ...

  5. 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.

  6. Solvothermal-induced 3D macroscopic SnO2/nitrogen-doped graphene aerogels for high capacity and long-life lithium storage.

    Science.gov (United States)

    Wang, Ronghua; Xu, Chaohe; Sun, Jing; Gao, Lian; Yao, Heliang

    2014-03-12

    3D macroscopic tin oxide/nitrogen-doped graphene frameworks (SnO2/GN) were constructed by a novel solvothermal-induced self-assembly process, using SnO2 colloid as precursor (crystal size of 3-7 nm). Solvothermal treatment played a key role as N,N-dimethylmethanamide (DMF) acted both as reducing reagent and nitrogen source, requiring no additional nitrogen-containing precursors or post-treatment. The SnO2/GN exhibited a 3D hierarchical porous architecture with a large surface area (336 m(2)g(-1)), which not only effectively prevented the agglomeration of SnO2 but also facilitated fast ion and electron transport through 3D pathways. As a result, the optimized electrode with GN content of 44.23% exhibited superior rate capability (1126, 855, and 614 mAh g(-1) at 1000, 3000, and 6000 mA g(-1), respectively) and extraordinary prolonged cycling stability at high current densities (905 mAh g(-1) after 1000 cycles at 2000 mA g(-1)). Electrochemical impedance spectroscopy (EIS) and morphological study demonstrated the enhanced electrochemical reactivity and good structural stability of the electrode.

  7. Raman scattering investigation of Bi2Te3 hexagonal nanoplates prepared by a solvothermal process in the absence of NaOH

    International Nuclear Information System (INIS)

    Liang Yujie; Wang Wenzhong; Zeng Baoqing; Zhang Guling; Huang Jing; Li Jin; Li Te; Song Yangyang; Zhang Xiuyu

    2011-01-01

    Research highlights: → Hexagonal Bi 2 Te 3 thin nanoplates were synthesized by a simple solvothermal method. → Optical properties of the nanoplates were investigated by micro-Raman spectroscopy. → Infrared (IR) active mode (A 1u ) is greatly activated in Raman scattering spectrum. → Infrared (IR) active mode (A 1u ) shows up in Raman spectrum of hexagonal nanoplates. → Raman spectrum clearly shows crystal symmetry breaking of hexagonal nanoplates. - Abstract: Hexagonal Bi 2 Te 3 nanoplates were synthesized by a simple solvothermal process in the absence of NaOH. The composition, morphology and size of the as-prepared products were characterized by powder X-ray diffraction (XRD) and transmission electron microscopy (TEM). Raman scattering optical properties of the as-prepared Bi 2 Te 3 nanoplates were investigated by micro-Raman spectroscopy. The Raman spectrum shows that infrared (IR) active mode (A 1u ), which must be odd parity and is Raman forbidden for bulk crystal due to its inversion symmetry, is greatly activated and shown up clearly in Raman scattering spectrum. We attribute the appearance of infrared active (A 1u ) in Raman spectrum to crystal symmetry breaking of Bi 2 Te 3 hexagonal nanoplates. The as-grown Bi 2 Te 3 hexagonal nanoplates, exhibiting novel Raman optical properties compared with bulk crystals, may find potential applications in thermoelectric devices.

  8. 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.

  9. Annealing temperatures influence luminescence of YBO{sub 3}: Ce{sup 3+}, Yb{sup 3+} prepared by solvothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Yue [Department of Physics, Northwest University, No. 229 Taibai North Road, Xi' an, Shaanxi, 710069 (China); Hu, Xiaoyun, E-mail: hxy3275@nwu.edu.cn [Department of Physics, Northwest University, No. 229 Taibai North Road, Xi' an, Shaanxi, 710069 (China); Zhan, Suchang; Sun, Xiao; Wang, Zhizhong; Miao, Tian; Miao, Hui [Department of Physics, Northwest University, No. 229 Taibai North Road, Xi' an, Shaanxi, 710069 (China); Fan, Jun [School of Chemical Engineering, Northwest University, No. 229 Taibai North Road, Xi' an, Shaanxi, 710069 (China)

    2014-08-01

    Near-infrared (NIR) quantum cutting (QC) YBO{sub 3}: Ce{sup 3+}, Yb{sup 3+} phosphors have been synthesized by solvothermal method with further heat treatment. The emission spectrum shows the Vis and NIR emission intensity of samples are both increasingly strong as annealing temperature rises when the annealing temperature is above 600 °C. Meanwhile the Vis emission of unannealed sample is observed. SEM images show that the sample annealed at different temperatures (200–900 °C) is mainly composed of nanosheets like potato chips, which is melt down granules after annealing treatment above 1000 °C.The crystal texture of all samples whether annealed or not is hexagonal through the analysis of XRD. The Raman and infrared spectrums indicate that the boron ions exist of BO{sub 4} units when the annealing temperature is above 600 °C. The infrared profile of unannealed sample shows that there are N–H units in the samples without annealing treatment. - Highlights: • The nanosheets like potato chips are synthesized by solvothermal method. • Annealing temperature is a great effect for luminescence of sample. • The boron ions exist of BO{sub 4} when the annealing temperature is above 600 °C, whose quantity determines the luminescent intensity. • According to the infrared profile of unannealed sample, there are N–H units, which are beneficial to the Vis emission.

  10. Synthesis of belt-like BiOBr hierarchical nanostructure with high photocatalytic performance

    Energy Technology Data Exchange (ETDEWEB)

    Li, Haiping [National Engineering Technology Research Center for Colloidal Materials, Shandong University, Jinan 250100 (China); Liu, Jingyi; Hu, Tingxia [Environment Research Institute, Shandong University, Jinan 250100 (China); Du, Na; Song, Shue [Key Laboratory of Colloid and Interface Chemistry (Ministry of Education), Shandong University, Jinan 250100 (China); Hou, Wanguo, E-mail: wghou@sdu.edu.cn [Key Laboratory of Colloid and Interface Chemistry (Ministry of Education), Shandong University, Jinan 250100 (China)

    2016-05-15

    Highlights: • BiOBr hierarchical nanobelts (NBs) were solvothermally prepared. • NBs show higher specific surface area and photoabsorption than BiOBr nanosheets. • NBs exhibit higher photoactivity than the nanosheets. - Abstract: One-dimensional (1D) bismuth oxyhalide (BiOX) hierarchical nanostructures are always difficult to prepare. Herein, we report, for the first time, a simple synthesis of BiOBr nanobelts (NBs) via a facile solvothermal route, using bismuth subsalicylate as the template and bismuth source. The BiOBr nanobelts are composed of irregular single crystal nanoparticles with highly exposed (0 1 0) facets. Compared with the BiOBr nanosheets (NSs) with dominant exposed (0 0 1) facets, they exhibit higher photocatalytic activity toward degradation of Rhodamine B and Methylene Blue under visible light irradiation. The higher photocatalytic performance of BiOBr NBs arises from their larger specific surface area and higher photoabsorption capability. This study provides a simple route for synthesis of belt-like Bi-based hierarchical nanostructures.

  11. 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.

  12. 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.

  13. 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.

  14. Solvothermal preparation of nanocrystalline anatase containing TiO{sub 2} and TiO{sub 2}/SiO{sub 2} coating agents for application of photocatalytic treatments

    Energy Technology Data Exchange (ETDEWEB)

    Mahltig, B., E-mail: boris.mahltig@hs-niederrhein.de [University of Applied Sciences Niederrhein, Faculty of Textile and Clothing Technology, Webschulstrasse 31, D-41065 Moenchengladbach (Germany); Gesellschaft zur Foerderung von Medizin-, Bio- und Umwelttechnologien e.V., GMBU e.V., Postfach 520165, D-01317 Dresden (Germany); Gutmann, E. [Technische Universitaet Dresden, Institut fuer Strukturphysik, D-01062 Dresden (Germany); Meyer, D.C. [Technische Universitaet Dresden, Institut fuer Strukturphysik, D-01062 Dresden (Germany); Technische Universitaet Bergakademie Freiberg, Institut fuer Experimentelle Physik, D-09596 Freiberg (Germany)

    2011-05-16

    Research highlights: {yields} TiO{sub 2} and TiO{sub 2}/SiO{sub 2} materials prepared by a solvothermal sol-gel process. {yields} Photodecomposition with oxygen increases with increasing solvothermal process temperature. {yields} In presence of H{sub 2}O{sub 2} the dye decomposition is observed even without UV light illumination. {yields} The materials contain potential for cleaning waste water containing dye stuffs. - Abstract: This paper reports on TiO{sub 2} and TiO{sub 2}/SiO{sub 2} materials prepared by a sol-gel process under solvothermal conditions with process temperatures between 120 deg. C and 180 deg. C. Under the preparation conditions chosen, the formation of anatase crystallites starts at a process temperature of 160 deg. C, as observed by X-ray diffraction. From TiO{sub 2} and TiO{sub 2}/SiO{sub 2} sols coatings on viscose fabrics and powders have been prepared. The photoactivity of both materials - coated textiles and powders - is determined by the decomposition of the dye AcidOrange under UV light illumination. Significant dye decomposition is only observed for samples containing a high ratio of TiO{sub 2} and that are solvothermally prepared at 180 deg. C. In contrast, when the photoactivity is determined in presence of H{sub 2}O{sub 2} totally different results are obtained and the degree of AcidOrange decomposition is higher for most of the samples. Furthermore, in presence of H{sub 2}O{sub 2} the dye decomposition is observed even without UV light illumination. Especially samples prepared with the polymer Pluronic P123 under lower solvothermal process temperatures exhibit strong dye decomposition without illumination in presence of H{sub 2}O{sub 2}. Therefore, these materials could be of high interest for cleaning waste water containing dye stuffs from textile industry.

  15. Synthesis and magnetic properties of superparamagnetic CoAs nanostructures

    Science.gov (United States)

    Desai, P.; Ashokaan, N.; Masud, J.; Pariti, A.; Nath, M.

    2015-03-01

    This article provides a comprehensive guide on the synthesis and characterization of superparamagnetic CoAs nanoparticles and elongated nanostructures with high blocking temperature, (TB), via hot-injection precipitation and solvothermal methods. Cobalt arsenides constitute an important family of magnetically active solids that find a variety of applications ranging from magnetic semiconductors to biomedical imaging. While the higher temperature hot-injection precipitation technique (300 °C) yields pure CoAs nanostructures, the lower temperature solvothermal method (200 °C) yields a mixture of CoAs nanoparticles along with other Co-based impurity phases. The synthesis in all these cases involved usage of triphenylarsine ((C6H5)3As) as the As precursor which reacts with solid Co2(CO)8 by ligand displacement to yield a single source precursor. The surfactant, hexadecylamine (HDA) further assists in controlling the morphology of the nanostructures. HDA also provides a basic medium and molten flux-like conditions for the redox chemistry to occur between Co and As at elevated temperatures. The influence of the length of reaction time was investigated by studying the evolution of product morphology over time. It was observed that while spontaneous nucleation at higher temperature followed by controlled growth led to the predominant formation of short nanorods, with longer reaction time, the nanorods were further converted to nanoparticles. The size of the nanoparticles obtained, was mostly in the range of 10-15 nm. The key finding of this work is exceptionally high coercivity in CoAs nanostructures for the first time. Coercivity observed was as high as 0.1 T (1000 Oe) at 2 K. These kinds of magnetic nanostructures find multiple applications in spintronics, whereas the superparamagnetic nanoparticles are viable for use in magnetic storage, ferrofluids and as contrast enhancing agents in MRI.

  16. 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).

  17. Graphene-supported SnO2 nanoparticles prepared by a solvothermal approach for an enhanced electrochemical performance in lithium-ion batteries.

    Science.gov (United States)

    Wang, Bei; Su, Dawei; Park, Jinsoo; Ahn, Hyojun; Wang, Guoxiu

    2012-04-13

    SnO2 nanoparticles were dispersed on graphene nanosheets through a solvothermal approach using ethylene glycol as the solvent. The uniform distribution of SnO2 nanoparticles on graphene nanosheets has been confirmed by scanning electron microscopy and transmission electron microscopy. The particle size of SnO2 was determined to be around 5 nm. The as-synthesized SnO2/graphene nanocomposite exhibited an enhanced electrochemical performance in lithium-ion batteries, compared with bare graphene nanosheets and bare SnO2 nanoparticles. The SnO2/graphene nanocomposite electrode delivered a reversible lithium storage capacity of 830 mAh g-1 and a stable cyclability up to 100 cycles. The excellent electrochemical properties of this graphene-supported nanocomposite could be attributed to the insertion of nanoparticles between graphene nanolayers and the optimized nanoparticles distribution on graphene nanosheets.

  18. Solvothermal method as a green chemistry solution for micro-encapsulation of phase change materials for high temperature thermal energy storage

    Science.gov (United States)

    Tudor, Albert Ioan; Motoc, Adrian Mihail; Ciobota, Cristina Florentina; Ciobota, Dan. Nastase; Piticescu, Radu Robert; Romero-Sanchez, Maria Dolores

    2018-05-01

    Thermal energy storage systems using phase change materials (PCMs) as latent heat storage are one of the main challenges at European level in improving the performances and efficiency of concentrated solar power energy generation due to their high energy density. PCM with high working temperatures in the temperature range 300-500 °C are required for these purposes. However their use is still limited due to the problems raised by the corrosion of the majority of high temperature PCMs and lower thermal transfer properties. Micro-encapsulation was proposed as one method to overcome these problems. Different micro-encapsulation methods proposed in the literature are presented and discussed. An original process for the micro-encapsulation of potassium nitrate as PCM in inorganic zinc oxide shells based on a solvothermal method followed by spray drying to produce microcapsules with controlled phase composition and distribution is proposed and their transformation temperatures and enthalpies measured by differential scanning calorimetry are presented.

  19. 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.

  20. 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.

  1. 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.

