Synthesis, characterization and structural refinement of polycrystalline uranium substituted zirconolite

International Nuclear Information System (INIS)

Shrivastava, O.P.; Narendra Kumar; Sharma, I.B.

2005-01-01

Ceramic precursors of Zirconolite (CaZrTi 2 O 7 ) family have a remarkable property of substitution Zr 4+ cationic sites. This makes them potential material for nuclear waste management in 'synroc' technology. In order to simulate the mechanism of partial substitution of zirconium by tetravalent actinides, a solid phase of composition CaZr 0.95 U 0.5 Ti 2 O 7 has been synthesized through ceramic route by taking calculated quantities of oxides of Ca, Ti and nitrates of uranium and zirconium respectively. Solid state synthesis has been carried out by repeated pelletizing and sintering the finely powdered oxide mixture in a muffle furnace at 1050 degC. The polycrystalline solid phase has been characterized by its typical powder diffraction pattern. Step analysis data has been used for ab initio calculation of structural parameters. The uranium substituted zirconolite crystallizes in monoclinic symmetry with space group C2/c (15). The following unit cell parameters have been calculated: a =12.4883(15), b =7.2448(5), c 11.3973(10) and β = 100.615(9)0. The structure was refined to satisfactory completion. The Rp and Rwp are found to be 7.48% and 9.74% respectively. (author)

Photocatalytic semiconductors synthesis, characterization, and environmental applications

CERN Document Server

Hernández-Ramírez, Aracely

2014-01-01

This critical volume examines the different methods used for the synthesis of a great number of photocatalysts, including TiO2, ZnO and other modified semiconductors, as well as characterization techniques used for determining the optical, structural and morphological properties of the semiconducting materials. Additionally, the authors discuss photoelectrochemical methods for determining the light activity of the photocatalytic semiconductors by means of measurement of properties such as band gap energy, flat band potential and kinetics of hole and electron transfer. Photocatalytic Semiconductors: Synthesis, Characterization and Environmental Applications provide an overview of the semiconductor materials from first- to third-generation photocatalysts and their applications in wastewater treatment and water disinfection. The book further presents economic and toxicological aspects in the production and application of photocatalytic materials.

Synthesis and characterization of rare-earth-doped calcium tungstate nanocrystals

Science.gov (United States)

Suneeta, P.; Rajesh, Ch.; Ramana, M. V.

2018-02-01

In this paper, we report synthesis and characterization of rare-earth-ion-doped calcium tungstate (CaWO4) nanocrystals (NCs). Rare-earth ions, such as gadolinium (Gd), neodymium (Nd), praseodymium (Pr), samarium (Sm) and holmium (Ho), were successfully doped in the CaWO4 NCs by changing the synthesis conditions. The adopted synthesis route was found to be fast and eco-friendly. Structural characterizations, such as X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and compositional analysis, were performed using energy dispersive analysis of X-rays (EDAX) on as-synthesized NCs. The results indicate the size of the NCs ranging between 47 to 68nm and incorporation of rare-earth ions in CaWO4 NCs.

Synthesis, characterization, thermal

Directory of Open Access Journals (Sweden)

Selma Bal

2017-09-01

Full Text Available This work explains the synthesis of a new azo-Schiff base compound, derived from condensation between N-ethylcarbazole-3-carbaldehyde and 1,3-diaminopropane, followed by azo coupling reaction with the diazonium salt of 2-amino-4-methyl phenol. The newly synthesized azo-Schiff base was further reacted with the acetate salts of Copper, Cobalt and Nickel to give three coordination compounds. All synthesized compounds have been characterized through spectral analysis. The coordination compounds have been examined for their thermal and catalytic features. Good and moderate yields were obtained for the oxidation of styrene and cyclohexene. Thermal features of the ligand and its complexes have been explained and the results obtained have supported the proposed structures.

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.

SYNTHESIS AND CHARACTERIZATION OF NEW HALOGENATED CURCUMINOIDS

Directory of Open Access Journals (Sweden)

Eugenio Torres

2013-12-01

Full Text Available In this work a novel procedure of synthesis of compounds analogues to curcumin with halogens atoms in its structure is described, which can increase its solubility and biological activity. Four halogenated curcuminoids were obtained with great pharmacological interest, none of them reported in literature before. Synthesis was carried out by means of the aldol condensation assisted by microwaves of halogenated aromatic aldehydes and acetylacetona, using morpholine as basic catalyst, in absence of solvent, and the reaction just needed 1 min. The products were purified by treatment of the reaction mixture with methanol under ultrasound irradiation, followed by chromatographic column. All obtained compounds were characterized by infrared spectroscopy, nuclear magnetic resonance, quantitative elementary analysis and high resolution mass spectrometry. The RMN-1H data demonstrate in all structures of synthesized curcuminoids the enol form is the most favored.

Novel biosynthesis of Ag-hydroxyapatite: Structural and spectroscopic characterization

Directory of Open Access Journals (Sweden)

Álvaro de Jesús Ruíz-Baltazar

2018-06-01

Full Text Available Silver-doped hydroxyapatite (Ag-HAP was obtained by green synthesis route. The dopant silver nanoparticles (AgNPs were obtained by biosynthesis based on Melissa officinalis extract. This research is focused on the characterization and the use of the nontoxic and environment-friendly Ag-HAP nanocomposite. The structural and morphological characterization of Ag-HAP nanocomposite was carried out by scanning electron microscopy (SEM, X-ray diffraction, Fourier-transform infrared (FT-IR and Raman spectroscopy. The obtained nanoparticles exhibited a great interaction with the HAP matrix, performing an Ag-HAP nanocomposite. Changes in the structure of the Ag-HAP nanocomposite were corroborated by the different characterization techniques. Additionally, a homogeneous distribution of the AgNPs on the HAP structure was observed. The heterogeneous nucleation process employed to doping the HAP, offer a functional route to obtain a green composite with potentials applications in multiple fields, such as tissue engineering, bone repair as well as protein. These properties can be evaluated in subsequent studies. Keywords: Green synthesis, Ag nanoparticles, Hydroxyapatite, Structural characterization, Spectroscopy

Synthesis, characterization and magnetic properties of selected Laves and MAX phases

International Nuclear Information System (INIS)

Hamm, Christin Maria

2017-01-01

In this work the rare-earth free Laves phases Ti 2 M 3 Si with M = Mn, Fe, Co, Ni were synthesized by microwave heating and were structurally and magnetically characterized. Furthermore, the solid solution Ti 2 (Co 1-x Fe x ) 3 Si was synthesized by arc melting and spark plasma sintering, as well as their magnetic behavior was studied. In addition to the Laves phases, the focus was on the synthesis and characterization of aluminum-based MAX phases. For the first time the ternary carbides were prepared by microwave heating. The phase-pure representation of MAX phases was particularly challenging for synthetic solid-state chemistry. The susceptor-assisted microwave heating allows the synthesis of high-quality samples, which was shown in this work on M 2 AlC (M = Ti, V, Cr) and V 4 AlC 3 . Furthermore, for the first time, the doping of these materials with Mn and Fe was successful. In addition to the structural characterization of the new phases, the microstructure and magnetic properties are discussed in this work. Using these doped compounds as well as the compound V 4 AlC 3 , it has been shown that field-activated synthesis, particularly susceptor-assisted microwave heating, are a very good synthesis method for compounds which are hard or sometimes not synthesized by conventional methods.

Synthesis by irradiation and mechanism and structural characterization study of high melt strength polypropylene

International Nuclear Information System (INIS)

Lugao, Ademar Benevolo

2004-01-01

Polypropylene molecular structure is made only by linear molecules interacting by weak forces. The resulting PP has very low melt strength (MS). MS is important to make feasible to process PP by all the transformation technologies based on the free expansion of the melt. The aim of this work was to develop a new process to synthesize PP with crosslinks and/or long chain branches, known as High Melt Strength Polypropylene (HMSPP) and to characterize its structure and synthesis mechanism. HMSPP was obtained by the irradiation of PP under a crosslinking (acetylene) atmosphere or inert or oxidative one, followed by thermal treatment for radical recombination and thermal treatment for annihilation of the remaining radicals under reactive or inert atmosphere. The results from rheological characterization showed that the highest levels of MS were obtained by conducting irradiation and thermal treatments under crosslinking atmospheres. The results for the elucidation of reaction mechanism by electron spin resonance (ESR) showed that acetylene irradiation is effective in promoting the creation of double bonds, based on the formation of polyenil radicals. The results of structural unraveling showed that radiation promotes predominantly the degradation of atactic molecules or molecules with atactic defects. These results support the hypothesis of formation of branched PP molecules based on the reaction of those fragments with the double bonds created in the PP molecules. (author)

Synthesis, structural characterization and in vitro testing of dysprosium containing silica particles as potential MRI contrast enhancing agents

International Nuclear Information System (INIS)

Chiriac, L.B.; Trandafir, D.L.; Turcu, R.V.F.; Todea, M.; Simon, S.

2016-01-01

Highlights: • Dysprosium containing silica microparticles obtained by freeze and spray drying. • Higher structural units interconnection achieved in freeze vs. spray dried samples. • Dy occurance on the outermost layer of the microparticles evidenced by XPS. • Enhanced MRI contrast observed for freeze dried samples with 5% mol Dy_2O_3. - Abstract: The work is focused on synthesis and structural characterization of novel dysprosium-doped silica particles which could be considered as MRI contrast agents. Sol-gel derived silica rich particles obtained via freeze-drying and spray-drying processing methods were structurally characterized by XRD, "2"9Si MAS-NMR and XPS methods. The occurrence of dysprosium on the outermost layer of dysprosium containing silica particles was investigated by XPS analysis. The MRI contrast agent characteristics have been tested using RARE-T_1 and RARE-T_2 protocols. The contrast of MRI images delivered by the investigated samples was correlated with their local structure. Dysprosium disposal on microparticles with surface structure characterised by decreased connectivity of the silicate network units favours dark T_2-weighted MRI contrast properties.

Synthesis and Characterization of Magnesium Substituted Aluminophosphate Molecular Sieves with AEL Structure

Institute of Scientific and Technical Information of China (English)

Benjing Xu; Ling Qian; Xinmei Liu; Chunmin Song; Zifeng Yan

2004-01-01

MAPO-11 molecular sieves were synthesized by hydrothermal methods. The influence of precursor of magnesium, Mg/Al ratio, synthesis temperature, synthesis time and the type of template on the formation and properties of MAPO-11 molecular sieves was examined. The samples were characterized by the techniques of X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric/differential thermogravimetric analysis (TG-DGA), etc. The results show that the shape and size of crystal were influenced by the precursor of Mg, the Mg/Al ratio and the type of template, and the TG-DGA analysis shows that MAPO-11 molecular sieves as-synthesized have poor thermal stability.

The Synthesis, Characterization and Catalytic Reaction Studies of Monodisperse Platinum Nanoparticles in Mesoporous Oxide Materials

Energy Technology Data Exchange (ETDEWEB)

Rioux, Robert M. [Univ. of California, Berkeley, CA (United States)

2006-01-01

A catalyst design program was implemented in which Pt nanoparticles, either of monodisperse size and/or shape were synthesized, characterized and studied in a number of hydrocarbon conversion reactions. The novel preparation of these materials enables exquisite control over their physical and chemical properties that could be controlled (and therefore rationally tuned) during synthesis. The ability to synthesize rather than prepare catalysts followed by thorough characterization enable accurate structure-function relationships to be elucidated. This thesis emphasizes all three aspects of catalyst design: synthesis, characterization and reactivity studies. The precise control of metal nanoparticle size, surface structure and composition may enable the development of highly active and selective heterogeneous catalysts.

Synthesis and structural characterization of coaxial nano tubes intercalated of molybdenum disulfide with carbon

International Nuclear Information System (INIS)

Reza San German, C.M.

2005-01-01

In this work the study of some fundamental aspects in the growth of unidimensional systems of coaxial nano tubes from the mold method is approached. This method is an inclusion technique of a precursor reagent into oxide nano porous alumina film (mold), and later applying some processes of synthesis it is gotten to obtain the wished material. The synthesized structures are identified later because they take place by means of the initial formation of nano tubes of MoS 2 , enclosing to carbon nano tubes by the same method, with propylene flow which generates a graphitization process that 'copy' the mold through as it flows. Binary phase MoS 2 + C nano tubes were synthesized by propylene pyrolysis inside MoS 2 nano tubes prepared by template assisted technique. The large coaxial nano tubes constituted of graphite sheets inserted between the MoS 2 layers forming the outer part, and coaxial multi wall carbon nano tubes (MWCNT) intercalated with MoS 2 inside. High resolution electron microscopy (HRTEM), electron energy loss spectroscopy (EELS), high angle annular dark field (HAADF), gatan image filter (GIF), nano beam electron diffraction patterns (NBEDP), along with molecular dynamics simulation and quantum mechanical calculations were used to characterize the samples. The one-dimensional structures exhibit diverse morphologies such as long straight and twisted nano tubes with several structural irregularities. The inter-planar spacing between MoS 2 layers was found to increase from 6.3 to 7.4 A due to intercalation with carbon. Simulated HREM images revealed the presence of these twisted nano structures, with mechanical stretch into intercalate carbon between MoS 2 layers. Our results open up the possibility of using MoS 2 nano tubes as templates for the synthesis of new one- dimensional binary phase systems. (Author)

Lanthanide phosphonates: Synthesis, thermal stability and magnetic characterization

Energy Technology Data Exchange (ETDEWEB)

Amghouz, Z., E-mail: amghouz.uo@uniovi.es [Departamentos de Quimica Fisica y Analitica y Quimica Organica e Inorganica, Universidad de Oviedo - CINN, 33006 Oviedo (Spain); Garcia, J.R.; Garcia-Granda, S. [Departamentos de Quimica Fisica y Analitica y Quimica Organica e Inorganica, Universidad de Oviedo - CINN, 33006 Oviedo (Spain); Clearfield, A. [Department of Chemistry, Texas A and M University, College Station, TX 77842-3012 (United States); Rodriguez Fernandez, J.; Pedro, I. de [CITIMAC, Facultad de Ciencias, Universidad de Cantabria, 39005 Santander (Spain); Blanco, J.A. [Departamento de Fisica, Universidad de Oviedo, 33007 Oviedo (Spain)

2012-09-25

Highlights: Black-Right-Pointing-Pointer Report of the complete series of lanthanide 1,4-phenylbis(phosphonate). Black-Right-Pointing-Pointer Synthesis under conventional hydrothermal synthesis or microwave-assisted hydrothermal synthesis. Black-Right-Pointing-Pointer Cation size is the key factor for the structural and particles size variations. Black-Right-Pointing-Pointer Thermal behaviour is characterized by unusual very high thermal stability. - Abstract: Series of novel organic-inorganic hybrids materials based on trivalent lanthanides (Ln = Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) and 1,4-phenylbis(phosphonate) obtained under hydrothermal conditions either by oven heat or microwave irradiation. The anhydrous compounds containing La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, and Ho, are isostructural. However, the compounds based on Y, Er, Tm, Yb, and Lu are hydrated and their structures have not yet been solved. The series of compounds are characterized by PXRD, TEM, SEM-EDX and thermal analyses (TG-MS and DSC). TEM study show a variable particles size with a minimum mean-particle size of ca. 30 nm. These compounds exhibit unusual very high thermal stability. The size of particles and the thermal stability are depending on lanthanide(III) cation features. All the investigated materials show paramagnetic behaviour. The magnetic susceptibility data follow a Curie-Weiss laws with paramagnetic effective moments in good agreement with those expected for Ln{sup 3+} free ions.

Synthesis, structural characterization and in vitro testing of dysprosium containing silica particles as potential MRI contrast enhancing agents

Energy Technology Data Exchange (ETDEWEB)

Chiriac, L.B.; Trandafir, D.L. [Faculty of Physics & National Magnetic Resonance Center, Babeş-Bolyai University, Cluj-Napoca, RO-400084 (Romania); Interdisciplinary Research Institute on Bio-Nano-Sciences & Faculty of Physics, Babeş-Bolyai University, Cluj-Napoca, RO-400084 (Romania); Turcu, R.V.F. [Faculty of Physics & National Magnetic Resonance Center, Babeş-Bolyai University, Cluj-Napoca, RO-400084 (Romania); Todea, M. [Interdisciplinary Research Institute on Bio-Nano-Sciences & Faculty of Physics, Babeş-Bolyai University, Cluj-Napoca, RO-400084 (Romania); Simon, S., E-mail: simons@phys.ubbcluj.ro [Faculty of Physics & National Magnetic Resonance Center, Babeş-Bolyai University, Cluj-Napoca, RO-400084 (Romania); Interdisciplinary Research Institute on Bio-Nano-Sciences & Faculty of Physics, Babeş-Bolyai University, Cluj-Napoca, RO-400084 (Romania)

2016-11-01

Highlights: • Dysprosium containing silica microparticles obtained by freeze and spray drying. • Higher structural units interconnection achieved in freeze vs. spray dried samples. • Dy occurance on the outermost layer of the microparticles evidenced by XPS. • Enhanced MRI contrast observed for freeze dried samples with 5% mol Dy{sub 2}O{sub 3}. - Abstract: The work is focused on synthesis and structural characterization of novel dysprosium-doped silica particles which could be considered as MRI contrast agents. Sol-gel derived silica rich particles obtained via freeze-drying and spray-drying processing methods were structurally characterized by XRD, {sup 29}Si MAS-NMR and XPS methods. The occurrence of dysprosium on the outermost layer of dysprosium containing silica particles was investigated by XPS analysis. The MRI contrast agent characteristics have been tested using RARE-T{sub 1} and RARE-T{sub 2} protocols. The contrast of MRI images delivered by the investigated samples was correlated with their local structure. Dysprosium disposal on microparticles with surface structure characterised by decreased connectivity of the silicate network units favours dark T{sub 2}-weighted MRI contrast properties.

Synthesis and characterization of new ionic liquids

International Nuclear Information System (INIS)

Oliveira, L.M.C. de; Mattedi, S.; Boaventura, J.S.; Iglesias, M.; Universidad de Santiago de Compostela

2010-01-01

In recent years, ionic liquids have been highlighted for its potential in various industrial applications. Among them, the salts of Broensted has a promising profile for the low toxicity, low cost and simple synthesis. This paper presents the synthesis and characterization of new salts of Bronsted with branched (lactate) or large chain anions (oleate) for future use as additives promoters of proton conductivity in fuel cells of ethanol. Experimental data were measured for density, sound velocity and conductivity of pure ionic liquids and mixtures. The density decreases linearly with increasing temperature, and sound velocity shows a similar trend, but not linear. The conductivity increases according to the Arrhenius model with activation energy less than 10 J/mol. Tests NMR, FTIR and TGA confirm ionic structure and thermal stability up to 165 deg C. (author)

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 ...

Synthesis and characterization of triangulene

Science.gov (United States)

Pavliček, Niko; Mistry, Anish; Majzik, Zsolt; Moll, Nikolaj; Meyer, Gerhard; Fox, David J.; Gross, Leo

2017-05-01

Triangulene, the smallest triplet-ground-state polybenzenoid (also known as Clar's hydrocarbon), has been an enigmatic molecule ever since its existence was first hypothesized. Despite containing an even number of carbons (22, in six fused benzene rings), it is not possible to draw Kekulé-style resonant structures for the whole molecule: any attempt results in two unpaired valence electrons. Synthesis and characterization of unsubstituted triangulene has not been achieved because of its extreme reactivity, although the addition of substituents has allowed the stabilization and synthesis of the triangulene core and verification of the triplet ground state via electron paramagnetic resonance measurements. Here we show the on-surface generation of unsubstituted triangulene that consists of six fused benzene rings. The tip of a combined scanning tunnelling and atomic force microscope (STM/AFM) was used to dehydrogenate precursor molecules. STM measurements in combination with density functional theory (DFT) calculations confirmed that triangulene keeps its free-molecule properties on the surface, whereas AFM measurements resolved its planar, threefold symmetric molecular structure. The unique topology of such non-Kekulé hydrocarbons results in open-shell π-conjugated graphene fragments that give rise to high-spin ground states, potentially useful in organic spintronic devices. Our generation method renders manifold experiments possible to investigate triangulene and related open-shell fragments at the single-molecule level.

Structural and Biochemical Characterization of Chlamydia trachomatis Hypothetical Protein CT263 Supports That Menaquinone Synthesis Occurs through the Futalosine Pathway*

Science.gov (United States)

Barta, Michael L.; Thomas, Keisha; Yuan, Hongling; Lovell, Scott; Battaile, Kevin P.; Schramm, Vern L.; Hefty, P. Scott

2014-01-01

The obligate intracellular human pathogen Chlamydia trachomatis is the etiological agent of blinding trachoma and sexually transmitted disease. Genomic sequencing of Chlamydia indicated this medically important bacterium was not exclusively dependent on the host cell for energy. In order for the electron transport chain to function, electron shuttling between membrane-embedded complexes requires lipid-soluble quinones (e.g. menaquionone or ubiquinone). The sources or biosynthetic pathways required to obtain these electron carriers within C. trachomatis are poorly understood. The 1.58Å crystal structure of C. trachomatis hypothetical protein CT263 presented here supports a role in quinone biosynthesis. Although CT263 lacks sequence-based functional annotation, the crystal structure of CT263 displays striking structural similarity to 5′-methylthioadenosine nucleosidase (MTAN) enzymes. Although CT263 lacks the active site-associated dimer interface found in prototypical MTANs, co-crystal structures with product (adenine) or substrate (5′-methylthioadenosine) indicate that the canonical active site residues are conserved. Enzymatic characterization of CT263 indicates that the futalosine pathway intermediate 6-amino-6-deoxyfutalosine (kcat/Km = 1.8 × 103 m−1 s−1), but not the prototypical MTAN substrates (e.g. S-adenosylhomocysteine and 5′-methylthioadenosine), is hydrolyzed. Bioinformatic analyses of the chlamydial proteome also support the futalosine pathway toward the synthesis of menaquinone in Chlamydiaceae. This report provides the first experimental support for quinone synthesis in Chlamydia. Menaquinone synthesis provides another target for agents to combat C. trachomatis infection. PMID:25253688

Electronic, electrical and magnetic ceramics synthesis and characterization

International Nuclear Information System (INIS)

Calix, V.S.; Saligan, P.P.; Naval, P.C.

1989-01-01

This paper describes the research and development activities of the Philippine Nuclear Research Institute (PNRI) on the synthesis and characterization of soft and hard ferrites and some beta alumina type superionic conductor materials. XRD, XRF and Moessbauer effect spectrometry are used to determine the structure phases, compositions and some magnetic properties of the materials. Effects of composition and preparation methods on the bulk electronic and magnetic properties are also discussed. (Auth.). 6 figs.; 3 tabs

Synthesis of Zinc Diethyldithiocarbamate (ZDEC) and Structure Characterization using Decoupling 1H NMR

International Nuclear Information System (INIS)

Sujarit, Jenjira; Phutdhawong, Weerachai

2003-10-01

A synthesis of zinc diethyldithiocarbamate (ZDEC) has been studied. The optimization mole ratio of the synthetic process was 2: 2: 2: 1 of diethylamine, carbondisulfide, sodium hydroxide, and zinc chloride. Characterization was carried out mainly by analyzing its spectroscopic properties especially decoupling 1 H NMR technique. ZDEC was obtained in 48.5% yield

Synthesis and structural characterization of a calcium coordination ...

Indian Academy of Sciences (India)

gly = glycine) has been isolated from the calcium chloride-glycine-water system and structurally characterized. Each Ca(II) in 1 is eight-coordinated and is bonded to eight oxygen atoms three of which are from terminal water molecules and five ...

Design, synthesis, and characterization of new phosphazene related materials, and study the structure property correlations

Science.gov (United States)

Tian, Zhicheng

The work described in this thesis is divided into three major parts, and all of which involve the exploration of the chemistry of polyphosphazenes. The first part (chapters 2 and 3) of my research is synthesis and study polyphoshazenes for biomedical applications, including polymer drug conjugates and injectable hydrogels for drug or biomolecule delivery. The second part (chapters 4 and 5) focuses on the synthesis of several organic/inorganic hybrid polymeric structures, such as diblock, star, brush and palm tree copolymers using living cationic polymerization and atom transfer radical polymerization techniques. The last part (chapters 6 and 7) is about exploratory synthesis of new polymeric structures with fluorinated side groups or cycloaliphatic side groups, and the study of new structure property relationships. Chapter 1 is an outline of the fundamental concepts for polymeric materials, as such the history, important definitions, and some introductory material for to polymer chemistry and physics. The chemistry and applications of phopshazenes is also briefly described. Chapter 2 is a description of the design, synthesis, and characterization of development of a new class of polymer drug conjugate materials based on biodegradable polyphosphazenes and antibiotics. Poly(dichlorophosphazene), synthesized by a thermal ring opening polymerization, was reacted with up to 25 mol% of ciprofloxacin or norfloxacin and three different amino acid esters (glycine, alanine, or phenylalanine) as cosubstituents via macromolecular substitutions. Nano/microfibers of several selected polymers were prepared by an electrospinning technique. Chapter 3 is concerned with the development of a class of injectable and biodegradable hydrogels based on water-soluble poly(organophosphazenes) containing oligo(ethylene glycol) methyl ethers and glycine ethyl esters. The hydrogels can be obtained by mixing alpha-cyclodextrin aqueous solution and poly(organophosphazenes) aqueous solution in

Design, synthesis, and characterization of 0-D, 1-D, and 2-D Zinc–Adeninate coordination assemblies

Energy Technology Data Exchange (ETDEWEB)

An, Ji Hyun [Dept. of Chemistry Education, Seoul National University, Seoul (Korea, Republic of); Geib, Steven J. [Dept. of Chemistry, University of Pittsburgh, Pittsburgh (United States); Kim, Myung Gil [Dept. of Chemistry, Chungang University, Seoul (Korea, Republic of)

2015-08-15

In this study, we demonstrate the synthesis and characterization of zinc– adeninate coordination polymers with 0-D, 1-D, and 2-D structures. We describe methods for controlling the structure of these materials by applying different synthetic conditions and discuss their structural relationships. 0-D, 1-D, and 2-D zinc–adeninate coordination polymers with the same metal–adeninate coordination mode were synthesized and characterized. By controlling the temperature, a material with 0-D macrocycle or 1-D chain coordination polymer was prepared. A replacement of pyridine with bipyridine formed 2-D sheet structure by connecting 1-D chains with each other. They exhibited an interesting relationship between synthetic methods and structures. Further study of metal–adeninate coordination chemistry will render a precise control of the structure in synthesis and will open a new venue to new materials with fascinating properties.

Synthesis and Characterization of Thermoelectric Oxides at Macro- and Nano-scales

Science.gov (United States)

Ma, Feiyue

Thermoelectric materials can directly convert a temperature difference into electrical voltage and vice versa. Due to this unique property, thermoelectric materials are widely used in industry and scientific laboratories for temperature sensing and thermal management applications. Waste heat harvesting, another potential application of thermoelectric materials, has long been limited by the low conversion efficiency of the materials. Potential high temperature applications, such as power plant waste heat harvesting and combustion engine exhaust heat recovery, make thermoelectric oxides a very promising class of thermoelectric materials. In this thesis, the synthesis and characterization of thermoelectric oxide materials are explored. In the first part of this thesis, the measurement methodologies and instrumentation processes employed to investigate different thermoelectric properties, such as the Seebeck coefficient and carrier concentration at the bulk scale and the thermal conductivity at the nanoscale, are detailed. Existing scientific and engineering challenges associated with these measurements are also reviewed. To overcome such problems, original parts and methodologies have been designed. Three fully functional systems were ultimately developed for the characterization of macroscale thermoelectric properties as well as localized thermal conductivity. In the second part of the thesis, the synthesis of NaxCo 2O4, a thermoelectric oxide material, is discussed. Modification of both composition and structure were carried out so as to optimize the thermoelectric performance of NaxCo2O4. Nanostructuring methods, such as ball milling, electrospinning, auto-combustion synthesis, and core-shell structure fabrication, have been developed to refine the grain size of NaxCo2O4 in order to reduce its thermal conductivity. However, the structure of the nanostructured materials is very unstable at high temperature and limited improvement on thermoelectric performance is

Synthesis and characterization of six-membered pincer ...

Indian Academy of Sciences (India)

0013167

SUPPORTING INFORMATION. REGULAR ARTICLE. Synthesis and characterization of six-membered pincer nickelacycles and application in alkylation of benzothiazole. †. HANUMANPRASAD PANDIRI,a DIPESH M SHARMA,a RAJESH G GONNADEb and. BENUDHAR PUNJI*,a. aOrganometallic Synthesis and Catalysis ...

Self-Assembled Structures of PMAA-PMMA Block Copolymers : Synthesis, Characterization, and Self-Consistent Field Computations

NARCIS (Netherlands)

Li, Feng; Schellekens, Mike; de Bont, Jens; Peters, Ron; Overbeek, Ad; Leermakers, Frans A. M.; Tuinier, Remco

2015-01-01

Block copolymers composed of methacrylic acid (MAA) and methyl methacrylate (MMA) blocks are interesting candidates for replacing surfactants in emulsion polymerization methods. Here the synthesis and experimental characterization of well-defined PMAA-PMMA block copolymers made via RAFT

Self-assembled structures of PMAA-PMMA block copolymers: Synthesis, characterization, and self-consistent field computations

NARCIS (Netherlands)

Li, F.; Schellekens, J.; Bont, de J.A.M.; Peters, R.; Overbeek, A.; Leermakers, F.A.M.; Tuinier, R.

2015-01-01

Block copolymers composed of methacrylic acid (MAA) and methyl methacrylate (MMA) blocks are interesting candidates for replacing surfactants in emulsion polymerization methods. Here the synthesis and experimental characterization of well-defined PMAA–PMMA block copolymers made via RAFT

Synthesis, structural and magnetic characterization of soft magnetic nanocrystalline ternary FeNiCo particles

Energy Technology Data Exchange (ETDEWEB)

Toparli, Cigdem [Department of Metallurgical & Materials Eng., Istanbul Technical University, 34469 Istanbul (Turkey); Max-Planck-Institut für Eisenforschung GmbH, Düsseldorf (Germany); Ebin, Burçak [Department of Metallurgical & Materials Eng., Istanbul Technical University, 34469 Istanbul (Turkey); Nuclear Chemistry and Industrial Material Recycling, Department of Chemistry and Chemical Engineering, Chalmers University of Technology, S-412 96 Gothenburg (Sweden); Gürmen, Sebahattin, E-mail: gurmen@itu.edu.tr [Department of Metallurgical & Materials Eng., Istanbul Technical University, 34469 Istanbul (Turkey)

2017-02-01

The present study focuses on the synthesis, microstructural and magnetic properties of ternary FeNiCo nanoparticles. Nanocrystalline ternary FeNiCo particles were synthesized via hydrogen reduction assisted ultrasonic spray pyrolysis method in single step. The effect of precursor concentration on the morphology and the size of particles was investigated. The syntheses were performed at 800 °C. Structure, morphology and magnetic properties of the as-prepared products were characterized through X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM) studies. Scherer calculation revealed that crystallite size of the ternary particles ranged between 36 and 60 nm. SEM and TEM investigations showed that the particle size was strongly influenced by the precursor concentration and Fe, Ni, Co elemental composition of individual particles was homogeneous. Finally, the soft magnetic properties of the particles were observed to be a function of their size. - Highlights: • Ternary FeNiCo alloy nanocrystalline particles were synthesized in a single step. • Cubic crystalline structure and spherical morphology was observed by XRD, SEM and TEM investigations. • The analysis of magnetic properties indicates the soft magnetic features of particles.

Synthesis and structural characterization of inorganic luminescent materials of Cs2NaErBr6 and Cs2NaHoBr6

International Nuclear Information System (INIS)

Poblete, V.H; Fack, G

2003-01-01

The synthesis and structural characterization is described of two luminescent materials, with technological [1] and spectroscopic [2] interest, whose crystallographic charts have not been published in the literature. The synthesis of both systems: Cs 2 NaErBr 6 and CS 2 NaHoBr 6 , was done using solid state reactions in a controlled environment. The thermal analyses DTA/TGA, applied with a temperature gradient of 10 o C/min., established crystallization ranges of 490,4 o C to 545,4 o C, for the elpasolite CS 2 NaHoBr 6 and 501 o C to 556 o C, for the structure CS 2 NaErBr 6 .. The heat vacuum treatments were carried out at 505 o C and 526 o C respectively, obtaining optimum crystallization. The structural characterization was performed with powdered X-ray diffraction (XRD). The range between 12 o and 80 o (2θ), was analyzed for 3352 points, measured steps of 0.02 o (2θ using the Rietveld profile refining program. The following crystallographic parameters were established: a 0 = 11,279(1), and 11,293(4) Angstroms, for the two structures analyzed, respectively. The relationship R exp wp in both cases is highly accurate for the 32 test lines that were analyzed. The structures present cubic closed packing Cs 1+ 3 Cl 1- , with Ho 3+ and Er 3+ atoms, filling the octahedral holes. The test data obtained will be very useful for completing the mass of experimental data needed to develop the design engineering, with specific applications for luminescent devices (au)

Boron-based nanostructures: Synthesis, functionalization, and characterization

Science.gov (United States)

Bedasso, Eyrusalam Kifyalew

Boron-based nanostructures have not been explored in detail; however, these structures have the potential to revolutionize many fields including electronics and biomedicine. The research discussed in this dissertation focuses on synthesis, functionalization, and characterization of boron-based zero-dimensional nanostructures (core/shell and nanoparticles) and one-dimensional nanostructures (nanorods). The first project investigates the synthesis and functionalization of boron-based core/shell nanoparticles. Two boron-containing core/shell nanoparticles, namely boron/iron oxide and boron/silica, were synthesized. Initially, boron nanoparticles with a diameter between 10-100 nm were prepared by decomposition of nido-decaborane (B10H14) followed by formation of a core/shell structure. The core/shell structures were prepared using the appropriate precursor, iron source and silica source, for the shell in the presence of boron nanoparticles. The formation of core/shell nanostructures was confirmed using high resolution TEM. Then, the core/shell nanoparticles underwent a surface modification. Boron/iron oxide core/shell nanoparticles were functionalized with oleic acid, citric acid, amine-terminated polyethylene glycol, folic acid, and dopamine, and boron/silica core/shell nanoparticles were modified with 3-(amino propyl) triethoxy silane, 3-(2-aminoethyleamino)propyltrimethoxysilane), citric acid, folic acid, amine-terminated polyethylene glycol, and O-(2-Carboxyethyl)polyethylene glycol. A UV-Vis and ATR-FTIR analysis established the success of surface modification. The cytotoxicity of water-soluble core/shell nanoparticles was studied in triple negative breast cancer cell line MDA-MB-231 and the result showed the compounds are not toxic. The second project highlights optimization of reaction conditions for the synthesis of boron nanorods. This synthesis, done via reduction of boron oxide with molten lithium, was studied to produce boron nanorods without any

Synthesis and characterization of mangan oxide coated sand from Capkala kaolin

Science.gov (United States)

Destiarti, Lia; Wahyuni, Nelly; Prawatya, Yopa Eka; Sasri, Risya

2017-03-01

Synthesis and characterization of mangan oxide coated sand from quartz sand fraction of Capkala kaolin has been conducted. There were two methods on synthesis of Mangan Oxide Coated Sand (MOCS) from Capkala Kaolin compared in this research. Characterization of MOCS was done by using Scanning Electron Microscope/Energy Dispersive X-Ray Spectrometer (SEM/EDX) and X-Ray Diffraction (XRD). The MOCS was tested to reduce phosphate in laundry waste. The result showed that the natural sand had bigger agregates and a relatively uniform structural orientation while both MOCS had heterogen structural orientation and manganese oxide formed in cluster. Manganese in first and second methods were 1,93% and 2,63%, respectively. The XRD spectrum showed clear reflections at 22,80°, 36,04°, 37,60° and a broad band at 26,62° (SiO2). Based on XRD spectrum, it can be concluded that mineral constituents of MOCS was verified corresponding to pyrolusite (MnO2). The former MOCS could reduce almost 60% while the later could reduce 70% phosphate in laundry waste.

Combustion synthesis by reaction and characterization of structural Ni-Zn ferrite doped with copper

International Nuclear Information System (INIS)

Dantas, J.; Santos, J.R.D.; Cunha, R.B.L.; Feitosa, C.A.; Costa, A.C.F.M.

2012-01-01

The present stud aims to evaluate the effect of doping with Cu 2+ ions concentrations of 0.0, 0.1, 0.2, 0.3 and 0.4 mol in the synthesis and structure of Ni-Zn ferrite. Samples were synthesized by the method of the combustion reaction and characterized by measuring the temperature as a function of reaction time, X-ray diffraction (XRD) and infrared spectroscopy in Fourier transform (FTIR). The combustion temperature and time were 646, 900, 989, 975 and 735°C and 210, 175, 220, 210 and 110 seconds for the sample doped with 0.0, 0.1, 0.2, 0.3 and 0.4 mol of copper, respectively. XRD results show that all concentrations of copper evaluated, there was only a training phase inverse spinel ferrite and Ni-Zn FTIR spectra show absorption bands below 1000cm -1 , which are characteristics of the spinel type AB 2 O 4- (author)

Synthesis and characterization of iron cobalt (FECO) nanorods ...

African Journals Online (AJOL)

Synthesis and characterization of iron cobalt (FECO) nanorods prepared by simple ... shaped by increasing annealing temperature from room temperature to 800 ... Keywords: FeCo nanoparticles, sodium borohydrid, CTAB, chemical synthesis ...

Synthesis and characterization of five-coordinated indium amidinates

Energy Technology Data Exchange (ETDEWEB)

Riahi, Yasaman

2016-07-29

The focus of this work is synthesis, characterization and exploring the reactivity of new indium amidinate compounds of the type R{sub 2}InX (R = R''NCR'NR''; R' = Ph, R'' = SiMe{sub 3}, iPr, dipp; X = Br, Cl) with the coordination number of five and R{sub 3}In (R = Me{sub 3}SiNCPhNSiMe{sub 3}) with the coordination number of six. By using amidinates as chelating ligands the electron deficiency of indium atom will be resolved. Additionally, by using different substituents the study of the different synthesized indium amidinates has become possible. The selected method for the synthesis allows the carbodiimides to react with organolithium compounds to get the corresponding lithium amidinates. Afterwards the resulting lithium amidinates take part in transmetalation reactions with InBr{sub 3} and InCl{sub 3}. The study of the reactivity of indium amidinate complexes including nucleophilic reactions as well as their reduction were also examined. Beside crystal structure analysis, nuclear magnetic resonance spectroscopy as well as elemental analysis has been applied to characterize the compounds.

Magnetic structures synthesized by controlled oxidative etching: Structural characterization and magnetic behavior

Directory of Open Access Journals (Sweden)

Álvaro de Jesús Ruíz-Baltazar

Full Text Available A facile strategy for the fabrication Fe3O4 nanostructures at room temperature and with well-defined morphology is proposed. In this methodology, the iron precursors were reduced by sodium borohydride. Subsequently an oxidative etching process promotes the formation of Fe2O3 nanostructures. Magnetic measurements revealed a well-defined superparamagnetic behavior for the material. The Zero-Field-Cooled (ZFC and Field-Cooled (FC magnetization curves reveals that critical and blocking temperature were 24 and 350 °C respectively. The Fe3O4 nanostructures were characterized using aberration-corrected (Cs scanning transmission electron microscopy (STEM and energy dispersive spectroscopy (EDS. Additionally, Raman spectra support the Fe3O4 presence and corroborate the efficiency of the synthesis process to obtain magnetite. Keywords: Chemical synthesis, Fe3O4 nanoparticles, Structural characterization, Magnetic properties

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.

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.

Characterization of nano structured metallic materials

International Nuclear Information System (INIS)

Marin A, M.; Gutierrez W, C.; Cruz C, R.; Angeles C, C.