  2. Immobilizing ternary Zn{sub X}Cd{sub 1−X}S on graphene via solvothermal method for enhanced photoelectric properties

    Energy Technology Data Exchange (ETDEWEB)

    Lei, Yun, E-mail: leiyun@whut.edu.cn; Chen, Feifei; Xu, Jun

    2015-12-01

    Graphical abstract: - Highlights: • Composition-tunable Zn{sub X}Cd{sub 1−X}S-graphene were prepared with a one-step solvothermal process by varying Zn/Cd ratios. • The diffraction peaks move to higher angle and UV–vis spectra present a progressive blue-shift with the increase of x value. • A more efficient separation of photo-induced carriers and a faster interfacial charge transfer occurs on graphene-Zn{sub 0.8}Cd{sub 0.2}S. - Abstract: Ternary Zn{sub X}Cd{sub 1−X}S particles were directly immobilized on graphene sheets by a facile solvothermal route with zinc acetate, cadmium acetate and thiourea as precursors, ethylene glycol as reaction solvent and graphene oxide as support. The value of x could be adjusted by controlling the molar ratio of Zn and Cd precursors. The products were characterized by X-ray diffraction, scanning electron microscope and ultraviolet–visible absorption. The photoelectric properties of the graphene-Zn{sub X}Cd{sub 1−X}S composites were investigated by transient photocurrent responses and electrochemical impedance spectra, and the results show that the obvious increase in the photocurrent density and decrease in electron-transfer resistance can be seen for graphene-Zn{sub 0.8}Cd{sub 0.2}S composites as compared to graphene-Zn{sub X}Cd{sub 1−X}S composites with other Zn/Cd ratios.

  3. 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

  4. 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.

  5. 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.

    2016-01-01

    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, Kd = 6.3 × 10−8 m), vancomycin (d = 250 nm, Kd = 3.4 × 10−9 m), a peptide (d = 350 nm, Kd = 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. PMID:26869870

  6. An Intrinsically Disordered Peptide from Ebola Virus VP35 Controls Viral RNA Synthesis by Modulating Nucleoprotein-RNA Interactions

    Directory of Open Access Journals (Sweden)

    Daisy W. Leung

    2015-04-01

    Full Text Available During viral RNA synthesis, Ebola virus (EBOV nucleoprotein (NP alternates between an RNA-template-bound form and a template-free form to provide the viral polymerase access to the RNA template. In addition, newly synthesized NP must be prevented from indiscriminately binding to noncognate RNAs. Here, we investigate the molecular bases for these critical processes. We identify an intrinsically disordered peptide derived from EBOV VP35 (NPBP, residues 20–48 that binds NP with high affinity and specificity, inhibits NP oligomerization, and releases RNA from NP-RNA complexes in vitro. The structure of the NPBP/ΔNPNTD complex, solved to 3.7 Å resolution, reveals how NPBP peptide occludes a large surface area that is important for NP-NP and NP-RNA interactions and for viral RNA synthesis. Together, our results identify a highly conserved viral interface that is important for EBOV replication and can be targeted for therapeutic development.

  7. An Intrinsically Disordered Peptide from Ebola Virus VP35 Controls Viral RNA Synthesis by Modulating Nucleoprotein-RNA Interactions.

    Science.gov (United States)

    Leung, Daisy W; Borek, Dominika; Luthra, Priya; Binning, Jennifer M; Anantpadma, Manu; Liu, Gai; Harvey, Ian B; Su, Zhaoming; Endlich-Frazier, Ariel; Pan, Juanli; Shabman, Reed S; Chiu, Wah; Davey, Robert A; Otwinowski, Zbyszek; Basler, Christopher F; Amarasinghe, Gaya K

    2015-04-21

    During viral RNA synthesis, Ebola virus (EBOV) nucleoprotein (NP) alternates between an RNA-template-bound form and a template-free form to provide the viral polymerase access to the RNA template. In addition, newly synthesized NP must be prevented from indiscriminately binding to noncognate RNAs. Here, we investigate the molecular bases for these critical processes. We identify an intrinsically disordered peptide derived from EBOV VP35 (NPBP, residues 20-48) that binds NP with high affinity and specificity, inhibits NP oligomerization, and releases RNA from NP-RNA complexes in vitro. The structure of the NPBP/ΔNPNTD complex, solved to 3.7 Å resolution, reveals how NPBP peptide occludes a large surface area that is important for NP-NP and NP-RNA interactions and for viral RNA synthesis. Together, our results identify a highly conserved viral interface that is important for EBOV replication and can be targeted for therapeutic development. Copyright © 2015 The Authors. Published by Elsevier Inc. All rights reserved.

  8. 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.

  9. A novel ethanol templating synthesis of ordered lamellar superstructured crystalline zirconia

    Energy Technology Data Exchange (ETDEWEB)

    Liu Chao, E-mail: liuchao_tj@yahoo.com; Wang Bin [Key Laboratory for New Type of Functional Materials in Hebei Province, Hebei University of Technology (China); Ji Xiujie, E-mail: jxjchem@yahoo.com [State Key Laboratory of Hollow Fiber Membrane Materials and Processes, Tianjin Polytechnic University (China); Zhao Shanshan; Wu Jie; Jia Jianlong; Ma Dongxia [Key Laboratory for New Type of Functional Materials in Hebei Province, Hebei University of Technology (China)

    2012-03-15

    Soft template technique has attracted great interest, because it is a facile, inexpensive and efficient synthesis strategy for ordered superstructural systems. Here, a novel ethanol template was used to synthesize the ordered lamellar superstructured crystalline zirconia (L{alpha}-ZrO{sub 2}) without post-treatments and surfactants. ZrOCl{sub 2} and NaOH were served as Zr source and precipitant, respectively. XRD analysis showed that L{alpha}-ZrO{sub 2} is crystalline. XPS spectra indicated the physical adsorption of ethanol molecules in L{alpha}-ZrO{sub 2}. TEM further observed and proved the 1.36-nm period of superstructure detected and calculated by SAXRD (1.35 nm), which is composed of 0.68-nm thick ZrO{sub 2} and pore alternatively. In contrast, the template-free ZrO{sub 2} (TF-ZrO{sub 2}) presents no superstructure and is poorly crystallized. As a soft template, ethanol presents the roles of (i) inducing the growth of zirconia layers, (ii) directing the self-assembly of ordered lamellar superstructure, and (iii) decreasing the crystallization temperature. The possible mechanism of ethanol serving as a soft template was proposed and discussed in thermodynamics.

  10. A novel ethanol templating synthesis of ordered lamellar superstructured crystalline zirconia

    International Nuclear Information System (INIS)

    Liu Chao; Wang Bin; Ji Xiujie; Zhao Shanshan; Wu Jie; Jia Jianlong; Ma Dongxia

    2012-01-01

    Soft template technique has attracted great interest, because it is a facile, inexpensive and efficient synthesis strategy for ordered superstructural systems. Here, a novel ethanol template was used to synthesize the ordered lamellar superstructured crystalline zirconia (Lα-ZrO 2 ) without post-treatments and surfactants. ZrOCl 2 and NaOH were served as Zr source and precipitant, respectively. XRD analysis showed that Lα-ZrO 2 is crystalline. XPS spectra indicated the physical adsorption of ethanol molecules in Lα-ZrO 2 . TEM further observed and proved the 1.36-nm period of superstructure detected and calculated by SAXRD (1.35 nm), which is composed of 0.68-nm thick ZrO 2 and pore alternatively. In contrast, the template-free ZrO 2 (TF-ZrO 2 ) presents no superstructure and is poorly crystallized. As a soft template, ethanol presents the roles of (i) inducing the growth of zirconia layers, (ii) directing the self-assembly of ordered lamellar superstructure, and (iii) decreasing the crystallization temperature. The possible mechanism of ethanol serving as a soft template was proposed and discussed in thermodynamics.

  11. Methylcellulose-Directed Synthesis of Nanocrystalline Zeolite NaA with High CO₂ Uptake.

    Science.gov (United States)

    Shakarova, Dilshod; Ojuva, Arto; Bergström, Lennart; Akhtar, Farid

    2014-07-28

    Zeolite NaA nanocrystals with a narrow particle size distribution were prepared by template-free hydrothermal synthesis in thermo-reversible methylcellulose gels. The effects of the amount of methylcellulose, crystallization time and hydrothermal treatment temperature on the crystallinity and particle size distribution of the zeolite NaA nanocrystals were investigated. We found that the thermogelation of methylcellulose in the alkaline Na₂O-SiO₂-Al₂O₃-H₂O system played an important role in controlling the particle size. The synthesized zeolite nanocrystals are highly crystalline, as demonstrated by X-ray diffraction (XRD), and scanning electron microscopy (SEM) shows that the nanocrystals can also display a well-defined facetted morphology. Gas adsorption studies on the synthesized nanocrystalline zeolite NaA showed that nanocrystals with a size of 100 nm displayed a high CO₂ uptake capacity (4.9 mmol/g at 293 K at 100 kPa) and a relatively rapid uptake rate compared to commercially available, micron-sized particles. Low-cost nanosized zeolite adsorbents with a high and rapid uptake are important for large scale gas separation processes, e.g., carbon capture from flue gas.

  12. Synthesis and gas-sensing characteristics of α-Fe2O3 hollow balls

    Directory of Open Access Journals (Sweden)

    Chu Manh Hung

    2016-03-01

    Full Text Available The synthesis of porous metal-oxide semiconductors for gas-sensing application is attracting increased interest. In this study, α-Fe2O3 hollow balls were synthesized using an inexpensive, scalable, and template-free hydrothermal method. The gas-sensing characteristics of the semiconductors were systematically investigated. Material characterization by XRD, SEM, HRTEM, and EDS reveals that single-phase α-Fe2O3 hollow balls with an average diameter of 1.5 μm were obtained. The hollow balls were formed by self assembly of α-Fe2O3 nanoparticles with an average diameter of 100 nm. The hollow structure and nanopores between the nanoparticles resulted in the significantly high response of the α-Fe2O3 hollow balls to ethanol at working temperatures ranging from 250 °C to 450 °C. The sensor also showed good selectivity over other gases, such as CO and NH3 promising significant application.

  13. 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.

  14. Fabrication and luminescence properties of Al{sub 2}O{sub 3}:Tb{sup 3+} microspheres via a microwave solvothermal route

    Energy Technology Data Exchange (ETDEWEB)

    Zhu Zhenfeng, E-mail: zhuzf@sust.edu.cn [School of Materials Science and Engineering, Shaanxi University of Science and Technology, Xi' an 710021 (China); Liu Dianguang; Liu Hui; Li Guangjun; Du Juan; He Zuoli [School of Materials Science and Engineering, Shaanxi University of Science and Technology, Xi' an 710021 (China)

    2012-02-15

    Al{sub 2}O{sub 3}:Tb{sup 3+} green phosphors were synthesized via a microwave solvothermal and thermal decomposition route, and characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), photoluminescence (PL) spectra, and decay curves. XRD results indicate that Tb{sup 3+} doped samples are {gamma}-Al{sub 2}O{sub 3} after being calcined at 773 K. SEM results show that the particles of Al{sub 2}O{sub 3}:Tb{sup 3+} are hierarchically nanostructured microspheres assembled from nanosheets. The PL spectra indicate that the {sup 5}D{sub 4}{yields}{sup 7}F{sub 5} (545 nm) electric dipole transition is the most intensive when excited at 235 nm. It is shown that 0.7 mol% of doping concentration of Tb{sup 3+} ions in {gamma}-Al{sub 2}O{sub 3}:Tb{sup 3+} is optimum. According to Dexter's theory, the critical distance between Tb{sup 3+} ions for energy transfer was determined to be 18.4 A. It is found that the curve followed the single-exponential decay. The excellent chromaticity coordinates of Al{sub 2}O{sub 3}:Tb{sup 3+} phosphors, as defined by the International Commission on Illumination (CIE), indicate that it is a good candidate for use in light display systems and optoelectronic devices. - Highlights: Black-Right-Pointing-Pointer Al{sub 2}O{sub 3}:Tb{sup 3+} phosphors prepared via a microwave solvothermal route. Black-Right-Pointing-Pointer The particles were hierarchically nanostructured microspheres packaged by nanosheets. Black-Right-Pointing-Pointer {sup 5}D{sub 4}{yields}{sup 7}F{sub 5} electric dipole transition is the most intensive when excited at 235 nm. Black-Right-Pointing-Pointer 0.7 mol% of doping concentration of Tb{sup 3+} ions in {gamma}-Al{sub 2}O{sub 3}:Tb{sup 3+} is optimum. Black-Right-Pointing-Pointer Critical distance between Tb{sup 3+} ions for energy transfer is 18.4 A.

  15. 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.

  16. Solvothermal method as a green chemistry solution for micro-encapsulation of phase change materials for high temperature thermal energy storage

    Directory of Open Access Journals (Sweden)

    Tudor Albert Ioan

    2018-01-01

    Full Text Available Thermal energy storage systems using phase change materials (PCMs as latent heat storage are one of the main challenges at European level in improving the performances and efficiency of concentrated solar power energy generation due to their high energy density. PCM with high working temperatures in the temperature range 300–500 °C are required for these purposes. However their use is still limited due to the problems raised by the corrosion of the majority of high temperature PCMs and lower thermal transfer properties. Micro-encapsulation was proposed as one method to overcome these problems. Different micro-encapsulation methods proposed in the literature are presented and discussed. An original process for the micro-encapsulation of potassium nitrate as PCM in inorganic zinc oxide shells based on a solvothermal method followed by spray drying to produce microcapsules with controlled phase composition and distribution is proposed and their transformation temperatures and enthalpies measured by differential scanning calorimetry are presented.

  17. 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.