1997-01-01

Nowadays the search of new materials with specific optical properties has carried out to realize a series of experiments through the polymer synthesis [(C 3 N 3 ) 2 (NH) 3 ] n doped with gold metallic nanoparticles. The thermal stability of a polymer is due to the presence of tyazine rings contained in the structure. The samples were characterized by High Resolution Transmission Electron Microscopy, X-ray diffraction by the Powder method, Ft-infrared and its thermal properties by Differential Scanning Calorimetry (DSC) and Thermogravimetry (TGA). One of the purposes of this work is to obtain nano structured materials over a polymeric matrix. (Author)

Hydrothermal synthesis, characterization and luminescent ...

Indian Academy of Sciences (India)

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

Synthesis and structural characterization of oaklin-catechins.

Science.gov (United States)

Sousa, André; Fernandes, Ana; Mateus, Nuno; De Freitas, Victor

2012-02-15

Condensation reactions of procyanidin dimer B4 with two representative oak wood cinnamic aldehydes (coniferaldehyde and sinapaldehyde) were conducted in winelike model solutions. Coniferaldehyde led to the formation of guaiacylcatechin-pyrylium-catechin (GCP-catechin, 737 m/z), whereas sinapaldehyde led to the formation of syringylcatechin-pyrylium-catechin (SCP-catechin, 767 m/z). The former was also structurally characterized by 1D and 2D NMR, allowing an elucidation of the formation mechanism of these oaklin-catechin adducts and demonstrating the importance of procyanidins in the formation of colored compounds through the reaction with cinnamic aldehydes extracted from oaks during storage.

Synthesis and characterization of tantalum organometallic complexes. Catalytic activity for olefins

International Nuclear Information System (INIS)

Baley, A.S.

1990-11-01

Synthesis of monoaryloxy (alcoxy) neopentyl compounds is investigated. The tantalum-oxygen bond is formed by two parallel ways from TaCl 5 or TaR 2 Cl 3 with R = neopentyl and the tantalum carbon bond from a neopentyl derivative of the main series. Some compounds were isolated and characterized by NMR, elemental analysis and sometimes X-ray structure, some others are characterized in solution only. Catalytic effect is tested by ethylene dimerization and olefin polymerization. Reactivity of tantalum aryloxy neopentyl in respect to complexing and chelating ligands is studied for preparation of neopentylidene complexes

Synthesis, characterization and magnetic properties of room-temperature nanofluid ferromagnetic graphite

OpenAIRE

Souza, N. S.; Sergeenkov, S.; Speglich, C.; Rivera, V. A. G.; Cardoso, C. A.; Pardo, H.; Mombru, A. W.; Rodrigues, A. D.; de Lima, O. F.; Araujo-Moreira, F. M.

2009-01-01

We report the chemical synthesis route, structural characterization, and physical properties of nanofluid magnetic graphite (NFMG) obtained from the previously synthesized bulk organic magnetic graphite (MG) by stabilizing the aqueous ferrofluid suspension with an addition of active cationic surfactant. The measured magnetization-field hysteresis curves along with the temperature dependence of magnetization confirmed room-temperature ferromagnetism in both MG and NFMG samples. (C) 2009 Americ...

Synthesis and Characterization of New Polyamides from 1,2-Bis hydrazine Derivatives

International Nuclear Information System (INIS)

Salaha, A.; Abdel-Bary, E.M.; Kandilea, N.G.

2005-01-01

Preparation of polyamides having different chemical structures allows obtaining new materials with different mechanical and physical properties. The difference in the chemical structure depends mainly on the starting reactants used in condensation polymerization of polyamides. In this paper the synthesis of new polyamides based on the condensation polymerization of 1,2- Bis(3-carboxyacryloyl or carboxybenzoyl) hydrazine derivatives and various diamines has been described. The polymers obtained were characterized using spectroscopic and X-ray analysis. Besides thermal stability and electrical conductivity have been evaluated and correlated with the chemical structure of the polyamides obtained

Synthesis and structural characterization of luminescent inorganic materials of the type CS2NaErBr6 and CS2NaHoBr6

International Nuclear Information System (INIS)

Poblete, V.H.; Fack, G.

2001-01-01

The synthesis and structural characterization is described of two luminescent materials, with technological [1] and spectroscopic [2] interest, whose crystallographic charts have not been published in the literature. The synthesis of both systems: Cs 2 NaErBr 6 and CS 2 NaHoBr 6 , was done using solid state reactions in a controlled environment. The thermal analyses DTA/TGA, applied with a temperature gradient of 10 o C/min., established crystallization ranges of 490,4 o C to 545,4 o C, for the elpasolite CS 2 NaHoBr 6 and 501 o C to 556 o C, for the structure CS 2 NaErBr 6 .. The heat vacuum treatments were carried out at 505 o C and 526 o C respectively, obtaining optimum crystallization. The structural characterization was performed with powdered X-ray diffraction (XRD). The range between 12 o and 80 o (2θ), was analyzed for 3352 points, measured steps of 0.02 o (2θ using the Rietveld profile refining program. The following crystallographic parameters were established: a 0 = 11,279(1), and 11,293(4) Angstroms, for the two structures analyzed, respectively. The relationship R exp wp in both cases is highly accurate for the 32 test lines that were analyzed. The structures present cubic closed packing Cs 1+ 3 Cl 1- , with Ho 3+ and Er 3+ atoms, filling the octahedral holes. The test data obtained will be very useful for completing the mass of experimental data needed to develop the design engineering, with specific applications for luminescent devices

Synthesis and structural characterization of the hexagonal anti-perovskite Na{sub 2}CaVO{sub 4}F

Energy Technology Data Exchange (ETDEWEB)

Green, Robert L., E-mail: rgreen@flpoly.org [Chemistry, Florida Polytechnic University, Lakeland, FL 33805 (United States); Avdeev, Maxim [Australian Science and Technology Organisation, Locked Bag 2001, Kirrawee DC, NSW 2232 (Australia); School of Chemistry, The University of Sydney, Sydney, NSW 2006 (Australia); Vogt, Thomas [NanoCenter and Department of Chemistry and Biochemistry, University of South Carolina, Columbia, SC 29208 (United States)

2017-06-15

The structural details of the ordered hexagonal oxyfluoride Na{sub 2}CaVO{sub 4}F prepared by solid-state synthesis using stoichiometric amounts of V{sub 2}O{sub 5}, CaCO{sub 3}, Na{sub 2}CO{sub 3} and NaF were characterized using high-resolution neutron powder diffraction. The structural changes between 25 °C and 750 °C revealed that the two structural subunits in this material behave different when heated: there is an expansion of the face-shared FNa{sub 4}Ca{sub 2} octahedra while the VO{sub 4} tetrahedra due to increased thermal disorder reveal marginal bond contractions. Bond valences and the global instability index point to significant structural disorder at 750 °C. - Graphical abstract: The structure of the novel oxyfluoride Na{sub 2}CaVO{sub 4}F is studied at room temperature and high-temperatures. The structure can be viewed as layers of compression and elongation of polyhedral subunits, which change as a function of temperature. - Highlights: • The novel oxyfluoride, Na{sub 2}CaVO{sub 4}F, is synthesized via solid-state method. • High-resolution neutron diffraction data is used to analyze the structure of Na{sub 2}CaVO{sub 4}F. • Structural subunits exhibit expansion and contraction with increasing temperature. • Higher temperatures increase instability within the structure of Na{sub 2}CaVO{sub 4}F.

Synthesis, characterization and comparison of polythiophene ...

Indian Academy of Sciences (India)

38

Synthesis, characterization and comparison of polythiophene-carbon ... b Nanotechnology Research Institute, School of Chemical Engineering, Babol University of Technology, Babol, ..... The scan range was from −0.24 to 1.2 V in reference to.

Synthesis and characterization of nano silicon and titanium nitride ...

Indian Academy of Sciences (India)

The characterization techniques indicated ... Scalable synthesis; microwave plasma; chemical synthesis; nanoparticles. 1. Introduction ... used but very few methods are available to produce silicon and titanium ... current (A). (m3/h). 1. Si. 2.1.

Boronate esters: Synthesis, characterization and molecular base receptor analysis

Science.gov (United States)

Gómez-Jaimes, Gelen; Barba, Victor

2014-10-01

The synthesis of three boronate esters obtained by reacting 4-fluorophenylboronic (1), 4-iodophenylboronic (2) and 3,4-chlorophenylboronic (3) acids with 2,4,5-trihidroxybenzaldehyde is reported. The structural characterization was determined by spectroscopic and spectrometric techniques. The boron atom was evaluated to acts as Lewis acid center in the reaction with pyridine (Py), triethylamine (TEA) and fluoride anion (F-). The titration method was followed by UV-Vis and 11B NMR spectroscopy; results indicate the good interaction with the fluoride ion but poor coordination towards pyridine in solution.

Synthesis and characterization of the polyaniline dopant Schiff base

Directory of Open Access Journals (Sweden)

Mirian Y. Matsumoto

2012-06-01

Full Text Available The Schiff base, N-salicilidenoanilina was used as dopant to induce polymerization of aniline and thus preparing polyaniline (PAni. The different conditions of preparation, including Schiff base structure, and the dosage of acidity reaction medium, were investigated to discuss the influence of these conditions relative conductivity of the resulting samples. The products were also characterized by Fourier transform infrared (FTIR, ultraviolet-visible (UV-Vis, electrochemical impedance spectroscopy (EIE. The results showed the synthesis conditions play an important in the formation and the final properties of the polyaniline

The Synthesis and Characterization of Gold-Core/LDH-Shell Nanoparticles

Science.gov (United States)

Rearick, Colton

In recent years, the field of nanomedicine has progressed at an astonishing rate, particularly with respect to applications in cancer treatment and molecular imaging. Although organic systems have been the frontrunners, inorganic systems have also begun to show promise, especially those based upon silica and magnetic nanoparticles (NPs). Many of these systems are being designed for simultaneous therapeutic and diagnostic capabilities, thus coining the term, theranostics. A unique class of inorganic systems that shows great promise as theranostics is that of layered double hydroxides (LDH). By synthesis of a core/shell structures, e.g. a gold nanoparticle (NP) core and LDH shell, the multifunctional theranostic may be developed without a drastic increase in the structural complexity. To demonstrate initial proof-of-concept of a potential (inorganic) theranostic platform, a Au-core/LDH-shell nanovector has been synthesized and characterized. The LDH shell was heterogeneously nucleated and grown on the surface of silica coated gold NPs via a coprecipitation method. Polyethylene glycol (PEG) was introduced in the initial synthesis steps to improve crystallinity and colloidal stability. Additionally, during synthesis, fluorescein isothiocyanate (FITC) was intercalated into the interlayer spacing of the LDH. In contrast to the PEG stabilization, a post synthesis citric acid treatment was used as a method to control the size and short-term stability. The heterogeneous core-shell system was characterized with scanning electron microscopy (SEM), energy dispersive x-ray spectroscopy (EDX), dynamic light scattering (DLS), and powder x-ray diffraction (PXRD). A preliminary in vitro study carried out with the assistance of Dr. Kaushal Rege's group at Arizona State University was to demonstrate the endocytosis capability of homogeneously-grown LDH NPs. The DLS measurements of the core-shell NPs indicated an average particle size of 212nm. The PXRD analysis showed that PEG

Synthesis, characterization, antimicrobial activity and molecular ...

African Journals Online (AJOL)

Synthesis, characterization, antimicrobial activity and molecular docking studies of combined pyrazol-barbituric acid pharmacophores. Assem Barakat, Bandar M. Al-Qahtani, Abdullah M. Al-Majid, M. Ali Mohammed Rafi Shaik, Mohamed H.M. Al-Agamy, Abdul Wadood ...

synthesis and optical characterization of acid-doped polyaniline thin

African Journals Online (AJOL)

HOD

SYNTHESIS AND OPTICAL CHARACTERIZATION OF ACID-DOPED. POLYANILINE THIN .... MATERIALS AND METHODS .... Characterization of Se Doped Polyaniline”,Current. Applied ... with Silver Nanoparticles”, Advances in Materials.

Synthesis, Characterization, Antimicrobial Activity and Antioxidant ...

African Journals Online (AJOL)

MBI

2015-12-08

Dec 8, 2015 ... Synthesis, Characterization, Antimicrobial Activity and Antioxidant. Studies of ... Transition metal complexes of Co(II) and Ni(II) with Schiff base ligand (HL) derived from condensation of 2- ..... 2-((5mercapto-1,3,4-thiadiazol-2-.

Synthesis and characterization of functional magnetic nanocomposites

Science.gov (United States)

Gass, J.; Sanders, J.; Srinath, S.; Srikanth, H.

2006-03-01

Magnetic nanoparticles and carbon nanotubes have been excellent functional materials that could be dispersed in polymer matrices for various applications. However, uniform dispersion of particles in polymers without agglomeration is quite challenging. We have fabricated PMMA/polypyrrole bilayer structures embedded with Fe3O4 magnetite nanoparticles synthesized using wet chemical synthesis. Agglomeration-free dispersion of nanoparticles was achieved by coating the particles with surfactants and by dissolving both the particles and PMMA in chlorobenzene. Structural characterization was done using XRD and TEM. Magnetic properties of the bilayer structures indicated superparamagnetic behavior that is desirable for RF applications as the magnetic losses are reduced. Our polymer nanocomposite bilayer films with conducting polymer coatings are potential candidates for tunable RF applications with integrated EMI suppression. We will also report on our studies of pumped ferrofluids flowing past carbon nanotubes that are arranged in microchannel arrays. Magnetization under various flow conditions is investigated and correlated with the hydrodynamic properties. This scheme provides a novel method of energy conversion and storage using nanocomposite materials.

Spectroscopic studies, theoretical models and structural characterization. II. Synthesis and X-ray powder diffraction of the elpasolites Cs2NaSmCl6

International Nuclear Information System (INIS)

Poblete, V.; Acevedo, R.

1998-01-01

In this research work, we report the synthesis and structural characterization of the stoichiometric elpasolite Cs 2 NaSmCl 6 . The synthesis was performed under a solid state reaction in nitrogen atmosphere from the chemicals CsCl, NaCl and SmCl 3 weighted stoichiometrically. The best possible crystallization temperature was obtained using thermal studies of the type DTA/TGA (the thermal treatment was allowed to proceed for 2.5 hours at 755 Centigrade, showing a temperature gradient of 10 Centigrade/minute). The structural characterization by powder X-ray diffraction (XDR) indicates that this elpasolite belongs to the Fm 3m (O h 5 ) space group and the optimized structural parameters are as follows: a 0 = 10.8342 Armstrong, V 1271.72 Armstrong 3 , Z=4, M=651.88, D x =3.406 y D exp=3.41 ± 0.01. The profile refinement, using the Rietveld method, allowed us to fit the experimental and the calculated intensities of a total of 32 lines. The above result indicates that the condition R exp 2+ + 3Cl -1 and the counter ions filling the octahedral holes, in full agreement with anti fluorite type crystal. According to the above description, these elpasolite adopt the form (M 1/3 □ 2/3 ) 4 X 2 , where M labels the central metal, X stand for the chlorine ions and □ represent the vacancies, which may accommodate a significant amount of defects without collapsing. This experimental study provides the necessary input to test theoretical models against experimental data. (Author)

Structural synthesis of parallel robots

CERN Document Server

Gogu, Grigore

This book represents the fifth part of a larger work dedicated to the structural synthesis of parallel robots. The originality of this work resides in the fact that it combines new formulae for mobility, connectivity, redundancy and overconstraints with evolutionary morphology in a unified structural synthesis approach that yields interesting and innovative solutions for parallel robotic manipulators.  This is the first book on robotics that presents solutions for coupled, decoupled, uncoupled, fully-isotropic and maximally regular robotic manipulators with Schönflies motions systematically generated by using the structural synthesis approach proposed in Part 1.  Overconstrained non-redundant/overactuated/redundantly actuated solutions with simple/complex limbs are proposed. Many solutions are presented here for the first time in the literature. The author had to make a difficult and challenging choice between protecting these solutions through patents and releasing them directly into the public domain. T...

Novel biosynthesis of Ag-hydroxyapatite: Structural and spectroscopic characterization

Science.gov (United States)

Ruíz-Baltazar, Álvaro de Jesús; Reyes-López, Simón Yobanny; Silva-Holguin, Pamela Nair; Larrañaga, Daniel; Estévez, Miriam; Pérez, Ramiro

2018-06-01

Silver-doped hydroxyapatite (Ag-HAP) was obtained by green synthesis route. The dopant silver nanoparticles (AgNPs) were obtained by biosynthesis based on Melissa officinalis extract. This research is focused on the characterization and the use of the nontoxic and environment-friendly Ag-HAP nanocomposite. The structural and morphological characterization of Ag-HAP nanocomposite was carried out by scanning electron microscopy (SEM), X-ray diffraction, Fourier-transform infrared (FT-IR) and Raman spectroscopy. The obtained nanoparticles exhibited a great interaction with the HAP matrix, performing an Ag-HAP nanocomposite. Changes in the structure of the Ag-HAP nanocomposite were corroborated by the different characterization techniques. Additionally, a homogeneous distribution of the AgNPs on the HAP structure was observed. The heterogeneous nucleation process employed to doping the HAP, offer a functional route to obtain a green composite with potentials applications in multiple fields, such as tissue engineering, bone repair as well as protein. These properties can be evaluated in subsequent studies.

Nanoscale Synthesis and Characterization Laboratory Annual Report 2005

Energy Technology Data Exchange (ETDEWEB)

Hamza, A V; Lesuer, D R

2006-01-03

The Nanoscale Synthesis and Characterization Laboratory's (NSCL) primary mission is to create and advance interdisciplinary research and development opportunities in nanoscience and technology. The initial emphasis of the NSCL has been on development of scientific solutions in support of target fabrication for the NIF laser and other stockpile stewardship experimental platforms. Particular emphasis has been placed on the design and development of innovative new materials and structures for use in these targets. Projects range from the development of new high strength nanocrystalline alloys to graded density materials to high Z nanoporous structures. The NSCL also has a mission to recruit and train personnel for Lab programs such as the National Ignition Facility (NIF), Defense and Nuclear Technologies (DNT), and Nonproliferation, Arms control and International security (NAI). The NSCL continues to attract talented scientists to the Laboratory.

Nano-ilmenite FeTiO3 : synthesis and characterization

OpenAIRE

Raghavender, A. T.; Hoa Hong, Nguyen; Lee, Kyu Joon; Jung, Myung-Hwa; Skoko, Z.; Vasilevskiy, Mikhail; Cerqueira, M. F.; Samantilleke, A. P.

2013-01-01

In general, ilmenite FeTiO3 is synthesized by solid-state reaction at very high pressure and high temperature. Synthesis of FeTiO3 is not an easy task as the Fe2+ ions are not stable. Therefore, it is really challenging to prepare this material. In this work nano-ilmenite FeTiO3 was synthesized by the sol-gel method. Structural, optical and magnetic characterizations were performed. The bandgap of FeTiO3 was determined to be 2.8 eV showing FeTiO3 as suitable wide bandgap material for technolo...

Synthesis and characterization of dihexyldithiocarbamate as a chelating agent in extraction of gold(III)

Energy Technology Data Exchange (ETDEWEB)

Fatimah, Soja Siti, E-mail: soja-sf@upi.edu [Departemen Pendidikan Kimia, Universitas Pendidikan Indonesia, Jl. Dr. Setiabudhi No. 229, Bandung 40154 (Indonesia); Department of Chemistry, Faculty of Mathematics and Natural Sciences, Padjadjaran University, Jl. Raya Bandung-Sumedang, Km. 21, Jatinangor (Indonesia); Bahti, Husein H.; Hastiawan, Iwan [Department of Chemistry, Faculty of Mathematics and Natural Sciences, Padjadjaran University, Jl. Raya Bandung-Sumedang, Km. 21, Jatinangor (Indonesia); Permanasari, Anna [Departemen Pendidikan Kimia, Universitas Pendidikan Indonesia, Jl. Dr. Setiabudhi No. 229, Bandung 40154 (Indonesia)

2016-02-08

The use of dialkyldithiocarbamates as chelating agents of transition metals have been developing for decades. Many chelating agents have been synthesized and used in the extraction of the metals. Studies on particular aspects of extraction of the metals, such as the effect of increasing hydrophobicity of chelating agents on the effectiveness of the extraction, have been done. However, despite the many studies on the synthesis and applications of this type of chelating agents, interests in the aspect of molecular structure of the synthesized ligands and of their complexes, have been limited. This study aimed at synthesizing and characterizing dihexylthiocarbamate, and using the ligand for the extraction of gold III). Characterization of the ligand and of its metal complex were done by using elemental analysis, DTG, and spectroscopic methods to include NMR, ({sup 1}H, and {sup 13}C), FTIR, and MS-ESI. Data on the synthesis, characterization, and the application of the ligand as a chelating agent are presented.

Synthesis and characterization of dihexyldithiocarbamate as a chelating agent in extraction of gold(III)

Science.gov (United States)

Fatimah, Soja Siti; Bahti, Husein H.; Hastiawan, Iwan; Permanasari, Anna

2016-02-01

The use of dialkyldithiocarbamates as chelating agents of transition metals have been developing for decades. Many chelating agents have been synthesized and used in the extraction of the metals. Studies on particular aspects of extraction of the metals, such as the effect of increasing hydrophobicity of chelating agents on the effectiveness of the extraction, have been done. However, despite the many studies on the synthesis and applications of this type of chelating agents, interests in the aspect of molecular structure of the synthesized ligands and of their complexes, have been limited. This study aimed at synthesizing and characterizing dihexylthiocarbamate, and using the ligand for the extraction of gold III). Characterization of the ligand and of its metal complex were done by using elemental analysis, DTG, and spectroscopic methods to include NMR, (1H, and 13C), FTIR, and MS-ESI. Data on the synthesis, characterization, and the application of the ligand as a chelating agent are presented.

Synthesis and transport characterization of electrochemically deposited CdTe nanowires

Science.gov (United States)

Kaur, Jaskiran; Kaur, Harmanmeet; Singh, R. C.

2018-04-01

This paper reports the synthesis and characterization of CdTe nanowires. A thin polymeric films were irradiated with 80MeV Ag ions at a fluence of 8E7 ions/cm2, followed by UV irradiation and chemically etching in aqueous NaOH. Nanosizes go-through pores so formed were filled using a specially designed cell via electrodeposition. Nanowires so formed were further studied using SEM, I-V, UV and XRD analysis. SEM images show very smooth and uniform CdTe nanowires freely standing on the substrate. The in-situ I-V characteristics of nano-/micro structures was carried out at room temperature by leaving the structures embedded in the insulating template membrane itself.

Synthesis, Spectroscopic and DFT Characterization of 4â-(4-tert ...

African Journals Online (AJOL)

In this work the synthesis, spectral characterization and non-linear optical properties of metal-free .... following literature methods23–26 The advantage of this method ..... Synthesis of phthalocyanine conjugates with gold nanoparticles and.

Synthesis and characterization of ceramic powders of pure and doped with trivalent erbium barium tungstate

International Nuclear Information System (INIS)

Sousa, R.B. de; Nascimento, V.A. do; Matos, J. M.E. de; Santos, M.R.M.C.

2014-01-01

This research proposes the synthesis and characterization of pure and doped with Er"3"+ (1 and 2 %) barium tungstate powders prepared by the coprecipitation method. In order to characterize the obtained powders were used X-Ray Diffractometry, Raman Spectroscopy and Fourier Transform Infrared Spectroscopy. According to the standard XRD spectra, the crystals exhibited the presence of tetragonal scheelite structure without the presence of secondary phases. Raman spectra showed the presence of eleven vibrational modes and two modes were observed in the infrared spectra. The synthesized oxides showed good crystallinity and structurally ordered at short and long-range. (author)

Synthesis and characterization of organic-inorganic hybrids formed between conducting polymers and crystalline antimonic acid

Directory of Open Access Journals (Sweden)

Beleze Fábio A.

2001-01-01

Full Text Available In this paper we report the synthesis and characterization of novel organic-inorganic hybrid materials between the crystalline antimonic acid (CAA and two conductive polymers: polypyrrole and polyaniline. The hybrids were obtained by in situ oxidative polymerization of monomers by the Sb(V present in the pyrochlore-like CAA structure. The materials were characterized by infrared and Raman spectroscopy, X-ray diffraction, cyclic voltammetry, CHN elemental analysis and electronic paramagnetic resonance spectroscopy. The results showed that both polymers were formed in their oxidized form, with the CAA structure acting as a counter anion.

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.

Nitridomanganates of alkaline-earth metals. Synthesis, structure, and physical properties

Energy Technology Data Exchange (ETDEWEB)

Ovchinnikov, Alexander

2016-12-02

The main goal of the present work was the synthesis of alkaline-earth nitridomanganates (AE{sub x}Mn{sub y}N{sub z}) with extended anionic structures and the characterization of their electronic and magnetic properties. Up to now, only compounds with isolated nitridomanganate anions have been reported in the discussed ternary systems. A systematic exploratory synthesis, employing high-temperature treatment of AE nitrides and Mn under controlled N2 pressure, yielded more than ten new nitridomanganates. Their crystal structures contain anionic building blocks of different dimensionalities, ranging from isolated species to three-dimensional frameworks. In general, the formation of Mn-rich compositions was found to be driven by the emergence of Mn-Mn interactions, which creates a link between nitridometalates and transition-metal-rich binary nitrides. The obtained nitridomanganates display a plethora of interesting phenomena, such as large spin-orbit coupling, magnetic frustration, quenching of magnetism due to Mn-Mn interactions, and metal-insulator transition.

Synthesis and characterization of dextran-coated iron oxide nanoparticles

Science.gov (United States)

Predescu, Andra Mihaela; Matei, Ecaterina; Berbecaru, Andrei Constantin; Pantilimon, Cristian; Drăgan, Claudia; Vidu, Ruxandra; Predescu, Cristian; Kuncser, Victor

2018-03-01

Synthesis and characterization of iron oxide nanoparticles coated with a large molar weight dextran for environmental applications are reported. The first experiments involved the synthesis of iron oxide nanoparticles which were coated with dextran at different concentrations. The synthesis was performed by a co-precipitation technique, while the coating of iron oxide nanoparticles was carried out in solution. The obtained nanoparticles were characterized by using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction spectrometry, Fourier transform infrared spectroscopy and superconducting quantum interference device magnetometry. The results demonstrated a successful coating of iron oxide nanoparticles with large molar weight dextran, of which agglomeration tendency depended on the amount of dextran in the coating solution. SEM and TEM observations have shown that the iron oxide nanoparticles are of about 7 nm in size.

Synthesis and Characterization of Stimuli Responsive Block Copolymers, Self-Assembly Behavior and Applications

Energy Technology Data Exchange (ETDEWEB)

Determan, Michael Duane [Iowa State Univ., Ames, IA (United States)

2005-12-17

The central theme of this thesis work is to develop new block copolymer materials for biomedical applications. While there are many reports of stimuli-responsive amphiphilic [19-21] and crosslinked hydrogel materials [22], the development of an in situ gel forming, pH responsive pentablock copolymer is a novel contribution to the field, Figure 1.1 is a sketch of an ABCBA pentablock copolymer. The A blocks are cationic tertiary amine methacrylates blocked to a central Pluronic F127 triblock copolymer. In addition to the prerequisite synthetic and macromolecular characterization of these new materials, the self-assembled supramolecular structures formed by the pentablock were experimentally evaluated. This synthesis and characterization process serves to elucidate the important structure property relationships of these novel materials, The pH and temperature responsive behavior of the pentablock copolymer were explored especially with consideration towards injectable drug delivery applications. Future synthesis work will focus on enhancing and tuning the cell specific targeting of DNA/pentablock copolymer polyplexes. The specific goals of this research are: (1) Develop a synthetic route for gel forming pentablock block copolymers with pH and temperature sensitive properties. Synthesis of these novel copolymers is accomplished with ATRP, yielding low polydispersity and control of the block copolymer architecture. Well defined macromolecular characteristics are required to tailor the phase behavior of these materials. (2) Characterize relationship between the size and shape of pentablock copolymer micelles and gel structure and the pH and temperature of the copolymer solutions with SAXS, SANS and CryoTEM. (3) Evaluate the temperature and pH induced phase separation and macroscopic self-assembly phenomenon of the pentablock copolymer. (4) Utilize the knowledge gained from first three goals to design and formulate drug delivery formulations based on the multi

A General Chemistry Experiment Incorporating Synthesis and Structural Determination

Science.gov (United States)

van Ryswyk, Hal

1997-07-01

An experiment for the general chemistry laboratory is described wherein gas chromatography-mass spectroscopy (GC-MS) and diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) are used to characterize the products of a series of microscale reactions on vanillin. A single sophisticated instrument can be incorporated into the laboratory given sufficient attention to the use of sampling accessories and software macros. Synthetic experiments coupled with modern instrumental techniques can be used in the general chemistry laboratory to illustrate the concepts of synthesis, structure, bonding, and spectroscopy.

Synthesis, structural characterization, and thermal stability studies of heteroleptic cadmium(II) dithiocarbamate with different pyridyl groups

Science.gov (United States)

Onwudiwe, Damian C.; Hosten, Eric C.

2018-01-01

The synthesis, characterization and crystal structures of three chloroform solvated adducts of cadmium with mixed ligands of N-alkyl-N-phenyldithiocarbamate and pyridine, 2,2-bipyridine and 1, 10 phenanthroline represented as [CdL1L2 (py)2]·CHCl3(1), [CdL1L2bpy]•CHCl3(2), and [CdL1L2phen]•CHCl3(3) (LI = N-methyl-N-phenyldithiocarbamate, L2 = N-ethyl-N-phenyldithiocarbamate, py = pyridine, bpy = 2,2-bipyridine and phen = 1,10-phenanthroline) respectively are reported. Complex 1, which crystallized in the monoclinic space group P-1, is a centrosymmetric dimeric structure where each Cd center is bonded to two monodentate pyridine, a bidentate terminal dithiocarbamate, and another bidentate bridging dithiocarbamate to form a four-membered ring. Complex 2 crystallized in the monoclinic space group P21/c, with four discrete monomeric molecules in the asymmetric unit. The structure presents a cadmium atom coordinated by two sulphur atoms of a dithiocarbamate ligand and two nitrogen atoms of the 2,2‧-bipyridine to form a CdS4N2 fragment, thus giving the structure around the Cd atom a distorted trigonal prism geometry. Complex 3 contains two discrete monomeric molecules of (phenanthroline) (N, N-methyl phenyl-N, N-ethyl phenyl dithiocarbamato)cadmium (II) per unit cell, and the complex crystallized in the triclinic space group P-1. The structure showed that the Cd atom is bonded to two bidentate dithiocarbamate ligands and to one bidentate phenanthroline ligand in a distorted trigonal prism geometry. All the compounds resulted in CdS as residue upon thermal decomposition process conducted under inert atmosphere.

Synthesis and study of nano-structured cellulose acetate based materials for energy applications

International Nuclear Information System (INIS)

Fischer, F.

2006-12-01

Nano-structured materials have unique properties (high exchange areas, containment effect) because of their very low characteristic dimensions. The elaboration way set up in this PhD work consists in applying the classical processes for the preparation of aerogel-like materials (combining sol-gel synthesis and CO 2 supercritical extraction) to cellulosic polymers. This work is divided in four parts: a literature review, the presentation and the study of the chemical synthesis that leads to cellulose acetate-based aerogel, the characterizations (chemical, structural and thermal) of the elaborated nano-materials, and finally the study of the first carbons that were obtained after pyrolysis of the organic matrix. The formulations and the sol-gel protocol lead to chemical gels by crosslinking cellulose acetate using a poly-functional iso-cyanate. The dry materials obtained after solvent extraction with supercritical CO 2 are nano-structured and mainly meso-porous. Correlations between chemical synthesis parameters (reagent concentrations, crosslinking rate and degree of polymerisation) and porous properties (density, porosity, pore size distribution) were highlighted thanks to structural characterizations. An ultra-porous reference aerogel, with a density equals to 0,245 g.cm -3 together with a meso-porous volume of 3,40 cm 3 .g -1 was elaborated. Once in granular shape, this material has a thermal conductivity of 0,029 W.m -1 .K -1 . In addition, carbon materials produced after pyrolysis of the organic matrix and after grinding are nano-structured and nano-porous, even if important structural modifications have occurred during the carbonization process. The elaborated materials are evaluated for applications in relation with energy such as thermal insulation (organic aerogels) but also for energy conversion and storage through electrochemical way (carbon aerogels). (author)

Component mode synthesis in structural dynamics

International Nuclear Information System (INIS)

Reddy, G.R.; Vaze, K.K.; Kushwaha, H.S.

1993-01-01

In seismic analysis of Nuclear Reactor Structures and equipments eigen solution requires large computer time. Component mode synthesis is an efficient technique with which one can evaluate dynamic characteristics of a large structure with minimum computer time. Due to this reason it is possible to do a coupled analysis of structure and equipment which takes into account the interaction effects. Basically in this the method large size structure is divided into small substructures and dynamic characteristics of individual substructure are determined. The dynamic characteristics of entire structure are evaluated by synthesising the individual substructure characteristics. Component mode synthesis has been applied in this paper to the analysis of a tall heavy water upgrading tower. Use of fixed interface normal modes, constrained modes, attachment modes in the component mode synthesis using energy principle and using Ritz vectors have been discussed. The validity of this method is established by solving fixed-fixed beam and comparing the results obtained by conventional and classical method. The eigen value problem has been solved using simultaneous iteration method. (author)

Synthesis and characterization of "1"3C_3-tristearin

International Nuclear Information System (INIS)

Wu Hangyu; Lin Lin; Li Lei; Chen Dazhou

2011-01-01

A highly efficient synthesis of "1"3C_3 labeled triglycerides of stearic acids from "1"3C_3-glycerol and stearic acids, by immobilized lipase-catalyzed in solvent-free medium was described. The structure of the product were characterized by fourier transform infrared spectrum (FT-IR), nuclear magnetic resonance (NMR), mass spectra (MS). The results showed that triglycerides of stearic acids contained three "1"3C atoms. The isotope abundance of "1"3C_3-tristearin was more than 99% and the yield was 80% of "1"3C_3-tristearin through calculation. Chemical purity (> 98%) was obtained by differential scanning calorimetry (DSC). (authors)

Synthesis and structural characterization of some trisulfide analoges of thiouracil-based antithyroid drugs

Science.gov (United States)

Bhabak, Krishna P.; Bhowmick, Debasish

2012-08-01

Thiourea-based antithyroid drugs are effectively used for the treatment of hyperthyroidism. In this paper, we describe the synthesis of new trisulfides (11-12) from the commonly used thiourea-based antithyroid drugs such as 6-n-propyl-2-thiouracil (PTU) and 6-methyl-2-thiouracil (MTU) in the reaction with I2/KI system. Structural analysis by single crystal X-ray diffraction studies revealed the stabilization of trisulfides by a lactam-lactim tautomerism facilitating effective intramolecular as well as intermolecular non-covalent interactions. Although the structures of both trisulfides were found to be quite similar, a notable difference in the intermolecular interactions was observed between compounds 11 and 12 leading to different structural patterns. Structural stabilization of these trisulfides by tautomerism followed by intramolecular as well as intermolecular H-bonds makes these molecules as perfect examples in molecular recognition with self-complementary donor and acceptor units within a single molecule.

V2O5 xerogel-poly(ethylene oxide) hybrid material: Synthesis, characterization, and electrochemical properties

International Nuclear Information System (INIS)

Guerra, Elidia M.; Ciuffi, Katia J.; Oliveira, Herenilton P.

2006-01-01

In this work, we report the synthesis, characterization, and electrochemical properties of vanadium pentoxide xerogel-poly(ethylene oxide) (PEO) hybrid materials obtained by varying the average molecular weight of the organic component as well as the components' ratios. The materials were characterized by X-ray diffraction, ultraviolet/visible and infrared spectroscopies, thermogravimetric analysis, scanning electron microscopy, electron paramagnetic resonance, and cyclic voltammetry. Despite the presence of broad and low intensity peaks, the X-ray diffractograms indicate that the lamellar structure of the vanadium pentoxide xerogel is preserved, with increase in the interplanar spacing, giving evidence of a low-crystalline structure. We found that the electrochemical behaviour of the hybrid materials is quite similar to that found for the V 2 O 5 xerogel alone, and we verified that PEO leads to stabilization and reproducibility of the Li + electrochemical insertion/de-insertion into the V 2 O 5 xerogel structure, which makes these materials potential components of lithium ion batteries. - Graphical abstract: The synthesis, structural and electrochemical properties of vanadium pentoxide xerogel-poly(ethylene oxide) hybrid materials have been described. Despite the presence of broad and low intensity peaks, the X-ray diffractograms indicate that the lamellar structure of the vanadium pentoxide xerogel is preserved. The cyclic voltammetry technique demonstrated that PEO intercalation provides an improvement in the electrochemical properties, mainly with respect to the lithium electroinsertion process into the oxide matrix

Magnetic ionic liquids: synthesis and characterization

International Nuclear Information System (INIS)

Medeiros, Anderson M.M.S.; Parize, Alexandre L.; Oliveira, Vanda M.; Neto, Brenno A.D.; Rubim, Joel C.

2010-01-01

The synthesis of magnetic ionic liquids (MILs) based on the stable dispersions of magnetic nanoparticles (MNPs) of γ-Fe 2 O 3 , Fe 3 O 4 , and CoFe 2 O 4 in the ionic liquid 1-n-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide (BMI.NTf 2 ) is reported. The MNPs were obtained by the coprecipitation method. The surface of the α-Fe 2 O 3 , Fe 3 O 4 , and CoFe 2 O 4 MNPs with mean sizes (XRD) of 9.3, 12.3, and 11.0 nm, respectively were functionalized by 1-n-butyl-3-(3'-trimethoxypropylsilane)- imidazolium chloride. The non functionalized and functionalized MNPs were further characterized by Raman, FTIR-ATR, and FTNIR spectroscopy and by TGA. The stability of the MILs was assigned to the formation of at least one monolayer of the surface modifier agent that mimics the structure of the BMI.NTf 2 IL. (author)

Synthesis of a hierarchically structured zeolite-templated carbon starting from fly ash-derived zeolite X

CSIR Research Space (South Africa)

Musyoka, Nicholas M

2014-05-01

Full Text Available A hierarchically structured zeolite derived from coal fly ash was used as a hard templating agent for the synthesis of a templated carbonaceous material. The samples were characterized using XRD, SEM, TEM, TGA, EDS and BET. The resulting carbon had...

Synthesis and structural characterization of nano-hydroxyapatite biomaterials prepared by microwave processing

Science.gov (United States)

Ramli, Rosmamuhamadani; Arawi, Ainaa Zafirah Omar; Talari, Mahesh Kumar; Mahat, Mohd Muzamir; Jais, Umi Sarah

2012-07-01

Synthetic hydroxyapatite, (HA, Ca10(PO4)6(OH)2), is an attractive and widely utilized bio-ceramic material for orthopedic and dental implants because of its close resemblance of native tooth and bone crystal structure. Synthetic HA exhibits excellent osteoconductive properties. Osteoconductivity means the ability to provide the appropriate scaffold or template for bone formation. Calcium phosphate biomaterials [(HA), tri-calcium phosphate (TCP) and biphasic calcium phosphate (HA/TCP)] with appropriate three-dimensional geometry are able to bind and concentrate endogenous bone morphogenetic proteins in circulation, and may become osteoinductive and can be effective carriers of bone cell seeds. This HA can be used in bio-implants as well as drug delivery application due to the unique properties of HA. Biomaterials synthesized from the natural species like mussel shells have additional benefits such as high purity, less expensive and high bio compatibility. In this project, HA-nanoparticles of different crystallite size were prepared by microwave synthesis of precursors. High purity CaO was extracted from the natural mussel shells for the synthesis of nano HA. Dried nano HA powders were analyzed using X-Ray Diffraction (XRD) technique for the determination of crystal structure and impurity content. Scanning Electron Microscopic (SEM) investigation was employed for the morphological investigation of nano HA powders. From the results obtained, it was concluded that by altering the irradiation time, nano HA powders of different crystallite sizes and morphologies could be produced. Crystallite sizes calculated from the XRD patterns are found to be in the range of 10-55 nm depending on the irradiation time.