  18. Electrophoretic deposition of Cu2ZnSn(S0.5Se0.5)4 films using solvothermal synthesized nanoparticles

    Science.gov (United States)

    Badkoobehhezaveh, Amir Masoud; Abdizadeh, Hossein; Golobostanfard, Mohammad Reza

    2018-01-01

    In this paper, a simple, practical, and fast solvothermal route is presented for synthesizing the Cu2ZnSn(S0.5Se0.5)4 nanoparticles (CZTSSe). In this method, the precursors were dissolved in triethylenetetramine and placed in an autoclave at 240 °C for 1 h under controlled pressure and constant stirring. After washing the samples for several times with absolute ethanol, the obtained CZTSSe nanoparticles were successfully deposited on fluorine doped tin oxide substrates by convenient electrophoretic deposition (EPD) using colloidal nanoparticles. The most appropriate parameters for EPD of pre-synthesized CZTSSe nanoparticles which result in proper surface properties, controlled thickness, and high film quality are investigated by adjusting applied voltage, pH, and deposition time. X-ray diffraction pattern and Raman spectroscopy of the pre-synthesized nanoparticles show kesterite structure formation. The particle size of the CZTSSe nanoparticles is in the range of 100 to 400 nm and for some agglomerates, it is about 2 µm confirmed by scanning electron microscope. The deposited film with optimized parameter has acceptable quality without any crack in it with the thickness of about 4-5 µm. Energy-dispersive X-ray spectroscopy confirms that the chemical composition of the samples is in near stoichiometric Cu-poor and Zn-rich region, which guarantees the p-type character of the film. The diffuse reflectance spectroscopy also demonstrates that the optical band gap of the sample is about 1.2 eV.

  19. 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.

  20. One-step solvothermal tailoring the compositions and phases of nickel cobalt sulfides on conducting oxide substrates as counter electrodes for efficient dye-sensitized solar cells

    International Nuclear Information System (INIS)

    Huang, Niu; Li, Guowang; Huang, Hua; Sun, Panpan; Xiong, Tianli; Xia, Zhifen; Zheng, Fang; Xu, Jixing; Sun, Xiaohua

    2016-01-01

    Highlights: • Co-Ni-S nanoparticles were in-suit grown on FTO via a facile method. • By varying thiourea amount, several Co-Ni-S alloys were obtained. • Amongst the Co-Ni-S alloys, NiCo_2S_4 exhibited the best electrocatalytic property. - Abstract: Several nickel cobalt sulfide (Ni-Co-S) counter electrodes (CEs) are prepared, and the Ni-Co-S nanoparticles are in-situ grown on SnO_2: F (FTO) transparent conductive glasses via a facile solvothermal process, in which thiourea is used as the sulfurizing reagent. The X-ray diffraction, scanning electron microscopy, and energy dispersive spectrometer are employed to measure the microstructure and composition of the Ni-Co-S CEs. When a proper amount of thiourea is adopted, fine crystalline NiCo_2S_4 CE is obtained. When the amount of thiourea is small or large, (Ni,Co)_4S_3 or (Ni,Co)_3S_4 CE is acquired, respectively. Cyclic voltammetry, electrochemical impedance spectroscopy, Tafel polarization and open-circuit voltage decay (OCVD) measurements all demonstrate that the electrocatalytic activities and electrical conductivities of these Ni-Co-S CEs all approach or exceed those of Pt-pyrolysis CE. Their superior electrochemical performances are further confirmed by fabricating DSSCs with the Ni-Co-S CEs, they display similar or better photo-electric conversion efficiencies to/than the Pt-pyrolysis counterpart.

  1. Solvothermal Vapor Annealing of Lamellar Poly(styrene)-block-poly(d,l-lactide) Block Copolymer Thin Films for Directed Self-Assembly Application.

    Science.gov (United States)

    Cummins, Cian; Mokarian-Tabari, Parvaneh; Andreazza, Pascal; Sinturel, Christophe; Morris, Michael A

    2016-03-01

    Solvothermal vapor annealing (STVA) was employed to induce microphase separation in a lamellar forming block copolymer (BCP) thin film containing a readily degradable block. Directed self-assembly of poly(styrene)-block-poly(d,l-lactide) (PS-b-PLA) BCP films using topographically patterned silicon nitride was demonstrated with alignment over macroscopic areas. Interestingly, we observed lamellar patterns aligned parallel as well as perpendicular (perpendicular microdomains to substrate in both cases) to the topography of the graphoepitaxial guiding patterns. PS-b-PLA BCP microphase separated with a high degree of order in an atmosphere of tetrahydrofuran (THF) at an elevated vapor pressure (at approximately 40-60 °C). Grazing incidence small-angle X-ray scattering (GISAXS) measurements of PS-b-PLA films reveal the through-film uniformity of perpendicular microdomains after STVA. Perpendicular lamellar orientation was observed on both hydrophilic and relatively hydrophobic surfaces with a domain spacing (L0) of ∼32.5 nm. The rapid removal of the PLA microdomains is demonstrated using a mild basic solution for the development of a well-defined PS mask template. GISAXS data reveal the through-film uniformity is retained following wet etching. The experimental results in this article demonstrate highly oriented PS-b-PLA microdomains after a short annealing period and facile PLA removal to form porous on-chip etch masks for nanolithography application.

  2. 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.

  3. High-performance macroporous bulk silicon anodes synthesized by template-free chemical etching

    Energy Technology Data Exchange (ETDEWEB)

    Bang, Byoung Man; Lee, Jung-In; Kim, Hyunjung; Cho, Jaephil; Park, Soojin [Interdisciplinary School of Green Energy, Ulsan National Institute of Science and Technology (UNIST), Ulsan (Korea, Republic of)

    2012-07-15

    Three-dimensional porous silicon particles can be produced via the combination of a galvanic displacement reaction and a metal-assisted chemical etching process. This simple synthetic route can be applied to make high-performance anode materials, including high specific capacity, stable cycling retention, and high rate capability, in lithium-ion batteries. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  4. Template-free electrosynthesis of aligned poly(p-phenylene) microtubules

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    Poly(p-phenylene) (PPP) microtubules with diameters of 0.2-0.8μm and lengths of~10 (m have been synthesized by direct oxidation of benzene in the mixed electrolyte of boron trifluoride diethyl etherate (BFEE) and trifluoroacetic acid (TFA) (BFEE:TFA= 2:1, by volume), containing a certain amount of sodium dodecylbenzene- sulfonate (SDBS) as surfactant. The microtubules were grown vertically on the working electrode surface. The tubular morphology has been confirmed by scanning and transmission electron microscopies and the chain structure of the skin of the tubules has been characterized by Raman spectroscopy. The electrode property, monomer/surfactant molar ratio and the value of applied potential have strong effects on the morphology of the microtubules.

  5. Template-free fabrication and morphology regulation of Ag@carbon composite structure

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Wenyan, E-mail: zhangwenyan8531@gmail.com [College of Material Engineering, Jinling Institute of Technology, Nanjing (China); Hao, Lingyun; Lin, Qin [College of Material Engineering, Jinling Institute of Technology, Nanjing (China); Lu, Chunhua; Xu, Zhongzi [College of Materials Science and Engineering, Nanjing Technology University, Nanjing (China); Chen, Xiaoyu [College of Material Engineering, Jinling Institute of Technology, Nanjing (China)

    2014-12-15

    Graphical abstract: - Highlights: • A simple and low-cost method to prepare Ag@C composite material. • AgNO{sub 3} plays an important role in tuning size and functional groups of products. • HTC reaction time is also a key factor for regulating the Ag@C structure. - Abstract: Ag–carbon composite materials were prepared without any template by hydrothermal carbonization of solvable starch. The composite materials are composed of Ag cores and carbonaceous shell to form a core–shell (Ag@carbon) structure. During the hydrothermal carbonization process, the aromatization and carbonization of solvable starch endowed the Ag@carbon composite structure with abundant aromatic, hydroxyl and carbonyl groups. The AgNO{sub 3} concentration and HTC reaction time are two important factors for regulating the size, morphology and functional groups of the composite material. With the increasing of AgNO{sub 3} concentration, morphologies of the composite material turned from spheres to wires.

  6. 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.

  7. 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.

  8. 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

  9. 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.

  10. Controllable synthesis of TiO2 nanomaterials by assisting with l-cysteine and ethylenediamine

    KAUST Repository

    Tao, Yugui; Cao, Ning; Pan, Jun; Sun, Yichen; Jin, Cheng; Song, Yang

    2013-01-01

    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.

  11. Inverted organic solar cells with solvothermal synthesized vanadium-doped TiO2 thin films as efficient electron transport layer

    Institute of Scientific and Technical Information of China (English)

    Mehdi Ahmadi; Sajjad Rashidi Dafeh; Samaneh Ghazanfarpour; Mohammad Khanzadeh

    2017-01-01

    We investigated the effects of using different thicknesses of pure and vanadium-doped thin films of TiO2 as the electron transport layer in the inverted configuration of organic photovoltaic cells based on poly (3-hexylthiophene) P3HT:[6-6] phenyl-(6) butyric acid methyl ester (PCBM).1% vanadium-doped TiO2 nanoparticles were synthesized via the solvothermal method.Crystalline structure,morphology,and optical properties of pure and vanadium-doped TiO2 thin films were studied by different techniques such as x-ray diffraction,scanning electron microscopy,transmittance electron microscopy,and UV-visible transmission spectrum.The doctor blade method which is compatible with roll-2-roll printing was used for deposition of pure and vanadium-doped TiO2 thin films with thicknesses of 30 nm and 60 nm.The final results revealed that the best thickness of TiO2 thin films for our fabricated cells was 30 nm.The cell with vanadium-doped TiO2 thin film showed slightly higher power conversion efficiency and great Jsc of 10.7 mA/cm2 compared with its pure counterpart.In the cells using 60 nm pure and vanadium-doped TiO2 layers,the cell using the doped layer showed much higher efficiency.It is remarkable that the extemal quantum efficiency of vanadium-doped TiO2 thin film was better in all wavelengths.

  12. In situ ligand generation for novel Mn(II) and Ni(II) coordination polymers with disulfide ligand: Solvothermal syntheses, structures and magnetic properties

    Energy Technology Data Exchange (ETDEWEB)

    Han, Yinfeng, E-mail: hanyinfeng@gmail.com; Wang, Chang' an; Zheng, Zebao; Sun, Jiafeng; Nie, Kun; Zuo, Jian; Zhang, Jianping

    2015-07-15

    Two coordination polymers, ([Mn{sub 2}(L1){sub 2}(μ{sub 2}-H{sub 2}O)(H{sub 2}O){sub 4}]·5H{sub 2}O){sub n}1 and ([Ni(L1)(H{sub 2}O){sub 2}]·2H{sub 2}O){sub n}2 (H{sub 2}L1=2,2′-dithiobisnicotinic acid), were prepared by the solvothermal reactions of the Mn(II) or Ni(II) ions with 2-mercaptonanicotinic acid. In 1, the [Mn{sub 2}(COO){sub 4}] units are connected by the 2,2′-dithiobisnicotinic dianion to form a two-dimensional (4,4)-connected network. In 2, the adjacent Ni(II) ions are connected by the carboxyl groups of the 2,2′-dithiobisnicotinic dianion to form an one-dimensional inorganic rod-shaped chain [Ni(COO){sub 2}]{sub n}, which are further interconnected by the 2,2′-dithiobisnicotinic ligand, giving rise to a two-dimensional framework. Variable-temperature magnetic susceptibilities of 1 and 2 exhibit overall weak antiferromagnetic coupling between the adjacent metal ions. - Graphical abstract: Two 2D coordination polymers were synthesized by transition-metal/in-situ oxidation of 2-mercaptonicotinic acid. The compounds pack into 2D frameworks by the carboxyl groups of 2,2′-dithiobisnicotinic dianion and exhibit overall weak antiferromagnetic coupling. - Highlights: • Two 2D coordination polymers containing 2,2′-dithiobisnicotinic dianion. • In situ oxidation and dehydro coupling reaction of 2-mercaptonbenzoic acid. • Two compounds display weak antiferromagnetic exchanges.

  13. Potassium-doped copper oxide nanoparticles synthesized by a solvothermal method as an anode material for high-performance lithium ion secondary battery

    Energy Technology Data Exchange (ETDEWEB)

    Thi, Trang Vu; Rai, Alok Kumar; Gim, Jihyeon; Kim, Jaekook, E-mail: jaekook@chonnam.ac.kr

    2014-06-01

    A simple and efficient approach was developed to synthesize CuO nanoparticles with improved electrochemical performance. Potassium (K{sup +})-doped CuO nanoparticles were synthesized by a simple and cost-effective solvothermal method followed by annealing at 500 °C for 5 h under air atmosphere. For comparison, an undoped CuO sample was also synthesized under the same conditions. X-ray diffraction analysis demonstrates that the K{sup +} ion doping caused no change in the phase structure, and highly crystalline K{sub x}Cu{sub 1−x}O{sub 1−δ} (x = 0.10) powder without any impurity was obtained. As an anode material for a lithium ion battery, the K{sup +}-doped CuO nanoparticle electrode exhibited better capacity retention with a reversible capacity of over 354.6 mA h g{sup −1} for up to 30 cycles at 0.1 C, as well as a high charge capacity of 162.3 mA h g{sup −1} at a high current rate of 3.2 C, in comparison to an undoped CuO electrode (275.9 mA h g{sup −1} at 0.1 C and 68.9 mA h g{sup −1} at 3.2 C). The high rate capability and better cycleability of the doped electrode can be attributed to the influence of the K{sup +} ion nanostructure on the increased electronic conductivity, diffusion efficiency, and kinetic properties of CuO during the lithiation and delithiation process.