Ultrasonic-assisted chemical reduction synthesis and structural characterization of copper nanoparticles

Science.gov (United States)

Anh-Nga, Nguyen T.; Tuan-Anh, Nguyen; Thanh-Quoc, Nguyen; Ha, Do Tuong

2018-04-01

Copper nanoparticles, due to their special properties, small dimensions and low-cost preparation, have many potential applications such as in optical, electronics, catalysis, sensors, antibacterial agents. In this study, copper nanoparticles were synthesized by chemical reduction method with different conditions in order to investigate the optimum conditions which gave the smallest (particle diameter) dimensions. The synthesis step used copper (II) acetate salt as precursor, ascorbic acid as reducing agent, glycerin and polyvinylpyrrolidone (PVP) as protector and stabilizer. The assistance of ultrasonic was were considered as the significant factor affecting the size of the synthesized particles. The results showed that the copper nanoparticles have been successfully synthesized with the diameter as small as 20-40 nm and the conditions of ultrasonic waves were 48 kHz of frequency, 20 minutes of treated time and 65-70 °C of temperature. The synthesized copper nanoparticles were characterized by optical absorption spectrum, scanning electron microscopy (SEM), and Fourier Transform Infrared Spectrometry.

Synthesis and characterization of a cerebral radiotracer

International Nuclear Information System (INIS)

Ben hamouda, Salem

2010-01-01

The development of nuclear medicine is based on research of new radiopharmaceuticals, in particular, relying on technetium-99m, the most used radioisotope in terms of availability and low cost. A similar study on Rhenium (185/187Re) is essential for monitoring physico-chemical studies due to the high specific activity of technetium-99m. During this work, we have synthesized and labeled with technetium the N-methyl-4-hydroxy piperidinyl ferrocenyl carboxylate. The marking is done by exchange of ligands between the iron group of ferrocene and tricabonyl technetium core. We have succeeded to synthesis the N-methyl-4-hydroxy piperidinyl carboxyl cyclopentadienyl tricarbonyl rhenium (the molecular analogue of the technetium). We characterized it by MS, IR and NMR (1H, 13C) The structure of N-methyl-4-hydroxy piperidinyl carboxyl cyclopentadienyl tricarbonyl technetium is well justified.

SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURES ...

African Journals Online (AJOL)

B. S. Chandravanshi

ABSTRACT. Reaction of [VO(acac)2] (acac = acetylacetonate) with ... Single crystal X-ray structural studies indicate that the hydrazone ligands coordinate to ..... Molecular structure of complex (1) at 30% probability displacement. Figure 4.

Synthesis, characterization and antimicrobial activity of mixed ...

African Journals Online (AJOL)

Synthesis, characterization and antimicrobial activity of mixed ascorbic acid - nicotinamide metal complexes. ... The result of the antimicrobial studies showed that the mixed complexes have higher inhibitory activity than the original ligands against the tested bacteria and fungi species. KEY WORDS: Ascorbic acid, ...

Synthesis, structural characterization and antitumor activity of a Ca(II) coordination polymer based on 4-formyl-1,3-benzenedisulfonate-2-furoic acid hydrazide ligands

Energy Technology Data Exchange (ETDEWEB)

Tai, Xi-Shi, E-mail: taixs@wfu.edu.cn [Weifang University, College of Chemistry and Chemical Engineering (China); Wang, Xin [Qinghai Normal University, Department of Chemistry (China)

2017-03-15

A new Ca(II) coordination polymer, ([CaL(H{sub 2}O){sub 4}] · (H{sub 2}O){sub 4}){sub n} (L = 4-formyl-1,3-benzenedisulfonate-2-furoic acid hydrazide) has been prepared by one-pot synthesis method. And it was characterized by elemental analysis, IR and thermal analysis. The result of X-ray single-crystal diffraction analysis shows that the Ca(II) complex molecules form one-dimensional chain structure by the bridging oxygen atoms. The anti-tumor activity of L ligand and the Ca(II) coordination polymer has also been studied.

Synthesis, Characterization, and Computational Modeling of N-(1-Ethoxyvinylpyridinium Triflates, an Unusual Class of Pyridinium Salts

Directory of Open Access Journals (Sweden)

Jonathan D. Shapiro

2018-02-01

Full Text Available N-Substituted pyridinium salts constitute one of the most valuable reagent classes in organic synthesis, due to their versatility and ease of use. Herein we report a preliminary synthesis and detailed structural analysis of several N-(1-ethoxyvinylpyridinium triflates, an unusual class of pyridinium salts with potentially broad use as a reagent in organic synthesis. Treatment of pyridines with trifluoromethane sulfonic acid and ethoxyacetylene generates stable, isolable adducts which have been extensively characterized, due to their novelty. Three-dimensional structural stability is perpetuated by an array of C–H•••O hydrogen bonds involving oxygen atoms from the –SO3 groups of the triflate anion, and hydrogen atoms from the aromatic ring and vinyl group of the pyridinium cation. Predictions from density functional theory calculations of the energy landscape for rotation about the exocyclic C–N bond of 2-chloro-1-(1-ethoxyvinylpyridine-1-ium trifluoromethanesulfonate (7 and 1-(1-ethoxyvinylpyridine-1-ium trifluoromethanesulfonate (16 are also reported. Notably, the predicted global energy minimum of 7 was nearly identical to that found within the crystal structure.

SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURE ...

African Journals Online (AJOL)

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Reaction of [MoO2(acac)2] (where acac = acetylacetonate) with N'-(2-hydroxy-4- ... Single crystal X-ray structural studies indicate that the hydrazone ligand coordinates .... Molecular structure of the complex at 30% probability displacement.

Green synthesis, characterization and antibacterial activity of copper ...

African Journals Online (AJOL)

Green synthesis, characterization and antibacterial activity of copper nanoparticles using L -ascorbic ... Journal Home > Vol 10, No 3 (2017) > ... In this study, simple, economical, convenient and environmentally-friendly chemical reduction ...

Synthesis of Carbon nano structures by plasma discharge

International Nuclear Information System (INIS)

Jimenez L, M.L.

2007-01-01

Due to the great quantity of applications of the carbon nano structures (NEC) in diverse areas like: synthesis of super-resistant materials, hydrogen storage, nano sensors generation and nano catalysts, it has seen the necessity to generate new processes of synthesis of this materials as well as to already improve those existent. The present work has as objective to optimize the NEC synthesis process by means of the electric arc method which uses alternating current to high frequencies (HF), obtaining relatively clean products; that is to say, it hardly presents amorphous material neither sludges. They stand out the obtaining of carbon nano fibers (NFC) by means of a luminescent-arch discharge, in a gas mixture of He-CH 4 with 34% at. Ni/10.32% at.Y like catalyst; at a frequency of 42 kHz and low power (300 W). This method benefits the amass of the particles in both electrodes due to the high frequencies. The time of duration of the process oscillates between 5 and 20 minutes. The obtained product was characterized by scanning electron microscopy (MEB), transmission electron microscopy (MET) to determine the NEC type obtained and by X-ray diffraction analysis and Raman spectroscopy for determining the purity of the samples. The NFC is relatively free of amorphous coal. The surface and structural analysis indicates that the fibers have a half diameter of 80 nm. It is also made, a study by optical emission spectroscopy of plasma using the Swan band for determining the temperature. (Author)

Ion beams provided by small accelerators for material synthesis and characterization

Science.gov (United States)

Mackova, Anna; Havranek, Vladimir

2017-06-01

The compact, multipurpose electrostatic tandem accelerators are extensively used for production of ion beams with energies in the range from 400 keV to 24 MeV of almost all elements of the periodic system for the trace element analysis by means of nuclear analytical methods. The ion beams produced by small accelerators have a broad application, mainly for material characterization (Rutherford Back-Scattering spectrometry, Particle Induced X ray Emission analysis, Nuclear Reaction Analysis and Ion-Microprobe with 1 μm lateral resolution among others) and for high-energy implantation. Material research belongs to traditionally progressive fields of technology. Due to the continuous miniaturization, the underlying structures are far beyond the analytical limits of the most conventional methods. Ion Beam Analysis (IBA) techniques provide this possibility as they use probes of similar or much smaller dimensions (particles, radiation). Ion beams can be used for the synthesis of new progressive functional nanomaterials for optics, electronics and other applications. Ion beams are extensively used in studies of the fundamental energetic ion interaction with matter as well as in the novel nanostructure synthesis using ion beam irradiation in various amorphous and crystalline materials in order to get structures with extraordinary functional properties. IBA methods serve for investigation of materials coming from material research, industry, micro- and nano-technology, electronics, optics and laser technology, chemical, biological and environmental investigation in general. Main research directions in laboratories employing small accelerators are also the preparation and characterization of micro- and nano-structured materials which are of interest for basic and oriented research in material science, and various studies of biological, geological, environmental and cultural heritage artefacts are provided too.

Synthesis, Characterization and Applications in Catalysis of Polyoxometalate/Zeolite Composites

Directory of Open Access Journals (Sweden)

Frédéric Lefebvre

2016-05-01

Full Text Available An overview of the synthesis, characterization and catalytic applications of polyoxometalates/zeolites composites is given. The solids obtained by direct synthesis of the polyoxometalate in the presence of the zeolite are first described with their applications in catalysis. Those obtained by a direct mixing of the two components are then reviewed. In all cases, special care is taken in the localization of the polyoxometalate, inside the zeolite crystal, in mesopores or at the external surface of the crystals, as deduced from the characterization methods.

Alternative chemical-based synthesis routes and characterization of nano-scale particles

International Nuclear Information System (INIS)

Brocchi, E.A.; Motta, M.S.; Solorzano, I.G.; Jena, P.K.; Moura, F.J.

2004-01-01

Different nano-scale particles have been synthesized by alternative routes: nitrates dehydratation and oxide, or co-formed oxides, reduction by hydrogen. Chemical-based synthesis routes are described and thermodynamics studies and kinetics data are presented to support the feasibility for obtaining single-phase oxides and co-formed two-phase oxides. In addition, the reduction reaction has been applied to successfully produce metal/ceramic nanocomposites. Structural characterization has been carried out by means of X-ray diffraction and, more extensively, transmission electron microscopy operating in conventional diffraction contrast mode (CTEM) and high-resolution mode (HRTEM). Nano-scale size distribution of oxide particles is well demonstrated together with their defect-free structure in the lower range, around 20 nm, size. Structural features related to the synthesized nano-composites are also presented

Recent progress in the direct synthesis of hierarchical zeolites: synthetic strategies and characterization methods

KAUST Repository

Liu, Zhaohui

2017-06-16

Hierarchically structured zeolites combine the merits of microporous zeolites and mesoporous materials to offer enhanced molecular diffusion and mass transfer without compromising the inherent catalytic activities and selectivity of zeolites. This short review gives an introduction to the synthesis strategies for hierarchically structured zeolites with emphasis on the latest progress in the route of ‘direct synthesis’ using various templates. Several characterization methods that allow us to evaluate the ‘quality’ of complex porous structures are also introduced. At the end of this review, an outlook is given to discuss some critical issues and challenges regarding the development of novel hierarchically structured zeolites as well as their applications.

CsPb2Br5 Single Crystals: Synthesis and Characterization

KAUST Repository

Dursun, Ibrahim

2017-08-02

CsPb2Br5 is a ternary halogen-plumbate material with close characteristics to well-reported halide perovskites. Due to its unconventional two-dimensional structure, CsPb2Br5 is being looked at broadly for potential applications in optoelectronics. CsPb2Br5 investigations are currently limited to nanostructures and powder forms of the material, which present unclear and conflicting optical properties. In this study, we present the synthesis and characterization of CsPb2Br5 bulk single crystals, which enabled us to finally clarify the material\\'s optical features. Our CsPb2Br5 crystal has a two-dimensional structure with Pb2Br5- layers spaced by Cs+ cations, and exhibits a ~3.1 eV indirect bandgap with no emission in the visible spectrum.

Synthesis, characterization and antibacterial property of ZnO:Mg nanoparticles

Science.gov (United States)

Kompany, A.; Madahi, P.; Shahtahmasbi, N.; Mashreghi, M.

2012-09-01

Sol-gel method was successfully used for the synthesis of ZnO nanoparticles (NPs) doped with different concentrations of Mg and the structural, optical and antibacterial properties of the nanoparticles were studied. The synthesized ZnO:Mg powders were characterized using x-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transformation Infrared (FTIR) and UV-Vis spectroscopy. It was revealed that the samples have hexagonal Wurtzite structure, and the phase segregation takes place for 15% Mg content. TEM images show that the average size of the particles is about 50 nm. Also, the antibacterial activities of the nanoparticles were tested against Escherichia coli (Gram negative) cultures. ZnO:Mg nanofluid showed good antibacterial activity which increases with the increase of NPs concentration, and decreases slightly with the amount of Mg.

Synthesis, stability range and characterization of Pr2Cu2O5

Science.gov (United States)

Fernández-Sanjulián, Javier; Morán, Emilio; Ángel Alario-Franco, Miguel

2010-03-01

A novel Pr2Cu2O5 phase has been prepared under high-pressure and high-temperature conditions (P ∼6 GPa and T ∼1673 K) in a Belt-type apparatus and characterized by X-ray diffraction and electron microscopy. The crystal structure appears to be an orthorhombic "oxygen-deficient perovskite" (M.T. Anderson, J.T. Vaughey, and K.R. Poeppelmeier, Structural similarities among oxygen-deficient perovskites, Chem. Mater. 5 (1993), pp. 151-165) isostructural with La2Cu2O5 (J.F. Bringley, B.A. Scott, S.J. La Placa, R.F. Boheme, T.M. Shaw, M.W. McElfresh, S.S. Trail, and D.E. Cox, Synthesis of the defect perovskite series LaCuO 3-δ with copper valence varying from 2+to 3+, Nature 347 (1990), pp. 263-265) and Nd2Cu2O5 (B.-H. Chen, D. Walker, E. Suard, B.A. Scott, B. Mercey, M. Hervieu, and B. Raveau, High pressure synthesis of NdCuO3-δ perovskites (0≤δ≤0.5). Inorg. Chem. 34 (1995), pp. 2077-2083).

Synthesis and characterization of waterborne polyurethane acrylate copolymers

International Nuclear Information System (INIS)

Sultan, Misbah; Bhatti, Haq Nawaz; Zuber, Mohammad; Barikani, Mehdi

2013-01-01

Polyurethane acrylate copolymers were synthesized by emulsion polymerization process. To reduce the environmental hazards, organic solvents were replaced by eco-friendly aqueous system. Concentration of polyurethane and acrylate monomer was varied to investigate the effect of chemical composition on performance properties of copolymers. FTIR spectroscopy was used as a key tool to record the chemical synthesis route. The synthesized copolymer emulsions were characterized by evaluating their particle size, viscosity, dry weight content, chemical and water resistance. Thermal decomposition was studied by thermogravimetric analysis. Scanning electron microscope was used to visualize the morphological structure of copolymers. The experimental results indicate better polyurethane acrylate compatibility till the ratio of 30/70. However, these copolymers exhibited synergistic effects between the two polymers and revealed a remarkable improvement in numerous coating properties

Synthesis and Single Crystal Structures of Substituted-1,3-Selenazol-2-amines

Directory of Open Access Journals (Sweden)

Guoxiong Hua

2016-12-01

Full Text Available The synthesis and X-ray single crystal structures of a series of new 4-substituted-1,3-selenazol-2-amines is reported. The efficient preparation of these compounds was carried out by two-component cyclization of the selenoureas with equimolar amounts of α-haloketones. The selenoureas were obtained from the reaction of Woollins’ reagent with cyanamides, followed by hydrolysis with water. All new compounds have been characterized by IR spectroscopy, multi-NMR (1H, 13C, 77Se spectroscopy, accurate mass measurement and single crystal X-ray structure analysis.

Synthesis, characterization and crystal structure of 6-Chloro-4,4‧-dimethyl-2,2‧-bipyridine and 4,4‧-Dimethyl 2,2‧-bipyridine N-Oxide

Science.gov (United States)

Conterosito, Eleonora; Magistris, Claudio; Barolo, Claudia; Croce, Gianluca; Milanesio, Marco

2016-03-01

The synthesis, the NMR characterization and the crystal structure of 6-Chloro 4,4‧-dimethyl 2,2‧-bipyridine and of the reaction intermediate 4,4‧-Dimethyl 2,2‧-bipyridine N-Oxide are here reported. The target compound crystallizes in the orthorhombic system while the intermediate is monoclinic. In both structures, the molecules are linked by weak interactions. The structure of the reaction intermediate N-oxide is characterized by a dihedral angle between the two phenyl rings of 161.77° while the other is almost planar with a dihedral angle of 179.15°. The crystal packing was investigated, also with the aid of Hirshfeld surface analysis. In the N-oxide reaction intermediate the packing is governed by CH-O interactions, while in the product the packing is simply driven by minimizing the voids and thus maximizing the density, with a prevalence of H•••H and C•••H contacts, as indicated by fingerprint decomposition analysis.

Design and synthesis of diverse functional kinked nanowire structures for nanoelectronic bioprobes.

Science.gov (United States)

Xu, Lin; Jiang, Zhe; Qing, Quan; Mai, Liqiang; Zhang, Qingjie; Lieber, Charles M

2013-02-13

Functional kinked nanowires (KNWs) represent a new class of nanowire building blocks, in which functional devices, for example, nanoscale field-effect transistors (nanoFETs), are encoded in geometrically controlled nanowire superstructures during synthesis. The bottom-up control of both structure and function of KNWs enables construction of spatially isolated point-like nanoelectronic probes that are especially useful for monitoring biological systems where finely tuned feature size and structure are highly desired. Here we present three new types of functional KNWs including (1) the zero-degree KNW structures with two parallel heavily doped arms of U-shaped structures with a nanoFET at the tip of the "U", (2) series multiplexed functional KNW integrating multi-nanoFETs along the arm and at the tips of V-shaped structures, and (3) parallel multiplexed KNWs integrating nanoFETs at the two tips of W-shaped structures. First, U-shaped KNWs were synthesized with separations as small as 650 nm between the parallel arms and used to fabricate three-dimensional nanoFET probes at least 3 times smaller than previous V-shaped designs. In addition, multiple nanoFETs were encoded during synthesis in one of the arms/tip of V-shaped and distinct arms/tips of W-shaped KNWs. These new multiplexed KNW structures were structurally verified by optical and electron microscopy of dopant-selective etched samples and electrically characterized using scanning gate microscopy and transport measurements. The facile design and bottom-up synthesis of these diverse functional KNWs provides a growing toolbox of building blocks for fabricating highly compact and multiplexed three-dimensional nanoprobes for applications in life sciences, including intracellular and deep tissue/cell recordings.

Synthesis, characterization, and photocatalytic properties of core/shell mesoporous silica nanospheres supporting nanocrystalline titania

International Nuclear Information System (INIS)

Cendrowski, K.; Chen, X.; Zielinska, B.; Kalenczuk, R. J.; Rümmeli, M. H.; Büchner, B.; Klingeler, R.; Borowiak-Palen, E.

2011-01-01

The facile bulk synthesis of silica nanospheres makes them an attractive support for the transport of chemical compounds such as nanocrystalline titanium dioxide. In this contribution we present a promising route for the synthesis of mesoporous silica nanospheres (m-SiO 2 ) with diameter in range 200 nm, which are ideal supports for nanocrystalline titanium dioxide (TiO 2 ). The detailed microscopic and spectroscopic characterizations of core/shell structure (m-SiO 2 /TiO 2 ) were conducted. Moreover, the photocatalytic potential of the nanostructures was investigated via phenol decomposition and hydrogen generation. A clear enhancement of photoactivity in both reactions as compared to commercial TiO 2 -Degussa P25 catalyst is detected.

Synthesis, characterization, and photocatalytic properties of core/shell mesoporous silica nanospheres supporting nanocrystalline titania

Science.gov (United States)

Cendrowski, K.; Chen, X.; Zielinska, B.; Kalenczuk, R. J.; Rümmeli, M. H.; Büchner, B.; Klingeler, R.; Borowiak-Palen, E.

2011-11-01

The facile bulk synthesis of silica nanospheres makes them an attractive support for the transport of chemical compounds such as nanocrystalline titanium dioxide. In this contribution we present a promising route for the synthesis of mesoporous silica nanospheres (m-SiO2) with diameter in range 200 nm, which are ideal supports for nanocrystalline titanium dioxide (TiO2). The detailed microscopic and spectroscopic characterizations of core/shell structure (m-SiO2/TiO2) were conducted. Moreover, the photocatalytic potential of the nanostructures was investigated via phenol decomposition and hydrogen generation. A clear enhancement of photoactivity in both reactions as compared to commercial TiO2-Degussa P25 catalyst is detected.

Synthesis and Structure Characterization of Phenol-Urea-Formaldehyde Resins in the Presence of Magnesium Oxide as Catalyst

Directory of Open Access Journals (Sweden)

Dong-Bin Fan

2014-08-01

Full Text Available The objective of this research was to provide a useful approach of polymer synthesis for accelerating the fast cure of phenol-urea-formaldehyde (PUF resin as wood adhesive by optimizing its structure and composition. The PUF resins containing high contents of very reactive groups such as para-methylol groups were synthesized by reacting methylolurea, phenol, and formaldehyde in the presence of magnesium oxide (MgO as catalyst. The effects of synthesis parameters including F/(P + U, OH/P, and MgO/P mole ratios on the structure, composition, curing characteristics, and their relationships of PUF resins were investigated. The results indicated that MgO seemed to be an efficacious catalyst for PUF resin synthesis and promote its faster cure. The increase in the F/(P + U mole ratio or/and OH/P mole ratio appeared to be beneficial for the formation of para-methylol groups and cocondensed methylene linkages between phenolic methylol groups and urea units, and for the removal of unreacted urea. In case of Catalyst/P mole ratio, an appropriate dosage of added metal-ion was very important for synthesizing the high-content reactive groups of PUF resins, otherwise leading to the reverse effects.

Synthesis, characterization and behaviour of trans-bis (argininate) copper (II) to gamma radiation

International Nuclear Information System (INIS)

Pereira, A.B.

1984-01-01

The synthesis, the characterization and the behaviour to gamma radiation of trans-bis (argininate) copper (II) are presented. The synthesis is made from copper sulfate, sodium hydroxide and hydrochloride of L (+) arginine, in aqueous medium, and the characterization by infrared spectroscopy, visible and ultraviolet spectroscopy and elementary analysis. (C.G.C.)

Synthesis, characterization, and molecular structure of tetraethylammonium pentakis(isothiocyanato)bis(2,2'-bipyridine)uranate(IV)

International Nuclear Information System (INIS)

Wiley, R.O.; Von Dreele, R.B.; Brown, T.M.

1980-01-01

The synthesis of tetraethylammonium pentakis(isothiocyanato)bis(2,2'-bipyridine)uranate(IV) has been accomplished, and it was characterized by classical physical methods. The crystal and molecular structure was determined from single-crystal x-ray data collected by the theta-2theta technique on an automated diffractometer. The compound consists of pentakis(isothiocyanato)bis (2,2'-bipyridine)uranate(IV) anions and disordered tetraethylammonium cations. Uranium is bound to nine nitrogen atoms in a highly distorted monocapped square antiprism in which one bipyridine occupies a position bridging the cap and the near square while the other bipyridine spans the opposite edge of the far square. Distortion from the ideal geometry is caused by the small ligand bite of the bipyridine ligand. An alternative description of the coordination geometry is derived from the seven-coordinate pentagonal bipyramid in which each bipyridine ligand is assumed to occupy an axial position with the five thiocyanato ligands forming the pentagonal girdle. The U-N bond distances vary from 2.35 to 2.47 A for the thiocyanato ligands and from 2.61 to 2.65 A for the bipyridine ligands. The structure was solved by standard heavy-atom techniques and refined by large-block matrix least squares to a final R value of 0.083 for 3878 independent observed reflections. The compound crystallized in the monoclinic space group P2 1 /c, Z = 4, with lattice parameters a = 14.427 (10) A, b = 18.612 (17) A, c = 15.710 (10) A, and β = 105.17 (7) 0 , rho/sub obsd/ = 1.57 g cm -3

Combustion synthesis and structural characterization of Li–Ti mixed ...

Indian Academy of Sciences (India)

pared by combustion method at lower temperatures compared to the conventional high temperature sintering for ... Li–Ti mixed ferrites; combustion synthesis; hysteresis. 1. ... Quantum model - VSM 6000) at an applied field of ±10 kOe.

Non linear structures seismic analysis by modal synthesis

International Nuclear Information System (INIS)

Aita, S.; Brochard, D.; Guilbaud, D.; Gibert, R.J.

1987-01-01

The structures submitted to a seismic excitation, may present a great amplitude response which induces a non linear behaviour. These non linearities have an important influence on the response of the structure. Even in this case (local shocks) the modal synthesis method remains attractive. In this paper we will present the way of taking into account, a local non linearity (shock between structures) in the seismic response of structures, by using the modal synthesis method [fr

Bio-assisted synthesis and characterization of nanostructured bismuth (III) sulphide using Clostridium acetobutylicum

International Nuclear Information System (INIS)

Kamaraj, Sathish Kumar; Venkatachalam, Ganesh; Arumugam, Palaniappan; Berchmans, Sheela

2014-01-01

Nanostructured bismuth (III) sulphide is synthesized at room temperature using a hydrogen sulphide producing microorganism namely Clostridium acetobutylicum. On contrary to chemical routes involving both the high and room temperature methods, the present experimental procedure involves a bio-assisted approach. This method is free from the usage of toxic and hazardous chemicals making it an environment friendly route. The synthesized bismuth sulphide is characterized using transmission electron microscope (TEM), powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV). From our experiments we find that bismuth sulphide produced using this bio-assisted approach exhibits a hexagonal shaped plate-like structures and is stabilized by the extracellular proteins present in the culture medium. - Graphical abstract: A green chemistry approach towards the synthesis of bismuth (III) sulphide nanostructures at room temperature using a hydrogen sulphide producing microorganism namely, Clostridium acetobutylicum is demonstrated. - Highlights: • Environmentally benign (greener) route towards synthesis of Bi 2 S 3 nanostructures. • Bio-assisted synthesis of Bi 2 S 3 at room temperature using Clostridium acetobutylicum. • Extracellular proteins in H 2 S producing microorganism as stabilizer for Bi 2 S 3 NPs. • Hexagonal platelets of Bi 2 S 3 possessing an orthorhombic crystalline structure

Synthesis and atomic scale characterization of Er2O3 nanoparticles: enhancement of magnetic properties and changes in the local structure

Science.gov (United States)

Corrêa, Eduardo L.; Bosch-Santos, Brianna; Freitas, Rafael S.; Potiens, Maria da Penha A.; Saiki, Mitiko; Carbonari, Artur W.

2018-05-01

In the investigation reported in this paper a modified thermal decomposition method was developed to produce very small Er2O3 nanoparticles (NPs). Particles structure, shape and size were characterized by x-ray diffraction and transmission electron microscopy which showed that the synthesis by thermal decomposition under O2 atmosphere produced very small and monodisperse NPs, allowing the investigation of finite-size and surface effects. Results of magnetization measurements showed that the smallest particles present the highest values of susceptibility that decrease as particle size increases. Specific heat measurements indicate that the sample with the smallest NPs (diameter ∼5 nm) has a Néel temperature of 0.54 K. The local structure of particles was investigated by measurements of hyperfine interactions with perturbed angular correlation spectroscopy using 111Cd as probe nuclei replacing the cationic sites. Results showed that the relative population of sites 8b increases in both the core and surface layer of particles.

Synthesis and characterization of germa[n]pericyclynes.

Science.gov (United States)

Tanimoto, Hiroki; Nagao, Tomohiko; Nishiyama, Yasuhiro; Morimoto, Tsumoru; Iseda, Fumiyasu; Nagato, Yuko; Suzuka, Toshimasa; Tsutsumi, Ken; Kakiuchi, Kiyomi

2014-06-14

The synthesis and characterization of novel pericyclynes comprising germanium atoms and acetylenes, germa[n]pericyclynes, are described. The prepared germa[4]-, [6]-, and [8]pericyclynes were compared by (13)C NMR spectroscopy, X-ray crystallography, cyclic voltammetry, UV-visible spectroscopy, fluorescence emission spectroscopy, Raman spectroscopy, and density functional theory calculation analyses.

Synthesis and characterization of composites HoMn_1_-_x(Ni,Co)_xO_3

International Nuclear Information System (INIS)

Santos, Cassio Morilla dos

2011-01-01

In this work was accomplished the synthesis process and structural and magnetic characterization of HoMn_1_-_X(Ni,Co)_XO_3 compounds of perovskite structure. The samples synthesis were performed through modified polymeric precursor method. After synthesis and solvent removal, the polymer resin formed was treated at 350 deg C/4h for organic constituents removal, followed by heating treatment at 500 deg C/4h and 900 deg C/20h to obtain the crystalline phase. For structural characterization, it was used D10B-XPD beam line of Laboratorio Nacional de Luz Sincrotron (LNLS), where X-rays wavelengths below cobalt, manganese and nickel absorption edge, were used. The formation of HoNi_0_._5_0Mn_0_._5_0O_3, HoCo_0_._5_0Mn_0_._5_0O_3 and HoNi_0_._2_5Co_0_._2_5Mn_0_._5_0O_3 phases were observed by X-ray diffraction technique. By Rietveld refinement method for sample HoNi_0_._2_5Co_0_._2_5Mn_0_._5_0O_3, it was determined that cobalt and nickel had similar occupations at the top and bottom of unit cell, while the manganese preferentially occupied plan 002. The magnetic response of samples was studied through magnetization curves according to the temperature function and the applied magnetic field. The ZFC curves showed a paramagnetic response associated to holmium magnetic moment, and ferromagnetism, antiferromagnetism and ferrimagnetism coexistence, due to sublattices formed by transition metals. The FC curves evidenced the spin reversal phenomenon, associated to the interaction between the sublattice formed by transition metals with sublattices formed by rare-earth, considering a mechanism of antiferromagnetic exchange interaction. (author)

Synthesis and Characterization of High Aluminum Zeolite X from Technical Grade Materials

Directory of Open Access Journals (Sweden)

Seyed Kamal Masoudian

2013-06-01

Full Text Available Zeolites are widely used as ion exchangers, adsorbents, separation materials and catalyst due to their well-tailored and highly-reproducible structures; therefore, the synthesis of zeolite from low grade resources can be interested. In the present work, high aluminum zeolite X was prepared from mixing technical grade sodium aluminate and sodium silicate solutions at temperatures between 70°C and 100°C. The synthesized zeolite X was characterized by SEM and X-ray methods according to ASTM standard procedures. The results showed that aging of the synthesis medium at the room temperature considerably increased the selectivity of zeolite X formation. On the other hand, high temperature of reaction mixture during crystallization formed zeolite A in the product; therefore, it decreased the purity of zeolite X. In addition, it was found that increasing H2O/Na2O and decreasing Na2O/SiO2 molar ratios in the reaction mixture resulted product with higher purity. © 2013 BCREC UNDIP. All rights reservedReceived: 7th January 2013; Revised: 7th April 2013; Accepted: 19th April 2013[How to Cite: Masoudian, S. K., Sadighi, S., Abbasi, A. (2013. Synthesis and Characterization of High Alu-minum Zeolite X from Technical Grade Materials. Bulletin of Chemical Reaction Engineering & Catalysis, 8 (1: 54-60. (doi:10.9767/bcrec.8.1.4321.54-60][Permalink/DOI: http://dx.doi.org/10.9767/bcrec.8.1.4321.54-60] | View in  |

Synthesis and Structural Characterization of ZnS Quantum Dots

International Nuclear Information System (INIS)

Selim, H.; Khalil, M.M.H.; Al-Kotb, M.S.; Kotkata, M.F.; Amer, H.H.

2013-01-01

Zinc sulfide QDs have been synthesized via a simple reaction of Zn (CH 3 COO) 2 and Na 2 S in the presence of sodium dodecyl sulphate (SDS) acting as an anionic capping material. The structure as well as characterization of the synthesized materials has been studied by XRD, EDX, SEM, TEM, TGA and FT-IR spectroscopy. Analysis of the obtained results revealed products of zinc blende ZnS nanoparticles with an average size of 5.3±0.2 nm in diameter distributed spherically and uniformly. The UV-visible absorption spectrum of the synthesized ZnS nanoparticles reflects an energy gap of 4.30 eV

Synthesis and characterization of Ce doped MFI zeolite

International Nuclear Information System (INIS)

Kalita, Banani; Talukdar, Anup K.

2012-01-01

Highlights: ► Cerium was incorporated into the tetrahedral position of MFI zeolite structure. ► Unit cell volume increases with an increase of Ce content in the framework of MFI. ► A band at 310 nm in the UV–vis spectra indicates Ce incorporation in MFI structure. ► The mass loss (%) in the region 373–423 K decreases with increase of Ce in MFI. - Abstract: Ce doped MFI (mobil five) zeolites with different Si to (Ce + Al) and different Ce to Al ratios were synthesized by a hydrothermal synthesis method. All the samples were characterized by different techniques such as X-ray diffraction, Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), UV–vis diffuse reflectance spectroscopy (DRS) and scanning electron microscopy (SEM). The results showed that almost pure MFI phase was obtained in all cases with incorporation of cerium metal into the framework. The increase in unit cell parameters observed with an increase in Ce content is indicative of incorporation of Ce into the framework structure of microporous material MFI. Corroboration of the framework incorporation of Ce into the MFI zeolite structure was also obtained from the UV–vis DRS spectra by the presence of an absorption band at 280 nm. TGA and SEM of the samples provide complementary evidence for Ce incorporation into the framework MFI structure.

Synthesis & Characterization of New bis-Symmetrical Adipoyl ...

African Journals Online (AJOL)

Full Title: Synthesis and Characterization of New bis-Symmetrical Adipoyl, Terepthaloyl, Chiral Diimido-di-L-alanine Diesters and Chiral Phthaloyl-L-alanine Ester of Tripropoxy p-tert-Butyl Calix[4]arene and Study of Their Hosting Ability for Alanine and Na+. Bis-symmetrical tripropoxy p-tert-butyl calix[4]arene esters were ...

Synthesis and characterization of the natural and burned hydrotalcite

International Nuclear Information System (INIS)

Granados C, F.

2006-01-01

The synthesis and the structural and surface properties of the natural and burned hydrotalcite using salts of AlCl 3 and MgCl 2 .6H 2 O its were studied. Its were used those analysis of BET, IR, XRD, TGA and SEM to characterize these materials. The obtained product was identified as the natural or carbonated hydrotalcite of chemical formula Mg 6 Al 2 (OH) 16 CO 3 .4H 2 O. The hydrotalcite was roasted at 500 C during 5 h and the was obtained roasted hydrotalcite (HTC) that is a material of high selectivity toward the anions that it can be efficiently used as adsorbent material in studies of adsorption for the treatment of anionic radioactive waste present in watery solution. (Author)

Synthesis and structural characterization of actinide oxalate compounds

International Nuclear Information System (INIS)

Tamain, C.

2011-01-01

Oxalic acid is a well-known reagent to recover actinides thanks to the very low solubility of An(IV) and An(III) oxalate compounds in acidic solution. Therefore, considering mixed-oxide fuel or considering minor actinides incorporation in ceramic fuel materials for transmutation, oxalic co-conversion is convenient to synthesize mixed oxalate compounds, precursors of oxide solid solutions. As the existing oxalate single crystal syntheses are not adaptable to the actinide-oxalate chemistry or to their manipulation constrains in gloves box, several original crystal growth methods were developed. They were first validate and optimized on lanthanides and uranium before the application to transuranium elements. The advanced investigations allow to better understand the syntheses and to define optimized chemical conditions to promote crystal growth. These new crystal growth methods were then applied to a large number of mixed An1(IV)-An2(III) or An1(IV)-An2(IV) systems and lead to the formation of the first original mixed An1(IV)-An2(III) and An1(IV)-An2(IV) oxalate single crystals. Finally thanks to the first thorough structural characterizations of these compounds, single crystal X-ray diffraction, EXAFS or micro-RAMAN, the particularly weak oxalate-actinide compounds structural database is enriched, which is essential for future studied nuclear fuel cycles. (author) [fr

Polypyrrole-silver Nanocomposite: Synthesis and Characterization

OpenAIRE

D. M. Nerkar; S. V. Panse; S. P. Patil; S. E. Jaware; G. G. Padhye

2016-01-01

Polypyrrole-Silver (PPy-Ag) nanocomposite has been successfully synthesized by the chemical oxidative polymerization of pyrrole with iron (III) chloride as an oxidant, in the presence of a colloidal suspension of silver nanoparticles. Turkevich method (Citrate reduction method) was used for the synthesis of silver nanoparticles (Ag NPs). The silver nanoparticles were characterized by UV-Visible spectroscopy which showed an absorption band at 423 nm confirming the formation of nanoparticles. P...

Synthesis and Characterization of Colloidal Metal and Photovoltaic Semiconductor Nanocrystals

KAUST Repository

Abulikemu, Mutalifu

2014-11-05

Metal and semiconducting nanocrystals have received a great deal of attention from fundamental scientists and application-oriented researchers due to their physical and chemical properties, which differ from those of bulk materials. Nanocrystals are essential building blocks in the development of nanostructured devices for energy conversion. Colloidal metals and metal chalcogenides have been developed for use as nanocrystal inks to produce efficient solar cells with lower costs. All high-performing photovoltaic nanocrystals contain toxic elements, such as Pb, or scarce elements, such as In; thus, the production of solution-processable nanocrystals from earth-abundant materials using environmentally benign synthesis and processing methods has become a major challenge for the inorganic semiconductor-based solar field. This dissertation, divided into two parts, addresses several aspects of these emerging challenges. The first portion of the thesis describes the synthesis and characterization of nanocrystals of antimony sulfide, which is composed of non-scarce and non-toxic elements, and examines their performance in photovoltaic devices. The effect of various synthetic parameters on the final morphology is explored. The structural, optical and morphological properties of the nanocrystals were investigated, and Sb2S3 nanocrystal-based solid-state semiconductor-sensitized solar cells were fabricated using different deposition processes. We achieved promising power conversion efficiencies of 1.48%. The second part of the thesis demonstrates a novel method for the in situ synthesis and patterning of nanocrystals via reactive inkjet printing. The use of low-cost manufacturing approaches for the synthesis of nanocrystals is critical for many applications, including photonics and electronics. In this work, a simple, low-cost method for the synthesis of nanocrystals with minimum size variation and waste using reactive inkjet printing is introduced. As a proof of concept, the

Zinc acetylacetonate hydrate adducted with nitrogen donor ligands: Synthesis, spectroscopic characterization, and thermal analysis

Science.gov (United States)

Brahma, Sanjaya; Shivashankar, S. A.

2015-12-01

We report synthesis, spectroscopic characterization, and thermal analysis of zinc acetylacetonate complex adducted by nitrogen donor ligands, such as pyridine, bipyridine, and phenanthroline. The pyridine adducted complex crystallizes to monoclinic crystal structure, whereas other two adducted complexes have orthorhombic structure. Addition of nitrogen donor ligands enhances the thermal property of these complexes as that with parent metal-organic complex. Zinc acetylacetonate adducted with pyridine shows much higher volatility (106 °C), decomposition temperature (202 °C) as that with zinc acetylacetonate (136 °C, 220 °C), and other adducted complexes. All the adducted complexes are thermally stable, highly volatile and are considered to be suitable precursors for metal organic chemical vapor deposition. The formation of these complexes is confirmed by powder X-ray diffraction, Fourier transform infrared spectroscopy, mass spectroscopy, and elemental analysis. The complexes are widely used as starting precursor materials for the synthesis of ZnO nanostructures by microwave irradiation assisted coating process.

Synthesis and characterization of activated lithium fluoride with silver

International Nuclear Information System (INIS)

Encarnacion E, E. K.; Guerrero S, Z.; Reyes A, J.

2017-10-01

The present work shows part of the results obtained in the development of the research that has been carried out since 2015 entitled -Synthesis and characterization of new thermoluminescent materials for the radiation dosimetry and its applications in health-. In the development of this research, the synthesis of crystals of pure lithium fluoride (LiF) and activated with different concentrations of silver (LiF:Ag); synthesized samples are also presented using different temperatures, as well as varying the concentration of the solvent (water-ethanol). The synthesized materials were characterized through different techniques: scanning electron microscopy and X-ray diffraction. Specifically, the results of the calculation of the size of the LiF crystals are presented using the Scherrer equation. Within the results, a dependence on the size of the crystals is highlighted by means of the following factors: the amount of activator in the sample, the temperature at which the sample was synthesized, as well as the amount of solvent in the synthesis. The samples have a simple cubic crystalline phase. (Author)

Synthesis and characterization of nanostructured powders of hydroxyapatite and β-calcium phosphate

Energy Technology Data Exchange (ETDEWEB)

Prants, W.T.; Muller, D.T.; Orzechowski, L.G.; Feit, G.; Delima, S.A.; Camargo, N.H.A.; Gemelli, E., E-mail: w_prants@hotmail.com, E-mail: danielt_muller@yahoo.com.br, E-mail: sarahamindelima@hotmail.com, E-mail: dem2nhac@joinville.udesc.br, E-mail: gemelli@joinville.udesc.br [Universidade do Estado de Santa Catarina (UDESC), Joinville, SC (Brazil). Campus Universitario Prof. Avelino Marcante

2009-07-01

Biphasic calcium phosphate (BCP) bioceramics are composed in a general manner from a mixture between hydroxyapatite (HA), and β-calcium phosphate. In the recent years, the BCP bioceramics are pointed out in researches from regeneration and reconstitution in osseous tissue, in reason of their similar mineralogical characteristics of the human bone structure, as great biodegradation, absorption and formation of precocious osseous tissue. The biphasic materials (BCP) are detached for use in medical and dental application, as filling bone cavities, maxillofacial treatment, medicaments discharge for treatment cancerous osteomyelitis and antibiotics discharge related with orthopedic injuries reparation. The aim of this work focused in synthesis and characterization of hydroxyapatite and β-calcium phosphate. The presented results are related with the mineralogical characterization with X-ray diffraction, thermal behavior with Differential Scanning Calorimetry and Dilatometer. The Scanning Electronic Microscopy (SEM) was used to help in the morphological characterization of the nanostructured powders. (author)

Synthesis and characterization of nanostructured powders of hydroxyapatite and β-calcium phosphate

International Nuclear Information System (INIS)

Prants, W.T.; Muller, D.T.; Orzechowski, L.G.; Feit, G.; Delima, S.A.; Camargo, N.H.A.; Gemelli, E.

2009-01-01

Biphasic calcium phosphate (BCP) bioceramics are composed in a general manner from a mixture between hydroxyapatite (HA), and β-calcium phosphate. In the recent years, the BCP bioceramics are pointed out in researches from regeneration and reconstitution in osseous tissue, in reason of their similar mineralogical characteristics of the human bone structure, as great biodegradation, absorption and formation of precocious osseous tissue. The biphasic materials (BCP) are detached for use in medical and dental application, as filling bone cavities, maxillofacial treatment, medicaments discharge for treatment cancerous osteomyelitis and antibiotics discharge related with orthopedic injuries reparation. The aim of this work focused in synthesis and characterization of hydroxyapatite and β-calcium phosphate. The presented results are related with the mineralogical characterization with X-ray diffraction, thermal behavior with Differential Scanning Calorimetry and Dilatometer. The Scanning Electronic Microscopy (SEM) was used to help in the morphological characterization of the nanostructured powders. (author)

Synthesis and structural characterization of amorphous alloys of the Fe-Ni-B type

International Nuclear Information System (INIS)

Cabral P, A.; Jimenez B, J.; Garcia S, I.

2004-01-01

It was prepared the alloy FeNiB for chemical reduction, using four p H values (5, 6, 7 and 7.5). To p H=6 partially oxidized particles were obtained, between 16 and 20%. In the synthesis to other p H values, the obtained particles were highly oxidized (65-90%) according to the X-ray diffraction results, in all the preparations the particles were partially crystallized, with crystal size that varied between 4 and 10 nm. The structure of these particles can be consider that they are formed by a nucleus due to the alloy and an oxide armor recovering it. (Author)

Synthesis and characterization of noble metal–titania core–shell nanostructures with tunable shell thickness

Directory of Open Access Journals (Sweden)

Bartosz Bartosewicz

2017-10-01

Full Text Available Core–shell nanostructures have found applications in many fields, including surface enhanced spectroscopy, catalysis and solar cells. Titania-coated noble metal nanoparticles, which combine the surface plasmon resonance properties of the core and the photoactivity of the shell, have great potential for these applications. However, the controllable synthesis of such nanostructures remains a challenge due to the high reactivity of titania precursors. Hence, a simple titania coating method that would allow better control over the shell formation is desired. A sol–gel based titania coating method, which allows control over the shell thickness, was developed and applied to the synthesis of Ag@TiO2 and Au@TiO2 with various shell thicknesses. The morphology of the synthesized structures was investigated using scanning electron microscopy (SEM. Their sizes and shell thicknesses were determined using tunable resistive pulse sensing (TRPS technique. The optical properties of the synthesized structures were characterized using UV–vis spectroscopy. Ag@TiO2 and Au@TiO2 structures with shell thickness in the range of ≈40–70 nm and 90 nm, for the Ag and Au nanostructures respectively, were prepared using a method we developed and adapted, consisting of a change in the titania precursor concentration. The synthesized nanostructures exhibited significant absorption in the UV–vis range. The TRPS technique was shown to be a very useful tool for the characterization of metal–metal oxide core–shell nanostructures.

SYNTHESIS AND CHARACTERIZATION OF N, N'-BIS-(3 ...

African Journals Online (AJOL)

user

base complexes derived from Salicylaldehyde and histidine with some divalent transition metal ions. Furthermore, Syed (1993) reported the synthesis, characterization and biological evaluation of some. Schiff base metal complexes derived from Anthranilic acid-sugar and naturally occurring amino acid-sugar. Schiff bases ...

Synthesis, Characterization and Application of Multiscale Porous Materials

Energy Technology Data Exchange (ETDEWEB)

Hussami, Linda

2010-07-01

This thesis work brings fresh insights and improved understanding of nano scale materials through introducing new hybrid composites, 2D hexagonal in MCM-41 and 3D random interconnected structures of different materials, and application relevance for developing fields of science, such as fuel cells and solar cells. New types of porous materials and organometallic crystals have been prepared and characterized in detail. The porous materials have been used in several studies: as hosts to encapsulate metal-organic complexes; as catalyst supports and electrode materials in devices for alternative energy production. The utility of the new porous materials arises from their unique structural and surface chemical characteristics as demonstrated here using various experimental and theoretical approaches. New single crystal structures and arene-ligand exchange properties of f-block elements coordinated to ligand arene and halogallates are described in Paper I. These compounds have been incorporated into ordered 2D-hexagonal MCM-41 and polyhedral silica nano foam (PNF-SiO{sub 2}) matrices without significant change to the original porous architectures as described in Paper II and III. The resulting inorganic/organic hybrids exhibited enhanced luminescence activity relative to the pure crystalline complexes. A series of novel polyhedral carbon nano foams (PNF-C's) and inverse foams were prepared by nano casting from PNF-SiO{sub 2}'s. These are discussed in Paper IV. The synthesis conditions of PNF-C's were systematically varied as a function of the filling ratio of carbon precursor and their structures compared using various characterization methods. The carbonaceous porous materials were further tested in Paper V and VI as possible catalysts and catalyst supports in counter- and working electrodes for solar- and fuel cell applications

Synthesis and characterization of ceramics BNO (BiNbO4) added to 10% of CuO

International Nuclear Information System (INIS)

Sales, A.J.M.; Silva, P.M.O.; Rodrigues Junior, C.A.; Sombra, A.S.B.

2012-01-01

The study of the synthesis and structural characterization of ceramic BiNbO4 and behavior of density when added 10% by weight of CuO, with a view to applications in ceramic capacitors, are presented in this work. The BiNbO4 was prepared by conventional ceramic method. The milled powders were calcined for 2 hours at 850 °C for 3 hours and characterized by using a diffractometer Rigaku DMAXB of Co-α radiation. A more detailed characterization by XRD was performed using the program DBWS9807a using the Rietveld refinement of crystal structures, which confirmed the achievement of the α-BNO phase with orthorhombic structure. Were produced buks with the calcined powder, they were sintered at 925 °C. In order to study the grain morphology and distribution of pores in the ceramic body, the surface of the sample by adding 10% of CuO was analyzed by Scanning Electron Microscopy which confirmed a better densification. (author)

Synthesis and characterization of cobalt sulfide nanoparticles by sonochemical method

Science.gov (United States)

Muradov, Mustafa B.; Balayeva, Ofeliya O.; Azizov, Abdulsaid A.; Maharramov, Abel M.; Qahramanli, Lala R.; Eyvazova, Goncha M.; Aghamaliyev, Zohrab A.

2018-03-01

Convenient and environmentally friendly synthesis of Co9S8/PVA, CoxSy/EG and CoxSy/3-MPA nanocomposites were carried out in the presence of ultrasonic irradiation by the liquid phase synthesis of the sonochemical method. For the synthesis, cobalt acetate tetrahydrate [Co(CH3COO)2·4H2O] and sodium sulfide (Na2S·9H2O) were used as a cobalt and sulfur precursor, respectively. Polyvinyl alcohol (PVA), ethylene glycol (EG) and 3-mercaptopropionic acid (3-MPA) were used as a capping agent and surfactant. The structural, optical properties and morphology of nanocomposites were characterized using X-ray diffractometer (XRD), Ultraviolet/Visible Spectroscopy (UV-Vis), Fourier-transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The optical band gap of Co9S8/PVA is 1.81 eV and for CoxSy/EG is 2.42 eV, where the direct band gap of bulk cobalt sulfide is (0.78-0.9 eV). The wide band gap indicates that synthesised nanocomposites can be used in the fabrication of optical and photonic devices. The growth mechanisms of the Co9S8, CoS2 and Co3S4 nanoparticles were discussed by the reactions. The effects of sonication time and annealing temperature on the properties of the nanoparticles have been studied in detail.

Synthesis and Physicochemical Characterization of Mesoporous SiO2 Nanoparticles

Directory of Open Access Journals (Sweden)

Dharani Das

2014-01-01

Full Text Available There exists a knowledge gap in understanding potential toxicity of mesoporous silica nanoparticles. A critical step in assessing toxicity of these particles is to have a wide size range with different chemistries and physicochemical properties. There are several challenges when synthesizing mesoporous silica nanoparticles over a wide range of sizes including (1 nonuniform synthesis protocols using the same starting materials, (2 the low material yield in a single batch synthesis (especially for particles below 60–70 nm, and (3 morphological instability during surfactant removal process and surface modifications. In this study, we synthesized a library of mesoporous silica nanoparticles with approximate particle sizes of 25, 70, 100, 170, and 600 nm. Surfaces of the silica nanoparticles were modified with hydrophilic-CH2–(CH22–COOH and relatively hydrophobic-CH2–(CH210–COOH functional groups. All silica nanoparticles were analysed for morphology, surface functionality, surface area/pore volume, surface organic content, and dispersion characteristics in liquid media. Our analysis revealed the synthesis of a spectrum of monodisperse bare and surface modified mesoporous silica nanoparticles with a narrow particle size distribution and devoid of cocontaminants critical for toxicity studies. Complete physicochemical characterization of these synthetic mesoporous silica nanoparticles will permit systematic toxicology studies for investigation of structure-activity relationships.

Synthesis and characterization of reactions by nanoferrites Co2Fe2O4 combustion

International Nuclear Information System (INIS)

Santos, P.T.A.; Dantas, B.B.; Costa, A.C.F.M.; Araujo, P.M.A.G.

2012-01-01

In this work CoFe 2 O 4 of magnetic nanoparticles were synthesized by combustion reaction and the structural and morphological characteristics of the synthesized samples as well as the parameters of synthesis temperature and reaction time were investigated in order to assess the reproducibility of the synthesis. The maximum temperature and time of the combustion flame were obtained with pyrometer coupled to a computer with online measurement and a stopwatch. The resulting samples were characterized by X-ray diffraction (XRD), infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The maximum temperature achieved during synthesis for all reactions ranged from 623 deg C and 755 deg C. The combustion flame time varied between 18 and 23 seconds. The XRD showed the formation of only CoFe 2 O 4 inverse spinel phase, with crystallite size 28 nm and crystallinity 78%, with typical morphology of the formation of agglomerates of uniform size, brittle and comprising nanoparticles together by weak forces. (author)

On-Surface Synthesis and Characterization of Honeycombene Oligophenylene Macrocycles.

Science.gov (United States)

Chen, Min; Shang, Jian; Wang, Yongfeng; Wu, Kai; Kuttner, Julian; Hilt, Gerhard; Hieringer, Wolfgang; Gottfried, J Michael

2017-01-24

We report the on-surface formation and characterization of [30]-honeycombene, a cyclotriacontaphenylene, which consists of 30 phenyl rings (C 180 H 120 ) and has a diameter of 4.0 nm. This shape-persistent, conjugated, and unsubstituted hexagonal hydrocarbon macrocycle was obtained by solvent-free synthesis on a silver (111) single-crystal surface, making solubility-enhancing alkyl side groups unnecessary. Side products include strained macrocycles with square, pentagonal, and heptagonal shape. The molecules were characterized by scanning tunneling microscopy and density functional theory (DFT) calculations. On the Ag(111) surface, the macrocycles act as molecular quantum corrals and lead to the confinement of surface-state electrons inside the central cavity. The energy of the confined surface state correlates with the size of the macrocycle and is well described by a particle-in-the-box model. Tunneling spectroscopy suggests conjugation within the planar rings and reveals influences of self-assembly on the electronic structure. While the adsorbed molecules appear to be approximately planar, the free molecules have nonplanar conformation, according to DFT.

Synthesis and characterization of PMMA/clay nanocomposites prepared by in situ polymerization assisted by sonication

International Nuclear Information System (INIS)

Prado, Bruna R.; Bartoli, Julio R.; Ito, Edson N.

2015-01-01

In this work is presented the synthesis of nanocomposites of poly(methyl methacrylate), PMMA, with organically montmorillonite (OMMT) modified clays by in situ polymerization assisted by sonication. A statistically designed experiment was used, central composing design (CCD), to study the effect of synthesis variables on the dispersion of nanoparticles in PMMA matrix. The processing and formulation factors studied were: energy of sonication and Flory-Huggins interaction parameter between PMMA and organoclay. The structural (XRD) and morphological (TEM) characterizations of the PMMA/OMMT nanocomposites are compared with the literature. It was observed significant exfoliation of OMMT modified with hydroxyl groups in the nanocomposites of PMMA, mainly at the low ultrasonic energy level (90 and 105 kJ) studied. (author)

Synthesis and characterization of bimetallic metal-organic framework Cu-Ru-BTC with HKUST-1 structure.

Science.gov (United States)

Gotthardt, Meike A; Schoch, Roland; Wolf, Silke; Bauer, Matthias; Kleist, Wolfgang

2015-02-07

The bimetallic metal-organic framework Cu-Ru-BTC with the stoichiometric formula Cu2.75Ru0.25(BTC)2·xH2O, which is isoreticular to HKUST-1, was successfully prepared in a direct synthesis using mild reaction conditions. The partial substitution of Cu(2+) by Ru(3+) centers in the paddlewheel structure and the absence of other Ru-containing phases was proven using X-ray absorption spectroscopy.

Synthesis and characterization of zeolite material from coal ashes modified by surfactant

International Nuclear Information System (INIS)

Fungaro, D.A.; Borrely, S.I.

2010-01-01

Coal ash was used as starting material for zeolite synthesis by means of hydrothermal treatment. The surfactant-modified zeolite (SMZ) was prepared by adsorbing the cationic surfactant hexadecyltrimethylammonium bromide (HDTMA-Br) on the external surface of the zeolite from coal ash. The zeolite structure stability was monitored during the characterization of the materials by FTIR, XDR and SEM. The structural parameters of surfactant-modified zeolite are very close to that of corresponding non-modified zeolite which indicates that the crystalline nature of the zeolite remained intact after required chemical treatment with HDTMA-Br molecules and heating treatment for drying. The most intense peaks in the FTIR spectrum of HDTMA-Br were observed in SMZ spectrum confirming adsorption of surfactant on zeolites. (author)

Synthesis and characterization of intercalated polyaniline-clay nanocomposite using supercritical CO2

Science.gov (United States)

Abdelraheem, A.; El-Shazly, A. H.; Elkady, M. F.

2018-05-01

Lately, supercritical CO2 (SCCO2) have been getting great interest. It can be used in numerous applications because it is environmentally friendly, safe, comparatively low cost, and nonflammable. One of its applications is being a solvent in the synthesis of polymeric-clay nanocomposite. In this paper, intercalated polyaniline-clay nanocomposite (PANC) was prepared using SCCO2. The intercalation structure of polyaniline chains between clay layers was verified by various characterization techniques. Scanning electron microscope and transmission electron microscope (SEM-TEM) were used to show the morphology of the synthesized nanocomposite. The molecular structure of PANC nanocomposite was confirmed using Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD). The BET surface area and the conductivity of the nanocomposite were determined.

Synthesis, spectroscopic, biological activity and thermal characterization of ceftazidime with transition metals

Science.gov (United States)

Masoud, Mamdouh S.; Ali, Alaa E.; Elasala, Gehan S.; Kolkaila, Sherif A.

2018-03-01

Synthesis, physicochemical characterization and thermal analysis of ceftazidime complexes with transition metals (Cr(III), Mn(II), Fe(III), Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Hg(II)) were discussed. It's obtained that ceftazidime act as bidentate ligand. From magnetic measurement and spectral data, octahedral structures were proposed for all complexes except for cobalt, nickel and mercury had tetrahedral structural. Hyper chemistry program confirmed binding sites of ceftazidime. Ceftazidime complexes show higher activity than ceftazidime for some strains. From TG and DTA curves the thermal decomposition mechanisms of ceftazidime and their metal complexes were suggested. The thermal decomposition of the complexes ended with the formation of metal oxides as a final product except in case of Hg complex.

Synthesis and characterization of reactive dye-cassava mesocarp ...

African Journals Online (AJOL)

The synthesis of triazine based reactive dyes was carried out. The resultant dyes were characterized by thin layers chromatography, molecular weight, infrared and ultra- violet spectroscopy, and used in dyeing cassava mesocarp to produce dye modified cellulosic substrates. The dyed substrates were tested for dye fixation, ...

Synthesis and characterization of new optically active poly(amide ...

African Journals Online (AJOL)

Synthesis and characterization of new optically active poly(amide-imide)s based on N -trimellitimido- ... Bulletin of the Chemical Society of Ethiopia ... (DMAc), dimethyl sulfoxide (DMSO) and N-methyl-2-pyrrolidone (NMP) at room temperature.

Selective synthesis and characterization of chlorins as sensitizers for photodynamic therapy

Science.gov (United States)

Montforts, Franz-Peter; Kusch, Dirk; Hoper, Frank; Braun, Stefan; Gerlach, Benjamin; Brauer, Hans-Dieter; Schermann, Guido; Moser, Joerg G.

1996-04-01

Chlorin type sensitizers have ideal photophysical properties for an application in PDT. The basic chlorin framework of these sensitizers has to be modified by attachment of lipophilic and hydrophilic residues to achieve a good cell uptake and tumor enrichment. In the present study we describe the selective synthesis of amphiphilic chlorins starting from the readily accessible red blood pigment heme. The photophysical properties of the well defined synthetic chlorins are characterized by photophysical investigations. The kinetic of cell uptake, the localization in the cell and the photodynamic behavior of the amphiphilic sensitizers are demonstrated by incubation of A 375 cancer cell lines with structurally different chlorins.

Ultrafine Magnetite Nanopowder: Synthesis, Characterization, and Preliminary Use as Filler of Polymethylmethacrylate Nanocomposites

Directory of Open Access Journals (Sweden)

Pietro Russo

2012-01-01

Full Text Available Magnetite (Fe3O4 nanoparticles prepared by microwave-assisted hydrothermal synthesis have been characterized in terms of morphological and structural features. Electron micrographs collected in both scanning (SEM and transmission (TEM modes and evaluations of X-ray powder diffraction (XRD patterns have indicated the achievement of a monodispersed crystallite structure with particles having an average size around 15–20 nm. Structural investigations by Micro-Raman spectroscopy highlighted the obtainment of magnetite nanocrystals with a partial surface oxidation to maghemite (γ-Fe3O4. Preliminary attention has been also paid to the use of these magnetite nanoparticles as filler for a commercial polymethylmethacrylate resin. Hybrid formulations containing up to 3 wt% of nanoparticles were prepared by melt blending and characterized by calorimetric and thermogravimetric tests. For sake of comparison, same formulations containing commercial Fe3O4 nanoparticles are also reported. Calorimetric characterization indicates an increase of both glass transition temperature and thermal stability of the nanocomposite systems when loaded with the synthesized magnetite nanoparticles rather then loaded with the same amount of commercial Fe3O4. This first observation represents just one aspect of the promising potentiality offered by the novel magnetic nanoparticles when mixed with PMMA.

Synthesis and thermoluminescent characterization of LiF doped with Ag; Sintesis y caracterizacion termoluminiscente de LiF dopado con Ag

Energy Technology Data Exchange (ETDEWEB)

Encarnacion, E. K.; Reyes, J.; Guerrero, Z. [Universidad Autonoma de Santo Domingo, Facultad de Ciencias, Ciudad Universitaria, Santo Domingo (Dominican Republic); Sosa, M. A.; Vallejo, M. A.; Rivera P, E., E-mail: emma.kee@gmail.com [Universidad de Guanajuato, Campus Leon, Division de Ciencias e Ingenierias, Loma del Bosque 103, Col. Lomas del Campestre, 37150 Leon, Guanajuato (Mexico)

2015-10-15

Full text: In this paper the synthesis and characterization of lithium fluoride (LiF) crystals pure and activated with silver (Ag) is reported. The synthesis was carried out by the method of co-precipitation; three samples were obtained one of pure LiF and two were activated with 0.02 and 0.04% of Ag. All samples were subjected to X-ray emission and the results were analyzed. The synthesized samples were characterized by X-ray diffraction, thermoluminescence and X-ray fluorescence. The XRD results show complete crystal structures. The radiation dosimetry responses are discussed. These are the first results of a research conducted at the Universidad Autonoma de Santo Domingo in collaboration with the Universidad de Guanajuato. (Author)

Relation between structural evolution and effective Ir moments upon applied pressure during synthesis in Ba{sub 3}YIr{sub 2}O{sub 9}

Energy Technology Data Exchange (ETDEWEB)

Stummer, Hannes; Dey, Tusharkanti; Wurmehl, Sabine; Buechner, Bernd [Leibniz Institute for Solid State and Materials Research, Dresden (Germany)

2015-07-01

The intensively investigated material class of Iridium oxide based materials provides a variety of new and unknown combinations of magnetic properties with interesting novel or exotic ground states. These Iridate compounds often appear in a perovskite type structure or a related derivative which are very favorable for crystal structure modifications under high pressure. High pressure synthesis therefore can be used to tune or change the magnetic properties appearing under normal pressure. The Iridate Ba{sub 3}YIr{sub 2}O{sub 9} crystallizes under ambient pressure synthesis in a hexagonal structure and exhibits magnetic ordering below 4 K. A synthesis pressure of 8 GPa advances the material to form a cubic double perovskite structure which is (meta-)stable at ambient pressure. For this high pressure configuration the magnetic ordering is suppressed. We will present our recent results about the systematic high pressure synthesis and characterization of Ba{sub 3}YIr{sub 2}O{sub 9} samples grown under different growth pressure. The main focus will be on the correlation between structural and magnetic properties depending on the applied pressure during the synthesis process.

Synthesis, Crystal structure and Characterization of a New Oxalate ...

Indian Academy of Sciences (India)

in a slightly distorted octahedral environment, by two O atoms from two water molecules and four O atoms of two oxalate anions acting as chelating ligands. ... component for building up supramolecular systems and for participating in hydrogen bonding ... heating rate of 10◦C min−1. 2.2 Synthesis of the complex. Aqueous ...

Structure of human DNA polymerase iota and the mechanism of DNA synthesis.

Science.gov (United States)

Makarova, A V; Kulbachinskiy, A V

2012-06-01

Cellular DNA polymerases belong to several families and carry out different functions. Highly accurate replicative DNA polymerases play the major role in cell genome replication. A number of new specialized DNA polymerases were discovered at the turn of XX-XXI centuries and have been intensively studied during the last decade. Due to the special structure of the active site, these enzymes efficiently perform synthesis on damaged DNA but are characterized by low fidelity. Human DNA polymerase iota (Pol ι) belongs to the Y-family of specialized DNA polymerases and is one of the most error-prone enzymes involved in DNA synthesis. In contrast to other DNA polymerases, Pol ι is able to use noncanonical Hoogsteen interactions for nucleotide base pairing. This allows it to incorporate nucleotides opposite various lesions in the DNA template that impair Watson-Crick interactions. Based on the data of X-ray structural analysis of Pol ι in complexes with various DNA templates and dNTP substrates, we consider the structural peculiarities of the Pol ι active site and discuss possible mechanisms that ensure the unique behavior of the enzyme on damaged and undamaged DNA.

SYNTHESIS, CHARACTERIZATION, AND CRYSTAL STRUCTURE ...

African Journals Online (AJOL)

a

KEY WORDS: Barium, Crystal structure, 2,6-Pyridinedicarboxylic acid .... The rational design of novel metal-organic frameworks has attracted great ..... Bond, A.D.; Jones, W. Supramolecular Organization and Materials Design, Jones, W.; Rao,.

Nanoparticles of the superconductor MgB2: structural characterization and in situ study of synthesis kinetics

International Nuclear Information System (INIS)

Cui Chunxiang; Liu Debao; Shen Yutian; Sun Jinbin; Meng Fanbin; Wang Ru; Liu Shuangjin; Greer, A.L.; Chen, S.K.; Glowacki, B.A.

2004-01-01

Single-crystal MgB 2 nanoparticles, with diameters in the range 20-100 nm, have been synthesized in situ in the sample chamber of an X-ray diffractometer. The reaction kinetics are analyzed and related to the atomic-level structure of the particles as observed by high-resolution electron microscopy. Synthesis conditions may have a significant influence on microstructure and superconducting properties

Synthesis and characterization of new ionic liquids; Sintese e caracterizacao de novos liquidos ionicos

Energy Technology Data Exchange (ETDEWEB)

Oliveira, L.M.C. de; Mattedi, S.; Boaventura, J.S., E-mail: luanaufrn@hotmail.co [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Escola Politecnica. Programa de Pos-Graduacao em Engenharia Quimica; Iglesias, M. [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Escola Politecnica. Programa de Pos-Graduacao em Engenharia Quimica; Universidad de Santiago de Compostela (Spain). Escuela Tecnica Superior de Ingenieria. Dept. de Ingenieria Quimica

2010-07-01

In recent years, ionic liquids have been highlighted for its potential in various industrial applications. Among them, the salts of Broensted has a promising profile for the low toxicity, low cost and simple synthesis. This paper presents the synthesis and characterization of new salts of Bronsted with branched (lactate) or large chain anions (oleate) for future use as additives promoters of proton conductivity in fuel cells of ethanol. Experimental data were measured for density, sound velocity and conductivity of pure ionic liquids and mixtures. The density decreases linearly with increasing temperature, and sound velocity shows a similar trend, but not linear. The conductivity increases according to the Arrhenius model with activation energy less than 10 J/mol. Tests NMR, FTIR and TGA confirm ionic structure and thermal stability up to 165 deg C. (author)

Synthesis and characterization of cadmium doped lead–borate ...

Indian Academy of Sciences (India)

Unknown

Mater. Sci., Vol. 29, No. 1, February 2006, pp. 55–58. © Indian Academy of Sciences. 55. Synthesis and characterization of cadmium doped lead–borate glasses. A A ALEMI*, H SEDGHI†, A R MIRMOHSENI and V GOLSANAMLU. Department of Inorganic Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, Iran.

Copper nanoparticles mediated by chitosan: synthesis and characterization via chemical methods.

Science.gov (United States)

Usman, Muhammad Sani; Ibrahim, Nor Azowa; Shameli, Kamyar; Zainuddin, Norhazlin; Yunus, Wan Md Zin Wan

2012-12-14

Herein we report a synthesis of copper nanoparticles (Cu-NPs) in chitosan (Cts) media via a chemical reaction method. The nanoparticles were synthesized in an aqueous solution in the presence of Cts as stabilizer and CuSO(4)·5H(2)O precursor. The synthesis proceeded with addition of NaOH as pH moderator, ascorbic acid as antioxidant and hydrazine( )as the reducing agent. The characterization of the prepared NPs was done using ultraviolet-visible spectroscopy, which showed a 593 nm copper band. The Field Emission Scanning Electron Microscope (FESEM) images were also observed, and found to be in agreement with the UV-Vis result, confirming the formation of metallic Cu-NPs. The mean size of the Cu-NPs was estimated to be in the range of 35-75 nm using X-ray diffraction. XRD was also used in analysis of the crystal structure of the NPs. The interaction between the chitosan and the synthesized NPs was studied using Fourier transform infrared (FT-IR) spectroscopy, which showed the capping of the NPs by Cts.

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.

Nanocrystalline hydroxyapatite doped with magnesium and zinc: Synthesis and characterization

Energy Technology Data Exchange (ETDEWEB)

Kalita, Samar J. [Department of Mechanical, Materials and Aerospace Engineering, University of Central Florida, Orlando, FL 32816-2450 (United States)]. E-mail: samar@mail.ucf.edu; Bhatt, Himesh A. [Department of Mechanical, Materials and Aerospace Engineering, University of Central Florida, Orlando, FL 32816-2450 (United States)

2007-05-16

During recent years, there have been efforts in developing nanocrystalline bioceramics, to enhance their mechanical and biological properties for use in tissue engineering applications. In this research, we made an attempt to synthesize nanocrystalline bioactive hydroxyapatite (Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}, HAp) ceramic powder in the lower-end of nano-range (2-10 nm), using a simple low-temperature sol-gel technique and studied its densification behavior. We further studied the effects of metal ion dopants during synthesis on powder morphology, and the properties of the sintered structures. Calcium nitrate and triethyl phosphite were used as precursors for calcium and phosphorous, respectively, for sol-gel synthesis. Calculated quantities of magnesium oxide and zinc oxide were incorporated as dopants into amorphous dried powder, prior to calcination at 250-550 {sup o}C. The synthesized powders were analyzed for their phases using X-ray diffraction technique and characterized for powder morphology and particle size using transmission electron microscopy (TEM). TEM analysis showed that the average particle size of the synthesized powders were in the range of 2-10 nm. The synthesized nano-powders were uniaxially compacted and then sintered at 1250 {sup o}C and 1300 {sup o}C for 6 h, separately, in air. A maximum average sintered density of 3.29 g/cm{sup 3} was achieved in structures sintered at 1300 {sup o}C, developed from nano-powder doped with magnesium. Vickers hardness testing was performed to determine the hardness of the sintered structures. Uniaxial compression tests were performed to evaluate the mechanical properties. Bioactivity and biodegradation behavior of the sintered structures were assessed in simulated body fluid (SBF) and maintained in a dynamic state.

Synthesis of a mixed-valent tin nitride and considerations of its possible crystal structures

International Nuclear Information System (INIS)

Caskey, Christopher M.; Holder, Aaron; Christensen, Steven T.; Biagioni, David; Ginley, David S.; Tumas, William; Perkins, John D.; Lany, Stephan; Zakutayev, Andriy; Shulda, Sarah; Diercks, David; Pylypenko, Svitlana; Richards, Ryan M.; Schwartz, Craig P.; Nordlund, Dennis; Kukliansky, Alon; Natan, Amir; Prendergast, David; Sun, Wenhao; Orvananos, Bernardo

2016-01-01

Recent advances in theoretical structure prediction methods and high-throughput computational techniques are revolutionizing experimental discovery of the thermodynamically stable inorganic materials. Metastable materials represent a new frontier for these studies, since even simple binary non-ground state compounds of common elements may be awaiting discovery. However, there are significant research challenges related to non-equilibrium thin film synthesis and crystal structure predictions, such as small strained crystals in the experimental samples and energy minimization based theoretical algorithms. Here, we report on experimental synthesis and characterization, as well as theoretical first-principles calculations of a previously unreported mixed-valent binary tin nitride. Thin film experiments indicate that this novel material is N-deficient SnN with tin in the mixed II/IV valence state and a small low-symmetry unit cell. Theoretical calculations suggest that the most likely crystal structure has the space group 2 (SG2) related to the distorted delafossite (SG166), which is nearly 0.1 eV/atom above the ground state SnN polymorph. This observation is rationalized by the structural similarity of the SnN distorted delafossite to the chemically related Sn 3 N 4 spinel compound, which provides a fresh scientific insight into the reasons for growth of polymorphs of metastable materials. In addition to reporting on the discovery of the simple binary SnN compound, this paper illustrates a possible way of combining a wide range of advanced characterization techniques with the first-principle property calculation methods, to elucidate the most likely crystal structure of the previously unreported metastable materials.

Synthesis of a mixed-valent tin nitride and considerations of its possible crystal structures

Energy Technology Data Exchange (ETDEWEB)

Caskey, Christopher M. [National Renewable Energy Laboratory, Golden, Colorado 80401 (United States); Colorado School of Mines, Golden, Colorado 80401 (United States); Larix Chemical Science, Golden, Colorado 80401 (United States); Holder, Aaron; Christensen, Steven T.; Biagioni, David; Ginley, David S.; Tumas, William; Perkins, John D.; Lany, Stephan; Zakutayev, Andriy, E-mail: andriy.zakutayev@nrel.gov [National Renewable Energy Laboratory, Golden, Colorado 80401 (United States); Shulda, Sarah; Diercks, David; Pylypenko, Svitlana; Richards, Ryan M. [Colorado School of Mines, Golden, Colorado 80401 (United States); Schwartz, Craig P.; Nordlund, Dennis [SLAC National Accelerator Laboratory, Menlo Park, California 94025 (United States); Kukliansky, Alon; Natan, Amir [Tel Aviv University, Tel Aviv-Yafo (Israel); Prendergast, David; Sun, Wenhao [Lawrence Berkeley National Laboratory, Berkley, California 94720 (United States); Orvananos, Bernardo [Massachusetts Institute of Technology, Cambridge, Massachusetts 02139 (United States); and others

2016-04-14

Recent advances in theoretical structure prediction methods and high-throughput computational techniques are revolutionizing experimental discovery of the thermodynamically stable inorganic materials. Metastable materials represent a new frontier for these studies, since even simple binary non-ground state compounds of common elements may be awaiting discovery. However, there are significant research challenges related to non-equilibrium thin film synthesis and crystal structure predictions, such as small strained crystals in the experimental samples and energy minimization based theoretical algorithms. Here, we report on experimental synthesis and characterization, as well as theoretical first-principles calculations of a previously unreported mixed-valent binary tin nitride. Thin film experiments indicate that this novel material is N-deficient SnN with tin in the mixed II/IV valence state and a small low-symmetry unit cell. Theoretical calculations suggest that the most likely crystal structure has the space group 2 (SG2) related to the distorted delafossite (SG166), which is nearly 0.1 eV/atom above the ground state SnN polymorph. This observation is rationalized by the structural similarity of the SnN distorted delafossite to the chemically related Sn{sub 3}N{sub 4} spinel compound, which provides a fresh scientific insight into the reasons for growth of polymorphs of metastable materials. In addition to reporting on the discovery of the simple binary SnN compound, this paper illustrates a possible way of combining a wide range of advanced characterization techniques with the first-principle property calculation methods, to elucidate the most likely crystal structure of the previously unreported metastable materials.

Synthesis, characterization and catalytic activity of stable [(NHC)H][ZnXY2] (NHC=N-Heterocyclic carbene, X, Y=Cl, Br) species

KAUST Repository

Santoro, Orlando; Nahra, Fady; Cordes, David B.; Slawin, Alexandra M.Z.; Nolan, Steven P.; Cazin, Catherine S. J.

2016-01-01

The synthesis and characterization of imidazol(in)ium-based zinc(II) halide salts are reported. These compounds present interesting structural features and exhibit high stability. Their catalytic activity was explored in the methylation of amines with CO2 and PhSiH3.

Synthesis, characterization and catalytic activity of stable [(NHC)H][ZnXY2] (NHC=N-Heterocyclic carbene, X, Y=Cl, Br) species

KAUST Repository

Santoro, Orlando

2016-06-04

The synthesis and characterization of imidazol(in)ium-based zinc(II) halide salts are reported. These compounds present interesting structural features and exhibit high stability. Their catalytic activity was explored in the methylation of amines with CO2 and PhSiH3.

Alpha amylase assisted synthesis of TiO2 nanoparticles: Structural characterization and application as antibacterial agents

International Nuclear Information System (INIS)

Ahmad, Razi; Mohsin, Mohd; Ahmad, Tokeer; Sardar, Meryam

2015-01-01

Graphical abstract: - Highlights: • Green synthesis of TiO 2 nanoparticles using an enzyme alpha amylase has been described. • The morphology and shape depends upon the concentration of the alpha amylase enzyme. • The biosynthesized nanoparticles show good bactericidal effect against both gram positive and gram negative bacteria. • The bactericidal effect was further confirmed by Confocal microscopy and TEM. - Abstract: The enzyme alpha amylase was used as the sole reducing and capping agent for the synthesis of TiO 2 nanoparticles. The biosynthesized nanoparticles were characterized by X-ray diffraction (XRD) and transmission electron microscopic (TEM) methods. The XRD data confirms the monophasic crystalline nature of the nanoparticles formed. TEM data shows that the morphology of nanoparticles depends upon the enzyme concentration used at the time of synthesis. The presence of alpha amylase on TiO 2 nanoparticles was confirmed by FTIR. The nanoparticles were investigated for their antibacterial effect on Staphylococcus aureus and Escherichia coli. The minimum inhibitory concentration value of the TiO 2 nanoparticles was found to be 62.50 μg/ml for both the bacterial strains. The inhibition was further confirmed using disc diffusion assay. It is evident from the zone of inhibition that TiO 2 nanoparticles possess potent bactericidal activity. Further, growth curve study shows effect of inhibitory concentration of TiO 2 nanoparticles against S. aureus and E. coli. Confocal microscopy and TEM investigation confirm that nanoparticles were disrupting the bacterial cell wall

Synthesis and characterization of nanocomposite powders of calcium phosphate/silica-gel; Sintese e caracterizacao de pos nanoestruturados de fosfato de calcio/silica-gel

Energy Technology Data Exchange (ETDEWEB)

Muller, D.T.; Delima, S.A. [Universidade do Estado de Santa Catarina (UDESC), Joinville, SC (Brazil). Dept. de Engenharia Mecanica; Santos, R.B.M.; Camargo, N.H.A., E-mail: dem2nhac@joinville.udesc.b [Universidade do Estado de Santa Catarina (UDESC), Joinville, SC (Brazil). Programa de Pos Graduacao em Ciencia e Engenharia de Materiais

2009-07-01

In the recent years ceramics of calcium phosphate are pointed out as an outstanding material in substitution and regeneration in defects from osseous tissue, in reason of their similar mineralogical characteristics of apatite of bone structure. However, the challenge with phosphate calcium ceramics find out about the mechanical properties and the development of biomaterials similar of the bone structure, what sometimes is not so easy, about fragile materials. The aim of this work focused in synthesis and characterization nanocomposites powders of calcium phosphate/silica-gel with percentages 1, 2, 3 e 5% of nanometric silica. The method synthesis used for the compositions elaboration was dissolution-precipitation. The presented results are related with the optimization to method elaboration of nanostructured powders, the mineralogical characterization with X-ray diffraction, thermal behavior with thermal differential analysis, differential scanning calorimetry here is ADT and dilatometer. The scanning electronic microscopy was used to help of morphological characterization the nanostructured powders and the surfaces from body test recovered from the mechanical test. (author)

Hydrothermal synthesis and characterization of zirconia based catalysts

Science.gov (United States)

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

2013-07-01

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

Synthesis and Characterization of Novel Ternary and Quaternary Alkali Metal Thiophosphates

KAUST Repository

Alahmary, Fatimah S.