  14. Potassium-doped copper oxide nanoparticles synthesized by a solvothermal method as an anode material for high-performance lithium ion secondary battery

    International Nuclear Information System (INIS)

    Thi, Trang Vu; Rai, Alok Kumar; Gim, Jihyeon; Kim, Jaekook

    2014-01-01

    A simple and efficient approach was developed to synthesize CuO nanoparticles with improved electrochemical performance. Potassium (K + )-doped CuO nanoparticles were synthesized by a simple and cost-effective solvothermal method followed by annealing at 500 °C for 5 h under air atmosphere. For comparison, an undoped CuO sample was also synthesized under the same conditions. X-ray diffraction analysis demonstrates that the K + ion doping caused no change in the phase structure, and highly crystalline K x Cu 1−x O 1−δ (x = 0.10) powder without any impurity was obtained. As an anode material for a lithium ion battery, the K + -doped CuO nanoparticle electrode exhibited better capacity retention with a reversible capacity of over 354.6 mA h g −1 for up to 30 cycles at 0.1 C, as well as a high charge capacity of 162.3 mA h g −1 at a high current rate of 3.2 C, in comparison to an undoped CuO electrode (275.9 mA h g −1 at 0.1 C and 68.9 mA h g −1 at 3.2 C). The high rate capability and better cycleability of the doped electrode can be attributed to the influence of the K + ion nanostructure on the increased electronic conductivity, diffusion efficiency, and kinetic properties of CuO during the lithiation and delithiation process.

  15. Potassium-doped copper oxide nanoparticles synthesized by a solvothermal method as an anode material for high-performance lithium ion secondary battery

    Science.gov (United States)

    Thi, Trang Vu; Rai, Alok Kumar; Gim, Jihyeon; Kim, Jaekook

    2014-06-01

    A simple and efficient approach was developed to synthesize CuO nanoparticles with improved electrochemical performance. Potassium (K+)-doped CuO nanoparticles were synthesized by a simple and cost-effective solvothermal method followed by annealing at 500 °C for 5 h under air atmosphere. For comparison, an undoped CuO sample was also synthesized under the same conditions. X-ray diffraction analysis demonstrates that the K+ ion doping caused no change in the phase structure, and highly crystalline KxCu1-xO1-δ (x = 0.10) powder without any impurity was obtained. As an anode material for a lithium ion battery, the K+-doped CuO nanoparticle electrode exhibited better capacity retention with a reversible capacity of over 354.6 mA h g-1 for up to 30 cycles at 0.1 C, as well as a high charge capacity of 162.3 mA h g-1 at a high current rate of 3.2 C, in comparison to an undoped CuO electrode (275.9 mA h g-1 at 0.1 C and 68.9 mA h g-1 at 3.2 C). The high rate capability and better cycleability of the doped electrode can be attributed to the influence of the K+ ion nanostructure on the increased electronic conductivity, diffusion efficiency, and kinetic properties of CuO during the lithiation and delithiation process.

  16. One-step solvothermal tailoring the compositions and phases of nickel cobalt sulfides on conducting oxide substrates as counter electrodes for efficient dye-sensitized solar cells

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Niu; Li, Guowang [College of Materials and Chemical Engineering, Hubei Provincial Collaborative Innovation Center for New Energy Microgrid, Collaborative Innovation Center for Energy Equipment of Three Gorges Region, China Three Gorges University, Yichang 443002 (China); Huang, Hua [Three Gorges Center for Product Quality Control, Yichang 443002 (China); Sun, Panpan; Xiong, Tianli; Xia, Zhifen; Zheng, Fang; Xu, Jixing [College of Materials and Chemical Engineering, Hubei Provincial Collaborative Innovation Center for New Energy Microgrid, Collaborative Innovation Center for Energy Equipment of Three Gorges Region, China Three Gorges University, Yichang 443002 (China); Sun, Xiaohua, E-mail: mksxh@163.com [College of Materials and Chemical Engineering, Hubei Provincial Collaborative Innovation Center for New Energy Microgrid, Collaborative Innovation Center for Energy Equipment of Three Gorges Region, China Three Gorges University, Yichang 443002 (China)

    2016-12-30

    Highlights: • Co-Ni-S nanoparticles were in-suit grown on FTO via a facile method. • By varying thiourea amount, several Co-Ni-S alloys were obtained. • Amongst the Co-Ni-S alloys, NiCo{sub 2}S{sub 4} exhibited the best electrocatalytic property. - Abstract: Several nickel cobalt sulfide (Ni-Co-S) counter electrodes (CEs) are prepared, and the Ni-Co-S nanoparticles are in-situ grown on SnO{sub 2}: F (FTO) transparent conductive glasses via a facile solvothermal process, in which thiourea is used as the sulfurizing reagent. The X-ray diffraction, scanning electron microscopy, and energy dispersive spectrometer are employed to measure the microstructure and composition of the Ni-Co-S CEs. When a proper amount of thiourea is adopted, fine crystalline NiCo{sub 2}S{sub 4} CE is obtained. When the amount of thiourea is small or large, (Ni,Co){sub 4}S{sub 3} or (Ni,Co){sub 3}S{sub 4} CE is acquired, respectively. Cyclic voltammetry, electrochemical impedance spectroscopy, Tafel polarization and open-circuit voltage decay (OCVD) measurements all demonstrate that the electrocatalytic activities and electrical conductivities of these Ni-Co-S CEs all approach or exceed those of Pt-pyrolysis CE. Their superior electrochemical performances are further confirmed by fabricating DSSCs with the Ni-Co-S CEs, they display similar or better photo-electric conversion efficiencies to/than the Pt-pyrolysis counterpart.

  17. 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}).

  18. Aqueous hydrodechlorination of 4-chlorophenol over an Rh/reduced graphene oxide synthesized by a facile one-pot solvothermal process under mild conditions

    International Nuclear Information System (INIS)

    Ren, Yanlin; Fan, Guangyin; Wang, Chenyu

    2014-01-01

    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 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 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

  19. 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.

  20. 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.

  1. A novel 3D nanoarchitecture of PrVO4 phosphor: Selective synthesis, characterization, and luminescence behavior

    International Nuclear Information System (INIS)

    Thirumalai, J.; Chandramohan, R.; Vijayan, T.A.

    2011-01-01

    Graphical abstract: Nanostructures of tetragonal PrVO 4 with novel 3D hierarchical architectures self-assembled nanorods were successfully synthesized by a hydrothermal method in ethylenediamine tetra-acetic acid (EDTA) mediated processes are ideal functional components for next generation luminescent devices. Research highlights: → Synthesis of self-assembled 3D nanoarchitecture of PrVO 4 phosphor. → Using template-free hydrothermal method. → pH, temperature and capping molecules control morphology of the products. → Detailed structural, morphology and luminescence were studied. - Abstract: Nanostructures of tetragonal PrVO 4 with novel 3D hierarchical architectures self-assembled nanorods were successfully synthesized by a hydrothermal method in ethylenediamine tetra-acetic acid (EDTA) mediated processes. Comprehensive structural, morphological studies like X-ray diffraction, scanning and transmission electron microscopy were employed to characterize the as-obtained products. In the hydrothermal process, EDTA not only acts as a chelating reagent to facilitate the formation of PrVO 4 , but also acts as a surface capping agent to adhere to the newly created surface and to promote the crystal splitting. The formation mechanisms of nanorods to hierarchical architectures were proposed on the basis of a series of surfactant and time-dependent experiments. Photoluminescence (PL) studies of PrVO 4 showed strong red emission upon UV illumination, and this implied potential application in the luminescent field. A possible growth mechanism of the sheaf-like PrVO 4 hierarchical nanocrystals is proposed and discussed.

  2. 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.

  3. Solution-based synthesis and design of late transition metal chalcogenide materials for oxygen reduction reaction (ORR).

    Science.gov (United States)

    Gao, Min-Rui; Jiang, Jun; Yu, Shu-Hong

    2012-01-09

    Late transition metal chalcogenide (LTMC) nanomaterials have been introduced as a promising Pt-free oxygen reduction reaction (ORR) electrocatalysts because of their low cost, good ORR activity, high methanol tolerance, and facile synthesis. Herein, an overview on the design and synthesis of LTMC nanomaterials by solution-based strategies is presented along with their ORR performances. Current solution-based synthetic approaches towards LTMC nanomaterials include a hydrothermal/solvothermal approach, single-source precursor approach, hot-injection approach, template-directed soft synthesis, and Kirkendall-effect-induced soft synthesis. Although the ORR activity and stability of LTMC nanomaterials are still far from what is needed for practical fuel-cell applications, much enhanced electrocatalytic performance can be expected. Recent advances have emphasized that decorating the surface of the LTMC nanostructures with other functional nanoparticles can lead to much better ORR catalytic activity. It is believed that new synthesis approaches to LTMCs, modification techniques of LTMCs, and LTMCs with desirable morphology, size, composition, and structures are expected to be developed in the future to satisfy the requirements of commercial fuel cells. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Solvothermal-assisted evaporation-induced self-assembly process for significant improvement in the textural properties of γ-Al2O3, and study dye adsorption efficiency

    Directory of Open Access Journals (Sweden)

    Sourav Ghosh

    2015-06-01

    Full Text Available A comparative study of the textural properties of γ-Al2O3 prepared by solvothermal-assisted evaporation-induced self-assembly (SA-EISA and conventional evaporation-induced self-assembly (EISA processes has been carried out using aluminum isopropoxide, triblock copolymer-type nonionic surfactant (Pluronic P123 and ethanol. The solvothermal reaction was carried out at 100 °C for 24 h followed by slow drying at 60 °C for 48 h. The synthesized products were characterized by thermogravimetry analysis (TGA, differential thermal analysis (DTA, X-ray diffraction (XRD analysis, N2 adsorption–desorption study and transmission electron microscopy (TEM. The γ-Al2O3 prepared by SA-EISA process became stable up to 1000 °C. The powder prepared by SA-EISA process resulted in a significant increase in textural properties (BET surface area, pore volume and pore diameter compared to that prepared by conventional EISA process. A better adsorption capacity for Congo red, a carcinogenic dye used in textile industry, was exhibited by the powders prepared by SA-EISA process. A proposed mechanism was illustrated for the formation of mesoporous γ-Al2O3 obtained by EISA and SA-EISA processes.

  5. 多级孔分子筛的合成及催化应用研究进展%Research progress of synthesis and catalytic applications of hierarchical molecular sieves

    Institute of Scientific and Technical Information of China (English)

    宋菁; 张君涛; 申志兵; 梁生荣

    2017-01-01

    综述了近几年国内外多级孔分子筛的研究进展,重点介绍了“自上而下”和“自下而上”两大类合成方法,并进一步阐述了脱硅法、重结晶法、硬模板法、软模板法、无模板自组装等具体合成方法的优势及局限性,同时介绍了不同方法制得的多级孔分子筛的催化应用,最后对多级孔分子筛的发展前景进行了展望.%The synthesis methods and catalytic applications of hierarchical molecular sieves in recent years have been reviewed.Various synthesis approaches of hierarchical molecular sieves are introduced,including Top-down approach and Bottom-up approach.Advantages and limitations of the different methods such as demetalization,recrystallization,hard template,soft template,template-free,and so on,will also be addressed.Meanwhile,the catalytic applications of the as-synthesized zeolites are discussed.The prospect of hierarchical molecular sieves is outlined in the end.

  6. Facile Synthesis of V2O5 Hollow Spheres as Advanced Cathodes for High-Performance Lithium-Ion Batteries

    Directory of Open Access Journals (Sweden)

    Xingyuan Zhang

    2017-01-01

    Full Text Available Three-dimensional V2O5 hollow structures have been prepared through a simple synthesis strategy combining solvothermal treatment and a subsequent thermal annealing. The V2O5 materials are composed of microspheres 2–3 μm in diameter and with a distinct hollow interior. The as-synthesized V2O5 hollow microspheres, when evaluated as a cathode material for lithium-ion batteries, can deliver a specific capacity as high as 273 mAh·g−1 at 0.2 C. Benefiting from the hollow structures that afford fast electrolyte transport and volume accommodation, the V2O5 cathode also exhibits a superior rate capability and excellent cycling stability. The good Li-ion storage performance demonstrates the great potential of this unique V2O5 hollow material as a high-performance cathode for lithium-ion batteries.

  7. Synthesis of nanostructured CuInS{sub 2} thin films and their application in dye-sensitized solar cells

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Yu; Zhuang, Mixue; Liu, Zhen; Wei, Aixiang [Guangdong University of Technology, Guangdong Provincial Key Laboratory of Functional Soft Condensed Matter, School of Material and Energy, Guangzhou (China); Luo, Fazhi [Guangdong University of Technology, Guangdong Provincial Key Laboratory of Functional Soft Condensed Matter, School of Material and Energy, Guangzhou (China); The Fifth Electronics Research Institute of Ministry of Industry and Information Technology, Guangzhou (China); Liu, Jun [Guangdong University of Technology, Guangdong Provincial Key Laboratory of Functional Soft Condensed Matter, School of Material and Energy, Guangzhou (China); Zhejiang University, State Key Lab of Silicon Materials, Hangzhou (China)

    2016-03-15

    CuInS{sub 2} (CIS) nanostructure thin films were successfully synthesized on FTO conductive glass substrates by solvothermal method. It is found that the surface morphology and microstructure of CIS thin films can be tailored by simply adjusting the concentration of oxalic acid. CIS nanostructure films with texture of ''nanosheet array'' and ''flower-like microsphere'' were obtained and used as Pt-free counter electrode for dye-sensitized solar cells (DSSCs). The nanosheet array CIS was found to have a better electrocatalytic activity than the flower-like microsphere one. DSSCs based on nanosheet array CIS thin film counter electrode show conversion efficiency of 3.33 %, which is comparable to the Pt-catalyzed DSSCs. The easy synthesis, low cost, morphology tunable and excellent electrocatalytic property may make the CuInS{sub 2} nanostructure competitive as counter electrode in DSSCs. (orig.)

  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. Use of organic precursors and graphenes in the controlled synthesis of carbon-containing nanomaterials for energy storage and conversion.