2014-05-01

The ongoing development of nonlinear optical (NLO) crystals such as coherent mid-IR sources focuses on various classes of materials such as ternary and quaternary metal chalcophosphates. In case of thiophosphates, the connection between PS4-tetrahedral building blocks and metals gives rise to a broad structural variety where approximately one third of all known ternary (A/P/S) and quaternary (A/M/P/S) (A = alkali metal, M = metal) structures are acentric and potential nonlinear optical materials. The molten alkali metal polychalcophosphate fluxes are a well-established method for the synthesis of new ternary and quaternary thiophosphate and selenophosphate compounds. It has been a wide field of study and investigation through the last two decades. Here, the flux method is used for the synthesis of new quaternary phases containing Rb, Ag, P and S. Four new alkali metal thiophosphates, Rb4P2S10, RbAg5(PS4), Rb2AgPS4 and Rb3Ag9(PS4)4, have been synthesized successfully from high purity elements and binary starting materials. The new compounds were characterized by single crystal and powder X-ray diffraction, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), ultraviolet-visible (UV-VIS), Raman spectroscopy, thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). These compounds show interesting structural variety and physical properties. The crystal structures feature 3D anionic framework built up of PS4 tetrahedral units and charge balanced by Ag and alkali metal cations. All prepared compounds are semiconductors with band gap between 2.3 eV to 2.6 eV and most of them are thermally stable up to 600ºC.

SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURE OF BIS-(2-HYDROXYBENZALDEHYDEDIAMINOGUANIZONE

Directory of Open Access Journals (Sweden)

Diana Dragancea, Vladimir B. Arion, Sergiu Shova

2008-12-01

Full Text Available The new ligand, bis(2-hydroxybenzaldehydediaminoguanizone (1 has been synthesized and characterized by elemental analysis, IR and 1H NMR spectroscopies. The crystal structure of the compound was determined by X-ray diffraction. The ligand C15H15N5O2·C2H5OH crystallizes in the monoclinic space group P21/c with unit cell parameters a = 8.9102(3, b = 10.0357(3, c = 19.7618(6 Å, β = 98.385(2°, Z = 4, V = 1748.21(9 Å3, R1 = 0.040. The amino form of the ligand adopts a planar conformation stabilized by two intramolecular hydrogen bonds of the type O–H···N, in which the H atoms of the central amino group are directed to the lone-pair regions of the azomethine nitrogen atoms.

Carbazole Containing Copolymers: Synthesis, Characterization, and Applications in Reversible Holographic Recording

Directory of Open Access Journals (Sweden)

Bénédicte Mailhot-Jensen

2010-01-01

Full Text Available Carbazolic copolymers have been developed to be used in reversible holographic recording. This paper describes a complete analysis, from synthesis of the material to its applications, together with the corresponding characterizations. The investigated materials were photosensitive copolymers obtained from carbazolylalkylmethacrylates (CEM and octylmethacrylate (OMA. A detailed investigation was undertaken involving infrared spectroscopy and NMR techniques, 1H, 13C, COSY, and HSQC, in order to establish the chemical structure and the composition of the copolymers. Holographic recording characteristics were investigated with one- and two-layer photothermoplastic carriers. The two-layer carrier contains separate photosensitive and thermoplastic layers and gives the best holographic response. The surface of microstructured samples has been characterized by atomic force microscopy analysis. It is shown that via a photothermoplastic recording process, it is possible to record and read holograms practically in real time (~3 s with a diffraction efficiency of 10% and a spatial resolution higher than 1000 mm−1.

Tuned apatitic materials: Synthesis, characterization and potential antimicrobial applications

Science.gov (United States)

Fierascu, Irina; Fierascu, Radu Claudiu; Somoghi, Raluca; Ion, Rodica Mariana; Moanta, Adriana; Avramescu, Sorin Marius; Damian, Celina Maria; Ditu, Lia Mara

2018-04-01

Inorganic antimicrobial materials can be viable for multiple applications (related to its use for new buildings with special requirements related to microbiological loading, such as hospital buildings and for consolidation of cultural heritage constructions); also the use of substituted hydroxyapatites for protection of stone artefacts against environmental factors (acidic rain) and biodeterioration it's an option to no longer use of toxic substances. This paper presents methods of synthesis and characterization of the material from the point of view of the obtained structures and final applications. The materials were characterized in terms of composition and morphology (using X-ray Diffraction, X-ray Fluorescence, Inductively coupled plasma-atomic emission spectrometry, Fourier Transform Infrared Spectroscopy, X-ray Photoelectron Spectroscopy, Surface area and pore size determination). Antimicrobial activity was tested against filamentous fungi strains and pathogenic bacteria strains, using both spot on lawn qualitative method (on agar medium) and serial microdilution quantitative method (in broth medium). Further, it was evaluated the anti-biofilm activity of the tested samples toward the most important microbial strains implicated in biofilm development, using crystal violet stained biofilms microtiter assay, followed by spectrophotometric quantitative evaluation.

Synthesis, structural characterization and quantum chemical studies of silicon-containing benzoic acid derivatives

Science.gov (United States)

Zaltariov, Mirela-Fernanda; Cojocaru, Corneliu; Shova, Sergiu; Sacarescu, Liviu; Cazacu, Maria

2016-09-01

The present paper is concerned with the synthesis and molecular structure investigation of two new benzoic acid derivatives having trimethylsilyl tails, 4-((trimethylsilyl)methoxy) and 4-(3-(trimethylsilyl)propoxy)benzoic acids. The structures of the novel compounds have been confirmed by X-ray crystallography, Fourier-transform infrared spectroscopy (FTIR) and nuclear magnetic resonance (1H and 13C NMR). The theoretical studies of molecules were conducted by using the quantum chemical methods, such as Density Functional Theory (DFT B3LYP/6-31 + G**), Hartree-Fock (HF/6-31 + G**) and semiempirical computations (PM3, PM6 and PM7). The optimized molecular geometries have been found to be in good agreement with experimental structures resulted from the X-ray diffraction. The maximum electronic absorption bands observed at 272-287 nm (UV-vis spectra) have been assigned to π → π* transitions, which were in reasonable agreement with the time dependent density functional theory (TD-DFT) calculations. The computed vibrational frequencies by DFT method were assigned and compared with the experimental FTIR spectra. The mapped electrostatic potentials revealed the reactive sites, which corroborated the observation of the dimer supramolecular structures formed in the crystals by hydrogen-bonding. The energies of frontier molecular orbitals (HOMO and LUMO), energy gap, dipole moment and molecular descriptors for the new compounds were calculated and discussed.

Synthesis and characterization of europium aluminophosphate

International Nuclear Information System (INIS)

Araujo, A.S.; Diniz, J.C.; Silva, A.O.S.

1998-01-01

Full text: Aluminophosphate molecular sieves (ALPO) represents a class of materials formed by AlO 2+ and PO 2- tetrahedra linked together through b the oxygen atom. The incorporation of metal cations, specifically rare earths, in the ALPO matrix, gives rise to generation of new materials that can be used as acid catalysts in chemical processes. In this work, it was synthesized hydrothermally a molecular sieve type Eu-ALPO-11, starting from an hydrated alumina (pseudobohemite), phosphoric acid solution, europium chloride, water, and di-isopropylamine (DIPA) as organic template. The gel of synthesis presented the following composition: 1.0 DIPA: 0.05 Eu 2 O 3 :0.95 Al 2 O 3 : 1.0 P 2 O 5 : 80 H 2 O The hydrogel was autoclaved at 170 deg C for a period of 3 days. After that the obtained solid was filtered, washed, dried and calcined at 500 deg C to remove the template. The sample was characterized by several physico-chemical methods, such a atomic absorption, FT-IR spectroscopy, X-ray diffraction, thermal analysis, scanning electron microscopy. Its spectroscopic properties was investigated by europium luminescence. The physico-chemical characterization of the Eu-ALPO-11 showed very good crystallinity, with AEL structure, and orthorhombic symmetry. Also, the material presents excellent thermal stability, with no structural collapse until 950 deg C. Through the luminescence spectra in the visible region, it was observed that the emission of the Eu 3+ is strongly influenced by the increasing of the 5d0 7f0 transition (Electric Dipole), as compared to the 5d0 7f1 transition (Magnetic Dipole) between the levels of 4f configuration perturbed by the crystalline field. The ED/MD ratio to the as synthesized sample was ca. 2.1, against ca. 1.1 relative to the calcined sample. The FT-IR spectra presented well defined absorption bands relative to Al-O and P-O bonds, of the structural internal tetrahedra (IT) and external links (EL): 1250- 950 cm -1 , symmetric stretching due to

Synthesis and characterization of Taurine

Directory of Open Access Journals (Sweden)

B Bayarmaa

2014-10-01

Full Text Available Have been obtained 2-aminoethanesulfonic acid (taurine from ethanolamine, sulfuric acid and sodium sulfite during the synthesis in laboratory condition. The process involves two steps of reactions, the first was esterification of ethanolamine with sulfuric acid to produce the intermediate product of 2-aminoethyl ester which than was extended to the second step by sulfonation with sodium sulfite to produce 2-aminoethanesulfonic acid. Resulting product was analyzed using 1H-NMR, IR, FAB-MS analysis and examined purity characterizations of the synthesized products. DOI: http://dx.doi.org/10.5564/mjc.v14i0.200 Mongolian Journal of Chemistry 14 (40, 2013, p57-60

Synthesis for Structure Rewriting Systems

Science.gov (United States)

Kaiser, Łukasz

The description of a single state of a modelled system is often complex in practice, but few procedures for synthesis address this problem in depth. We study systems in which a state is described by an arbitrary finite structure, and changes of the state are represented by structure rewriting rules, a generalisation of term and graph rewriting. Both the environment and the controller are allowed to change the structure in this way, and the question we ask is how a strategy for the controller that ensures a given property can be synthesised.

Synthesis and characterization of iron nano particles for the arsenic removal in water

International Nuclear Information System (INIS)

Gutierrez M, O. E.

2011-01-01

The synthesis of iron nanoparticles for the removal of metallic ions in polluted waters has been during the last years study topic for different world organizations. This work presents a synthesis method of conditioned coal with iron nanoparticles starting from the use of leaves of pineapple crown, with the purpose of using it in arsenic removal processes in aqueous phase. For the synthesis of this material, the leaves of the pineapple crown were used like supports structure of the iron nanoparticles. First, the pyrolysis appropriate temperature was determined. For the preparation of the support material, this had contact with a ferric nitrate and hexamine solution, because the preparation of the material and the coal synthesis were realized during the pyrolysis process, where the hexamine molecules and the ferric nitrate react, causing the reduction of the iron particles and their dispersion on the support material, obtaining as product a conditioned coal with iron nanoparticles. For the characterization of the materials were used techniques as: Scanning electron microscopy, Transmission electron microscopy, X-Rays Diffraction), X-Ray photoelectron spectroscopy and Moessbauer spectroscopy; moreover was determined the isoelectric point and the density of surface sites. The arsenic sorption capacity of the materials was evaluated by means of the methodology type lots where was determined the sorption kinetics and isotherms in terms of arsenic concentration and mass. (Author)

Synthesis and characterization of BNO (BiNbO4) ceramics added to 3% of ZnO

International Nuclear Information System (INIS)

Sales, A.J.M.; Pires Junior, G.F.M.; Rodrigues, H.O.; Sousa, D.G.; Sales, J.C.; Sombra, A.S.B.

2012-01-01

This work describes the synthesis and study of the structural characterization of ceramic BiNbO4 and density behavior when added 3% by weight of ZnO with a view to use in capacitors. The manufacture of BiNbO4 was made by conventional ceramic method. The powders were milled for two hours, calcined at 850 ° C for 3 h and characterized by XRD with Diffractometer Rigaku DMAXB of Co-α radiation. A more detailed XRD characterization was performed with the program DBWS9807a using the Rietveld refinement of crystal structures, which confirmed the achievement of phase -α-BiNbO4. Were made 'buks' with the calcined powder and these were sintered at 1025 ° C. In order to study the grain morphology and distribution of pores in the ceramic body, the surface of the sample with addition of 3% by weight of ZnO was analyzed by Scanning Electron Microscopy which confirmed a better densification. (author)

Comparison among structural characteristics of Ce1-xCuxO2 nanocatalysts obtained by two methods of distinct synthesis

International Nuclear Information System (INIS)

Neiva, L.S.; Bispo, A.; Santos, P.T.A.; Costa, A.C.F.M.; Gama, L.; Mascarenhas, A.J.S.

2009-01-01

The objective this work is to synthesize nano catalysts Ce 1-x Cu x O 2 type by the synthesis methods of the combustion reaction and Pechini. The value of the concentration (x) of the element dope (Cu) varies between 0,1 and 0,5 mols. It intends evaluate that form the synthesis method influences in the physical structural characteristics of this material. nano catalysts were characterized by ray- X diffraction. The results showed nano catalysts formation with a formed structure for the most part by the phase CeO 2 , as it was expected, since this is the hostess matrix of the element dope (Cu). Nano catalysts obtained by the method Pechini presents crystallinity larger deg, according with patterns of ray-X. Thus, it was concluded that synthesis employee method the kind in the methodology, as well as the value of the concentration of the element dope has influence on the final structural characteristics of the developed material. (author)

Synthesis and characterization of a nanostructured matrix hydroxyapatite ceramic bone reconstruction

International Nuclear Information System (INIS)

Correa, P.; Camargo, N.H.A.; Silva, D.F.

2012-01-01

The nanostructured ceramics have been shown promise as biomaterials for bone reconstruction. Among calcium phosphates, hydroxyapatite Ca/P ratio = 1.67 mol stands out because of its crystallographic similarity with the mineral bone phase and biocompatibility. This work was based on synthesis and characterization of a nanostructured hydroxyapatite for use in reconstituting bone tissue. The synthesis method for obtaining the bioceramic powder occurred at process of dissolution/precipitation, involving CaO solid/liquid and phosphoric acid required for forming the composition of Ca/P = 1.67 mole. The material recovered from the synthesis was calcined at 900 ° C/2h, providing the hydroxyapatite powder nanometer. This was subjected to mechanical fragmentation process in mill attritor, providing a hydroxyapatite with modified surface morphology. The results presented relate to morphological characterization studies (SEM), mineralogical (XRD), chemical (FTIR) and particle size distribution, using the laser particle size analysis method. Such results showed the formation of hydroxyapatite phase and morphology satisfactory for use in reconstituting bone tissue

Synthesis of carbon nano structures by plasma discharge

International Nuclear Information System (INIS)

Jimenez L, M.L.

2007-01-01

Due to the great quantity of applications of carbon neocarcinostatin (NEC) in diverse areas like: synthesis of super-resistant materials, hydrogen storage, nano sensors generation and nano catalysts, one has seen the necessity to generate new synthesis processes of these materials as well as to already improve those existent. The present work has as objective to optimize the NEC synthesis process by means of the electric arc method which uses alternating current to high frequencies (HF), obtaining relatively clean products; that is to say, it hardly presents amorphous material neither impurities. They stand out the obtaining of carbon nano fibers (NFC) by means of a luminescent-arc discharge, in a gas mixture He-CH 4 with 34% at.Ni/10.32%at.Y like catalyst; to a frequency of 42 k Hz and low power (300 W). This method benefits the agglomeration of the particles in both electrodes due to the high frequencies. The time of duration of the process oscillates between 5 and 20 minutes. The obtained product was characterized by scanning electron microscopy (MEB), transmission electron microscopy (MET) to determine the type of obtained NEC and by X-ray diffraction analysis and Raman spectroscopy to determine the purity of the samples. The NFC are relatively free of amorphous coal. The surface and structural analysis indicates that the fibers have a half diameter of 80 nm. It is also made, a study by optical emission spectroscopy of the plasma using the Swan band to determine the temperature. (Author)

Synthesis, characterization and photochemistry of a new ...

Indian Academy of Sciences (India)

The synthesis, crystal structure, redox characteristics and photochemistry of a new heptamolyb- ... The ability of [Mo7O24]−6 to function as a pure “inor- .... Abbreviations used: bpp = 1,3-bis(4-pyridyl)propane; 2-amp = 2-aminopyridine; DMSO ...

Synthesis of imine bond containing insoluble polymeric ligand and its transition metal complexes, structural characterization and catalytic activity on esterification reaction.

Science.gov (United States)

Gönül, İlyas; Ay, Burak; Karaca, Serkan; Saribiyik, Oguz Yunus; Yildiz, Emel; Serin, Selahattin

2017-01-01

In this study, synthesis of insoluble polymeric ligand (L) and its transition metal complexes [Cu(L)Cl 2 ]·2H 2 O (1) , [Co(L)Cl 2 (H 2 O) 2 ] (2) and [Ni(L)Cl 2 (H 2 O) 2 ] (3) , having the azomethine groups, were synthesized by the condensation reactions of the diamines and dialdehydes. The structural properties were characterized by the analytical and spectroscopic methods using by elemental analysis, Fourier Transform Infrared, Thermo Gravimetric Analysis, Powder X-ray Diffraction, magnetic susceptibility and Inductively Coupled Plasma. The solubilities of the synthesized polymeric materials were also investigated and found as insoluble some organic and inorganic solvents. Additionally, their catalytic performance was carried out for the esterification reaction of acetic acid and butyl acetate. The highest conversion rate is 75.75% by using catalyst 1 . The esterification of butanol gave butyl acetate with 100% selectivity.

Synthesis and Characterization of Metal Phosphates for Photocatalytic Applications

KAUST Repository

Al-Sabban, Bedour

2012-07-01

Solar energy is the most abundant efficient and important source of renewable energy. The objective of this study is to develop highly efficient visible light responsive photocatalysts for overall water splitting. This is done by using silver or copper containing materials. Phosphate compounds have caught much attention due to their rigid structure, thermal stability and resistance to chemical attacks. Solid phosphates can be prepared by direct solid-state reaction between metal cations and phosphate anions at high temperatures. Double metal phosphates of the Nasion-type structure had shown further technological importance. It has been reported that well-crystallized double metal phosphate particles have excellent ordering and cationic conduction channels in the Nasicon framework. In this study, several Nasion-type structured materials have been synthesized by solid-state method (e.g. CuTi2(PO4)3 and AgTi2(PO4)3) heated up under different temperatures (400–1100C) in N2 or air atmosphere. These materials were characterized by XRD, SEM, DR-UV-Vis spectroscopy and tested for photocatalytic applications. A new method for direct synthesis of photoelectrode on Ti Plate had been demonstrated. Further investigations on controlling the size and morphology for better performance of single and double metal phosphates will be done.

Characterization of nano structured metallic materials; Caracterizacion de materiales metalicos nanoestructurados

Energy Technology Data Exchange (ETDEWEB)

Marin A, M.; Gutierrez W, C.; Cruz C, R.; Angeles C, C. [Instituto Nacional de Investigaciones Nucleares, A.P. 18-1027, 11801 Mexico D.F. (Mexico)

1997-07-01

Nowadays the search of new materials with specific optical properties has carried out to realize a series of experiments through the polymer synthesis [(C{sub 3}N{sub 3}){sub 2} (NH){sub 3}]{sub n} doped with gold metallic nanoparticles. The thermal stability of a polymer is due to the presence of tyazine rings contained in the structure. The samples were characterized by High Resolution Transmission Electron Microscopy, X-ray diffraction by the Powder method, Ft-infrared and its thermal properties by Differential Scanning Calorimetry (DSC) and Thermogravimetry (TGA). One of the purposes of this work is to obtain nano structured materials over a polymeric matrix. (Author)

Synthesis, Properties Characterization and Applications of Various Organobismuth Compounds

Directory of Open Access Journals (Sweden)

Jingfei Luan

2011-05-01

Full Text Available Organobismuth chemistry was emphasized in this review article due to the low price, low toxicity and low radioactivity characteristics of bismuth. As an environmentally-friendly class of organometallic compounds, different types of organobismuth compounds have been used in organic synthesis, catalysis, materials, etc. The synthesis and property characterization of many organobismuth compounds had been summarized. This review article also presented a survey of various applications of organobismuth compounds in organic transformations, as reagents or catalysts. The reactivity, reaction pathways and mechanisms of reactions with organobismuths were discussed. Less common and limiting aspects of organobismuth compounds were also briefly mentioned.

A short designed semi-aromatic organic nanotube – synthesis, chiroptical characterization, and host properties

DEFF Research Database (Denmark)

Wixe, Torbjörn; Christensen, Niels Johan; Lidin, Sven

2014-01-01

to molecular dynamics simulations in chloroform). The synthesis of the tube, a heptamer, is based on a series of Friedländer condensations and the use of pyrido[3,2-d]pyrimidine units as masked 2-amino aldehydes, as a general means to propagate organic tubular structures and the introduction of a methoxy group...... for modification toward solubility and functionalization are described. The electronic CD spectra of the tube and molecular intermediates are correlated with theoretical spectra calculated with time-dependent density functional theory to characterize the chirality of the tube. Both experimental (NMR...

Synthesis and characterization of thermally oxidized ZnO films

Indian Academy of Sciences (India)

Administrator

Synthesis and characterization of thermally oxidized ZnO films. A P RAMBU1,* and N IFTIMIE2 .... R. −. Δ. = = (1) where Ra is the sensor resistance in the air and Rg is the .... ple, Aida and coworkers (2006) reported that the total oxidation is ...

Synthesis and characterization of nanostructured CaSiO3 biomaterial

Science.gov (United States)

Jagadale, Pramod N.; Kulal, Shivaji R.; Joshi, Meghanath G.; Jagtap, Pramod P.; Khetre, Sanjay M.; Bamane, Sambhaji R.

2013-04-01

Here we report a successful preparation of nanostructured calcium silicate by wet chemical approach. The synthesized sample was characterized by various physico-chemical methods. Thermal stability was investigated using thermo-gravimetric and differential thermal analysis (TG-DTA). Structural characterization of the sample was carried out by the X-ray diffraction technique (XRD) which confirmed its single phase hexagonal structure. Transmission electron microscopy (TEM) was used to study the nanostructure of the ceramics while homogeneous grain distribution was revealed by scanning electron microscopy studies (SEM). The elemental analysis data obtained from energy dispersive X-ray spectroscopy (EDAX) were in close agreement with the starting composition used for the synthesis. Superhydrophilic nature of CaSiO3 was investigated at room temperature by sessile drop technique. Effect of porous nanosized CaSiO3 on early adhesion and proliferation of human bone marrow mesenchymal stem cells (BMMSCs) and cord blood mesenchymal stem (CBMSCs) cells was measured in vitro. MTT cytotoxicity test and cell adhesion test showed that the material had good biocompatibility and promoted cell viability and cell proliferation. It has been stated that the cell viability and proliferation are significantly affected by time and concentration of CaSiO3. These findings indicate that the CaSiO3 ceramics has good biocompatibility and that it is promising as a biomaterial.

Synthesis, molecular modeling and structural characterization of vanillin derivatives as antimicrobial agents

Science.gov (United States)

Sun, Juan; Yin, Yong; Sheng, Gui-Hua; Yang, Zhi-Bo; Zhu, Hai-Liang

2013-05-01

Two vanillin derivatives have been designed and synthesized and their biological activities were also evaluated for antimicrobial activity. Their chemical structures are characterized by single crystal X-ray diffraction studies, 1H NMR, MS, and elemental analysis. Structural stabilization of them followed by intramolecular as well as intermolecular H-bonds makes these molecules as perfect examples in molecular recognition with self-complementary donor and acceptor units within a single molecule. Docking simulations have been performed to position compounds into the FtsZ active site to determine their probable binding model. Compound 3a shows the most potent biological activity, which may be a promising antimicrobial leading compound for the further research.

Template-Assisted Synthesis and Characterization of Passivated Nickel Nanoparticles

Directory of Open Access Journals (Sweden)

Al-Omari IA

2010-01-01

Full Text Available Abstract Potential applications of nickel nanoparticles demand the synthesis of self-protected nickel nanoparticles by different synthesis techniques. A novel and simple technique for the synthesis of self-protected nickel nanoparticles is realized by the inter-matrix synthesis of nickel nanoparticles by cation exchange reduction in two types of resins. Two different polymer templates namely strongly acidic cation exchange resins and weakly acidic cation exchange resins provided with cation exchange sites which can anchor metal cations by the ion exchange process are used. The nickel ions which are held at the cation exchange sites by ion fixation can be subsequently reduced to metal nanoparticles by using sodium borohydride as the reducing agent. The composites are cycled repeating the loading reduction cycle involved in the synthesis procedure. X-Ray Diffraction, Scanning Electron Microscopy, Transmission Electron microscopy, Energy Dispersive Spectrum, and Inductively Coupled Plasma Analysis are effectively utilized to investigate the different structural characteristics of the nanocomposites. The hysteresis loop parameters namely saturation magnetization and coercivity are measured using Vibrating Sample Magnetometer. The thermomagnetization study is also conducted to evaluate the Curie temperature values of the composites. The effect of cycling on the structural and magnetic characteristics of the two composites are dealt in detail. A comparison between the different characteristics of the two nanocomposites is also provided.

Synthesis, characterization, bioactivity and potential application of phenolic acid grafted chitosan: A review.

Science.gov (United States)

Liu, Jun; Pu, Huimin; Liu, Shuang; Kan, Juan; Jin, Changhai

2017-10-15

In recent years, increasing attention has been paid to the grafting of phenolic acid onto chitosan in order to enhance the bioactivity and widen the application of chitosan. Here, we present a comprehensive overview on the recent advances of phenolic acid grafted chitosan (phenolic acid-g-chitosan) in many aspects, including the synthetic method, structural characterization, biological activity, physicochemical property and potential application. In general, four kinds of techniques including carbodiimide based coupling, enzyme catalyzed grafting, free radical mediated grafting and electrochemical methods are frequently used for the synthesis of phenolic acid-g-chitosan. The structural characterization of phenolic acid-g-chitosan can be determined by several instrumental methods. The physicochemical properties of chitosan are greatly altered after grafting. As compared with chitosan, phenolic acid-g-chitosan exhibits enhanced antioxidant, antimicrobial, antitumor, anti-allergic, anti-inflammatory, anti-diabetic and acetylcholinesterase inhibitory activities. Notably, phenolic acid-g-chitosan shows potential applications in many fields as coating agent, packing material, encapsulation agent and bioadsorbent. Copyright © 2017 Elsevier Ltd. All rights reserved.

Novel polymeric potassium complex: Its synthesis, structural characterization, photoluminescence and electrochemical properties

Energy Technology Data Exchange (ETDEWEB)

Ceyhan, Goekhan [Chemistry Department, K.Maras Suetcue Imam University, 46100 K.Maras (Turkey); Tuemer, Mehmet, E-mail: mtumer@ksu.edu.tr [Chemistry Department, K.Maras Suetcue Imam University, 46100 K.Maras (Turkey); Koese, Muhammet; McKee, Vickie [Chemistry Department, Loughborough University, LE11 3TU Leicestershire (United Kingdom)

2012-03-15

In this paper, we obtained a novel poly(vanillinato potassium) complex (PVP) as a single crystal and characterized by analytical and spectroscopic methods. A single crystal of the PVP was obtained from the acetone solution. X-ray structural data show that crystals contain polymeric K{sup +} complex of vanillin. Each potassium ion in the polymeric structure is identical and seven-coordinate, bonded to two methoxy, two phenoxy and three aldehyde oxygen atoms from four vaniline molecules. Two aldehyde oxygen atoms are bridging between potassium ions. It crystallizes in the monoclinic system, space group P2{sub 1}/c, with lattice parameters a=9.6215(10) A, b=17.4139(19) A, c=9.6119(10) A, {beta}=100.457(2) Degree-Sign and Z=4. Thermal properties of the PVP were investigated by TGA, DTA and DSC methods. The electrochemical properties of the complex were studied in different solvents and at various scan rates. The luminescence properties of the complex in different solvents and at different pH values have been investigated. The results show that the complex exhibits more efficient luminescence property in CH{sub 3}CN and n-butanol. - Highlights: Black-Right-Pointing-Pointer Novel polymeric potassium complex was prepared and fully characterized. Black-Right-Pointing-Pointer X-ray crystal structure of complex was reported. Black-Right-Pointing-Pointer Electrochemical properties of compound were investigated. Black-Right-Pointing-Pointer Thermal and DSC measurements of complex were examined.

Incorporation of the zosteric sodium salt in silica nanocapsules: synthesis and characterization of new fillers for antifouling coatings

Science.gov (United States)

Ruggiero, Ludovica; Crociani, Laura; Zendri, Elisabetta; El Habra, Naida; Guerriero, Paolo

2018-05-01

In the last decade many commercial biocides were gradually banned for toxicity. This work reports, for the first time, the synthesis and characterization of silica nanocontainers loaded with a natural product antifoulant (NPA), the zosteric sodium salt which is a non-commercial and environmentally friendly product with natural origin. The synthesis approach is a single step dynamic self-assembly with tetraethoxysilane (TEOS) as silica precursor. Unlike conventional mesoporous silica nanoparticles, the structure of these silica nanocontainers provides loading capacity and allows prolonged release of biocide species. The obtained nanocapsules have been characterized morphologically by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The encapsulation was checked by FTIR ATR spectroscopy and thermogravimetric analyses. The results of the release studies show the great potential of the here presented newly developed nanofillers in all applications where a controlled release of non-toxic and environmentally friendly biocides is required.

Synthesis and characterization of graphene oxide using modified Hummer's method

Science.gov (United States)

Kaur, Manpreet; Kaur, Harsimran; Kukkar, Deepak

2018-05-01

In the present study, a simple approach has been followed for the synthesis of graphene oxide (GO) using modified Hummers method in which graphite powder was oxidized in the presence of concentrated H2SO4 and KMnO4. The amount of NaNO3 and KMnO4 was varied to produce sheet like structure. The varied concentrations of NaNO3 and KMnO4 resulted in yielding large amount of the product. Structural, morphological and physicochemical features of the product were studied using UV-Visible spectrophotometer, Fourier Transform infrared spectroscopy (FTIR), and crystal structure was determined using X-ray powder diffraction (XRD). UV-Vis spectra of GO was observed at a maximum absorption of 230 nm due to (π-π*) transition of atomic carbon-carbon bonds. FTIR spectra revealed the presence of oxygen containing functional groups which ensures the complete exfoliation of graphite into graphene oxide X-ray powder diffraction pattern of the product showed the diffraction peak at (2θ = 26.7°) with an interlayer spacing of 0.334 nm. All the above characterizations successfully confirmed the formation of GO.

Polypyrrole-silver Nanocomposite: Synthesis and Characterization

Directory of Open Access Journals (Sweden)

D. M. Nerkar

2016-07-01

Full Text Available Polypyrrole-Silver (PPy-Ag nanocomposite has been successfully synthesized by the chemical oxidative polymerization of pyrrole with iron (III chloride as an oxidant, in the presence of a colloidal suspension of silver nanoparticles. Turkevich method (Citrate reduction method was used for the synthesis of silver nanoparticles (Ag NPs. The silver nanoparticles were characterized by UV-Visible spectroscopy which showed an absorption band at 423 nm confirming the formation of nanoparticles. PPy-Ag nanocomposite was characterized by Transmission Electron Microscopy (TEM, Scanning Electron Microscopy (SEM, Fourier Transform Infrared Spectroscopy (FTIR and X-ray diffraction (XRD techniques for morphological and structural confirmations. TEM and SEM images revealed that the silver nanoparticles were well dispersed in the PPy matrix. XRD pattern showed that PPy is amorphous but the presence of the peaks at 2q values of 38.24°, 44.57°, 64.51° and 78.45° corresponding to a cubic phase of silver, revealed the incorporation of silver nanoparticles in the PPy matrix. A possible formation mechanism of PPy-Ag nanocomposite was also proposed. The electrical conductivity of PPy-Ag nanocomposite was studied using two probe method. The electrical conductivity of the PPy-Ag nanocomposite prepared was found to be 4.657´10- 2 S/cm, whereas that of pure PPy was found to be 9.85´10-3 S/cm at room temperature (303 K. The value of activation energy (Ea for pure PPy was 0.045 eV while it decreased to 0.034 eV for PPy-Ag nanocomposite. The synthesized nanocomposite powder can be utilized as a potential material for fabrication of gas sensors operating at room temperature.

Synthesis and characterization of In{sub 2}O{sub 3} nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Ayeshamariam, A. [KhadirMohideen College, Adirampattinam (India); Kashif, M. [Universiti Malaysia Perlis, Perlis (Malaysia); Raja, S. Muthu [Vellore Institute of Technology, Vellore (India); Sivaranjani, S. [SBM College of Engineering and technology, Dindigul (India); Sanjeeviraja, C. [Alagappa University, Karaikudi (India); Bououdina, M. [University of Bahrain, Bahrain (Bahrain)

2014-01-15

Metal-oxide nanostructures have elicited increasing interest in both fundamental and applied sciences. Among metal oxide nanostructures, In{sub 2}O{sub 3} has the potential for use asa semiconductor material. This article provides details on studies carried out thus far for the synthesis and the characterization of In{sub 2}O{sub 3} nanostructures. In this research, various techniques were investigated for the fabrication of diverse and fascinating spherical shaped In{sub 2}O{sub 3} nanostructures. BrunauerEmmett-Teller (BET) analyses of the In{sub 2}O{sub 3} nanostructures through detailed refinements of the structure of the In{sub 2}O{sub 3} nanoparticles by using the Rietveld method, followed by microstructural analyses using scanning electron microscopy/ transmission electron microscopy (SEM/TEM) and a chemical composition analysis are presented and discussed. Decreasing crystallinity with an improvement in specific surface area was observed from the structural characterization. The energy dispersive analysis results showed that the as-prepared In{sub 2}O{sub 3} powder sample was stoichiometric, containing almost equal proportions of indium and oxygen. The microstructural analysis (TEM and SEM) demonstrated precise control over the diameters of the nanoparticles, which is an important advantage of the solution combustion approach.

A Comparative Characterization of the HPA-MCM-48 Type Catalysts Produced by the Direct Hydrothermal and Room Temperature Synthesis Methods

International Nuclear Information System (INIS)

Gucbilmez, Y.; Calis, I.; Yargic, A. S.

2012-01-01

MCM-48 type support materials synthesized by the direct hydrothermal synthesis (HTS) and room temperature synthesis (RTS) methods were incorporated with tungstophosphoric acid (TPA) in the range of 10-40 wt% by using a wet impregnation technique in methanol solutions. Resulting HPA-MCM-48 catalysts were characterized by the XRD, Nitrogen Physisorption, SEM, TEM, EDS, and FT-IR methods in order to determine the effects of different initial synthesis conditions on the catalyst properties. RTS samples were found to have better crystalline structures, higher BET surface areas, and higher BJH pore volumes than HTS samples. They also had slightly higher TPA incorporation, except for the 40 wt% samples, as evidenced by the EDS results. Keggin ion structure was preserved, for both methods, even at the highest acid loading of 40 wt%. It was concluded that the simpler and more economical RTS method was more successful than the HTS method for hetero poly acid incorporation into MCM-48 type materials

Soft chemistry routes to transparent metal oxide thin films. The case of sol–gel synthesis and structural characterization of Ta2O5 thin films from tantalum chloromethoxide

International Nuclear Information System (INIS)

Epifani, Mauro; Zamani, Reza; Arbiol, Jordi; Fabrega, Cristian; Andreu, Teresa; Pace, Giovanni Battista; Siciliano, Pietro; Morante, Joan R.

2014-01-01

Ta 2 O 5 thin films were prepared by spin-coating methanol solutions of Ta chloromethoxide. It was prepared by reacting TaCl 5 with methanol, followed by water addition (H 2 O: Ta molar ratio was 16). Thin films were deposited by spin-coating onto SiO 2 /Si substrates, followed by drying at 90 °C and heat-treatment up to 700 °C. The films were characterized by X-ray diffraction, transmission electron microscopy and field emission scanning electron microscopy. Crystallization was obtained only after heating at 700 °C, in the Ta 2 O 5 orthorhombic phase. The resulting films had a thickness of 100 nm. Their structure was constituted by porous crystals with size up to 50 nm, while the pores had a size of about 10 nm. The results demonstrated that TaCl 5 is very convenient precursor for the wet chemical synthesis of Ta 2 O 5 thin films. - Highlights: • Development of convenient solution synthesis of Ta 2 O 5 thin films; • The precursor chemistry was established and related to the synthesis process; • Uniform films crystallized in the most stable orthorombic Ta 2 O 5 phase;

Synthesis and characterization of amorphous cellulose from triacetate of cellulose

International Nuclear Information System (INIS)

Vega-Baudrit, Jose; Sibaja, Maria; Nikolaeva, Svetlana; Rivera A, Andrea

2014-01-01

It was carried-out a study for the synthesis and characterization of amorphous cellulose starting from cellulose triacetate. X-rays diffraction was used in order to obtain the cellulose crystallinity degree, also infrared spectroscopy FTIR was used. (author)

A2TiF5.nH2O (A=K, Rb, or Cs; n=0 or 1): Synthesis, structure, characterization, and calculations of three new uni-dimensional titanium fluorides

International Nuclear Information System (INIS)

Jo, Vinna; Woo Lee, Dong; Koo, Hyun-Joo; Ok, Kang Min

2011-01-01

Three new uni-dimensional alkali metal titanium fluoride materials, A 2 TiF 5 .nH 2 O (A=K, Rb, or Cs; n=0 or 1) have been synthesized by hydrothermal reactions. The structures of A 2 TiF 5 .nH 2 O have been determined by single-crystal X-ray diffraction. The Ti 4+ cations have been reduced to Ti 3+ during the synthesis reactions. All three A 2 TiF 5 .nH 2 O materials contain novel 1-D chain structures that are composed of the slightly distorted Ti 3+ F 6 corner-sharing octahedra attributable to the Jahn-Teller distortion. The coordination environment of the alkali metal cations plays an important role to determine the degree of turning in the chain structures. Complete structural analyses, Infrared and UV-vis diffuse reflectance spectra, and thermal analyses are presented, as are electronic structure calculations. -- Graphical abstract: Ball-and-stick and polyhedral representations for (a) β-K 2 TiF 5 and (b) Rb 2 TiF 5 .H 2 O or Cs 2 TiF 5 .H 2 O with the K + and Rb + (or Cs + ) coordination environment emphasized. Display Omitted Research highlights: → Synthesis, structure, characterization, and calculation of new titanium fluorides. → Study of reduction of starting Ti 4+ cations to Ti 3+ by DMF. → Novel 1-D chain structures with Jahn-Teller distorted TiF 6 octahedra.

Synthesis and characterization of the silver methacrylate and its polymerization with gamma radiation

International Nuclear Information System (INIS)

Figueroa de Paz, Y. M.

2014-01-01

One of the traditional objectives in research has been the development of new and useful materials that combine the properties of polymers with metals. Synthesis of monomers containing metal, followed by a polymerization process, is a method to introduce metal ions in the structure of a polymer, and the gamma radiation was easily applied to initiate polymerization. The coordination polymers have high insolubility, which is a general problem of these materials, besides the lack of structural information available. Also, due to the difficulty of obtaining single crystals, it has hindered the identification of the structures of some coordination polymers, requiring the use of indirect methods for structural characterization. In this work the synthesis of silver poly-methacrylate (PMAAg), was performed using the gamma radiation as polymerization initiator, having as precursor to silver methacrylate monomer (MAAg). The combination of spectroscopic methods revealed structural changes in the coordination polymers. With scanning electron microscopy, it was observed that the morphology of the monomer and its polymers is fiber, which grows with increasing radiation dose; furthermore, this increase in size is related to Bet analysis result, since the monomer has a bigger superficial area to the irradiated polymers. In monomer and irradiated polymers the crystalline structure CCC was observed by X-ray diffraction. By thermogravimetric analysis the decomposition temperature of the products was determined, finding around 150 degrees C. The infrared spectroscopy confirmed the silver methacrylate polymerization, as with increasing radiation dose, also increases the degree of polymerization; likewise the form of coordination of the monomer was determined and its irradiated polymers which corresponds to a bi-dentate chelate, confirmed by X-ray photoelectron spectroscopy. (Author)

Polymer Brushes: Synthesis, Characterization, Applications

Science.gov (United States)

Advincula, Rigoberto C.; Brittain, William J.; Caster, Kenneth C.; Rühe, Jürgen

2004-09-01

Materials scientists, polymer chemists, surface physicists and materials engineers will find this book a complete and detailed treatise on the field of polymer brushes, their synthesis, characterization and manifold applications. In a first section, the various synthetic pathways and different surface materials are introduced and explained, followed by a second section covering important aspects of characterization and analysis in both flat surfaces and particles. These specific surface initiated polymerization (SIP) systems such as linear polymers, homopolymers, block copolymers, and hyperbranched polymers are unique compared to previously reported systems by chemisorption or physisorption. They have found their way in both large-scale and miniature applications of polymer brushes, which is covered in the last section. Such 'hairy' surfaces offer fascinating opportunities for addressing numerous problems of both academic and, in particular, industrial interest: high-quality, functional or protective coatings, composite materials, surface engineered particles, metal-organic interfaces, biological applications, micro-patterning, colloids, nanoparticles, functional devices, and many more. It is the desire of the authors that this book will be of benefit to readers who want to "brush-up on polymers".

Tungsten disilicide (WSi{sub 2}). Synthesis, characterization, and prediction of new crystal structures

Energy Technology Data Exchange (ETDEWEB)

Lukovic, Jelena; Zagorac, Dejan; Zagorac, Jelena; Jordanov, Dragana; Matovic, Branko [Institute of Nuclear Sciences Vinca, Materials Science Laboratory, University of Belgrade (Serbia); Materials Science Laboratory, Center for the Synthesis, Processing and Characterization of Materials for Use in Extreme Conditions, Belgrade (Serbia); Schoen, J. Christian [Materials Science Laboratory, Max Planck Institute for Solid State Research, Stuttgart (Germany); Volkov-Husovic, Tatjana [Faculty of Technology and Metallurgy, Department for Metallurgical Engineering, University of Belgrade (Serbia)

2017-12-13

Transition metal silicides have attracted great attention due to their potential applications in microelectronics, ceramics, and the aerospace industry. In this study, experimental and theoretical investigations of tungsten based silicides were performed. Tungsten disilicide (WSi{sub 2}) was synthesized by simple thermal treatment at 1350 C for 4 h in an argon atmosphere. These optimal synthesis conditions were obtained by variation of temperatures and times of heating, and the structure of the final synthesized compound was determined by XRPD analysis. In addition, new modifications for WSi{sub 2} were proposed and investigated using first-principles calculations within density-functional theory (DFT). Both LDA and PBE calculations show excellent agreement with experimental observations and previous calculations for the existing modifications, where available. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Fused 1,2,3-Dithiazoles: Convenient Synthesis, Structural Characterization, and Electrochemical Properties

Directory of Open Access Journals (Sweden)

Lidia S. Konstantinova

2016-05-01

Full Text Available A new general protocol for synthesis of fused 1,2,3-dithiazoles by the reaction of cyclic oximes with S2Cl2 and pyridine in acetonitrile has been developed. The target 1,2,3-dithiazoles fused with various carbocycles, such as indene, naphthalenone, cyclohexadienone, cyclopentadiene, and benzoannulene, were selectively obtained in low to high yields. In most cases, the hetero ring-closure was accompanied by chlorination of the carbocyclic moieties. With naphthalenone derivatives, a novel dithiazole rearrangement (15→13 featuring unexpected movement of the dithiazole ring from α- to β-position, with respect to keto group, was discovered. Molecular structure of 4-chloro-5H-naphtho[1,2-d][1,2,3]dithiazol-5-one 13 was confirmed by single-crystal X-ray diffraction. Electrochemical properties of 13 were studied by cyclic voltammetry and a complex behavior was observed, most likely including hydrodechlorination at a low potential.

Chemical synthesis, characterization and evaluation of antimicrobial properties of Cu and its oxide nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Moshalagae Motlatle, Abesach, E-mail: AMotlatle@csir.co.za; Kesavan Pillai, Sreejarani, E-mail: skpillai@csir.co.za; Rudolf Scriba, Manfred, E-mail: MRscriba@csir.co.za; Sinha Ray, Suprakas, E-mail: Rsuprakas@csir.co.za [Council for Scientific and Industrial Research, DST/CSIR Nanotechnology Innovation Centre, National Centre for Nano-Structured Materials (South Africa)

2016-10-15

Cu nanoparticles were synthesized using low-temperature aqueous reduction method at pH 3, 5, 7, 9 and 11 in presence of ascorbic acid and polyvinylpyrrolidone. The nanoparticles were characterized using transmission electron microscopy, scanning electron microscopy, energy-dispersive X-ray spectroscopy, and X-ray diffraction techniques. Results demonstrated a strong dependence of synthesis pH on the size, shape, chemical composition and structure of Cu nanoparticles. While lower pH conditions of 3 and 5 produced Cu{sup 0}, higher pH levels (more than 7) led to the formation of Cu{sub 2}O/CuO nanoparticles. The reducing capacity of ascorbic acid, capping efficiency of PVP and the resulting particle sizes were strongly affected by solution pH. The results of in vitro disk diffusion tests showed excellent antimicrobial activity of Cu{sub 2}O/CuO nanoparticles against a mixture of bacterial strains (Staphylococcus aureus, Escherichia coli and Pseudomonas aeruginosa), indicating that the size as well as oxidation state of Cu contributes to the antibacterial efficacy. The results indicate that varying synthesis pH is a strategy to tailor the composition, structure and properties of Cu nanoparticles.

[Synthesis and Characterization of a Sugar Based Electrolyte for Thin-film Polymer Batteries

Science.gov (United States)

1998-01-01

The work performed during the current renewal period, March 1,1998 focused primarily on the synthesis and characterization of a sugar based electrolyte for thin-film polymer batteries. The initial phase of the project involved developing a suitable sugar to use as the monomer in the polymeric electrolyte synthesis. The monomer has been synthesized and characterized completely. Overall the yield of this material is high and it can be produced in relatively large quantity easily and in high purity. The scheme used for the preparation of the monomer is outlined along with pertinent yields.

Mineralizer-assisted high-pressure high-temperature synthesis and characterization of novel phosphorus nitride imides and luminescent alkaline earth metal (oxo)nitridophosphates

International Nuclear Information System (INIS)

Marchuk, Alexey

2016-01-01

The main objectives of this thesis were the synthesis, identification and structural characterization of new alkaline earth metal (oxo)nitridophopshates and phosphorus nitrides. Furthermore, luminescence properties of the resulting materials should be investigated and a connection between these properties and the respective structures should be established. For this purpose, a range of synthesis strategies was employed, including conventional solid-state syntheses in silica ampoules and high-pressure high-temperature syntheses using the multianvil technique. The emphasis of the synthetic part of this thesis lies on the development of new synthetic strategies in order to increase crystallinity of alkaline earth metal (oxo)nitridophosphates and thus accelerate their structure determination. This involves the selection of a suitable mineralizer and the investigation of its interaction with the respective starting materials. In addition, the analytical methods applied in this thesis in order to identify and characterize the compounds are just as essential as the synthesis strategies. X-ray diffraction on single crystals and on powders was carried out as the main analytical method while being supported by quantitative and qualitative 1 H and 31 P solid-state NMR measurements, FTIR and energy-dispersive X-ray (EDX) spectroscopy, as well as electron microscopy methods including both imaging and diffraction techniques. Implied by the large number of novel structures investigated, theoretical studies including topological analysis, calculations of lattice energies and bond-valence sums also played a major role in this thesis. Optical analysis methods such as reflectance spectroscopy, luminescence microscopy and photoluminescence measurements helped to determine the luminescence properties of some of the presented compounds.

Hydrothermal synthesis, structure and characterization of new ...

Indian Academy of Sciences (India)

Unknown

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

Structural characterization of copper (II) tetradecanoate with 2,2′-bipyridine and 4,4′-bipyridine to study magnetic properties

OpenAIRE

Noha Said Bedowr; Rosiyah Binti Yahya; Nesrain Farhan

2018-01-01

This paper presents synthesis, structural characterization and spintronic applications of copper (II) tetradecanoate derived magnetic complexes. The complexes were prepared by a chemical reaction between [Cu2(CH3(CH2)12COO)4](EtOH)2 and 2,2′-bipyridine-4,4′-bipyridine ligands respectively. The complexes were further reacted between the product of the first reaction and 4,4′-bipyridine-2,2′-bipyridine respectively. The structural characterization techniques included elemental analysis, Fourier...

Novel synthesis and characterization of a collagen-based biopolymer initiated by hydroxyapatite nanoparticles.

Science.gov (United States)

Bhuiyan, D; Jablonsky, M J; Kolesov, I; Middleton, J; Wick, T M; Tannenbaum, R

2015-03-01

In this study, we developed a novel synthesis method to create a complex collagen-based biopolymer that promises to possess the necessary material properties for a bone graft substitute. The synthesis was carried out in several steps. In the first step, a ring-opening polymerization reaction initiated by hydroxyapatite nanoparticles was used to polymerize d,l-lactide and glycolide monomers to form poly(lactide-co-glycolide) co-polymer. In the second step, the polymerization product was coupled with succinic anhydride, and subsequently was reacted with N-hydroxysuccinimide in the presence of dicyclohexylcarbodiimide as the cross-linking agent, in order to activate the co-polymer for collagen attachment. In the third and final step, the activated co-polymer was attached to calf skin collagen type I, in hydrochloric acid/phosphate buffer solution and the precipitated co-polymer with attached collagen was isolated. The synthesis was monitored by proton nuclear magnetic resonance, infrared and Raman spectroscopies, and the products after each step were characterized by thermal and mechanical analysis. Calculations of the relative amounts of the various components, coupled with initial dynamic mechanical analysis testing of the resulting biopolymer, afforded a preliminary assessment of the structure of the complex biomaterial formed by this novel polymerization process. Copyright © 2015. Published by Elsevier Ltd.

Synthesis and Characterization of Novel Quaternary Thioaluminogermanates

KAUST Repository

Al-Bloushi, Mohammed

2013-05-01

Metal chalcogenides form an important class of inorganic materials, which include several technologically important applications. The design of metal chlcogenides is of technological interest and has encouraged recent research into moderate temperature solid-state synthetic methods for the single crystal growth of new materials. The aim of this project is the investigation and development of synthetic methodology for the synthesis of novel metal chlcogenides. The new inorganic compounds of the type “M(AlS2)(GeS2)” (M = Na and K) are new metal-chalcogenides, synthesized by the classical solid state approach. The characterization of these compounds was carried out by Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDS), Single crystal and powder X-ray diffraction, solid state Nuclear Magnetic Resonance (NMR), Ultraviolet-visible (UV-VIS), Infrared (IR) and Raman spectroscopy. These theses study the synthesis of metal chalcogenides through the use of standard chemical techniques. The systematic studies demonstrate the effect of the reactants ratio and reaction temperature on the synthesis and growth of the single crystals. Metal chalcogenides have several potential applications in gas separation, ion exchange, environmental remediation, and energy storage. Especially, the ion exchange materials have found\\tpossible applications in waste-water treatment, water softening, metal separation, and production of high purity water.

Synthesis and Characterization of Fluoro- and Chlorobimetallic Alkoxides as Precursors for Luminescent Metal Oxide Materials via Sol-Gel Technique

Institute of Scientific and Technical Information of China (English)

ATHAR, Taimur; SEOK, Sang II; KWON, Jeong Oh

2007-01-01

Heterobimetallic alkoxides are broadly recognized as versatile precursors for luminescence materials, and efforts are being made to develop novel routes by applying the concept of geometrical molecular design, for their synthesis and to design a single source precursor suited to photoluminescent materials. Novel and new series of bimetallic alkoxides has been prepared by metathesis route. They exhibit a lower sensitivity towards hydrolysis and so they are easier to handle as compared to other alkoxides. All the compounds were characterized by elemental analysis, FT-IR and multinuclear NMR spectroscopies. FT-IR revealed that the molecular structure of these metal spectroscopy provided useful information about chemical shifts for better understanding the likely structure based on interactions with their coordinate metals. The mass spectra show similar types of fragmentation pattern.SEM-EDS analyses showed consistency with the formulation. XRD patterns show an enhanced homogeneity at high temperature. TGA measurements show that thermal decomposition occured in steps that depended entirely on the chemical compositions and the synthesis routes. SEM observation reveals that the morphology and particle size strongly depend on synthesis routes for their precursors.

Synthesis and characterization of zeolite P using technical-grade materials

CERN Document Server

Aghabozorg, H R; Aghabozorg, H R; Sharif, M

2001-01-01

Research attempts on zeolites show structural and industrial importance of these inorganic compounds. In this regard, the synthesis of zeolites is of great importance, because their natural occurring counterparts are often impure. Zeolite Na-P with a silicon to aluminium ratio of one has a better ion exchange capacity than Na-A and can be used as a detergent builder. In this work, zeolite Na-P of high purity was successfully synthesized using commercial silica and alumina sources. parameters such as H sub 2 O:A1 sub 2 O sub 3 and SiO sub 2 :A1 sub 2 O sub 3 molar ratios and crystallization temperature and time were investigated. So that the optimum condition was obtained. X-ray powder diffraction, infrared, scanning electron microscopy and elemental analysis were utilized for the characterization of the product.

Synthesis, characterization, spectroscopic properties and DFT study of a new pyridazinone family

Science.gov (United States)

Arrue, Lily; Rey, Marina; Rubilar-Hernandez, Carlos; Correa, Sebastian; Molins, Elies; Norambuena, Lorena; Zarate, Ximena; Schott, Eduardo

2017-11-01

Nitrogen compounds are widely investigated due to their pharmacological properties such as antihypertensive, antinociceptive, antibacterial, antifungal, analgesic, anticancer and inhibition activities and lately even as pesticide. In this context, we present the synthesis of new compounds: (E)-6-(3,4-dimethoxyphenyl)-3-(3-(3,4-dimethoxyphenyl)acryloyl)-1-(4-R-phenyl)- 5,6-dihydropyridazin-4(1H)-one (with R = sbnd H(1), -Cl(2), -Br(3), sbnd I(4) and sbnd COOH(5)) that was carried out by reaction of (1E, 6E)-1,7-bis(3,4-dimethoxyphenyl)hepta-1,6-diene-3,5-dione with a substituted phenylamine with general formula p-R-C6H4sbnd NH2 (R = sbnd H (1), sbnd Cl (2), -Br(3), sbnd I(4) and sbnd COOH(5)). This is the first synthesis report of a pyridazinone using as precursors a curcuminoid derivative and a diazonium salt formed in situ. All compounds were characterized by EA, FT-IR, UV-Vis, Emission,1H- and13C-NMR spectroscopy and the crystalline and molecular structure of 4 was solved by X-rays diffraction method. DFT and TD-DFT quantum chemical calculations were also employed to characterize the compounds and provide a rational explanation to the spectroscopic properties. To assess the biological activity of the systems, we focused on pesticide tests on compound 2, which showed an inhibitory effect in plant growth of Agrostis tenuis Higland.

Total synthesis of the proposed structure of trichodermatide A.

Science.gov (United States)

Myers, Eddie; Herrero-Gómez, Elena; Albrecht, Irina; Lachs, Jennifer; Mayer, Peter; Hanni, Matti; Ochsenfeld, Christian; Trauner, Dirk

2014-10-17

A short total synthesis of the published structure of racemic trichodermatide A is reported. Our synthesis involves a Knoevenagel condensation/Michael addition sequence, followed by the formation of tricyclic hexahydroxanthene-dione and a diastereoselective bis-hydroxylation. The final product, the structure of which was confirmed by X-ray crystallography, has NMR spectra that are very similar, but not identical, to those of the isolated natural product. Quantum chemically computed (13)C shifts agree well with the present NMR measurements.

Designing Selectivity in Metal-Semiconductor Nanocrystals: Synthesis, Characterization, and Self-Assembly

Science.gov (United States)

Pavlopoulos, Nicholas George

This dissertation contains six chapters detailing recent advances that have been made in the synthesis and characterization of metal-semiconductor hybrid nanocrystals (HNCs), and the applications of these materials. Primarily focused on the synthesis of well-defined II-VI semiconductor nanorod (NR) and tetrapod (TP) based constructs of interest for photocatalytic and solar energy applications, the research described herein discusses progress towards the realization of key design rules for the synthesis of functional semiconductor nanocrystals (NCs). As such, a blend of novel synthesis, advanced characterization, and direct application of heterostructured nanoparticles are presented. The first chapter is a review summarizing the design, synthesis, properties, and applications of multicomponent nanomaterials composed of disparate semiconductor and metal domains. By coupling two compositionally distinct materials onto a single nanocrystal, synergistic properties can arise that are not present in the isolated components, ranging from self-assembly to photocatalysis. For semiconductor nanomaterials, this was first realized in the ability to tune nanomaterial dimensions from 0-D quantum dot (QD) structures to cylindrical (NR) and branched (TP) structures by exploitation of advanced colloidal synthesis techniques and understandings of NC facet reactivities. The second chapter is focused on the synthesis and characterization of well-defined CdSe-seeded-CdS (CdSe CdS) NR systems synthesized by overcoating of wurtzite (W) CdSe quantum dots with W-CdS shells. 1-dimensional NRs have been interesting constructs for applications such as solar concentrators, optical gains, and photocatalysis. Through synthetic control over CdSe CdS NR systems, materials with small and large CdSe seeds were prepared, and for each seed size, multiple NR lengths were prepared. Through transient absorption studies, it was found that band alignment did not affect the efficiency of charge localization

Synthesis and characterization of iron (II and III) phosphates by X-ray diffraction and Scanning Electron Microscopy of high vacuum

International Nuclear Information System (INIS)

Diaz F, J.C.; Solis M, L.; Garcia R, G.; Romero G, E.T.

2002-01-01

The XRD and Sem techniques for determining the mineralogical and structural composition of iron II and III phosphates have been used. The mineralogical and structural composition of the materials revealed that they are the ferrous phosphate and the ferric phosphate. The contribution of the synthesis and characterization of these phosphates is that they can be used as components in the geological barriers capable to avoiding the dispersion from the hazardous radioactive materials to the environment. (Author)

Functional coordination polymers and MOFs from reactions of the lanthanides and barium with azole ligands. Synthesis and characterization with a focus on structure determination from X-ray powder diffraction data

International Nuclear Information System (INIS)

Rybak, Jens-Christoph

2012-01-01

This thesis deals with the synthesis and characterization of coordination polymers and MOFs of the lanthanides and barium with different azolic N-heterocycles. A total of 18 new organic-inorganic hybrid materials, as well as a series of co-doped compounds is presented. Besides the structural characterization of these materials from X-ray diffraction powder data, the focus of the investigations is on the thermal and photoluminescence spectroscopic properties. The lanthanides La - Lu, except Eu and Pm, can be reacted with 1H-1,2,3-triazole to give the series of the isotypic dense 3D-MOFs 3 ∞ [Ln(Tz * ) 3 ]. Investigation of the photoluminescence properties of these compounds reveals a broad range of different luminescence phenomena, including the first observation of an intrinsic inner-filter effect of the Ln 3+ -ions. The structure of this isotypic series of compounds was solved and refined from X-ray powder diffraction data. A 2D-polymorph of these compounds 2 ∞ [Ln(Tz * ) 3 ], is observed for Ln = Sm, Tb and was characterized by single crystal data. The reaction of Eu with 1H-benzotriazole yields the 1D-coordination polymer 1 ∞ [Eu(Btz) 2 (BtzH) 2 ], which is the first example of a divalent rare earth benzotriazolate. Analysis of the thermal properties reveals the transformation to the 3D-MOF 3 ∞ [Eu(Btz) 2 ] at higher temperatures. The structure of this material was also solved from X-ray powder diffraction data. Investigation of the photoluminescence properties of the co-doped compounds 3 ∞ [Ba 1-x Eu x (Im) 2 ], which were obtained from reaction of the salt-like hydrides BaH 2 and EuH 2 with imidazole, show that the synthesis of luminescent MOF materials by co-doping of non-luminescent networks with luminescence centers is possible. The structure of these materials was solved from X-ray powder diffraction data of the undoped compound 3 ∞ [BaEu(Im) 2 ]. Structural characterization of materials from X-ray powder diffraction data is an important aspect

Synthesis and characterization of thorium(IV) and uranium(IV) complexes with Schiff bases

Energy Technology Data Exchange (ETDEWEB)

Radoske, Thomas; Maerz, Juliane; Kaden, Peter; Patzschke, Michael; Ikeda-Ohno, Atsushi [Helmholtz-Zentrum Dresden-Rossendorf e.V., Dresden (Germany). Chemistry of the F-Elements

2017-06-01

We report herein the synthesis and characterization of several imine complexes of tetravalent thorium (Th(IV)) and uranium (U(IV)). The ligands investigated in this study are a Schiff base type, including the well-known salen ligand (H{sub 2}Le, Fig. 1). The complexation in solution was investigated by NMR measurements indicating paramagnetic effects of unpaired f-electrons of U(IV) on the ligand molecule. We also determined the solid-state molecular structures of the synthesized complexes by single crystal X-ray diffraction. The synthesized complexes show an eight-fold coordination geometry around the actinide center surrounded by two tetradentate ligands with 2N- and 2O-donor atoms.

Microwave Synthesis and Characterization of Waste Soybean Oil-Based Gemini Imidazolinium Surfactants with Carbonate Linkage

Science.gov (United States)

Tripathy, Divya Bajpai; Mishra, Anuradha

Gemini surfactants are presently gaining attention due to their unusual self-assembling characteristics and incomparable interfacial activity. Current research work involves the cost-effective microwave (MW) synthesis of waste soybean oil-based gemini imidazolinium surfactants (GIS) having a carbonate linkage in its spacer moiety. Structural characterizations of the materials have been done using FT-IR, 1H-NMR and 13C-NMR. Using indigenous and natural material as base and MW as energy source for synthesizing the GIS with easily degradable chemical moiety make them to be labeled as green surfactants.

Synthesis and characterization of innovative insulation materials

Directory of Open Access Journals (Sweden)

Skaropoulou Aggeliki

2018-01-01

Full Text Available Insulation elements are distinguished in inorganic fibrous and organic foamed materials. Foamed insulation materials are of great acceptance and use, but their major disadvantage is their flammability. In case of fire, they tend to transmit the flame producing toxic gases. In this paper, the synthesis and characterization of innovative inorganic insulation materials with properties competitive to commercial is presented. Their synthesis involves the mixing of inorganic raw material and water with reinforcing agent or/and foaming agent leading to the formation of a gel. Depending on raw materials nature, the insulation material is produced by freeze drying or ambient drying techniques of the gel. The raw material used are chemically benign and abundantly available materials, or industrial by-products and the final products are non-toxic and, in some cases, non-flammable. Their density and thermal conductivity was measured and found 0.02-0.06 g/cm3 and 0.03-0.04 W/mK, respectively.

Facile Synthesis of Yolk/Core-Shell Structured TS-1@Mesosilica Composites for Enhanced Hydroxylation of Phenol

KAUST Repository

Zou, Houbing

2015-12-14

© 2015 by the authors. In the current work, we developed a facile synthesis of yolk/core-shell structured TS-1@mesosilica composites and studied their catalytic performances in the hydroxylation of phenol with H2O2 as the oxidant. The core-shell TS-1@mesosilica composites were prepared via a uniform coating process, while the yolk-shell TS-1@mesosilica composite was prepared using a resorcinol-formaldehyde resin (RF) middle-layer as the sacrificial template. The obtained materials were characterized by X-ray diffraction (XRD), N2 sorption, Fourier transform infrared spectoscopy (FT-IR) UV-Visible spectroscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The characterization results showed that these samples possessed highly uniform yolk/core-shell structures, high surface area (560–700 m2 g−1) and hierarchical pore structures from oriented mesochannels to zeolite micropores. Importantly, owing to their unique structural properties, these composites exhibited enhanced activity, and also selectivity in the phenol hydroxylation reaction.

Synthesis and Characterization of Two New p-tert-Butylcalix[4]-arene Schiff Bases

Directory of Open Access Journals (Sweden)

Saeed Taghvaee Ganjali

2001-03-01

Full Text Available Synthesis and characterization of two new Schiff bases of p-tertbuthylcalix[4]arene (H2L1 and HL2 is described. The synthesis of H2L1 and HL2 has been achieved by the condensation of salicylaldehyde with the amine group of upper rim monoamine p-tert-butylcalix[4]arene in ethanol. These compounds have been characterized on the basis of elemental analysis and spectral data. Solvatochromicity and fluorescence properties were observed and measured for H2L1 and HL2. Solvatochromicity of these ligands indicates their potential for NLO applications.

Synthesis and characterization of LiFePO{sub 4} cathode preparation by low temperature method

Energy Technology Data Exchange (ETDEWEB)

Rajesh, Desapogu, E-mail: rajesh.desapogu@gmail.com; Srinivas Naik, V.; Sunandana, C.S., E-mail: sunandana@gmail.com

2015-05-01

We review in detail the physics and technology of the novel material LiFePO{sub 4}, a potential cathode material for Li-ion batteries. In the present work, nano crystalline LiFePO{sub 4} film has been synthesized in both powder and thin film forms from a non-aqueous sol–gel synthesis route based on oxalates of Li and Fe (II). Ferrous oxalate has been synthesized indigenously using a ferrous sulphate based chemical reaction and characterized. Nano powders and thin films of LiFePO{sub 4} have been fabricated and coated on stainless steel substrates with the aim of device development in future. The material has been characterized extensively by XRD for crystal structure, FESEM for microstructure, EDS for elemental analysis and FTIR for the internal modes of phosphate ion. Fe{sup 3+} impurity characterization has been done by using ESR.

Structural Characterization of Bimetallic Nanocrystal Electrocatalysts

Energy Technology Data Exchange (ETDEWEB)

Cullen, David A [ORNL

2016-01-01

Late transition metal nanocrystals find applications in heterogeneous catalysis such as plasmon-enhanced catalysis and as electrode materials for fuel cells, a zero-emission and sustainable energy technology. Their commercial viability for automotive transportation has steadily increased in recent years, almost exclusively due to the discovery of more efficient bimetallic nanocatalysts for the oxygen reduction reaction (ORR) at the cathode. Despite improvements to catalyst design, achieving high activity while maintaining durability is essential to further enhance their performance for this and other important applications in catalysis. Electronic effects arising from the generation of metal-metal interfaces, from plasmonic metals, and from lattice distortions, can vastly improve sorption properties at catalytic surfaces, while increasing durability.[1] Multimetallic lattice-strained nanoparticles are thus an interesting opportunity for fundamental research.[2,3] A colloidal synthesis approach is demonstrated to produce AuPd alloy and Pd@Au core-shell nanoicosahedra as catalysts for electro-oxidations. The nanoparticles are characterized using aberration-corrected scanning transmission electron microscopy (ac-STEM) and large solid angle energy dispersive X-ray spectroscopy (EDS) on an FEI Talos 4-detector STEM/EDS system. Figure 1 shows bright-field (BF) and high-angle annular dark-field (HAADF) ac-STEM images of the alloy and core-shell nanoicosahedra together with EDS line-scans and elemental maps. These structures are unique in that the presence of twin boundaries, alloying, and core-shell morphology could create highly strained surfaces and interfaces. The shell thickness of the core-shell structures observed in HAADF-STEM images is tuned by adjusting the ratio between metal precursors (Figure 2a-f) to produce shells ranging from a few to several monolayers. Specific activity was measured in ethanol electro-oxidation to examine the effect of shell thickness on

Synthesis and physicochemical characterizations and antimicrobial activity of ZnO nanoparticles

Science.gov (United States)

Sharma, Bhumika K.; Patel, Kinjal; Roy, Debesh R.

2018-05-01

Nanoparticles exhibit very interesting and useful physicochemical properties when they interact with substrates and goes through some physicochemical and/or biological processes. ZnO is known to be a highly demanding nanomaterial due to its discreet properties, shapes and sizes. A detail experimental study on the synthesis, characterization and antibacterial activity of ZnO nanoparticles (NPs) is performed. ZnO NPs are synthesized using chemical precipitation method. The understanding of crystal structure, morphology and elemental compositions are explained using Powder X-Ray Diffraction (XRD) and Field Emission Scanning Electron Microscope (FE-SEM) respectively. Fourier transform infrared spectroscopy (FTIR) is performed to achieve the information on the presence of various functional groups. The antibacterial activity of these ZnO NPs is investigated in terms of Zone of Inhibition (ZOI) against Escherichia coli (Gram negative) microorganisms.

Graphene optoelectronics synthesis, characterization, properties, and applications

CERN Document Server

bin M Yusoff, Abdul Rashid

2014-01-01

This first book on emerging applications for this innovative material gives an up-to-date account of the many opportunities graphene offers high-end optoelectronics.The text focuses on potential as well as already realized applications, discussing metallic and passive components, such as transparent conductors and smart windows, as well as high-frequency devices, spintronics, photonics, and terahertz devices. Also included are sections on the fundamental properties, synthesis, and characterization of graphene. With its unique coverage, this book will be welcomed by materials scientists, solid-

Alpha amylase assisted synthesis of TiO{sub 2} nanoparticles: Structural characterization and application as antibacterial agents

Energy Technology Data Exchange (ETDEWEB)

Ahmad, Razi; Mohsin, Mohd [Department of Biosciences, Jamia Millia Islamia, New Delhi 110025 (India); Ahmad, Tokeer [Department of Chemistry, Jamia Millia Islamia, New Delhi 110025 (India); Sardar, Meryam, E-mail: msardar@jmi.ac.in [Department of Biosciences, Jamia Millia Islamia, New Delhi 110025 (India)

2015-02-11

Graphical abstract: - Highlights: • Green synthesis of TiO{sub 2} nanoparticles using an enzyme alpha amylase has been described. • The morphology and shape depends upon the concentration of the alpha amylase enzyme. • The biosynthesized nanoparticles show good bactericidal effect against both gram positive and gram negative bacteria. • The bactericidal effect was further confirmed by Confocal microscopy and TEM. - Abstract: The enzyme alpha amylase was used as the sole reducing and capping agent for the synthesis of TiO{sub 2} nanoparticles. The biosynthesized nanoparticles were characterized by X-ray diffraction (XRD) and transmission electron microscopic (TEM) methods. The XRD data confirms the monophasic crystalline nature of the nanoparticles formed. TEM data shows that the morphology of nanoparticles depends upon the enzyme concentration used at the time of synthesis. The presence of alpha amylase on TiO{sub 2} nanoparticles was confirmed by FTIR. The nanoparticles were investigated for their antibacterial effect on Staphylococcus aureus and Escherichia coli. The minimum inhibitory concentration value of the TiO{sub 2} nanoparticles was found to be 62.50 μg/ml for both the bacterial strains. The inhibition was further confirmed using disc diffusion assay. It is evident from the zone of inhibition that TiO{sub 2} nanoparticles possess potent bactericidal activity. Further, growth curve study shows effect of inhibitory concentration of TiO{sub 2} nanoparticles against S. aureus and E. coli. Confocal microscopy and TEM investigation confirm that nanoparticles were disrupting the bacterial cell wall.

Neutral, seven-coordinate dioxime complexes of technetium(III): Synthesis and characterization

International Nuclear Information System (INIS)

Linder, K.E.; Malley, M.F.; Gougoutas, J.Z.; Unger, S.E.; Nunn, A.D.

1990-01-01

The tin-capped complexes 99 Tc(oxime) 3 (μ-OH)SnCl 3 [oxime = dimethylglyoxime (DMG) or cyclohexanedione dioxime (CDO)] can be prepared by the reduction of NH 4 TcO 4 with 2 equiv of SnCl 2 in the presence of dioxime and HCl. These tin-capped complexes can be readily converted into a new class of uncapped Tc-dioxime compounds, TcCl(oxime) 3 , by treatment with HCl. This reaction is reversible. Both the tin-capped and uncapped tris(dioxime) complexes can be converted to the previously reported boron-capped Tc-dioxime complexes TcCl(oxime) 3 BR (R = alkyl, OH) by reaction with boronic acids or with boric acid at low pH. All of these complexes [Tc(oxime) 3 (μ-OH)SnCl 3 , TcCl(oxime) 3 , and TcCl(oxime) 3 BR] appear to be neutral, seven-coordinate compounds of technetium(III). They have been characterized by elemental analysis, 1 H NMR and UV/visible spectroscopy, conductivity, and fast atom bombardment mass spectrometry. The synthesis, characterization, and reactivity of these compounds is discussed. The x-ray crystal structure analysis of TcCl(DMG) 3 and an abbreviated structure report on TcCl(DMG) 3 MeB are described. Crystal data for TcCl(DMG) 3 are reported. 23 refs., 6 figs., 5 tabs

Facile synthesis of gold nanomaterials with unusual crystal structures.

Science.gov (United States)

Fan, Zhanxi; Huang, Xiao; Chen, Ye; Huang, Wei; Zhang, Hua

2017-11-01

Gold (Au) nanomaterials have attracted wide research attention, owing to their high chemical stability, promising catalytic properties, excellent biocompatibility, unique electronic structure and outstanding localized surface plasmon resonance (LSPR) absorption properties; all of which are closely related to their size and shape. Recently, crystal-phase-controlled synthesis of noble metal nanomaterials has emerged as a promising strategy to tune their physicochemical properties. This protocol describes the detailed experimental procedures for the crystal-phase-controlled syntheses of Au nanomaterials with unusual crystal structures under mild conditions. Briefly, pure hexagonal close-packed (hcp) Au square sheets (AuSSs) with a thickness of ∼2.4 nm are synthesized using a graphene-oxide-assisted method in which HAuCl 4 is reduced by oleylamine in a mixture of hexane and ethanol. By using pure hexane as the solvent, well-dispersed ultrathin hcp/face-centered cubic (fcc) Au nanowires with a diameter of ∼1.6 nm on graphene oxide can be obtained. Meanwhile, hcp/fcc Au square-like plates with a side length of 200-400 nm are prepared via the secondary growth of Au on the hcp AuSSs. Remarkably, hexagonal (4H) Au nanoribbons with a thickness of 2.0-6.0 nm can be synthesized with a one-pot colloidal method in which HAuCl 4 is reduced by oleylamine in a mixed solvent of hexane and 1,2-dichloropropane. It takes 17-37 h for the synthesis of these Au nanomaterials with unusual crystal structures. Transmission electron microscopy (TEM) and atomic force microscopy (AFM) are used to characterize the resultant Au nanomaterials, which could have many promising applications, such as biosensing, near-IR photothermal therapy, catalysis and surface-enhanced Raman scattering (SERS).

Stop Flow Lithography Synthesis and Characterization of Structured Microparticles

Directory of Open Access Journals (Sweden)

David Baah

2014-01-01

Full Text Available In this study, the synthesis of nonspherical composite particles of poly(ethylene glycol diacrylate (PEG-DA/SiO2 and PEG-DA/Al2O3 with single or multiple vias and the corresponding inorganic particles of SiO2 and Al2O3 synthesized using the Stop Flow Lithography (SFL method is reported. Precursor suspensions of PEG-DA, 2-hydroxy-2-methylpropiophenone, and SiO2 or Al2O3 nanoparticles were prepared. The precursor suspension flows through a microfluidic device mounted on an upright microscope and is polymerized in an automated process. A patterned photomask with transparent geometric features masks UV light to synthesize the particles. Composite particles with vias were synthesized and corresponding inorganic SiO2 and Al2O3 particles were obtained through polymer burn-off and sintering of the composites. The synthesis of porous inorganic particles of SiO2 and Al2O3 with vias and overall dimensions in the range of ~35–90 µm was achieved. BET specific surface area measurements for single via inorganic particles were 56–69 m2/g for SiO2 particles and 73–81 m2/g for Al2O3 particles. Surface areas as high as 114 m2/g were measured for multivia cubic SiO2 particles. The findings suggest that, with optimization, the particles should have applications in areas where high surface area is important such as catalysis and sieving.

Synthesis and structural characterization of manganese olivine lithium phosphate

Energy Technology Data Exchange (ETDEWEB)

Herrera Robles, Joel O. [Basic Science Department, IIT, Universidad Autónoma de Ciudad Juárez, Av. del Charro 460 norte Cd. Juárez, Chih. C.P. 32310 (Mexico); Fuentes Cobas, Luis E. [Centro de Investigación en Materiales Avanzados CIMAV, Complejo Industrial, M. Cervantes 120, Chihuahua C.P. 31109 (Mexico); Díaz de la Torre, Sebastián [Instituto Politécnico Nacional, Centro de Investigación e Innovación Tecnológica CIITEC, Azcapotzalco, México, D.F. C.P. 02250 (Mexico); Camacho Montes, Héctor, E-mail: hcamacho@uacj.mx [Basic Science Department, IIT, Universidad Autónoma de Ciudad Juárez, Av. del Charro 460 norte Cd. Juárez, Chih. C.P. 32310 (Mexico); Elizalde Galindo, José T.; García Casillas, Perla E.; Rodríguez González, Claudia A. [Basic Science Department, IIT, Universidad Autónoma de Ciudad Juárez, Av. del Charro 460 norte Cd. Juárez, Chih. C.P. 32310 (Mexico); Álvarez Contreras, Lorena [Centro de Investigación en Materiales Avanzados CIMAV, Complejo Industrial, M. Cervantes 120, Chihuahua C.P. 31109 (Mexico)

2015-09-15

Highlights: • LiMnPO{sub 4} was obtained by sol gel method and crystallization in reducing atmosphere. • Magnetic and electric properties are reported for LiMnPO{sub 4}. • Electrochemical properties are also found and enhanced by adding carbon. • SEM and HRTEM show the submicron powder nature. • The multifunctional behavior of LiMnPO{sub 4} is experimentally demonstrated. - Abstract: The manganese olivine lithium phosphate is a multifunctional material. If carbon is added to form a composite LiMnPO{sub 4}–C, electrochemical properties can be enhanced, making this material a good candidate for battery cathode. High magnetic susceptibility is reported for this compound at room temperature. In this work, the magnetic response was measured through a Field Cooling/Zero Field Cooling technique at temperature below 100 K. Weak ferroelectric properties at room temperature were measured. Even though, the promising applications and the interesting properties of this system, the attention received in the literature is relatively low. The synthesis of this material is difficult because of the rapid manganese oxidation and the need of a reducing atmosphere. In fact, only few authors report the synthesis of the pure phase. In the present work, nanostructured LiMnPO{sub 4} is obtained by sol gel chemical method and according to X-ray diffraction patterns, pure LiMnPO{sub 4} is obtained after calcination in a reducing atmosphere (10% H{sub 2} – 90% Ar). Nanostructured LiMnPO{sub 4} is a material with very interesting properties that deserves attentions.

Hydrothermal synthesis, characterization, and thermal properties of alumino silicate azide sodalite, Na8[AlSiO4]6(N3)2

Science.gov (United States)

Borhade, A. V.; Wakchaure, S. G.; Dholi, A. G.; Kshirsagar, T. A.