    Science.gov (United States)

    Yang, Shubin; Bachman, Robert E; Feng, Xinliang; Müllen, Klaus

    2013-01-15

    The development of high-performance electrochemical energy storage and conversion devices, including supercapacitors, lithium-ion batteries, and fuel cells, is an important step on the road to alternative energy technologies. Carbon-containing nanomaterials (CCNMs), defined here as pure carbon materials and carbon/metal (oxide, hydroxide) hybrids with structural features on the nanometer scale, show potential application in such devices. Because of their pronounced electrochemical activity, high chemical and thermal stability and low cost, researchers are interested in CCNMs to serve as electrodes in energy-related devices. Various all-carbon materials are candidates for electrochemical energy storage and conversion devices. Furthermore, carbon-based hybrid materials, which consist of a carbon component with metal oxide- or metal hydroxide-based nanostructures, offer the opportunity to combine the attractive properties of these two components and tune the behavior of the resulting materials. As such, the design and synthesis of CCNMs provide an attractive route for the construction of high-performance electrode materials. Studies in these areas have revealed that both the composition and the fabrication protocol employed in preparing CCNMs influence the morphology and microstructure of the resulting material and its electrochemical performance. Consequently, researchers have developed several synthesis strategies, including hard-templated, soft-templated, and template-free synthesis of CCNMs. In this Account, we focus on recent advances in the controlled synthesis of such CCNMs and the potential of the resulting materials for energy storage or conversion applications. The Account is divided into four major categories based on the carbon precursor employed in the synthesis: low molecular weight organic or organometallic molecules, hyperbranched or cross-linked polymers consisting of aromatic subunits, self-assembling discotic molecules, and graphenes. In each case

  10. LiFePO4 mesocrystals for lithium-ion batteries.

    Science.gov (United States)

    Popovic, Jelena; Demir-Cakan, Rezan; Tornow, Julian; Morcrette, Mathieu; Su, Dang Sheng; Schlögl, Robert; Antonietti, Markus; Titirici, Maria-Magdalena

    2011-04-18

    Olivine LiFePO(4) is considered one of the most promising cathode materials for Li-ion batteries. A simple one-step, template-free, low-temperature solvothermal method is developed for the synthesis of urchinlike hierarchical mesocrystals of pristine LiFePO(4) as well as carbon-coated LiFePO(4) composites. Each urchinlike mesocrystal consists of LiFePO(4) sheets self-assembled via a dipolar field in spheres during a solvothermal process under the influence of Cl(-) anions. The obtained primary sheets of LiFePO(4) are single crystalline in nature and can be coated in situ with an amorphous nitrogen-doped carbonaceous layer several nanometers in thickness. To increase the conductivity of the carbon coating, the materials are subjected to further temperature treatment (700 °C) under an inert atmosphere. The lithium storage performance of the pure LiFePO(4) is compared with that of its carbon-coated counterparts. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. 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.

  12. Morphology-controllable synthesis of cobalt oxalates and their conversion to mesoporous Co3O4 nanostructures for application in supercapacitors.

    Science.gov (United States)

    Wang, Dewei; Wang, Qihua; Wang, Tingmei

    2011-07-18

    In this work, one-dimensional and layered parallel folding of cobalt oxalate nanostructures have been selectively prepared by a one-step, template-free, water-controlled precipitation approach by simply altering the solvents used at ambient temperature and pressure. Encouragingly, the feeding order of solutions played an extraordinary role in the synthesis of nanorods and nanowires. After calcination in air, the as-prepared cobalt oxalate nanostructures were converted to mesoporous Co(3)O(4) nanostructures while their original frame structures were well maintained. The phase composition, morphology, and structure of the as-obtained products were studied in detail. Electrochemical properties of the Co(3)O(4) electrodes were carried out using cyclic voltammetry (CV) and galvanostatic charge-discharge measurements by a three-electrode system. The electrochemical experiments revealed that the layered parallel folding structure of mesoporous Co(3)O(4) exhibited higher capacitance compared to that of the nanorods and nanowires. A maximum specific capacitance of 202.5 F g (-1) has been obtained in 2 M KOH aqueous electrolyte at a current density of 1 A g(-1) with a voltage window from 0 to 0.40 V. Furthermore, the specific capacitance decay after 1000 continuous charge-discharge cycles was negligible, revealing the excellent stability of the electrode. These characteristics indicate that the mesoporous Co(3)O(4) nanostructures are promising electrode materials for supercapacitors.

  13. 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.

  14. 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.

  15. Solvothermal coating LiNi_0_._8Co_0_._1_5Al_0_._0_5O_2 microspheres with nanoscale Li_2TiO_3 shell for long lifespan Li-ion battery cathode materials

    International Nuclear Information System (INIS)

    Wu, Naiteng; Wu, Hao; Liu, Heng; Zhang, Yun

    2016-01-01

    LiNi_0_._8Co_0_._1_5Al_0_._0_5O_2 (NCA) microspheres covered by a nanoscale Li_2TiO_3-based shell were synthesized by a facile strategy based on a solvothermal pre-coating treatment combined with a post-sintering lithiation process. The morphology, structure and composition of the Li_2TiO_3-coated NCA samples were investigated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning scanning electron microscope (SEM) with an energy-dispersive X-ray spectroscope (EDS), and transmission electron microscopy (TEM). Owing to the complete, uniform and nanoscale Li_2TiO_3 coating shell, the resultant surface-modified NCA microspheres used as Li-ion battery cathode materials manifest remarkably enhanced cycling performances, attaining 94% and 84% capacity retention after 200 and 400 cycles at 0.5 C, respectively, which is much better than the pristine NCA counterpart (60% retention, 200 cycles). More impressively, the surface-modified NCA also shows an intriguing storage stability. After being stored at 30 °C for 50 days, the coated NCA-based cells are subjected to be cycled both at room and elevated temperatures, in which the aged cells can still remain 84% capacity retention after 200 cycles at 25 °C and 77% capacity retention after 200 cycles at 55 °C, respectively. All these results demonstrate that the Li_2TiO_3-coated LiNi_0_._8Co_0_._1_5Al_0_._0_5O_2 microsphere is a promising cathode material for Li-ion batteries with long lifespan. - Graphical abstract: Nanoscale Li_2TiO_3-based shell encapsulated LiNi_0_._8Co_0_._1_5Al_0_._0_5O_2 (NCA) microspheres are fabricated through a solvothermal pre-coating treatment combined with post-lithiation process. The surface-coated NCA as cathode materials shows a remarkably enhanced cycling performance and storage stability for long lifespan Li-ion batteries. - Highlights: • Li_2TiO_3 is used as coating materials for layer structured LiNi_0_._8Co_0_._1_5Al_0_._0_5O_2 cathode. • Solvothermal coating

  16. Rapid and facile preparation of zinc ferrite (ZnFe{sub 2}O{sub 4}) oxide by microwave-solvothermal technique and its catalytic activity in heterogeneous photo-Fenton reaction

    Energy Technology Data Exchange (ETDEWEB)

    Anchieta, Chayene G.; Severo, Eric C.; Rigo, Caroline; Mazutti, Marcio A. [Department of Chemical Engineering, Federal University of Santa Maria, 97105-900, Santa Maria (Brazil); Kuhn, Raquel C., E-mail: raquelckuhn@yahoo.com.br [Department of Chemical Engineering, Federal University of Santa Maria, 97105-900, Santa Maria (Brazil); Muller, Edson I.; Flores, Erico M.M. [Department of Chemistry, Federal University of Santa Maria, 97105-900, Santa Maria (Brazil); Moreira, Regina F.P.M. [Department of Chemical Engineering and Food Engineering, Federal University of Santa Catarina, 88040-970, Florianópolis (Brazil); Foletto, Edson L. [Department of Chemical Engineering, Federal University of Santa Maria, 97105-900, Santa Maria (Brazil)

    2015-06-15

    In this work zinc ferrite (ZnFe{sub 2}O{sub 4}) oxide was rapidly and easily prepared by microwave-solvothermal route and its catalytic property in photo-Fenton reaction was evaluated. The effects of microwave heating time and power on the properties of produced particles were investigated. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), atomic force microscopy (AFM) and nitrogen adsorption–desorption isotherms were the techniques used for characterizing the solid products. The synthesized material was tested as a catalyst in the degradation of the textile dye molecule by the heterogeneous photo-Fenton process. Characterization results showed that the microwave heating time and power have significant influences on the formation of the phase spinel as well as on its physical properties. The reaction results showed that the ZnFe{sub 2}O{sub 4} oxide has good photocatalytic activity, which can be attributed to high surface area and pore volume, and large pore size. The ZnFe{sub 2}O{sub 4} oxide produced by the microwave irradiation exhibited promising photocatalytic activity for the removal of textile dye, reaching nearly 100% of decolorization at 40 min and 60% of mineralization at 240 min. Therefore, ZnFe{sub 2}O{sub 4} particles rapidly prepared by the microwave route have the potential for use in treatment of textile wastewater by the heterogeneous photo-Fenton process. - Highlights: • ZnFe{sub 2}O{sub 4} was synthesized by microwave-solvothermal method. • ZnFe{sub 2}O{sub 4} was prepared by different microwave heating times and powers. • ZnFe{sub 2}O{sub 4} was used as heterogeneous photo-Fenton catalyst. • Degradation of Procion red dye using heterogeneous photo-Fenton process. • ZnFe{sub 2}O{sub 4} was highly efficient to degrade textile dye under visible light.

  17. Solvothermal syntheses of Bi and Zn co-doped TiO_2 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.

  18. Structure-directing effects of ionic liquids in the ionothermal synthesis of metal-organic frameworks.

    Science.gov (United States)

    Vaid, Thomas P; Kelley, Steven P; Rogers, Robin D

    2017-07-01

    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.

  19. 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.

  20. All-gas-phase synthesis of UiO-66 through modulated atomic layer deposition

    Science.gov (United States)

    Lausund, Kristian Blindheim; Nilsen, Ola

    2016-11-01

    Thin films of stable metal-organic frameworks (MOFs) such as UiO-66 have enormous application potential, for instance in microelectronics. However, all-gas-phase deposition techniques are currently not available for such MOFs. We here report on thin-film deposition of the thermally and chemically stable UiO-66 in an all-gas-phase process by the aid of atomic layer deposition (ALD). Sequential reactions of ZrCl4 and 1,4-benzenedicarboxylic acid produce amorphous organic-inorganic hybrid films that are subsequently crystallized to the UiO-66 structure by treatment in acetic acid vapour. We also introduce a new approach to control the stoichiometry between metal clusters and organic linkers by modulation of the ALD growth with additional acetic acid pulses. An all-gas-phase synthesis technique for UiO-66 could enable implementations in microelectronics that are not compatible with solvothermal synthesis. Since this technique is ALD-based, it could also give enhanced thickness control and the possibility to coat irregular substrates with high aspect ratios.

  1. Ultrasound-assisted synthesis and processing of carbon materials

    Science.gov (United States)

    Fortunato, Maria E.

    2011-12-01

    Part I: Porous carbons are of interest in many applications because of their high surface areas and other physicochemical properties, and much effort has been directed towards developing new methods for controlling the porosity of carbons. Ultrasonic spray pyrolysis (USP) is an aerosol method suitable for large-scale, continuous synthesis of materials. Ultrasound is used to create aerosol droplets of a precursor solution which serve as micron-sized spherical reactors for materials synthesis. This work presents a precursor system for the template-free USP synthesis of porous carbons using low-cost precursors that do not evolve or require hazardous chemicals: sucrose was used as the carbon source, and sodium carbonate, sodium bicarbonate, or sodium nitrate was added as a decomposition catalyst and porogen. The USP carbons had macroporous interiors and microporous shells with surface areas as high as 800 m2/g and a narrow pore size distribution. It was determined that the interior porosity was a result of the gas evolution from salt decomposition and not from the presence of a salt template. Porous carbon is frequently used as a catalyst support because it provides high surface area and it is chemically and physically stable under many anoxic reaction conditions. Typically, the preparation of supported catalysts requires multiple steps for carbonization and metal impregnation. In this work, iron-impregnated porous carbon microspheres (Fe-C) were prepared by a one-step USP process by incorporating both the carbon and metal sources into the precursor solution. Carbonization, pore formation, metal impregnation, and metal activation occurred simultaneously to produce Fe-C materials with surface areas as high as 800 m2/g and up to 10 wt% Fe incorporated as nanoparticles carbon support. Part II: The effects of high intensity ultrasound arise from acoustic cavitation: the formation, growth, and collapse of bubbles in a liquid. Bubble collapse produces intense localized

  2. 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.

  3. 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

  4. Solvothermal syntheses of Bi and Zn co-doped TiO{sub 2} with enhanced electron-hole separation and efficient photodegradation of gaseous toluene under visible-light

    Energy Technology Data Exchange (ETDEWEB)

    Li, Juan-Juan [Center for Excellence in Regional Atmospheric Environment, and Key Laboratory of Urban Pollutant Conversion, Institute of Urban Environment, Chinese Academy of Sciences, Xiamen 361021 (China); Cai, Song-Cai [Center for Excellence in Regional Atmospheric Environment, and Key Laboratory of Urban Pollutant Conversion, Institute of Urban Environment, Chinese Academy of Sciences, Xiamen 361021 (China); University of Chinese Academy of Sciences, Beijing, 100049 (China); Xu, Zhen [Center for Excellence in Regional Atmospheric Environment, and Key Laboratory of Urban Pollutant Conversion, Institute of Urban Environment, Chinese Academy of Sciences, Xiamen 361021 (China); Chen, Xi [Center for Excellence in Regional Atmospheric Environment, and Key Laboratory of Urban Pollutant Conversion, Institute of Urban Environment, Chinese Academy of Sciences, Xiamen 361021 (China); University of Chinese Academy of Sciences, Beijing, 100049 (China); Chen, Jin [Center for Excellence in Regional Atmospheric Environment, and Key Laboratory of Urban Pollutant Conversion, Institute of Urban Environment, Chinese Academy of Sciences, Xiamen 361021 (China); Jia, Hong-Peng, E-mail: hpjia@iue.ac.cn [Center for Excellence in Regional Atmospheric Environment, and Key Laboratory of Urban Pollutant Conversion, Institute of Urban Environment, Chinese Academy of Sciences, Xiamen 361021 (China); Chen, Jing, E-mail: jing.chen@fjirsm.ac.cn [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002 (China)

    2017-03-05

    Highlights: • Bi-Zn co-doped TiO{sub 2} catalysts were prepared by solvothermal route. • The incorporation of Bi doping into the TiO{sub 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{sub 1.9%}Zn{sub 1%}O{sub 2} exhibited high photocatalytic degradation for toluene. - Abstract: This study investigated the effects of Bi doped and Bi-Zn co-doped TiO{sub 2} on photodegradation of gaseous toluene. The doped TiO{sub 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{sub 1.9%}O{sub 2} and TiBi{sub 1.9%}Zn{sub 1%}O{sub 2} can reach to 51% and 93%, respectively, which are much higher than 25% of TiO{sub 2}. Bi doping into TiO{sub 2} lattice generates new intermediate energy level of Bi below the CB edge of TiO{sub 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{sub 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.