2017-07-01

First time we report the synthesis, structural characterization and thermal behavior of an unusual N3 - containing alumino-silicate sodalite mineral. Azide sodalite, Na8[AlSiO4]6(N3)2 has been synthesized under hydrothermal conditions at 433 K in steel lined Teflon autoclave. The structural and microstructural properties of azide sodalite mineral was characterized by various methods including FT-IR, XRD, SEM, TGA, and MAS NMR. Crystal structure have been refined by Rietveld method in P\\bar 43n space group, indicating that the N3 - sodalite has cubic in lattice. High temperature study was carried out to see the effect of thermal expansion on cell dimension ( a o) of azide sodalite. Thermal behavior of sodalite was also assessed by thermogravimetric method.

Synthesis and structure of the unligated carbene of chromium

Energy Technology Data Exchange (ETDEWEB)

Billups, W.E.; Souchan Chang; Hauge, R.H.; Margrave, J.L. (Rice Univ., Houston, TX (United States))

1993-04-14

Complexes with metal-carbon double bonds have found applications as intermediates in many important catalytic reactions including cyclopropanation of alkenes by diazoalkanes, Fischer-Tropsch synthesis, olefin metathesis, Ziegler-Natta polymerization, alkane activation, and in the decomposition of transition metal alkyl complexes. However, complexes with the simplest carbene, CH[sub 2], coordinated to the metal center are relatively rare. In this paper the authors report the synthesis and characterization of the simple unligated carbene of chromium by FTIR matrix isolation spectroscopy. 7 refs., 3 figs., 4 tabs.

Synthesis and magnetic characterization of LaMnO{sub 3} nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Hernandez, E.; Sagredo, V. [Universidad de Los Andes, Facultad de Ciencias, Laboratorio de Magnetismo, 5101 Merida (Venezuela, Bolivarian Republic of); Delgado, G. E. [Universidad de Los Andes, Facultad de Ciencias, Laboratorio de Cristalografia, 5101 Merida (Venezuela, Bolivarian Republic of)

2015-07-01

LaMnO{sub 3} nanoparticles system were prepared by the sol-gel auto-combustion method, in order to analyze the structure and magnetic behavior presented by the compound prepared following a new alternative route of synthesis. Structural characterization, morphology and crystallite size was performed by X-ray diffraction (XRD), infrared spectroscopy (IR) and electron microscopy. The XRD study together with a Rietveld analysis showed that the LaMnO{sub 3} compound crystallized in a perovskite hexagonal structure. The IR spectra showed that the compound has tensile energy bands in the Mn-O-Mn bonds related with the octahedron MnO{sub 6}; which are attributed to a characteristic vibration of the ABO{sub 3} perovskite. An estimated size and morphological analysis was carried out by applying the Scherrer formula and using transmission electron microscopy, revealing non-spherical shape and particle sizes between 13 nm and 18 nm. The magnetic measurements M(T) were performed by using zero field-cooled and field-cooled protocols which revealed a positive Weiss temperature indicating the presence of ferromagnetic interactions with a Curie temperature, T{sub C} = 150 K. (Author)

Synthesis and Structural Characterization of 1- and 2-Substituted Indazoles: Ester and Carboxylic Acid Derivatives

Directory of Open Access Journals (Sweden)

Isabel Bento

2006-11-01

Full Text Available A series of indazoles substituted at the N-1 and N-2 positions with ester-containing side chains -(CH2nCO2R of different lengths (n = 0-6, 9, 10 are described.Nucleophilic substitution reactions on halo esters (X(CH2nCO2R by 1H-indazole inalkaline solution lead to mixtures of N-1 and N-2 isomers, in which the N-1 isomerpredominates. Basic hydrolysis of the ester derivatives allowed the synthesis of thecorresponding indazole carboxylic acids. All compounds were fully characterised bymultinuclear NMR and IR spectroscopies, MS spectrometry and elemental analysis; theNMR spectroscopic data were used for structural assignment of the N-1 and N-2 isomers.The molecular structure of indazol-2-yl-acetic acid (5b was determined by X-raydiffraction, which shows a supramolecular architecture involving O2-H...N1intermolecular hydrogen bonds.

Structural Studies of Silver Nanoparticles Obtained Through Single-Step Green Synthesis

Science.gov (United States)

Prasad Peddi, Siva; Abdallah Sadeh, Bilal

2015-10-01

Green synthesis of silver Nanoparticles (AGNP's) has been the most prominent among the metallic nanoparticles for research for over a decade and half now due to both the simplicity of preparation and the applicability of biological species with extensive applications in medicine and biotechnology to reduce and trap the particles. The current article uses Eclipta Prostrata leaf extract as the biological species to cap the AGNP's through a single step process. The characterization data obtained was used for the analysis of the sample structure. The article emphasizes the disquisition of their shape and size of the lattice parameters and proposes a general scheme and a mathematical model for the analysis of their dependence. The data of the synthesized AGNP's has been used to advantage through the introduction of a structural shape factor for the crystalline nanoparticles. The properties of the structure of the AGNP's proposed and evaluated through a theoretical model was undeviating with the experimental consequences. This modus operandi gives scope for the structural studies of ultrafine particles prepared using biological methods.

Radiation synthesis and characterization of network structure of natural/synthetic double-network superabsorbent polymers

International Nuclear Information System (INIS)

Sen, M.; Hayrabolulu, H.

2011-01-01

Complete text of publication follows. Superabsorbent polymers (SAPs) are moderately cross linked, 3-D, hydrophilic network polymers that can absorb and conserve considerable amounts of aqueous fluids even under certain heat or pressure. Because of the unique properties superior to conventional absorbents, SAPs have found potential application in many fields such as hygienic products, disposable diapers, horticulture, gel actuators, drug-delivery systems, as well as water-blocking tapes coal dewatering, water managing materials for the renewal of arid and desert environment, etc. In recent years, naturally available resources, such as polysaccharides have drawn considerable attention for the preparation of SAPs. Since the mechanical properties of polysaccharide based natural polymers are low, researchers have mostly focused on natural/synthetic polymer/monomer mixtures to obtain novel SAPs. The aim of this study is to synthesize and characterization of network structure of novel double-network (DN) hydrogels as a SAP. Hydrogels with high mechanical strength have been prepared by radiation induced polymerization and crosslink of acrylic acid sodium salt in the presence of natural polymer locust bean gum. Liquid retention capacities and absorbency under load (AUL) analysis of synthesized SAPs was performed at different temperatures in water and synthetic urine solution, in order to determine their SAP character. For the characterization of network structure of the semi-IPN hydrogels, the average molecular weight between cross links (M c ) were evaluated by using uniaxial compression and oscillatory dynamical mechanical analyses and the advantage and disadvantage of these two technique for the characterization of network structures were compared.

Ultrasound-assisted synthesis of nano-structured Zinc(II)-based metal-organic frameworks as precursors for the synthesis of ZnO nano-structures.

Science.gov (United States)

Bigdeli, Fahime; Ghasempour, Hosein; Azhdari Tehrani, Alireza; Morsali, Ali; Hosseini-Monfared, Hassan

2017-07-01

A 3D, porous Zn(II)-based metal-organic framework {[Zn 2 (oba) 2 (4-bpmn)]·(DMF) 1.5 } n (TMU-21), (4-bpmn=N,N'-Bis-pyridin-4-ylmethylene-naphtalene-1,5-diamine, H 2 oba=4,4'-oxybis(benzoic acid)) with nano-rods morphology under ultrasonic irradiation at ambient temperature and atmospheric pressure was prepared and characterized by scanning electron microscopy. Sonication time and concentration of initial reagents effects on the size and morphology of nano-structured MOFs were studied. Also {[Zn 2 (oba) 2 (4-bpmn)] (TMU-21) and {[Zn 2 (oba) 2 (4-bpmb)] (TMU-6), 4-bpmb=N,N'-(1,4-phenylene)bis(1-(pyridin-4-yl)methanimine) were easily prepared by mechanochemical synthesis. Nanostructures of Zinc(II) oxide were obtained by calcination of these compounds and their de-solvated analogue as activated MOFs, at 550°C under air atmosphere. As a result of that, different Nanostructures of Zinc(II) oxide were obtained. The ZnO nanoparticles were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and FT-IR spectroscopy. Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis and conductivity of heptadecatungstovanadodiphosphoric heteropoly acid with Dawson structure

Energy Technology Data Exchange (ETDEWEB)

Tong Xia; Zhu Weiming [Department of Chemistry, Zhejiang University, Hangzhou 310027 (China); Wu Qingyin, E-mail: qywu@zju.edu.cn [Department of Chemistry, Zhejiang University, Hangzhou 310027 (China); Qian Xueyu; Liu Zhen [Department of Chemistry, Zhejiang University, Hangzhou 310027 (China); Yan Wenfu [State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, Jilin University, Changchun 130012 (China); Gong Jian [Key Lab of Polyoxometalate Science, the Ministry of Education, Northeast Normal University, Changchun 130024 (China)

2011-07-21

A new solid high-proton conductor, heptadecatungstovanadodiphosphoric heteropoly acid H{sub 7}P{sub 2}W{sub 17}VO{sub 62}.28H{sub 2}O with Dawson structure was synthesized by the stepwise acidification and the stepwise addition of element solutions. The optimal proportion of component compounds in the synthesis reaction was given. The product was characterized by chemical analysis, potentiometric titration, IR, UV, XRD, {sup 31}P NMR, TG-DTA and electrochemical impedance spectroscopy (EIS). The results indicate that H{sub 7}P{sub 2}W{sub 17}VO{sub 62}.28H{sub 2}O possesses the Dawson structure. EIS measurements show a high conductivity (3.10 x 10{sup -2} S cm{sup -1} at 26 deg. C and 75% relative humidity), with an activation energy of 32.23 kJ mol{sup -1} for proton conduction. The mechanism of proton conduction for this heteropoly acid is Vehicle mechanism.

Microwave hydrothermal synthesis and characterization of PZT 52/48 powders

International Nuclear Information System (INIS)

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

2009-01-01

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

PROSPECTIVE TEACHERS’ COGNITIVE STRUCTURES CONCERNING PROTEIN SYNTHESIS AND THEIR DEGREE OF UNDERSTANDING

Directory of Open Access Journals (Sweden)

Cem Gerçek

2018-02-01

Full Text Available The purpose of education is to actualise meaningful learning. Therefore, researching the issues on how students process information and how they configure it is important for meaningful learning. The issue of protein synthesis contains a number of abstract topics and concepts. Hence, it is important in biology teaching to be informed of students’ cognitive structures concerning protein synthesis. This research aims to analyse prospective teachers’ cognitive structures about protein synthesis and their degree of understanding the subject. The research group was composed of 17 volunteering prospective teachers who had been chosen through purposeful sampling. The data were collected via semi-structured interviews. Flow maps and content analysis were used in analysing the data. The results demonstrated that prospective teachers had too many misconceptions about protein synthesis and that their knowledge extent and rich connection are inadequate. The prospective teachers’ degree of understanding protein synthesis was divided into three categories. The results obtained in this research suggested that teachers should be careful in teaching the subject of protein synthesis. Students’ prior knowledge and their misconceptions should be determined and content or contexts to facilitate them to learn an abstract subject such as protein synthesis should be presented.

Nickel oxide/polypyrrole/silver nanocomposites with core/shell/shell structure: Synthesis, characterization and their electrochemical behaviour with antimicrobial activities

Energy Technology Data Exchange (ETDEWEB)

Das, Dhaneswar; Nath, Bikash C. [Department of Chemical Sciences, Tezpur University, Tezpur 784028, Assam (India); Phukon, Pinkee [Department of Molecular Biology and Biotechnology, Tezpur University, Tezpur 784028, Assam (India); Saikia, Bhaskar J.; Kamrupi, Isha R. [Department of Chemical Sciences, Tezpur University, Tezpur 784028, Assam (India); Dolui, Swapan K., E-mail: dolui@tezu.ernet.in [Department of Chemical Sciences, Tezpur University, Tezpur 784028, Assam (India)

2013-10-01

Magnetic and conducting Nickel oxide–polypyrrole (NiO/PPy) nanoparticles with core–shell structure were prepared in the presence of Nickel oxide (NiO) in aqueous solution containing sodium dodecyl benzenesulfonate (SDBS) as a surfactant as well as dopant. A stable dispersion of silver (Ag) nanoparticles was synthesized by chemical (citrate reduction) method. NiO/PPy nanocomposites were added to the Ag colloid under stirring. Ag nanoparticles could be electrostatically attracted on the surface of NiO/PPy nanocomposites, leading to formation of NiO/PPy/Ag nanocomposites with core/shell/shell structure. The morphology, structure, particle size and composition of the products were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, cyclic voltammetry (CV) and current–voltage (I–V) analysis. The resultant nanocomposites have the good conductivity and excellent electrochemical and catalytic properties of PPy and Ag nanoparticles. Furthermore, the nanocomposites showed excellent antibacterial behaviour due to the presence of Ag nanoparticles in the composite. The thermal stability of NiO–PPy as well as NiO/PPy/Ag nanocomposites was higher than that of pristine PPy. Studies of IR spectra suggest that the increased thermal stability may be due to interactions between NiO and Ag nanoparticles with the PPy backbone. - Highlights: • NiO nanoparticles were synthesized by two step soft chemical synthesis route. • Ag nanoparticles were prepared by using citrate reduction method. • NiO/PPy nanocomposites are synthesized by chemical oxidative polymerization process. • NiO/PPy/Ag nanocomposites can be used in the water purification technology.

Nickel oxide/polypyrrole/silver nanocomposites with core/shell/shell structure: Synthesis, characterization and their electrochemical behaviour with antimicrobial activities

International Nuclear Information System (INIS)

Das, Dhaneswar; Nath, Bikash C.; Phukon, Pinkee; Saikia, Bhaskar J.; Kamrupi, Isha R.; Dolui, Swapan K.

2013-01-01

Magnetic and conducting Nickel oxide–polypyrrole (NiO/PPy) nanoparticles with core–shell structure were prepared in the presence of Nickel oxide (NiO) in aqueous solution containing sodium dodecyl benzenesulfonate (SDBS) as a surfactant as well as dopant. A stable dispersion of silver (Ag) nanoparticles was synthesized by chemical (citrate reduction) method. NiO/PPy nanocomposites were added to the Ag colloid under stirring. Ag nanoparticles could be electrostatically attracted on the surface of NiO/PPy nanocomposites, leading to formation of NiO/PPy/Ag nanocomposites with core/shell/shell structure. The morphology, structure, particle size and composition of the products were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, cyclic voltammetry (CV) and current–voltage (I–V) analysis. The resultant nanocomposites have the good conductivity and excellent electrochemical and catalytic properties of PPy and Ag nanoparticles. Furthermore, the nanocomposites showed excellent antibacterial behaviour due to the presence of Ag nanoparticles in the composite. The thermal stability of NiO–PPy as well as NiO/PPy/Ag nanocomposites was higher than that of pristine PPy. Studies of IR spectra suggest that the increased thermal stability may be due to interactions between NiO and Ag nanoparticles with the PPy backbone. - Highlights: • NiO nanoparticles were synthesized by two step soft chemical synthesis route. • Ag nanoparticles were prepared by using citrate reduction method. • NiO/PPy nanocomposites are synthesized by chemical oxidative polymerization process. • NiO/PPy/Ag nanocomposites can be used in the water purification technology

Synthesis and characterization of magnetite nanoparticles encapsulated in a bovine hemoglobin microgel

Science.gov (United States)

Mody, Puja J.

This study shows the successful synthesis and characterization of a novel material that is composed of iron oxide particles within a protein gel. During the synthesis, bovine hemoglobin surrounds the forming Fe 3O4 nanoparticles, resulting in a biocompatible hydrogel, which has the potential to be used as a targeted drug delivery vehicle and as an MRI contrast agent. The structure, size, and thermal stability of these hydrogel complexes were analyzed using a range of techniques. Powder x-ray diffraction and infrared spectroscopy indicated the presence of Fe3O 4 and hemoglobin without significant interactions between particles in the solid state. Microscopy analysis determined the average size of these microgel complexes to be 4-9 mum2 in area (˜2-3 mum in diameter), and DSC analysis indicated that none of the microgels exhibited a denaturing or unfolding transition below 54°C regardless of the iron: hemoglobin ratio. Initial testing has been performed on the ability of these materials to act as magnetically activated drug delivery vehicles. Other pertinent tests (for magnetic properties and MRI applicability) are currently proceeding at external labs.

Synthesis and molecular characterization of chitosan based polyurethane elastomers using aromatic diisocyanate.

Science.gov (United States)

Zia, Khalid Mahmood; Anjum, Sohail; Zuber, Mohammad; Mujahid, Muhammad; Jamil, Tahir

2014-05-01

The present research work was performed to synthesize a new series of chitosan based polyurethane elastomers (PUEs) using poly(ɛ-caprolactone) (PCL). The chitosan based PUEs were prepared by step-growth polymerization technique using poly(ɛ-caprolactone) (PCL) and 2,4-toluene diisocyanate (TDI). In the second step the PU prepolymer was extended with different mole ratios of chitosan and 1,4-butane diol (BDO). Molecular engineering was carried out during the synthesis. The conventional spectroscopic characterization of the synthesized samples using FT-IR confirms the existence of the proposed chitosan based PUEs structure. Internal morphology of the prepared PUEs was studied using SEM analysis. The SEM images confirmed the incorporation of chitosan molecules into the PU backbone. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis and Characterization of a Sulfonyl- and Iminophosphoryl-Functionalized Methanide and Methandiide

Directory of Open Access Journals (Sweden)

Kai-Stephan Feichtner

2016-12-01

Full Text Available The synthesis of [H2C(PPh2=NSiMe3(SO2Ph] (1 and its mono- and dimetalation are reported. Due to the strong anion-stabilizing abilities of the iminophosphoryl and the sulfonyl group monometalation to 1-K and dimetalation to 1-Li2 proceed smoothly with potassium hydride and methyllithium, respectively. Both compounds could be isolated in high yields and were characterized by NMR spectroscopy as well as XRD analysis. The methanide 1-K forms a coordination polymer in the solid state, while in case of the methandiide a tetrameric structure is observed. The latter features an unusual structural motif consisting of two (SO2Li2 eight-membered rings, which are connected with each other via the methandiide carbon atoms and additional lithium atoms. With increasing metalation a contraction of the P–C–S linkage is observed, which is well in line with the increased charge at the central carbon atom and involved electrostatic interactions.

Synthesis, characterization, and application of two Al(OR(F))3 Lewis superacids.

Science.gov (United States)

Kraft, Anne; Trapp, Nils; Himmel, Daniel; Böhrer, Hannes; Schlüter, Peter; Scherer, Harald; Krossing, Ingo

2012-07-23

We report herein the synthesis and full characterization of the donor-free Lewis superacids Al(OR(F))(3) with OR(F) = OC(CF(3))(3) (1) and OC(C(5)F(10))C(6)F(5) (2), the stabilization of 1 as adducts with the very weak Lewis bases PhF, 1,2-F(2)C(6)H(4), and SO(2), as well as the internal C-F activation pathway of 1 leading to Al(2)(F)(OR(F))(5) (4) and trimeric [FAl(OR(F))(2)](3) (5, OR(F) = OC(CF(3))(3)). Insights have been gained from NMR studies, single-crystal structure determinations, and DFT calculations. The usefulness of these Lewis acids for halide abstractions has been demonstrated by reactions with trityl chloride (NMR; crystal structures). The trityl salts allow the introduction of new, heteroleptic weakly coordinating [Cl-Al(OR(F))(3)](-) anions, for example, by hydride or alkyl abstraction reactions. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

SYNTHESIS, SPECTRAL CHARACTERIZATIONS AND ...

African Journals Online (AJOL)

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A series of 4-chloro-2-[(arylmethylidene)amino]phenols (1–11) including methoxy group ... The structures of the Schiff bases were characterized by FT-IR, .... The characteristic ν(C-H) modes of ring residues are observed at near 3050 cm–1.

Synthesis and characterization of composites of mixed oxides of iron ...

Indian Academy of Sciences (India)

Home; Journals; Bulletin of Materials Science; Volume 34; Issue 4. Synthesis and characterization of composites of mixed oxides of iron and neodymium in polymer matrix of aniline–formaldehyde. Sajdha H N Sheikh B L Kalsotra N Kumar S Kumar. Volume 34 Issue 4 July 2011 pp 843-851 ...

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

International Nuclear Information System (INIS)

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

2015-01-01

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

Synthesis and characterization of cationic lipid coated magnetic nanoparticles using multiple emulsions as microreactors

Energy Technology Data Exchange (ETDEWEB)

Akbaba, Hasan; Karagöz, Uğur [Ege University, Faculty of Pharmacy, Department of Pharmaceutical Biotechnology, 35100 Izmir (Turkey); Selamet, Yusuf [Izmir Institute of Technology, Faculty of Science, Department of Physics, 35433 Izmir (Turkey); Kantarcı, A. Gülten, E-mail: gulten.kantarci@ege.edu.tr [Ege University, Faculty of Pharmacy, Department of Pharmaceutical Biotechnology, 35100 Izmir (Turkey)

2017-03-15

The aim of this study was to develop a novel iron oxide nanoparticle synthesis method with in-situ surface coating. For this purpose multiple emulsions were used as microreactors for the first time and magnetic iron oxide particles synthesized in the core of cationic solid lipid nanoparticles. DLS, SEM, TEM, VSM, Raman Spectrometer, XRD, and XPS techniques were performed for characterization of the magnetic nanoparticles. Obtained magnetic nanoparticles are superparamagnetic and no additional process was needed for surface adjustments. They are positively charged as a result of cationic lipid coating and has appropriate particle size (<30 nm) for drug or nucleic acid delivery. Structure analysis showed that magnetic core material is in the form of magnetite. Saturation magnetization value was measured as 15–17 emu g{sup −1} for lipid coated magnetic nanoparticles obtained by multiple emulsion method which is reasonably sufficient for magnetic targeting. - Highlights: • A novel iron oxide nanoparticle synthesis method with in-situ surface coating. • Combining advantages of microemulsions and multiple emulsion methods. • Multiple emulsions were used as microreactors for magnetic nanoparticle synthesis. • Superparamagnetic iron oxide particles synthesized in the core of cationic lipids. • Possible delivery systems for nucleic acids, oil soluble compounds or drugs.

Synthesis and Characterization of Birnessite and Cryptomelane Nanostructures in Presence of Hoffmeister Anions

Directory of Open Access Journals (Sweden)

Marcos A. Cheney

2009-01-01

Full Text Available The effect of Hoffmeister anions Cl−, SO42−, and ClO4− on the structure and morphology of birnessite and cryptomelane-type manganese dioxide nanostructures, produced by the reduction reaction of KMnO4 and MnSO4 in aqueous acidic media, was studied. The syntheses were based on the decomposition of aqueous KMnO4 in presence of HCl for birnessite-type and acidified MnSO4 for cryptomelane-type manganese dioxide under soft hydrothermal conditions. They were characterized using X-ray diffraction (XRD, transmission electron microscopy (TEM, and high-resolution transmission electron microscopy (HRTEM techniques. XRD patterns show the formation of birnessite for the first synthesis and a mixture of cryptomelane and birnessite-types MnO2 for the second synthesis. XRD data revealed that the Hoffmeister anions have a significant effect on the nanostructures of birnessite. The sulphate ion-treated birnessite has the smallest crystals, whereas the chloride ion-treated birnessite has the largest crystals. Their TEM and HRTEM studies revealed a transformation from nanoplatelet morphology for chloride-treated samples to nanofibrous morphology for sulphate-treated birnessite. For the cryptomelane nanostructures, Hoffmeister anions also show a profound effect on their crystalline structures as determined by XRD analyses revealing a transformation of the cryptomelane phase to birnessite phase of MnO2. This transformation is also supported by TEM and HRTEM studies.

Mechanochemical synthesis and structural characterization of three novel cocrystals of dimethylglyoxime with N-heterocyclic aromatic compounds and acetamide

Science.gov (United States)

Abidi, Syed Sibte Asghar; Azim, Yasser; Gupta, Abhishek Kumar; Pradeep, Chullikkattil P.

2017-12-01

With an aim to explore the interactions of (RR'Cdbnd Nsbnd OH) oxime moiety of dimethylglyoxime (DMG) with pyridyl ring of N-heterocyclic aromatic compounds and acetamide, three novel cocrystals of dimethylglyoxime with acridine (ACR), 1,10-phenanthroline monohydrate (PT) and acetamide (ACT) are reported. These three cocrystals were obtained with a mechanochemical synthesis approach and were characterized by single crystal X-ray diffraction (SCXRD), powder X-ray diffraction (PXRD), fourier transform-infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Additionally, Hirshfeld surface analysis is used to investigate the intermolecular interaction and the crystal packing of cocrystals.

Synthesis and Characterization of Zeolite Na−Y and Its Conversion to the Solid Acid Zeolite H−Y

DEFF Research Database (Denmark)

Warner, Terence Edwin; Galsgaard Klokker, Mads; Nielsen, Ulla Gro

2017-01-01

Zeolite Y has an iconic crystal structure, but more importantly, the hydrogen modification zeolite H−Y is the classic example of a solid acid which is used extensively as a catalyst in the oil industry. This metastable compound cannot be synthesized directly, which creates an opportunity to discuss...... various preparative strategies with the students, such as the three-stage procedure described here. Stage I concerns the hydrothermal synthesis of zeolite Na−Y, followed by ion-exchange with an ammonium acetate solution to form zeolite NH4−Y, and the latter is subsequently converted to zeolite H......−Y by thermolysis. Stages II and III may instead be performed using commercially available zeolites, Na−Y and NH4−Y, respectively, which shifts the learning objectives to structural characterization of zeolites. The characterization of the product and intermediate materials gives the students a practical insight...

Structural characterization of birnessite: influence of the way of synthesis; Caracterisation structurale de la birnessite: influence du protocole de synthese

Energy Technology Data Exchange (ETDEWEB)

Gaillot, A.C.

2002-01-15

Birnessite is a lamellar manganese oxide whose layers are built up of edge sharing MnO{sub 6} octahedra. The presence of hetero-valent Mn cations and/or of vacant sites in these layers leads to a charge deficit compensated for by the presence of hydrated cations in the interlayer space. Because of their high specific area and of their strong oxidative character, these ubiquitous manganese oxides play a fundamental role in the fate of organic and metallic pollutants in the environment, but our imperfect knowledge of their structure limits the understanding and the modeling of this impact. This study aimed at classifying all different kinds of birnessite obtained using existing synthesis protocols according to two relevant criteria: layer symmetry and layer stacking mode, and at determining the structure of several essential varieties using X-ray and electron diffraction. Layers of hydrothermal birnessite contain vacant sites and, as a result, possess an hexagonal symmetry. Their stacking mode is 3R. In high-temperature birnessites, adjacent layers have an opposite orientation, which results in a two-layer polytype. The symmetry of these layers, linked to the origin of the layer charge deficit, depends on the temperature of synthesis. At 800 C the presence of vacant sites results in an hexagonal symmetry (2H polytype). At 1000 C, the layer charge deficit originates from the presence of Mn{sup 3+} cations in the layer lowering the layer symmetry (2O polytype). A variety of chemical and structural heterogeneities was also described in these samples, along with the occurrence of a new type of structural disorder. Finally we proved both the fundamental link between the origin of the layer charge and the layer symmetry, and the influence of physico-chemical parameters during synthesis (temperature, average manganese oxidation degree, nature of the interlayer cation) on the structure of the obtained compound. The chemical and thermal stabilities of these birnessites are

Tunable synthesis of copper nanotubes

International Nuclear Information System (INIS)

Kaniukov, E; Yakimchuk, D; Kozlovsky, A; Shlimas, D; Zdorovets, M; Kadyrzhanov, K

2016-01-01

Simple method of tunable synthesis of copper nanotubes based on template synthesis was developed. A comprehensive study of the structural, morphological and electrical characteristics of the obtained nanostructures was carried out. Characterization of structural features was made by methods of scanning electron microscopy, energy dispersive spectroscopy and X-ray diffractometry analysis. Evaluation of wall thickness is made by methods of gas permeability. Electrical conductivity of nanotubes was define in the study of their current-voltage characteristics. The possibility to control of copper nanotubes physical properties by variation of the deposition parameters was shown. (paper)

Synthesis and characterization of energetic thermoplastic elastomers for propellant formulations

Directory of Open Access Journals (Sweden)

Aparecida M. Kawamoto

2009-01-01

Full Text Available Synthesis and characterization of energetic ABA-type thermoplastic elastomers for propellant formulations has been carried out. Following the working plan elaborated, the synthesis and characterization of Poly 3- bromomethyl-3-methyl oxetane (PolyBrMMO, Poly 3- azidomethyl-3-methyl oxetane (PolyAMMO, Poly 3,3-bis-azidomethyl oxetane (PolyBAMO and Copolymer PolyBAMO/AMMO (by TDI end capping has been successfully performed. The thermoplastic elastomers (TPEs were synthesized using the chain elongation process PolyAMMO, GAP and PolyBAMO by diisocyanates. In this method 2.4-toluene diisocyanate (TDI is used to link block A (hard and mono- functional to B (soft and di-functional. For the hard A-block we used PolyBAMO and for the soft B-block we used PolyAMMO or GAP.This is a joint project set up, some years ago, between the Chemistry Division of the Institute of Aeronautics and Space (IAE - subordinated to the Brazilian Ministry of Defense - and the Fraunhofer Institut Chemische Technologie (ICT, in Germany. The products were characterized by different techniques as IR- and (1H,13CNMR spectroscopies, elemental and thermal analyses. New methodologies based on FT-IR analysis have been developed as an alternative for the determination of the molecular weight and CHNO content of the energetic polymers.

Preparation and Characterization of Nano-structured Ceramic Powders Synthesized by Emulsion Combustion Method

International Nuclear Information System (INIS)

Takatori, Kazumasa; Tani, Takao; Watanabe, Naoyoshi; Kamiya, Nobuo

1999-01-01

The emulsion combustion method (ECM), a novel powder production process, was originally developed to synthesize nano-structured metal-oxide powders. Metal ions in the aqueous droplets were rapidly oxidized by the combustion of the surrounding flammable liquid. The ECM achieved a small reaction field and a short reaction period to fabricate the submicron-sized hollow ceramic particles with extremely thin wall and chemically homogeneous ceramic powder. Alumina, zirconia, zirconia-ceria solid solutions and barium titanate were synthesized by the ECM process. Alumina and zirconia powders were characterized to be metastable in crystalline phase and hollow structure. The wall thickness of alumina was about 10 nm. The zirconia-ceria powders were found to be single-phase solid solutions for a wide composition range. These powders were characterized as equiaxed-shape, submicron-sized chemically homogeneous materials. The powder formation mechanism was investigated through the synthesis of barium titanate powder with different metal sources

synthesis and structural characterization of n-(2-{[(2e)-2-(2 ...

African Journals Online (AJOL)

E.J. Research Institute of Chemistry, International Center for Chemical and Biological ... Benzamide and its analogues have various application in synthesis of ..... Symmetry codes: (i) x+3/2, y+1/2, z; (ii) −x+1/2, −y+1/2, −z; (iii) x, y−1, z.

The synthesis of CuO nanoleaves, structural characterization, and their glucose sensing application

International Nuclear Information System (INIS)

Ibupoto, Z. H.; Khun, K.; Willander, M.; Lu, J.

2013-01-01

The present study describes the synthesis of well aligned and highly dense polyethylene glycol template assisted cupric oxide (CuO) nanoleaves on the gold coated glass substrate by hydrothermal growth method. The structural study based investigations of CuO nanoleaves were performed by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), energy dispersive X-ray (EDX), infrared reflection-absorption spectroscopy (IRAS), and high resolution transmission electron microscopy (HRTEM). The glucose sensor based on the glucose oxidase immobilized CuO nanoleaves electrode detected the wide range of glucose concentrations with good linearity and exhibited high sensitivity of 61.9 ± 2.0 mV/decade. The linear detection range was observed from 1.0 × 10 −5 to 2.0 × 10 −2 M with detection limit of 5.0 × 10 −6 M and a fast response time of less than 5 s was also observed. The glucose sensor electrode possesses good anti-interference ability, stability, repeatability, and reproducibility.

The synthesis of CuO nanoleaves, structural characterization, and their glucose sensing application

Energy Technology Data Exchange (ETDEWEB)

Ibupoto, Z. H.; Khun, K.; Willander, M. [Department of Science and Technology, Campus Norrkoeping, Linkoeping University, SE-60174 Norrkoeping (Sweden); Lu, J. [Department of Physics, Chemistry, and Biology (IFM), Linkoeping University, 58183 Linkoeping (Sweden)

2013-03-11

The present study describes the synthesis of well aligned and highly dense polyethylene glycol template assisted cupric oxide (CuO) nanoleaves on the gold coated glass substrate by hydrothermal growth method. The structural study based investigations of CuO nanoleaves were performed by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), energy dispersive X-ray (EDX), infrared reflection-absorption spectroscopy (IRAS), and high resolution transmission electron microscopy (HRTEM). The glucose sensor based on the glucose oxidase immobilized CuO nanoleaves electrode detected the wide range of glucose concentrations with good linearity and exhibited high sensitivity of 61.9 {+-} 2.0 mV/decade. The linear detection range was observed from 1.0 Multiplication-Sign 10{sup -5} to 2.0 Multiplication-Sign 10{sup -2} M with detection limit of 5.0 Multiplication-Sign 10{sup -6} M and a fast response time of less than 5 s was also observed. The glucose sensor electrode possesses good anti-interference ability, stability, repeatability, and reproducibility.

Synthesis, characterization and a.c. magnetic analysis of magnetite nanoparticles

International Nuclear Information System (INIS)

Riani, P.; Napoletano, M.; Canepa, F.

2011-01-01

In the last years, the study of Fe-based magnetic nanoparticles (MNP) has attracted increasing interest either for the physical properties shown by nanosized materials (electric and magnetic properties are strongly affected by dimension and surface effects) either for the different technological applications of these materials (catalysis, drug delivery, magnetic resonance imaging, contaminants removal from groundwater, new exchange coupled magnets, soft nanomagnets for high frequency applications, etc.). In this article, the results obtained in the synthesis and characterization of the Fe 3 O 4 MNP is reported. The magnetite nanoparticles were synthesized by a modified Massart method. Structural characterization was performed using X-ray diffraction analysis and a complete morphological and dimensional study was carried out by means of Transmission Electron Microscopy, and a.c. magnetic susceptibility measured as a function of the frequency of the applied magnetic field. Diameters of the superparamagnetic Fe 3 O 4 nanoparticles are ranging from 2 to 10 nm, as evidenced by all the techniques employed. The size distribution of the hydrated aggregates in solution has been obtained by quantitative analysis of the frequency dependence of the a.c. susceptibility. The mathematical approach adopted will be described and all the obtained results will be compared and discussed.

Synthesis and characterization of irradiated injectable bone substitute paste based on hydroxyapatite

International Nuclear Information System (INIS)

Yessy Warastuti; Basril Abbas

2011-01-01

Synthesis and characterization of hydroxyapatite, chitosan and hydroxypropyl methylcellulose (HPMC) composite in injectable paste form have been done. The composite was synthesized by stirring hydroxyapatite, chitosan and HPMC until homogen. IBS paste was irradiated at the dose of 25 kGy (sterile dose). Characterization of IBS paste was conducted by measuring of the water content, identification of functional group with Fourier Transform Infra Red Spectrophotometer (FTIR), and identification of sample morphology with Scanning Electron Microscope Energy Dispersive Spectrophotometer (SEM EDS). The result showed that the water content of irradiated sample was higher than unirradiated sample due to water radiolysis. Several specific bands of IBS paste were identified, i.e., carbonate (CO 3 2- ), at 1420 cm -1 , phosphate (PO 4 3- ) at 1043 cm -1 , 605 cm -1 , 568 cm -1 and chitosan (NH 2 ) at 1599 cm -1 . There is no significant difference in absorbed band between irradiated and unirradiated samples. IBS paste has a microstructure with the size of 0.05 – 0.1 μm. Electron beam irradiation did not change the structure and morphology of sample. (author)

Synthesis and Characterization of Poly(Amidoamine Dendrimers Encapsulatd 198Au Nanoparticles

Directory of Open Access Journals (Sweden)

R. Ritawidya1,2

2012-12-01

Full Text Available Brachytherapy or internal radiotherapy is one of many methods used for treatment of cancer. This modality requires an agent with radionuclides that emits  or β particle with a proper energy. 198Au (99% β max = 0.96 MeV and t1/2 = 2.69 days is one of radionuclides that has been considered to be effective for the above-mentioned purpose. The purpose of this research was to synthesis and characterize poly(amidoamine (PAMAM G3.0 dendrimers encapsulated 198Au nanoparticles as a new brachytherapy agent. PAMAM G3.0 dendrimers encapsulated 198Au nanoparticles was successfully synthesized by a bottom-up method using sodium borohydride as a reductor. Purification was then performed by a size exclusion chromatography in order to separate large Au nanoparticles that were formed outside the cavity of PAMAM G3.0 dendrimers. Prior to the synthesis of PAMAM G3.0 dendrimers encapsulated 198Au nanoparticles, the synthetic procedure was first established by using a non-radioactive Au. The PAMAM G3.0 dendrimers encapsulated Au nanoparticles produced was then characterized by using an UV-Vis spectroscopy, a transmission electron microscopy (TEM, particle size analyzer (PSA, and an atomic absorption spectroscopy (AAS. Characterization results revealed that PAMAM G3.0 dendrimers encapsulated Au nanoparticles that were prepared from a reaction mixture of PAMAM G3.0 dendrimers and Au HAuCl4 with mol ratio of 2.8, was found to be a proper formula. It produced PAMAM G3.0 dendrimers encapsulated Au nanoparticles with diameter of 1.743 nm, spheris, uniform and drug loading value of 26.34%. This formula was then used in synthesis using radioactive Au, 198Au. Characterization results of PAMAM G3.0 dendrimers encapsulated 198Au nanoparticles gave a radiochemical purity of 99.4% and zero charge.

Chromium(III) Complex Obtained from Dipicolinic Acid: Synthesis, Characterization, X-Ray Crystal Structure and Electrochemical Studies

Energy Technology Data Exchange (ETDEWEB)

Ghasemi, Khaled; Rezvani, Ali Reza; Ghasemi, Fatemeh [Univ. of Sistan and Baluchestan, Zahedan (Iran, Islamic Republic of); Razak, Ibrahim Abdul; Rosli, Mohd Mustaqim [Universiti Sains Malaysia, Penang (Malaysia)

2013-10-15

The synthesis, X-ray crystallography, spectroscopic (IR, UV-vis), and electrochemical properties of the title compound, [H{sub 3}O][Cr(dipic){sub 2}] [H{sub 3}O{sup +}.Cl{sup -}] (1), (H{sub 2}dipic = 2,6-pyridinedicarboxylic acid), are reported. This complex crystallizes in the monoclinic space group Cc with a = 14.9006(10) A, b = 12.2114(8) A, c = 8.6337(6) A, α = 90.00 .deg., β = 92.7460(10) .deg., γ = 90.00 .deg., and V = 1569.16(18) A3 with Z = 4. The hydrogen bonding and noncovalent interactions play roles in the stabilization of the structure. In order to gain a better understanding of the most important geometrical parameters in the structure of the complex, atoms in molecules (AIM) method at B3LYP/6-31G level of theory has been employed.

Synthesis and characterization of dental composites

Science.gov (United States)

Djustiana, Nina; Greviana, Nadia; Faza, Yanwar; Sunarso

2018-02-01

During the last few decades, the increasing demands in esthetic dentistry have led to the development of dental composites material that provide similar appearance to the natural teeth. Recently, esthetic trend was an issue which increase the demand for teeth restorations that is similar with the origin. The esthetics of dental composite are more superior compared to amalgam, since its color look similar with natural teeth. Various dental composites have been developed using many type of fillers such as amorphous silica, quartz), borosilicate, Li-Sr-Ba-Al glass and oxide: zirconia and alumina. Researchers in Faculty of Dentistry University of Padjadjaran have prepared dental composites using zirconia-alumina-silica (ZAS) system as the filler. The aim is to improve the mechanical properties and the esthetic of the dental composites. The ZAS was obtained from chemical grade purity chemicals and Indonesia's natural sand as precursors its characterization were also presented. This novel method covers the procedure to synthesis and characterize dental composites in Padjadjaran University and some review about dental composites in global research.