  5. 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.

  6. 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

  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. A template-free approach for determining the latency of single events of auditory evoked M100

    Energy Technology Data Exchange (ETDEWEB)

    Burghoff, M [Physikalisch-Technische Bundesanstalt (PTB), Berlin (Germany); Link, A [Physikalisch-Technische Bundesanstalt (PTB), Berlin (Germany); Salajegheh, A [Cognitive Neuroscience of Language Laboratory, University of Maryland College Park, MD (United States); Elster, C [Physikalisch-Technische Bundesanstalt (PTB), Berlin (Germany); Poeppel, D [Cognitive Neuroscience of Language Laboratory, University of Maryland College Park, MD (United States); Trahms, L [Physikalisch-Technische Bundesanstalt (PTB), Berlin (Germany)

    2005-02-07

    The phase of the complex output of a narrow band Gaussian filter is taken to define the latency of the auditory evoked response M100 recorded by magnetoencephalography. It is demonstrated that this definition is consistent with the conventional peak latency. Moreover, it provides a tool for reducing the number of averages needed for a reliable estimation of the latency. Single-event latencies obtained by this procedure can be used to improve the signal quality of the conventional average by latency adjusted averaging. (note)

  9. 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

  10. 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

  11. Facile Template-Free Fabrication of the hollow sea cucumber-like TbF{sub 3} and luminescent properties

    Energy Technology Data Exchange (ETDEWEB)

    Gao, Yu, E-mail: gaoy777@126.com [College of Materials Science and Engineering, Shenyang University of Chemical Technology, Shenyang, 100142 (China); Shi, Shan; Fang, Qinghong; Yang, Feng [College of Materials Science and Engineering, Shenyang University of Chemical Technology, Shenyang, 100142 (China); Xu, Zhenhe [College of Applied Chemistry, Shenyang University of Chemical Technology, Shenyang, 100142 (China)

    2014-12-15

    Graphical abstract: Hollow sea cucumber-like TbF{sub 3} has been prepared via a facile hydrothermal route. The possible growth mechanism and the luminescent properties of the as-prepared sample have been discussed. - Highlights: • TbF3 particles were prepared by a facile hydrothermal route. • TbF3 product show strong green emission. • This method may be more widely applicable in the design of other rare-earth compounds. - Abstract: Hollow sea cucumber-like TbF{sub 3} was successfully fabricated by a self-assembled hydrothermal method. The crystal structure, morphology and photoluminescence properties of the as-prepared TbF{sub 3} crystals were investigated. The results revealed that the as-prepared TbF{sub 3} sample has orthorhombic structure and composed of monodispersed 3D hollow sea cucumber-like particles. The possible formation mechanism for sea cucumber-like TbF{sub 3} is presented in detail. Additionally, the as-prepared sample possesses property of down-conversion photoluminescence. The excitation spectrum of TbF{sub 3} sample was obtained by monitoring the emission of Tb{sup 3+} at 545 nm was composed of the characteristics f–f transition lines within the Tb{sup 3+} 4f{sup 8} configuration. Under the UV light irradiation, the emission spectrum exhibited four obvious lines centered at 491, 545, 588, and 620 nm, which was corresponding to the {sup 5}D{sub 4} → {sup 7}F{sub J} (J = 6, 5, 4, 3) transitions of the Tb{sup 3+} ions in the TbF{sub 3} nanoparticles.

  12. Template free fabrication of hollow hematite spheres via a one-pot polyoxometalate-assisted hydrolysis process

    International Nuclear Information System (INIS)

    Mao Baodong; Kang Zhenhui; Wang Enbo; Tian Chungui; Zhang Zhiming; Wang Chunlei; Song Yanli; Li Meiye

    2007-01-01

    Uniform hollow hematite (α-Fe 2 O 3 ) spheres with diameter of about 600-700 nm and shell thickness lower than 100 nm are obtained by direct hydrothermal treatment of dilute FeCl 3 and tungstophosphoric acid H 3 PW 12 O 40 solution at 180 deg. C. The hollow spheres are composed of robust shells with small nanoparticles standing out of the surface and present a high-surface area and a weak ferromagnetic behavior at room temperature. The effect of concentration of H 3 PW 12 O 40 , reaction time and temperature for the formation of the hollow spheres are investigated in series of experiments. The formation of the hollow spheres may be ascribed to a polyoxometalte-assisted forced hydrolysis and dissolution process. - Graphical abstract: Uniform hollow hematite (α-Fe 2 O 3 ) spheres with diameter of about 600-700 nm and shell thickness lower than 100 nm are obtained by direct hydrothermal treatment of dilute FeCl 3 and tungstophosphoric acid H 3 PW 12 O 40 solution at 180 deg. C. The hollow spheres present a high surface area and weak ferromagnetic behavior at room temperature

  13. 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.

  14. The synthesis and photocatalytic activity of ZnSe microspheres

    International Nuclear Information System (INIS)

    Cao Huaqiang; Xiao Yujiang; Zhang Sichun

    2011-01-01

    This paper reports the synthesis of semiconductor ZnSe microspheres composed of nanoparticles via a solvothermal route between the organic molecule selenophene (C 4 H 4 Se) and ZnCl 2 without adding any surfactant. The ZnSe microspheres were characterized by x-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), specific surface area measurement, and photoluminescence (PL) spectra. A strong and broad blue PL emission at 443 nm in wavelength (∼2.79 eV in photon energy) is attributed to the near-band-edge (NBE) emission of ZnSe, while the 530 nm peak is a defect-related (DL) emission. The photocatalytic activity of the as-prepared ZnSe microspheres was evaluated by photodegradation of methyl orange (MO) dye under ultraviolet (UV) light and visible light irradiation. The degradations of MO reach 94% or 95.1%, close to 100%, in the presence of the as-synthesized ZnSe microspheres or commercial ZnSe powder after 7 or 10 h under UV irradiation, respectively. Meanwhile the degradations of MO reach 94.3% or 60.6% in the presence of the as-synthesized ZnSe microspheres or commercial ZnSe powder after 12 h, respectively. The degradation rate of ZnSe microspheres is twice that of ZnSe commercial powder under UV light irradiation, and three times under visible light irradiation. The degradation process of MO dye on ZnSe microspheres under UV or visible light is also discussed.

  15. Synthesis of highly c-oriented ZIF-69 membranes by secondary growth and their gas permeation properties

    KAUST Repository

    Liu, Yunyang; Zeng, Gaofeng; Pan, Yichang; Lai, Zhiping

    2011-01-01

    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.

  16. 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.

  17. 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.

  18. 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.

  19. Synthesis of ZnO particles using water molecules generated in esterification reaction

    Science.gov (United States)

    Šarić, Ankica; Gotić, Marijan; Štefanić, Goran; Dražić, Goran

    2017-07-01

    Zinc oxide particles were synthesized without the addition of water by autoclaving (anhydrous) zinc acetate/alcohol and zinc acetate/acetic acid/alcohol solutions at 160 °C. The solvothermal synthesis was performed in ethanol or octanol. The structural, optical and morphological characteristics of ZnO particles were investigated by X-ray diffraction (XRD), UV-Vis spectroscopy, FE-SEM and TEM/STEM microscopy. 13C NMR spectroscopy revealed the presence of ester (ethyl- or octyl-acetate) in the supernatants which directly indicate the reaction mechanism. The formation of ester in this esterification reaction generated water molecule in situ, which hydrolyzed anhydrous zinc acetate and initiated nucleation and formation of ZnO. It was found that the size and shape of ZnO particles depend on the type of alcohol used as a solvent and on the presence of acetic acid in solution. The presence of ethanol in the ;pure; system without acetic acid favoured the formation of fine and uniform spherical ZnO nanoparticles (∼20 nm). With the addition of small amount of acetic acid the size of these small nanoparticles increased significantly up to a few hundred nanometers. The addition of small amount of acetic acid in the presence of octanol caused even more radical changes in the shape of ZnO particles, favouring the growth of huge rod-like particles (∼3 μm).

  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 of manganese coordination polymer microspheres for lithium-ion batteries with good cycling performance

    International Nuclear Information System (INIS)

    Fei, Hailong; Liu, Xin; Li, Zhiwei; Feng, Wenjing

    2015-01-01

    Highlights: • We achieve controllable synthesis of manganese 2,5-thiophene dicarboxylate microspheres with DMF and CTABr. • We perform research on changes in morphologies and crystalline structure. • It is a new anode material for lithium-ion batteries with high capacity and good cycle stability. - Abstract: A simple and versatile method for preparation of novel manganese 2,5-thiophene dicarboxylate microspheres is developed via a surfactant-assisted solvo-thermal route, which are found to be a new high-energy anode material for lithium-ion batteries. It shows better cycling performance and higher discharge capacity than its counterpart of irregular shapes. A reversible capacity was achieved as high as 645.7 mA h g −1 after 250 cycles at a current density of 400 mA g −1 . Furthermore, the coulombic efficiency can be close to 100% even after 650 charge-discharge cycles at a current density of 500 mA g −1

  2. 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.

  3. Synthesis, characterization and application of metal organic frameworks in the adsorption of dimethylamine

    International Nuclear Information System (INIS)

    Sun-Kou, Maria del Rosario; Bravo Hualpa, Fabiola; Beltran Suito, Rodrigo; Samanamu, Christian; Picasso Escobar, Gino

    2014-01-01

    This study investigated the removal of dimethylamine (DMA) by an adsorption mechanism using metal-organic frameworks (MOFs). The synthesis of the MOFs was performed by solvothermal methods. The characterization of the MOF obtained was made by attenuated total reflectance spectroscopy (ATR), proton nuclear magnetic resonance spectroscopy ("1H-NMR), X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDX) and scanning electron microscopy (SEM). The XRD diffractograms allowed to identify the structure of MOF as Dashkovaite, which has the molecular formula Mg(HCOO)_2.2H_2O; while the ATR studies revealed the presence of carbonyl group as most important functional group in the MOF structure. The morphological analysis showed that the MOF crystalline particles had a hexagonal shape, formed from filaments of around 7,5-8 microns in length. Adsorption experiments showed that the MOF had a high adsorption capacity of DMA (q_e= 307,96 mg.g"-"1). The kinetic data were fitted to the pseudo second order equation and the Elovich equation, while the adsorption isotherm was fitted to the Temkin equation and the Dubinin - Radushkevich equation, processes related to chemisorptions preferably on a heterogeneous surface. (author)

  4. Green synthesis of AgI-reduced graphene oxide nanocomposites: Toward enhanced visible-light photocatalytic activity for organic dye removal

    International Nuclear Information System (INIS)

    Reddy, D. Amaranatha; Lee, Seunghee; Choi, Jiha; Park, Seonhwa; Ma, Rory; Yang, Haesik; Kim, Tae Kyu

    2015-01-01

    Graphical abstract: - Highlights: • A novel green synthesis of AgI-RGO nanocomposites. • Significant improvement of the photocatalytic activity in RGO wrapped composites. • Additive promoted photocatalytic performance in AgI-RGO composites. • AgI-RGO nanocomposites may find applications in luminescent and catalytic devices. - Abstract: Novel reduced graphene oxide (RGO) enwrapped AgI nanocomposites were successfully fabricated by a facile template-free ultrasound-assisted method at room temperature. The structural, morphological, and optical studies demonstrate that the obtained nanostructures have good crystallinity and that the graphene nanosheets are decorated densely with AgI nanostructures. The photocatalytic activity of the composite was evaluated by the degradation of an organic dye, Rhodamine B (RhB), under visible-light irradiation. The results indicate that AgI with incorporated graphene exhibited much higher photocatalytic activity than the pure AgI due to the improved separation efficiency of the photogenerated carriers and that it prolonged the lifetime of the electron–hole pairs due to the chemical bonding between AgI and graphene. AgI (0.4 mg mL −1 of graphene oxide) nanocomposites displayed the highest photocatalytic degradation efficiency and the corresponding catalytic efficiencies within 70 min were ∼96%. Moreover, with the assistance of H 2 O 2 the photocatalytic ability of the as-obtained AgI-RGO nanocomposites was enhanced. The corresponding catalytic efficiencies within 30 min were ∼96.8% (for 1 mL H 2 O 2 ) under the same irradiation conditions. The excellent visible-light photocatalytic efficiency and luminescence properties make the AgI-RGO nanocomposites promising candidates for the removal of organic dyes for water purification and enable their application in near-UV white LEDs

  5. 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

  6. Synthesis and characterization of microporous inorganic membranes for propylene/propane separation

    Science.gov (United States)

    Ma, Xiaoli

    Membrane-based gas separation is promising for efficient propylene/propane (C3H6/C3H8) separation with low energy consumption and minimum environment impact. Two microporous inorganic membrane candidates, MFI-type zeolite membrane and carbon molecular sieve membrane (CMS) have demonstrated excellent thermal and chemical stability. Application of these membranes into C3H6/C3H 8 separation has not been well investigated. This dissertation presents fundamental studies on membrane synthesis, characterization and C3H 6/C3H8 separation properties of MFI zeolite membrane and CMS membrane. MFI zeolite membranes were synthesized on α-alumina supports by secondary growth method. Novel positron annihilation spectroscopy (PAS) techniques were used to non-destructively characterize the pore structure of these membranes. PAS reveals a bimodal pore structure consisting of intracrystalline zeolitic micropores of ~0.6 nm in diameter and irregular intercrystalline micropores of 1.4 to 1.8 nm in size for the membranes. The template-free synthesized membrane exhibited a high permeance but a low selectivity in C3H 6/C3H8 mixture separation. CMS membranes were synthesized by coating/pyrolysis method on mesoporous gamma-alumina support. Such supports allow coating of thin, high-quality polymer films and subsequent CMS membranes with no infiltration into support pores. The CMS membranes show strong molecular sieving effect, offering a high C3H 6/C3H8 mixture selectivity of ~30. Reduction in membrane thickness from 500 nm to 300 nm causes an increase in C3H8 permeance and He/N2 selectivity, but a decrease in the permeance of He, N 2 and C3H6 and C3H6/C 3H8 selectivity. This can be explained by the thickness dependent chain mobility of the polymer film resulting in final carbon membrane of reduced pore size with different effects on transport of gas of different sizes, including possible closure of C3H6-accessible micropores. CMS membranes demonstrate excellent C3H6/C 3H8 separation

  7. 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

  8. Hamiltonian Algorithm Sound Synthesis

    OpenAIRE

    大矢, 健一

    2013-01-01

    Hamiltonian Algorithm (HA) is an algorithm for searching solutions is optimization problems. This paper introduces a sound synthesis technique using Hamiltonian Algorithm and shows a simple example. "Hamiltonian Algorithm Sound Synthesis" uses phase transition effect in HA. Because of this transition effect, totally new waveforms are produced.

  9. 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...

  10. 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....

  11. 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...

  12. Solvothermal syntheses, crystal structures, and properties of lanthanide(III) thioarsenates [Ln(dien)2(μ-1κ,2κ2-AsS4)]n (Ln==Sm, Eu, Gd) and [Ln(dien)2(1κ2-AsS4)] (Ln==Tb, Dy, Ho)

    International Nuclear Information System (INIS)

    Wang, Fang; Tang, Chunying; Chen, Ruihong; Zhang, Yong; Jia, Dingxian

    2013-01-01

    Solvothermal reactions of Ln 2 O 3 , As and S in diethylenetriamine (dien) at 170 °C for 6 days afforded two structural types of lanthanide thioarsenates with the general formulae [Ln(dien) 2 (μ-1κ,2κ 2 -AsS 4 )] n [Ln=Sm(1), Eu(2), Gd(3)] and [Ln(dien) 2 (1κ 2 -AsS 4 )] [Ln=Tb(4), Dy(5), Ho(6)]. The Ln 2 O 3 oxides were converted to [Ln(dien) 2 ] 3+ complex units in the solvothermal reactions. The As atom binds four S atoms, forming a tetrahedral AsS 4 unit. In 1−3, the AsS 4 units interconnect the [Ln(dien) 2 ] 3+ cations via Ln−S bonds as tridentate μ-1κ,2κ 2 -AsS 4 bridging ligands, resulting in the neutral coordination polymers [Ln(dien) 2 (μ-1κ,2κ 2 -AsS 4 )] n (Ln1). In 4−6, the AsS 4 units coordinate with the Ln 3+ ion of [Ln(dien) 2 ] 3+ as 1κ 2 -AsS 4 chelating ligands to form neutral coordination compounds [Ln(dien) 2 (1κ 2 -AsS 4 )] (Ln2). The Ln 3+ ions are in nine- and eight-coordinated environments in Ln1 and Ln2, respectively. The formation of Ln1 and Ln2 is related with ionic size of the Ln 3+ ions. Optical absorption spectra showed that 1−6 have potential use as semiconductors with the band gaps in the range 2.18−3.21 eV. - Graphical abstract: Two types of Ln-thioarsenates [Ln(dien) 2 (μ-1κ,2κ 2 -AsS 4 )] n and [Ln(dien) 2 (1κ 2 -AsS 4 )] were prepared by solvothermal methods and the soft Lewis basic AsS 4 3– ligand to Ln(III) centers with polyamine co-ligand was obtained. Display Omitted - Highlights: • Lanthanide thioarsenates were prepared by solvothermal methods. • The soft Lewis basic AsS 4 ligand coordinate Ln 3+ ions with coexistence polyamine ligands. • Two structural types of Ln-thioarsenates with structural turnover at Tb were obtained along Ln series. • The Ln-thioarsenates are potential semiconductors with optical band gaps in the range 2.18−3.21 eV

  13. Integrated biofuels process synthesis

    DEFF Research Database (Denmark)

    Torres-Ortega, Carlo Edgar; Rong, Ben-Guang

    2017-01-01

    Second and third generation bioethanol and biodiesel are more environmentally friendly fuels than gasoline and petrodiesel, andmore sustainable than first generation biofuels. However, their production processes are more complex and more expensive. In this chapter, we describe a two-stage synthesis......% used for bioethanol process), and steam and electricity from combustion (54%used as electricity) in the bioethanol and biodiesel processes. In the second stage, we saved about 5% in equipment costs and 12% in utility costs for bioethanol separation. This dual synthesis methodology, consisting of a top......-level screening task followed by a down-level intensification task, proved to be an efficient methodology for integrated biofuel process synthesis. The case study illustrates and provides important insights into the optimal synthesis and intensification of biofuel production processes with the proposed synthesis...

  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. Synthesis and characterization of titanium oxide/bismuth sulfide nanorods for solar cells applications

    International Nuclear Information System (INIS)

    Solis, M.; Rincon, M. E.

    2008-01-01

    In the present work is showed the synthesis and characterization of titanium oxide/bismuth sulfide nanowires hetero-junctions for solar cells applications. Conductive glass substrates (Corning 25 x 75 mm) were coated with a thin layer of sol-gel TiO2 and used as substrates for the subsequent deposition of bismuth sulfide nanorods (BN). TiO2 films (∼400 nm) were deposited with a semiautomatic immersion system with controlled immersion/withdraw velocity, using titanium isopropoxide as the titania precursor [1]. For BN synthesis and deposition, the solvo-thermal method was used, introducing air annealed TiO2-substrates in the autoclave. The typical bilayer TiO2/BN hetero-junction was 600 nm thick. The synthesized materials (powders and films) were characterized by X-Ray Diffraction, Scanning Electron Microscopy, and UV-Visible Spectroscopy. Anatase was the crystalline phase of TiO2, while bismuth sulfide nanotubes show a diffraction pattern characteristic of bismuthinite distorted by the preferential growth of some planes [2-4]. The optoelectronic characterization of TiO2/NB hetero-junctions was compared with hetero-junctions obtained by sensitizing TiO2 with chemically deposited bismuth sulfide films. Bismuth sulfide nanowires are 2µm long and 70nm wide (aspect ratio L/D = 43), while chemically deposited bismuth sulfide have L/D = 1, therefore the effect of particle size evaluation and geometry in the photosensitization phenomena will be discussed in the context of new materials for solar-cells applications. (Full text)

  16. Gas Phase Nanoparticle Synthesis

    Science.gov (United States)

    Granqvist, Claes; Kish, Laszlo; Marlow, William

    This book deals with gas-phase nanoparticle synthesis and is intended for researchers and research students in nanomaterials science and engineering, condensed matter physics and chemistry, and aerosol science. Gas-phase nanoparticle synthesis is instrumental to nanotechnology - a field in current focus that raises hopes for environmentally benign, resource-lean manufacturing. Nanoparticles can be produced by many physical, chemical, and even biological routes. Gas-phase synthesis is particularly interesting since one can achieve accurate manufacturing control and hence industrial viability.

  17. Radiation chemical synthesis

    International Nuclear Information System (INIS)

    Zagoretz, P.A.; Poluetkov, V.A.; Shostenko, A.G.

    1986-01-01

    The authors consider processes in radiation chemical synthesis which are being developed in various scientific-research organizations. The important advantages of radiation chlorination, viz. the lower temperature compared with the thermal method and the absence of dehydrochlorination products are discussed. The authors examine the liquid-phase chlorination of trifluorochloroethyltrichloromethyl ether to obtain the pentachloro-contining ether, trifluorodichloroethyltrichloromethyl ether. The authors discuss radiation synthesis processes that have be used formulated kinetic equations on which models have been based. It is concluded that the possibilities of preparative (micro- and low-tonnage) radiation synthesis are promising

  18. In Situ Tracking Kinetic Pathways of Li+/Na+ Substitution during Ion-Exchange Synthesis of LixNa1.5-xVOPO4F0.5.

    Science.gov (United States)

    Park, Young-Uk; Bai, Jianming; Wang, Liping; Yoon, Gabin; Zhang, Wei; Kim, Hyungsub; Lee, Seongsu; Kim, Sung-Wook; Looney, J Patrick; Kang, Kisuk; Wang, Feng

    2017-09-13

    Ion exchange is a ubiquitous phenomenon central to wide industrial applications, ranging from traditional (bio)chemical separation to the emerging chimie douce synthesis of materials with metastable structure for batteries and other energy applications. The exchange process is complex, involving substitution and transport of different ions under non-equilibrium conditions, and thus difficult to probe, leaving a gap in mechanistic understanding of kinetic exchange pathways toward final products. Herein, we report in situ tracking kinetic pathways of Li + /Na + substitution during solvothermal ion-exchange synthesis of Li x Na 1.5-x VOPO 4 F 0.5 (0 ≤ x ≤ 1.5), a promising multi-Li polyanionic cathode for batteries. The real-time observation, corroborated by first-principles calculations, reveals a selective replacement of Na + by Li + , leading to peculiar Na + /Li + /vacancy orderings in the intermediates. Contradicting the traditional belief of facile topotactic substitution via solid solution reaction, an abrupt two-phase transformation occurs and predominantly governs the kinetics of ion exchange and transport in the 1D polyanionic framework, consequently leading to significant difference of Li stoichiometry and electrochemical properties in the exchanged products. The findings may help to pave the way for rational design of ion exchange synthesis for making new materials.

  19. 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.

  20. 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

  1. Principles of asymmetric synthesis

    CERN Document Server

    Gawley, Robert E; Aube, Jeffrey

    2012-01-01

    The world is chiral. Most of the molecules in it are chiral, and asymmetric synthesis is an important means by which enantiopure chiral molecules may be obtained for study and sale. Using examples from the literature of asymmetric synthesis, this book presents a detailed analysis of the factors that govern stereoselectivity in organic reactions. After an explanation of the basic physical-organic principles governing stereoselective reactions, the authors provide a detailed, annotated glossary of stereochemical terms. A chapter on "Practical Aspects of Asymmetric Synthesis" provides a critical overview of the most common methods for the preparation of enantiomerically pure compounds, techniques for analysis of stereoisomers using chromatographic, spectroscopic, and chiroptical methods. The authors then present an overview of the most important methods in contemporary asymmetric synthesis organized by reaction type. Thus, there are four chapters on carbon-carbon bond forming reactions, one chapter on reductions...

  2. Synthesis of protargol

    International Nuclear Information System (INIS)

    Baratova, Z.R.; Sattarova, M.A.; Abdurakhmanov, A.Kh.; Solojenkin, P.M.

    1997-01-01

    This paper is devoted to synthesis of protargol containing 7,5-8,3% of silver. The flowsheet of obtaining of protargol was elaborated. The obtained protargol contains 7,5% of silver, insoluble in alcohol, ether and chloroform.

  3. Synthesis Polarimetry Calibration

    Science.gov (United States)

    Moellenbrock, George

    2017-10-01

    Synthesis instrumental polarization calibration fundamentals for both linear (ALMA) and circular (EVLA) feed bases are reviewed, with special attention to the calibration heuristics supported in CASA. Practical problems affecting modern instruments are also discussed.

  4. SYNTHESIS, CHARACTERIZATION AND PHOTOCATALYTIC ...

    African Journals Online (AJOL)

    ISSN 1011-3924. © 2018 Chemical Society of Ethiopia and The Authors. Printed in Ethiopia ... SYNTHESIS, CHARACTERIZATION AND PHOTOCATALYTIC ACTIVITY OF .... cm−1 to determine the surface functional groups. 10 mg of sample ...

  5. 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

  6. 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

  7. Two-directional synthesis as a tool for diversity-oriented synthesis: Synthesis of alkaloid scaffolds

    Directory of Open Access Journals (Sweden)

    Kieron M. G. O’Connell

    2012-06-01

    Full Text Available Two-directional synthesis represents an ideal strategy for the rapid elaboration of simple starting materials and their subsequent transformation into complex molecular architectures. As such, it is becoming recognised as an enabling technology for diversity-oriented synthesis. Herein, we provide a thorough account of our work combining two-directional synthesis with diversity-oriented synthesis, with particular reference to the synthesis of polycyclic alkaloid scaffolds.

  8. 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.

  9. Nitrocyclopropanes: synthesis and properties

    Energy Technology Data Exchange (ETDEWEB)

    Averina, Elena B; Yashin, N V; Kuznetsova, Tamara S; Zefirov, Nikolai S [Department of Chemistry, M.V. Lomonosov Moscow State University, Moscow (Russian Federation)

    2009-10-31

    State-of-the-art data on the methods of synthesis, properties and transformations of nitro- and- dinitrocyclopropanes of different structure is generalized and described systematically. The attention is focused on stereoselective cyclopropanation methods, new approaches to the synthesis of natural products and their synthetic analogues with diversified biological activities, in particular, of aminocyclopropane acids based on nitrocyclopropanes, and the formation of structures of energetic compounds.

  10. Controllable synthesis and electrochemical hydrogen storage properties of Sb₂Se₃ ultralong nanobelts with urchin-like structures.

    Science.gov (United States)

    Jin, Rencheng; Chen, Gang; Pei, Jian; Sun, Jingxue; Wang, Yang

    2011-09-01

    The controlled synthesis of one-dimensional and three-dimensional Sb(2)Se(3) nanostructures has been achieved by a facile solvothermal process in the presence of citric acid. By simply controlling the concentration of citric acid, the nucleation, growth direction and exposed facet can be readily tuned, which brings the different morphologies and nanostructures to the final products. The as-prepared products have been characterized by means of X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscopy (TEM), high-resolution TEM and selected area electron diffraction. Based on the electron microscope observations, a possible growth mechanism of Sb(2)Se(3) with distinctive morphologies including ultralong nanobelts, hierarchical urchin-like nanostructures is proposed and discussed in detail. The electrochemical hydrogen storage measurements reveal that the morphology plays a key role on the hydrogen storage capacity of Sb(2)Se(3) nanostructures. The Sb(2)Se(3) ultralong nanobelts with high percentage of {-111} facets exhibit higher hydrogen storage capacity (228.5 mA h g(-1)) and better cycle stability at room temperature.

  11. 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.

  12. Microwave-assisted synthesis of CuInSe{sub 2} nanoparticles in low-absorbing solvents

    Energy Technology Data Exchange (ETDEWEB)

    Oleksak, Richard P.; Flynn, Brendan T.; Herman, Gregory S. [School of Chemical, Biological and Environmental Engineering, Oregon State University, Corvallis, OR (United States); Schut, David M. [Voxtel Inc., Eugene, OR (United States)

    2014-01-15

    Copper indium diselenide (CIS) nanoparticles were synthesized using a microwave-assisted one-pot solvothermal approach. For these studies high microwave-absorbing precursors were used in combination with low microwave absorbing solvents tri-n-octylphosphine (TOP) and oleic acid (OA) to investigate the effect of selective heating of the precursors on nanoparticle synthesis. High-resolution transmission electron microscopy (TEM) results indicated that the nanoparticles were spherical, crystalline and 4-5 nm in diameter. X-ray diffraction (XRD) results indicated that the nanoparticles had a body-centered tetragonal structure with planar defects that decreased in concentration with increasing reaction temperature and reaction time. The nanoparticle compositions varied depending on the reaction conditions and the compositions were found to approach stoichiometry for increased reaction times. Fourier transform infrared (FTIR) spectroscopy indicated both solvents adsorbed to the nanoparticle surface and energy dispersive spectroscopy indicated that these ligands became chlorinated during the reaction. The uniform temperature profile offered by the microwave heating allowed for highly reproducible batch-to-batch reactions, allowing for tight control over composition and defect concentration. (copyright 2014 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  13. Designed synthesis of tunable amorphous carbon nanotubes (a ...

    Indian Academy of Sciences (India)

    Administrator

    The as-prepared a-CNTs were a kind of hydrogenated a-CNTs containing both ... aluminium oxide (AAO) template, solvothermal method, etc., have been developed to ... above products were treated by dilute HCl solution to remove VOx in the ...

  14. Room temperature synthesis of hydrophilic Ln(3+)-doped KGdF4 (Ln = Ce, Eu, Tb, Dy) nanoparticles with controllable size: energy transfer, size-dependent and color-tunable luminescence properties.

    Science.gov (United States)

    Yang, Dongmei; Li, Guogang; Kang, Xiaojiao; Cheng, Ziyong; Ma, Ping'an; Peng, Chong; Lian, Hongzhou; Li, Chunxia; Lin, Jun

    2012-06-07

    In this paper, we demonstrate a simple, template-free, reproducible and one-step synthesis of hydrophilic KGdF(4): Ln(3+) (Ln = Ce, Eu, Tb and Dy) nanoparticles (NPs) via a solution-based route at room temperature. X-Ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), photoluminescence (PL) and cathodoluminescence (CL) spectra are used to characterize the samples. The results indicate that the use of water-diethyleneglycol (DEG) solvent mixture as the reaction medium not only allows facile particle size control but also endows the as-prepared samples with good water-solubility. In particular, the mean size of NPs is monotonously reduced with the increase of DEG content, from 215 to 40 nm. The luminescence intensity and absolute quantum yields for KGdF(4): Ce(3+), Tb(3+) NPs increase remarkably with particle sizes ranging from 40 to 215 nm. Additionally, we systematically investigate the magnetic and luminescence properties of KGdF(4): Ln(3+) (Ln = Ce, Eu, Tb and Dy) NPs. They display paramagnetic and superparamagnetic properties with mass magnetic susceptibility values of 1.03 × 10(-4) emu g(-1)·Oe and 3.09 × 10(-3) emu g(-1)·Oe at 300 K and 2 K, respectively, and multicolor emissions due to the energy transfer (ET) process Ce(3+)→ Gd(3+)→ (Gd(3+))(n)→ Ln(3+), in which Gd(3+) ions play an intermediate role in this process. Representatively, it is shown that the energy transfer from Ce(3+) to Tb(3+) occurs mainly via the dipole-quadrupole interaction by comparison of the theoretical calculation and experimental results. This kind of magnetic/luminescent dual-function materials may have promising applications in multiple biolabels and MR imaging.

  15. 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...

  16. Solvothermal syntheses, crystal structures, optical and thermal ...

    Indian Academy of Sciences (India)

    compounds 1–3 exhibit optical band gaps between 2.06 and 2.35 eV. Keywords. .... under a nitrogen stream of 100 mL min. −1 . 2.3 X-ray diffraction. Single-crystal ..... Liu G N, Guo G C, Wang M S, Cai L Z and Huang J S. 2010 Five dimeric ...

  17. Detonation-synthesis nanodiamonds: synthesis, structure, properties and applications

    Energy Technology Data Exchange (ETDEWEB)

    Dolmatov, Valerii Yu [Federal State Unitary Enterprise Special Design-Technology Bureau (FSUE SDTB) ' ' Tekhnolog' ' at the St Petersburg State Institute of Technology (Technical University) (Russian Federation)

    2007-04-30

    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.

  18. 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.

  19. Noncovalent synthesis of protein dendrimers

    NARCIS (Netherlands)

    Lempens, E.H.M.; Baal, van I.; Dongen, van J.L.J.; Hackeng, T.M.; Merkx, M.; Meijer, E.W.

    2009-01-01

    The covalent synthesis of complex biomolecular systems such as multivalent protein dendrimers often proceeds with low efficiency, thereby making alternative strategies based on noncovalent chemistry of high interest. Here, the synthesis of protein dendrimers using a strong but noncovalent

  20. 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...

  1. Click synthesis of PET radiopharmaceuticals

    International Nuclear Information System (INIS)

    Xu Mei; Kuang Chunxiang

    2009-01-01

    Increasing attention has been focused on synthesis radiopharmaceuticals for positron emission tomography (PET). The recent years witnessed applications of click chemistry to PET radiopharmaceutical synthesis,because of its distinctive advantages including high speed,yield and stereospecificity under mild conditions. Synthesis of 18 F-labeled and 11 C-labeled radiopharmaceuticals and intermediates via click chemistry are reviewed. The future trend of click chemistry for the synthesis of PET radiopharmaceutical is prospected. (authors)

  2. 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.

  3. 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.

  4. Toleration, Synthesis or Replacement?

    DEFF Research Database (Denmark)

    Holtermann, Jakob v. H.; Madsen, Mikael Rask

    2016-01-01

    , in order to answer is not yet another partisan suggestion, but rather an attempt at making intelligible both the oppositions and the possibilities of synthesis between normative and empirical approaches to law. Based on our assessment and rational reconstruction of current arguments and positions, we...... therefore outline a taxonomy consisting of the following three basic, ideal-types in terms of the epistemological understanding of the interface of law and empirical studies: toleration, synthesis and replacement. This tripartite model proves useful with a view to teasing out and better articulating...

  5. Synthesis and photocatalytic activity of mesoporous – (001) facets TiO_2 single crystals

    International Nuclear Information System (INIS)

    Dong, Yeshuo; Fei, Xuening; Zhou, Yongzhu

    2017-01-01

    Highlights: • The (001) facets of TiO_2 single crystals with mesoporous structure. • The (010) and (100) facets of TiO_2 single crystals were covered by the flower – shaped TiO_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_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_2 single crystals, we synthesized these mesoporous – (001) facets TiO_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_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_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_2 single crystals.

  6. Synthesis imaging in radio astronomy

    International Nuclear Information System (INIS)

    Perley, R.A.; Schwab, F.R.; Bridle, A.H.

    1989-01-01

    Recent advances in techniques and instrumentation for radio synthesis imaging in astronomy are discussed in a collection of review essays. Topics addressed include coherence in radio astronomy, the interferometer in practice, primary antenna elements, cross correlators, calibration and editing, sensitivity, deconvolution, self-calibration, error recognition, and image analysis. Consideration is given to wide-field imaging (bandwidth and time-average smearing, noncoplanar arrays, and mosaicking), high-dynamic-range imaging, spectral-line imaging, VLBI, solar imaging with a synthesis telescope, synthesis imaging of spatially coherent objects, noise in images of very bright sources, synthesis observing strategies, and the design of aperture-synthesis arrays

  7. Solvothermal syntheses, crystal structures, and properties of lanthanide(III) thioarsenates [Ln(dien){sub 2}(μ-1κ,2κ{sup 2}-AsS{sub 4})]{sub n} (Ln==Sm, Eu, Gd) and [Ln(dien){sub 2}(1κ{sup 2}-AsS{sub 4})] (Ln==Tb, Dy, Ho)

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Fang; Tang, Chunying; Chen, Ruihong; Zhang, Yong; Jia, Dingxian, E-mail: jiadingxian@suda.edu.cn

    2013-10-15

    Solvothermal reactions of Ln{sub 2}O{sub 3}, As and S in diethylenetriamine (dien) at 170 °C for 6 days afforded two structural types of lanthanide thioarsenates with the general formulae [Ln(dien){sub 2}(μ-1κ,2κ{sup 2}-AsS{sub 4})]{sub n} [Ln=Sm(1), Eu(2), Gd(3)] and [Ln(dien){sub 2}(1κ{sup 2}-AsS{sub 4})] [Ln=Tb(4), Dy(5), Ho(6)]. The Ln{sub 2}O{sub 3} oxides were converted to [Ln(dien){sub 2}]{sup 3+} complex units in the solvothermal reactions. The As atom binds four S atoms, forming a tetrahedral AsS{sub 4} unit. In 1−3, the AsS{sub 4} units interconnect the [Ln(dien){sub 2}]{sup 3+} cations via Ln−S bonds as tridentate μ-1κ,2κ{sup 2}-AsS{sub 4} bridging ligands, resulting in the neutral coordination polymers [Ln(dien){sub 2}(μ-1κ,2κ{sup 2}-AsS{sub 4})]{sub n} (Ln1). In 4−6, the AsS{sub 4} units coordinate with the Ln{sup 3+} ion of [Ln(dien){sub 2}]{sup 3+} as 1κ{sup 2}-AsS{sub 4} chelating ligands to form neutral coordination compounds [Ln(dien){sub 2}(1κ{sup 2}-AsS{sub 4})] (Ln2). The Ln{sup 3+} ions are in nine- and eight-coordinated environments in Ln1 and Ln2, respectively. The formation of Ln1 and Ln2 is related with ionic size of the Ln{sup 3+} ions. Optical absorption spectra showed that 1−6 have potential use as semiconductors with the band gaps in the range 2.18−3.21 eV. - Graphical abstract: Two types of Ln-thioarsenates [Ln(dien){sub 2}(μ-1κ,2κ{sup 2}-AsS{sub 4})]{sub n} and [Ln(dien){sub 2}(1κ{sup 2}-AsS{sub 4})] were prepared by solvothermal methods and the soft Lewis basic AsS{sub 4}{sup 3–} ligand to Ln(III) centers with polyamine co-ligand was obtained. Display Omitted - Highlights: • Lanthanide thioarsenates were prepared by solvothermal methods. • The soft Lewis basic AsS{sub 4} ligand coordinate Ln{sup 3+} ions with coexistence polyamine ligands. • Two structural types of Ln-thioarsenates with structural turnover at Tb were obtained along Ln series. • The Ln-thioarsenates are potential semiconductors

  8. Stellar population synthesis

    International Nuclear Information System (INIS)

    Pickles, A.J.

    1989-01-01

    The techniques used to derive astrophysically useful information from observations of the integrated light of composite stellar systems are briefly reviewed. A synthesis technique, designed to separate and describe on a standard system the competing effects of age and metallicity variations is introduced, and illustrated by its application to the study of the history of star formation in bright elliptical galaxies in clusters. (author)

  9. 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

  10. 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

  11. 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

  12. 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)

  13. 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)

  14. 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...

  15. [Synthesis of new nitrosoureas].

    Science.gov (United States)

    Papadaki-Valiraki, A; Siatra-Papastaikoudi, T; Skaltsounis, A L; Roussakis, C

    1989-01-01

    Two chemical pathways were used for the synthesis of three new N'-(2-chloroethyl)-N-[2-(4-alkoxyphenylthio)ethyl]-N'-nitrosoureas and two new N'-(2-chloroethyl)-N)[2-(4-alkoxyphenyl-thio)ethyl]-N-nitrosoureas . The study of the cytotoxicity of the three N'-nitrosoureas, was carried out in two experimental models (P 388 and NSCLCN6).

  16. MICROWAVES IN ORGANIC SYNTHESIS

    Science.gov (United States)

    The effect of microwaves, a non-ionizing radiation, on organic reactions is described both in polar solvents and under solvent-free conditions. The special applications are highlighted in the context of solventless organic synthesis which involve microwave (MW) exposure of neat r...

  17. SYNTHESIS, CHARACTERIZATION AND ANTIBACTERIAL ...

    African Journals Online (AJOL)

    Preferred Customer

    In the present study, synthesis, and biological evaluation of some novel ... Then slowly cooled and resultant mixture was basified with aqueous sodium hydroxide ... mol), anhydrous potassium carbonate (5.52 g, 0.04 mol) in acetone (25 mL), ...

  18. Synthesis, characterization and properties

    Indian Academy of Sciences (India)

    Unknown

    work, we report herein the synthesis, structural cha- racterization and properties of a chiral Mn(IV) mononuclear ... atmosphere with a platinum disc working electrode, a platinum wire auxiliary electrode and a Ag/AgCl ... SMART APEX CCD area detector system [λ(Mo-. Kα) = 0⋅71073 Å], graphite monochromator, 2400.

  19. 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 sy