Synthesis and characterization of CuGeO3 photocatalyst using Green Chemistry and its application for the degradation of direct black dye

Directory of Open Access Journals (Sweden)

Ashok. V. Borhade

2013-03-01

Full Text Available In this paper, we report synthesis of CuGeO3 photocatalyst by mechanochemical, solid state synthesis, method with green chemistry approach. The product obtained was characterized by various investigative techniques like UV-Diffuse Reflectance Spectroscopy, Fourier Transform Infrared Spectroscopy, X-ray Diffraction, Scanning Electron Microscopy, with Energy Dispersive X-ray Spectroscopy, and BET Surface area. The study confirm orthorhombic pervoskite crystal structure of photocatalyst with band gap 3.7 eV. The photocatalytic activity of the catalysts CuGeO3 was evaluated by photochemical bleaching of Direct black dye, under sun light.

Synthesis and characterization of tricalcium phosphate ceramics doped with zinc

International Nuclear Information System (INIS)

Kai, K.C.; Marchi, J.; Ussui, V.; Bressiani, A.H.A.

2011-01-01

Due to its biocompatibility, the tricalcium phosphate (TCP) is used as a biomaterial for bone replacement and reconstruction. Zinc (Zn) can replace calcium in the crystal structure of TCP to be added in small quantities, can result in stimulatory effects on bone formation in vitro and in vivo. In this work, pure TCP and Zn-TCP, with general formula (Ca_1_-_xZn_x)_3 (PO_4)_2 and 0 ≤ x ≤ 0.0225, were prepared by wet synthesis, from precursors Ca(OH)_2, H_3PO_4 and ZnO, after calcinated at 800 deg C and characterized by X-ray diffraction, specific surface area, agglomerate size distribution, differential thermal analysis and scanning electron microscopy. The results showed that the addition of small amounts of Zn resulted in TCP with suitable densification and higher specific surface area, may be promising as biomaterial due to the stimulatory effects of zinc associated with suitable mechanical properties of the final material. (author)

Competing Pathways for Nucleation of the Double Perovskite Structure in the Epitaxial Synthesis of La ₂ MnNiO ₆

Energy Technology Data Exchange (ETDEWEB)

Spurgeon, Steven R.; Du, Yingge; Droubay, Timothy; Devaraj, Arun; Sang, Xiahan; Longo, Paolo; Yan, Pengfei; Kotula, Paul G.; Shutthanandan, Vaithiyalingam; Bowden, Mark E.; LeBeau, James M.; Wang, Chongmin; Sushko, Peter V.; Chambers, Scott A.

2016-06-14

Over the past decades a confluence of advanced synthesis techniques, data-driven characterization, and rapid increases in computing power has sparked a renaissance in materials engineering. The emerging “materials-by-design” approach, while radically transforming the development of multicomponent systems, has tended to overlook the complex kinetic pathways that define materials synthesis. Although we are able to envision almost limitless materials combinations, we are unable to synthesize all of them in practice, since existing characterization and modeling approaches often fail to capture the inherent complexity of such systems. There is currently a disconnect between highly local structural characterization and macroscale properties measurements, resulting in oversimplified or incomplete structure-property models. Here we describe a multi-technique approach that combines aberration-corrected transmission electron microscopy with emerging oxide atom probe tomography to measure chemical ordering and extended defects in the model complex oxide, La2MnNiO6. We visualize cation ordering, as well as a three-dimensional network of secondary phases, which we describe in terms of ab initio structure calculations. We propose a defect model in which these phases alter their surrounding octahedral environment, severely disrupting cation superexchange. Through this array of experimental and theoretical techniques, we uncover fundamental structure-property relationships and illustrate a new approach to engineer complex, multicomponent systems.

Synthesis, characterization and gas sensing performance of SnO2 ...

Indian Academy of Sciences (India)

Synthesis, characterization and gas sensing performance of SnO2 thin films prepared by spray pyrolysis. GANESH E PATIL, D D KAJALE, D N CHAVAN†, N K PAWAR††, P T AHIRE, S D SHINDE#,. V B GAIKWAD# and G H JAIN. ∗. Materials Research Laboratory, Arts, Commerce and Science College, Nandgaon 423 106, ...

Synthesis and characterization of polyglycerols dendrimers for applications in tissue engineering biological

International Nuclear Information System (INIS)

Passos, E.D.; Queiroz, A.A.A. de

2014-01-01

Full text: Introduction: Over the last twenty years is the growing development in the manufacture of synthetic scaffold in tissue engineering applications. These new materials are based on polyglycerol dendrimers (PGLD's). PGLD's are highly functional polymers with hydroxymethyl side groups, fulfill all structural prerequisites to replace poly(ethylene glycol)s in medical applications. Furthermore, since these materials are based on naturally occurring compounds that degrades over time in the body and can be safely excreted. The objective of this work was the synthesis, physicochemical, biological characterization of HPGL's with potential use as scaffolds in tissue engineering. HPGL's with oligomeric cores, of diglycerol triglycerol and tetraglycerol was used. Theoretical and Experimental Simulation Details: The synthesis of PGLD procedures involves the etherification of glycerol through anionic polymerization of glycidol. The PGLD's were characterized by chromatographic techniques (SEC and HPLC), spectroscopic (FTIR, 1H-NMR and 13C - NMR) electrochemical (zeta potential) and thermal analysis (DSC and TGA) techniques. The structure- activity relationships (SAR's) of compound prototype and its analogs were studied to determine the generation number (G) of the molecule responsible for the biological activity on the adhesion and cell proliferation process. A detailed study of the structure of PGLD's of G=0-4 was performed using the Hyperchem 7. 5 and Gromacs 4 software packages. The biocompatibility studies were studied by scanning electron microscopy (SEM) and fluorescence microscopy (EPF) technique after PGLD (G=0-4) blood contact. The overall electro-negativity/total charge density, dipole moment, frontier orbital's (HOMO - LUMO) and electrostatic potential maps (EPM) were calculated. The most stable form of the resulting compounds was determined by estimating the hydration energy and energy conformation. Results and Discussion: The techniques SEM and EPF

Synthesis, Structural Characterization, Antimicrobial Activity, and In Vitro Biocompatibility of New Unsaturated Carboxylate Complexes with 2,2'-Bipyridine.

Science.gov (United States)

Vasile Scăețeanu, Gina; Chifiriuc, Mariana Carmen; Bleotu, Coralia; Kamerzan, Crina; Măruţescu, Luminiţa; Daniliuc, Constantin G; Maxim, Cătălin; Calu, Larisa; Olar, Rodica; Badea, Mihaela

2018-01-12

The synthesis, structural characterization, cytotoxicity, and antimicrobial properties of four new complexes formed by employing acrylate anion and 2,2'-bipyridine are reported herein. X-ray crystallography revealed the trinuclear nature of [Mn₃(2,2'-bipy)₂(C₃H₃O₂)₆] ( 1 ), meanwhile complexes with general formula [M(2,2'-bipy)(C₃H₃O₂)₂(H₂O) x ]∙ y H₂O (( 2 ) M: Ni, x = 1, y = 0; ( 3 ) M: Cu, x = 1, y = 0; ( 4 ) M: Zn, x = 0, y = 1; 2,2'-bipy: 2,2'-bipyridine; C₃H₃O₂: acrylate anion) were shown to be mononuclear. The lowest minimum inhibitory concentration (MIC) of 128 μg mL -1 was recorded for all four tested complexes against Candida albicans , for complex ( 3 ) against Escherichia coli , and for complex ( 4 ) against Staphylocococcus aureus . Compounds ( 3 ) and ( 4 ) were also potent efflux pumps activity inhibitors (EPI), proving their potential for use in synergistic combinations with antibiotics. Complexes ( 1 )-( 4 ) revealed that they were not cytotoxic to HCT-8 cells. They also proved to interfere with the cellular cycle of tumour HCT-8 cells by increasing the number of cells found in the S and G2/M phases. Taken together, these results demonstrate the potential of zinc and copper complexes for use in the development of novel antimicrobial and anti-proliferative agents.

Synthesis, Structural Characterization and Up-Conversion Luminescence Properties of NaYF4:Er3+,Yb3+@MOFs Nanocomposites

Science.gov (United States)

Giang, Lam Thi Kieu; Marciniak, Lukasz; Huy, Tran Quang; Vu, Nguyen; Le, Ngo Thi Hong; Binh, Nguyen Thanh; Lam, Tran Dai; Minh, Le Quoc

2017-10-01

This paper describes a facile synthesis of NaYF4:Er3+,Yb3+ nanoparticles embraced in metal-organic frameworks (MOFs), known as NaYF4:Er3+, Yb3+@MOFs core/shell nanostructures, by using iron(III) carboxylate (MIL-100) and zeolitic imidazolate frameworks (ZIF-8). Morphological, structural and optical characterization of these nanostructures were investigated by field emission-scanning electron microscopy, Fourier transform infrared spectroscopy, x-ray diffraction, and up-conversion luminescence measurements. Results showed that spherical-shaped NaYF4:Er3+,Yb3+@MIL-100 nanocomposites with diameters of 150-250 nm, and rod-shaped NaYF4:Er3+,Yb3+@ZIF-8 nanocomposites with lengths of 300-550 nm, were successfully synthesized. Under a 980-nm laser excitation at room temperature, the NaYF4:Er3+,Yb3+@MOFs nanocomposites exhibited strong up-conversion luminescence with two emission bands in the green part of spectrum at 520 nm and 540 nm corresponding to the 2H11/2 → 4I15/2 and 4S3/2 → 4I15/2 transitions of Er3+ ions, respectively, and a red emission band at 655 nm corresponding to the 4F9/2 → 4I15/2 transition of Er3+ ions. The above properties of NaYF4:Er3+,Yb3+@MOFs make them promising candidates for applications in biotechnology.

Materials Research Society Symposium Proceedings Volume 635. Anisotropic Nanoparticles - Synthesis, Characterization and Applications

National Research Council Canada - National Science Library

Lyon, L

2000-01-01

This volume contains a series of papers originally presented at Symposium C, "Anisotropic Nanoparticles Synthesis, Characterization and Applications," at the 2000 MRS Fall Meeting in Boston, Massachusetts...

Synthesis and Structural Characterization of Silver Nanoparticles Stabilized with 3-Mercapto-1-Propansulfonate and 1-Thioglucose Mixed Thiols for Antibacterial Applications

Science.gov (United States)

Porcaro, Francesco; Carlini, Laura; Ugolini, Andrea; Visaggio, Daniela; Visca, Paolo; Fratoddi, Ilaria; Venditti, Iole; Meneghini, Carlo; Simonelli, Laura; Marini, Carlo; Olszewski, Wojciech; Ramanan, Nitya; Luisetto, Igor; Battocchio, Chiara

2016-01-01

The synthesis, characterization and assessment of the antibacterial properties of hydrophilic silver nanoparticles (AgNPs) were investigated with the aim to probe their suitability for innovative applications in the field of nanobiotechnology. First, silver nanoparticles were synthetized and functionalized with two capping agents, namely 3-mercapto-1-propansulfonate (3MPS) and 1-β-thio-d-glucose (TG). The investigation of the structural and electronic properties of the nano-systems was carried out by means of X-ray Photoelectron Spectroscopy (XPS) and X-ray Absorption Spectroscopy (XAS). XPS data provided information about the system stability and the interactions between the metallic surface and the organic ligands. In addition, XPS data allowed us to achieve a deep understanding of the influence of the thiols stoichiometric ratio on the electronic properties and stability of AgNPs. In order to shed light on the structural and electronic local properties at Ag atoms sites, XAS at Ag K-Edge was successfully applied; furthermore, the combination of Dynamic Light Scattering (DLS) and XAS results allowed determining AgNPs sizes, ranging between 3 and 13 nm. Finally, preliminary studies on the antibacterial properties of AgNPs showed promising results on four of six multidrug-resistant bacteria belonging to the ESKAPE group (Enterococcus faecium, Staphylococcus aureus, Klebsiella pneumoniae, Acinetobacter baumannii, Pseudomonas aeruginosa, and Enterobacter sp.). PMID:28774148

Synthesis, characterization, x-ray structure and antimicrobial activity ...

African Journals Online (AJOL)

Methods: Pyridine-based thiosemicarbazide was synthesized, characterized and evaluated for antimicrobial activity. ... homogeneity of the compounds was checked by. TLC performed ..... properties of novel N-methyl-1,3,4-thiadiazol-2- amine.

Synthesis and characterization of ferrous phosphate (vivianite) and its behavior in aqueous media

International Nuclear Information System (INIS)

Diaz F, J.C.

2003-01-01

The synthesis and characterization of materials that can be useful in Environmental Chemistry is very important because their characteristics are exposed and its behavior in chemical phenomena as the sorption in aqueous media is understand to use it in the human being benefit. With the object of using, in a future, the octa hydrated ferrous phosphate (vivianite) as a potential candidate for matrix confinement in contention walls for the storage of radioactive waste of long half life, it was synthesized and it characterized physico chemically and their properties of surface of this compound were evaluated. Presently work was carried out the synthesis and structural characterization of the iron phosphate II by infrared spectroscopy with having Fourier transform, high vacuum scanning electron microscopy, X-ray diffraction, thermal gravimetric analysis, the BET multipoint surface area and Moessbauer spectroscopy; as well as, the determination between aqueous media of the isoelectric point and the density of sites of surface of the compound. The octa hydrated ferrous phosphate was obtained pure. The results indicate that the product corresponds to the prospective mineral, the vivianite. The thermal gravimetric analysis demonstrated that the ferrous phosphate is a stable salt after the lost of water. The isoelectric point is since an important parameter because allows to know the behavior of the surface of the material in aqueous systems, in this case the isoelectric point, of the octa hydrated ferrous phosphate, in distilled water is of pH 4.20 and in solution of potassium nitrate 0.5 M is of pH = 3.75. This indicates that the material has an amphoteric surface depending on the pH. On the other hand, the density of active sites of surface obtained by titrations acid-base is of 20 sites by nm 2 . (Author)

Nano-/micro metallic wire synthesis on Si substrate and their characterization

International Nuclear Information System (INIS)

Kaur, Jaskiran; Kaur, Harmanmeet; Singh, Surinder; Kanjilal, Dinakar; Chakarvarti, Shiv Kumar

2014-01-01

Nano-/micro wires of copper are grown on semiconducting Si substrate using the template method. It involves the irradiation of 8 um thick polymeric layer coated on Si with150 MeV Ni ion beam at a fluence of 2E8. Later, by using the simple technique of electrodeposition, copper nano-/micro wires were grown via template synthesis. Synthesized wires were morphologically characterized using SEM and electrical characterization was carried out by finding I-V plot

Investigating the Synthesis, Structure, and Catalytic Properties of Versatile Gold-Based Nanocatalvsts

Science.gov (United States)

Pretzer, Lori A.

Transition metal nanomaterials are used to catalyze many chemical reactions, including those key to environmental, medicinal, and petrochemical fields. Improving their catalytic properties and lifetime would have significant economic and environmental rewards. Potentially expedient options to make such advancements are to alter the shape, size, or composition of transition metal nanocatalysts. This work investigates the relationships between structure and catalytic properties of synthesized Au, Pd-on-Au, and Au-enzyme model transition metal nanocatalysts. Au and Pd-on-Au nanomaterials were studied due to their wide-spread application and structure-dependent electronic and geometric properties. The goal of this thesis is to contribute design procedures and synthesis methods that enable the preparation of more efficient transition metal nanocatalysts. The influence of the size and composition of Pd-on-Au nanoparticles (NPs) was systematically investigated and each was found to affect the catalyst's surface structure and catalytic properties. The catalytic hydrodechlorination of trichloroethene and reduction of 4-nitrophenol by Pd-on-Au nanoparticles were investigated as these reactions are useful for environmental and pharmaceutical synthesis applications, respectively. Structural characterization revealed that the dispersion and oxidation state of surface Pd atoms are controlled by the Au particle size and concentration of Pd. These structural changes are correlated with observed Pd-on-Au NP activities for both probe reactions, providing new insight into the structure-activity relationships of bimetallic nanocatalysts. Using the structure-dependent electronic properties of Au NPs, a new type of light-triggered biocatalyst was prepared and used to remotely control a model biochemical reaction. This biocatalyst consists of a model thermophilic glucokinase enzyme covalently attached to the surface of Au nanorods. The rod-like shape of the Au nanoparticles made the

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-09-15

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

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.

Znx-1CuxMn2O4 spinels; synthesis, structural characterization and electrical evaluation

International Nuclear Information System (INIS)

Mendez M, F.; Lima, E.; Bosch, P.; Pfeiffer, H.; Gonzalez, F.

2010-01-01

This work presents the structural characterization and electrical evaluation of Zn x-1 Cu x Mn 2 O 4 spinels, which are materials presented as secondary phases into the vari stor ceramic systems. Samples were analyzed by X-ray diffraction, solid-state nuclear magnetic resonance, infrared spectroscopy, scanning electron microscopy and impedance spectroscopy. Although, the addition of copper to the ZnMn 2 O 4 spinel did not produce morphological changes, the structure and electrical behaviors changed considerably. Structurally, copper addition induced the formation of partial inverse spinels, and its addition increases significantly the electrical conductivity. Therefore, the formation of Zn x-1 Cu x Mn 2 O 4 spinels, as secondary phases into the vari stor materials, may compromise significantly the vari stor efficiency. (Author)

CdTe and CdSe quantum dots: synthesis, characterizations and applications in agriculture

International Nuclear Information System (INIS)

Ung, Thi Dieu Thuy; Tran, Thi Kim Chi; Pham, Thu Nga; Nguyen, Quang Liem; Nguyen, Duc Nghia; Dinh, Duy Khang

2012-01-01

This paper highlights the results of the whole work including the synthesis of highly luminescent quantum dots (QDs), characterizations and testing applications of them in different kinds of sensors. Concretely, it presents: (i) the successful synthesis of colloidal CdTe and CdSe QDs, their core/shell structures with single- and/or double-shell made by CdS, ZnS or ZnSe/ZnS; (ii) morphology, structural and optical characterizations of the synthesized QDs; and (iii) testing examples of QDs as the fluorescence labels for agricultural-bio-medical objects (for tracing residual pesticide in agricultural products, residual clenbuterol in meat/milk and for detection of H5N1 avian influenza virus in breeding farms). Overall, the results show that the synthesized QDs have very good crystallinity, spherical shape and strongly emit at the desired wavelengths between ∼500 and 700 nm with the luminescence quantum yield (LQY) of 30–85%. These synthesized QDs were used in fabrication of the three testing fluorescence QD-based sensors for the detection of residual pesticides, clenbuterol and H5N1 avian influenza virus. The specific detection of parathion methyl (PM) pesticide at a content as low as 0.05 ppm has been realized with the biosensors made from CdTe/CdS and CdSe/ZnSe/ZnS QDs and the acetylcholinesterase (AChE) enzymes. Fluorescence resonance energy transfer (FRET)-based nanosensors using CdTe/CdS QDs conjugated with 2-amino-8-naphthol-6-sulfonic acid were fabricated that enable detection of diazotized clenbuterol at a content as low as 10 pg ml −1 . For detection of H5N1 avian influenza virus, fluorescence biosensors using CdTe/CdS QDs bound on the surface of chromatophores extracted and purified from bacteria Rhodospirillum rubrum were prepared and characterized. The specific detection of H5N1 avian influenza virus in the range of 3–50 ng μl −1 with a detection limit of 3 ng μL −1 has been performed based on the antibody-antigen recognition. (review)

Synthesis and characterization of poly aniline for electrochemical biosensor construction

International Nuclear Information System (INIS)

Magalhaes, Gleice S.L.; Southgate, Erica F.; Alhadeff, Eliana M.; Guimaraes, Maria Jose O.C.

2011-01-01

Conductors polymers have many attractive interests to the industry due their highly technological applications. This work treats specially of polyaniline because it's large electrical conductivity, electrochemical properties, associate to the chemical stability in environmental conditions and synthesis facility. The main of this work is the application in a construction of an electrochemical biosensor for ethanol detection and quantification. Different conditions of synthesis of the conductor emeraldine polyaniline form were studied, investigated the influence of the dopant agent and the reactional environment conditions temperature on the reaction yield and conductivities. The polyaniline that showed the best conductivity were characterized by differential and thermal gravimetric analysis, infrared spectroscopy, X ray diffraction, and cycle voltammetry, comparing with the commercial polyaniline. (author)

InSe monolayer: synthesis, structure and ultra-high second-harmonic generation

Science.gov (United States)

Zhou, Jiadong; Shi, Jia; Zeng, Qingsheng; Chen, Yu; Niu, Lin; Liu, Fucai; Yu, Ting; Suenaga, Kazu; Liu, Xinfeng; Lin, Junhao; Liu, Zheng

2018-04-01

III–IV layered materials such as indium selenide have excellent photoelectronic properties. However, synthesis of materials in such group, especially with a controlled thickness down to monolayer, still remains challenging. Herein, we demonstrate the successful synthesis of monolayer InSe by physical vapor deposition (PVD) method. The high quality of the sample was confirmed by complementary characterization techniques such as Raman spectroscopy, atomic force microscopy (AFM) and high resolution annular dark field scanning transmission electron microscopy (ADF-STEM). We found the co-existence of different stacking sequence (β- and γ-InSe) in the same flake with a sharp grain boundary in few-layered InSe. Edge reconstruction is also observed in monolayer InSe, which has a distinct atomic structure from the bulk lattice. Moreover, we discovered that the second-harmonic generation (SHG) signal from monolayer InSe shows large optical second-order susceptibility that is 1–2 orders of magnitude higher than MoS2, and even 3 times of the largest value reported in monolayer GaSe. These results make atom-thin InSe a promising candidate for optoelectronic and photosensitive device applications.

Synthesis and characterization of Au incorporated Alq3 nanowires

Science.gov (United States)

Khan, Mohammad Bilal; Ahmad, Sultan; Parwaz, M.; Rahul, Khan, Zishan H.

2018-05-01

We report the synthesis and characterization of pure and Au incorporated Alq3 nanowires. These nanowires are synthesized using thermal vapor transport method. The luminescence intensity of Au incorporated Alq3 nanowires are recorded to be higher than that of pure Alq3 nanowires, which is found to increase with the increase in Au concentration. Fluorescence quenching is also observed when Au concentration is increased beyond the certain limit.

Synthesis and Characterization of Highly Intercalated Graphite Bisulfate

Science.gov (United States)

Salvatore, Marcella; Carotenuto, Gianfranco; De Nicola, Sergio; Camerlingo, Carlo; Ambrogi, Veronica; Carfagna, Cosimo

2017-03-01

Different chemical formulations for the synthesis of highly intercalated graphite bisulfate have been tested. In particular, nitric acid, potassium nitrate, potassium dichromate, potassium permanganate, sodium periodate, sodium chlorate, and hydrogen peroxide have been used in this synthesis scheme as the auxiliary reagent (oxidizing agent). In order to evaluate the presence of delamination, and pre-expansion phenomena, and the achieved intercalation degree in the prepared samples, the obtained graphite intercalation compounds have been characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), X-ray powder diffraction (XRD), infrared spectroscopy (FT-IR), micro-Raman spectroscopy ( μ-RS), and thermal analysis (TGA). Delamination and pre-expansion phenomena were observed only for nitric acid, sodium chlorate, and hydrogen peroxide, while the presence of strong oxidizers (KMnO4, K2Cr2O7) led to stable graphite intercalation compounds. The largest content of intercalated bisulfate is achieved in the intercalated compounds obtained from NaIO4 and NaClO3.

Synthesis and characterization of DC magnetron sputtered nano structured molybdenum thin films

Energy Technology Data Exchange (ETDEWEB)

Rondiya, S. R.; Rokade, A. V.; Jadhavar, A. A.; Pandharkar, S. M.; Kulkarni, R. R.; Karpe, S. D.; Diwate, K. D. [School of Energy Studies, Savitribai Phule Pune University, Pune 411007 (India); Jadkar, S. R., E-mail: sandesh@physics.unipune.ac.in [Department of Physics, Savitribai Phule Pune University, Pune 411007 (India)

2016-04-13

Molybdenum (Mo) thin films were deposited on corning glass (#7059) substrates using DC magnetron sputtering system. The effect of substrate temperature on the structural, morphology and topological properties have been investigated. Films were characterized by variety of techniques such as low angle x-ray diffraction (low angle XRD), field emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM). The low angle XRD analysis revealed that the synthesized Mo films are nanocrystalline having cubic crystal structure with (110) preferential orientation. The microstructure of the deposited Mo thin films observed with FE-SEM images indicated that films are homogeneous and uniform with randomly oriented leaf shape morphology. The AFM analysis shows that with increase in substrate temperature the rms roughness of Mo films increases. The obtained results suggest that the synthesized nanostructured Mo thin films have potential application as a back contact material for high efficiency solar cells like CdTe, CIGS, CZTS etc.

Synthesis and characterization of alumina-coated aluminum sponges manufactured by sintering and dissolution process as possible structured reactors

International Nuclear Information System (INIS)

Méndez, Franklin J.; Rivero-Prince, Sayidh; Escalante, Yelisbeth; Villasana, Yanet; Brito, Joaquín L.

2016-01-01

Al_2O_3–Al sponges were manufactured by sintering and dissolution process with the aim of using these materials as structured catalytic reactors. For this purpose, several synthesis conditions were examined for the design of the cellular material, such as: particle size of NaCl, weight fraction of Al, compaction pressure, and sintering temperature or time. An alumina layers was grown on top of the aluminum surfaces during both: sintering and thermal treatment. The obtained results showed that the synthesized materials could be promising as structured reactors for endothermic or exothermic reactions. - Highlights: • An efficient method for manufactured of aluminum sponges is reported. • Methods for productions of superficial Al_2O_3 are studied. • Al_2O_3–Al sponges could be used as structured reactors.

Green synthesis and characterization of graphene nanosheets

Energy Technology Data Exchange (ETDEWEB)

Tavakoli, Farnosh [School of Chemistry, College of Science, University of Tehran, Tehran (Iran, Islamic Republic of); Salavati-Niasari, Masoud, E-mail: salavati@kashanu.ac.ir [Institute of Nano Science and Nano Technology, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of); Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of); Badiei, Alireza [School of Chemistry, College of Science, University of Tehran, Tehran (Iran, Islamic Republic of); Mohandes, Fatemeh [Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of)

2015-03-15

Highlights: • For the first time, we have synthesized graphene nanosheets in the presence of pomegranate juice. • Here pomegranate juice was used not only as reductant but also as capping agent. • FT-IR, XRD, SEM, EDS and TEM were used to characterize the samples. • According to TEM image, graphene nanosheet is individually exfoliated after stirring for 24 h. • As shown in the TEM image, graphene monolayer is obtained. - Abstract: For the first time, we have successfully synthesized graphene nanosheets in the presence of pomegranate juice. In this approach, pomegranate juice was used not only as reductant but also as capping agent to form graphene nanosheets. At first, the improved Hummer method to oxidize graphite for the synthesis of graphene oxide (GO) was applied, and then the as-produced graphene oxide was reduced by pomegranate juice to form graphene nanosheets. Fourier transformed infrared (FT-IR), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and raman were used to characterize the samples. The results obtained from the characterization techniques proved high purity of the final products.

Green synthesis and characterization of graphene nanosheets

International Nuclear Information System (INIS)

Tavakoli, Farnosh; Salavati-Niasari, Masoud; Badiei, Alireza; Mohandes, Fatemeh

2015-01-01

Highlights: • For the first time, we have synthesized graphene nanosheets in the presence of pomegranate juice. • Here pomegranate juice was used not only as reductant but also as capping agent. • FT-IR, XRD, SEM, EDS and TEM were used to characterize the samples. • According to TEM image, graphene nanosheet is individually exfoliated after stirring for 24 h. • As shown in the TEM image, graphene monolayer is obtained. - Abstract: For the first time, we have successfully synthesized graphene nanosheets in the presence of pomegranate juice. In this approach, pomegranate juice was used not only as reductant but also as capping agent to form graphene nanosheets. At first, the improved Hummer method to oxidize graphite for the synthesis of graphene oxide (GO) was applied, and then the as-produced graphene oxide was reduced by pomegranate juice to form graphene nanosheets. Fourier transformed infrared (FT-IR), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and raman were used to characterize the samples. The results obtained from the characterization techniques proved high purity of the final products

Synthesis, characterization and crystal structure of N,N'-Bis(2,3-Dimethoxybenzylidene)-1,2-Diaminoethane

Czech Academy of Sciences Publication Activity Database

Khalaji, A.D.; Fejfarová, Karla; Dušek, Michal; Bijanzadeh, H.R.

2011-01-01

Roč. 41, č. 12 (2011), 1955-1960 ISSN 1074-1542 Institutional research plan: CEZ:AV0Z10100521 Keywords : Shiff bases * X-ray diffraction * Jana2006 * crystal structure * characterization Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.566, year: 2011

Synthesis and characterization of silver nanoparticles by sol-gel route from silver nitrate

International Nuclear Information System (INIS)

Morales, Jorge; Moran, Jose; Quintana, Maria; Estrada, Walter

2009-01-01

Silver nanoparticles colloids have been synthesized by sol-gel method. This synthesis consists in silver nitrate reduction by ethylene glycol in a process called polyol. The growth of the nanoparticles have been controlled by the steric stabilization of the colloid with polyvinylpyrrolidone (PVP, M w = 40 000). The silver nanoparticle size and structure was depending on the control of parameters such as: molar concentrations ratio of silver nitrate and PVP, temperature of reaction and the reflux time. Colloids have been characterized by UV-vis spectroscopy in the range from 300 to 1000 nm. The results show that the typical peak of surface plasmon resonance is formed at 400-450 nm indicating the formation of silver nanoparticles. The presences of silver nanoparticles of spherical shape with size among 20-40 nm were observed by transmission electronic microscopy (TEM). Electron diffraction patterns confirmed that synthesized colloids contain metallic silver with a crystal structure face centered cubic FCC. (author)

Synthesis, characterization, and application of surface-functionalized ordered mesoporous nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Chung, Po-Wen [Iowa State Univ., Ames, IA (United States)

2009-01-01

The dissertation begins with Chapter 1, which is a general introduction of the fundamental synthesis of mesoporous silica materials, the selective functionlization of mesoporous silica materials, and the synthesis of nanostructured porous materials via nanocasting. In Chapter 2, the thermo-responsive polymer coated mesoporous silica nanoparticles (MSN) was synthesized via surface-initated polymerization and exhibited unique partition activities in a biphasic solution with the thermally induced change. In Chapter 3, the monodispersed spherical MSN with different mesoporous structure (MCM-48) was developed and employed as a template for the synthesis of mesoporous carbon nanoparticles (MCN) via nanocasting. MCN was demonstrated for the delivery of membrane impermeable chemical agents inside the cells. The cellular uptake efficiency and biocompabtibility of MCN with human cervical cancer cells were also investigated. In addition to the biocompabtibility of MCN, MCN was demonstrated to support Rh-Mn nanoparticles for catalytic reaction in Chapter 4. Owing to the unique mesoporosity, Rh-Mn nanoparticles can be well distributed inside the mesoporous structure and exhibited interesting catalytic performance on CO hydrogenation. In Chapter 5, the synthesis route of the aforementioned MCM-48 MSN was discussed and investigated in details and other metal oxide nanoparticles were also developed via nanocasting by using MCM-48 MSN as a template. At last, there is a general conclusion summarized in Chapter 6.

Soft chemistry routes to transparent metal oxide thin films. The case of sol–gel synthesis and structural characterization of Ta{sub 2}O{sub 5} thin films from tantalum chloromethoxide

Energy Technology Data Exchange (ETDEWEB)

Epifani, Mauro, E-mail: mauro.epifani@le.imm.cnr.it [Istituto per la Microelettronica e i Microsistemi, IMM-CNR, Via Monteroni, 73100 Lecce (Italy); Zamani, Reza [Catalonia Institute for Energy Research, IREC c/Jardins de les Dones de Negre, 1, 08930-Sant Adria del Besos, Barcelona (Spain); Institut de Ciència de Materials de Barcelona, ICMAB-CSIC, 08193 Bellaterra, CAT (Spain); Arbiol, Jordi [Institut de Ciència de Materials de Barcelona, ICMAB-CSIC, 08193 Bellaterra, CAT (Spain); Institucio Catalana de Recerca i Estudis Avançats, ICREA, 08010, Barcelona (Spain); Fabrega, Cristian; Andreu, Teresa [Catalonia Institute for Energy Research, IREC c/Jardins de les Dones de Negre, 1, 08930-Sant Adria del Besos, Barcelona (Spain); Pace, Giovanni Battista; Siciliano, Pietro [Istituto per la Microelettronica e i Microsistemi, IMM-CNR, Via Monteroni, 73100 Lecce (Italy); Morante, Joan R. [Catalonia Institute for Energy Research, IREC c/Jardins de les Dones de Negre, 1, 08930-Sant Adria del Besos, Barcelona (Spain); M2E-IN2UB-XaRMAE, Departament d’Electrònica, Universitat de Barcelona, C. Martí i Franquès 1, 08028 Barcelona, CAT (Spain)

2014-03-31

Ta{sub 2}O{sub 5} thin films were prepared by spin-coating methanol solutions of Ta chloromethoxide. It was prepared by reacting TaCl{sub 5} with methanol, followed by water addition (H{sub 2}O: Ta molar ratio was 16). Thin films were deposited by spin-coating onto SiO{sub 2}/Si substrates, followed by drying at 90 °C and heat-treatment up to 700 °C. The films were characterized by X-ray diffraction, transmission electron microscopy and field emission scanning electron microscopy. Crystallization was obtained only after heating at 700 °C, in the Ta{sub 2}O{sub 5} orthorhombic phase. The resulting films had a thickness of 100 nm. Their structure was constituted by porous crystals with size up to 50 nm, while the pores had a size of about 10 nm. The results demonstrated that TaCl{sub 5} is very convenient precursor for the wet chemical synthesis of Ta{sub 2}O{sub 5} thin films. - Highlights: • Development of convenient solution synthesis of Ta{sub 2}O{sub 5} thin films; • The precursor chemistry was established and related to the synthesis process; • Uniform films crystallized in the most stable orthorombic Ta{sub 2}O{sub 5} phase;.

Structured mesoporous Mn, Fe, and Co oxides: Synthesis, physicochemical, and catalytic properties

Science.gov (United States)

Maerle, A. A.; Karakulina, A. A.; Rodionova, L. I.; Moskovskaya, I. F.; Dobryakova, I. V.; Egorov, A. V.; Romanovskii, B. V.

2014-02-01

Structured mesoporous Mn, Fe, and Co oxides are synthesized using "soft" and "hard" templates; the resulting materials are characterized by XRD, SEM, TEM, BET, and TG. It is shown that in the first case, the oxides have high surface areas of up to 450 m2/g that are preserved after calcination of the material up to 300°C. Even though, the surface area of the oxides prepared by the "hard-template" method does not exceed 100 m2/g; it is, however, thermally stable up to 500°C. Catalytic activity of mesoporous oxides in methanol conversion was found to depend on both the nature of the transition metal and the type of template used in synthesis.

Molybdenum oxide nanocubes: Synthesis and characterizations

Energy Technology Data Exchange (ETDEWEB)

Muthamizh, S.; Suresh, R.; Giribabu, K.; Manigandan, R.; Kumar, S. Praveen; Munusamy, S.; Narayanan, V., E-mail: vnnara@yahoo.co.in [Department of Inorganic Chemistry, University of Madras, Guindy Campus, Chennai -600025 (India); Stephen, A. [Department of Nuclear Physics, University of Madras, Guindy Campus, Chennai-600025 (India)

2015-06-24

Molybdenum oxide nanoparticles were prepared by Solid state synthesis. The MoO{sub 3} nanoparticles were synthesized by using commercially available ammonium heptamolybdate. The XRD pattern reveals that the synthesized MoO{sub 3} has orthorhombic structure. In addition, lattice parameter values were also calculated using XRD data. The Raman analysis confirm the presence of Mo-O in MoO{sub 3} nanoparticles. DRS-UV analysis shows that MoO{sub 3} has a band gap of 2.89 eV. FE-SEM analysis confirms the material morphology in cubes with nano scale.

An alternative gas sensor material: Synthesis and electrical characterization of SmCoO3

International Nuclear Information System (INIS)

Michel, Carlos Rafael; Delgado, Emilio; Santillan, Gloria; Martinez, Alma H.; Chavez-Chavez, Arturo

2007-01-01

Single-phase perovskite SmCoO 3 was prepared by a wet-chemical synthesis technique using metal-nitrates and citric acid; after its characterization by thermal analyses and X-ray diffraction, sintering at 900 deg. C in air, gave single phase and well crystallized powders. The powders were mixed with an organic solvent to prepare a slurry, which was deposited on alumina substrates as thick films, using the screen-printing technique. Electrical and gas sensing properties of sintered SmCoO 3 films were investigated in air, O 2 and CO 2 , the results show that sensitivity reached a maximum value at 420 deg. C, for both gases. Dynamic tests revealed a better behavior of SmCoO 3 in CO 2 than O 2 , due to a fast response and a larger electrical resistance change to this gas. X-ray diffraction made on powders after electrical characterization in gases, showed that perovskite-type structure was preserved

Synthesis and characterization of a new porphyrin-polyoxometalate hybrid material and investigation of its catalytic activity.

Science.gov (United States)

Araghi, Mehdi; Mirkhani, Valiollah; Moghadam, Majid; Tangestaninejad, Shahram; Mohammdpoor-Baltork, Iraj

2012-03-14

In the present work, the preparation of a new organic-inorganic hybrid material in which tetrakis(p-aminophenylporphyrin) is covalently linked to a Lindqvist structure of polyoxometalate, is reported. This new porphyrin-polyoxometalate hybrid material was characterized by (1)H NMR, FT-IR and UV-Vis spectroscopic methods and cyclic voltammetry. These spectro- and electrochemical studies provided spectral data of the synthesis of this compound. Cyclic voltammetry showed the influence of the porphyrin on the redox process of the polyoxometalate. The catalytic activity of this hybrid material was investigated in the alkene epoxidation with NaIO(4).

A series of fluorene-based two-photon absorbing molecules: synthesis, linear and nonlinear characterization, and bioimaging

Science.gov (United States)

Andrade, Carolina D.; Yanez, Ciceron O.; Rodriguez, Luis; Belfield, Kevin D.

2010-01-01

The synthesis, structural, and photophysical characterization of a series of new fluorescent donor–acceptor and acceptor-acceptor molecules, based on the fluorenyl ring system, with two-photon absorbing properties is described. These new compounds exhibited large Stokes shifts, high fluorescent quantum yields, and, significantly, high two-photon absorption cross sections, making them well suited for two-photon fluorescence microscopy (2PFM) imaging. Confocal and two-photon fluorescence microscopy imaging of COS-7 and HCT 116 cells incubated with probe I showed endosomal selectivity, demonstrating the potential of this class of fluorescent probes in multiphoton fluorescence microscopy. PMID:20481596

Synthesis and Characterization of CdS/CdSxSe1-x Nanowires

Science.gov (United States)

Agueda Lopez, Kleyser; Wu, Marvin

Semiconductor nanowire heterostructures are of interest for potential applications in solar cells and other advanced optoelectronic devices. We report here on synthesis of CdS/CdSxSe1-x nanowires (NWs) using a dual source vapor = liquid - solid technique, and characterization of these NWs with scanning electron microscopy and optical microscopy. We determine the effect of growth parameters, including source / substrate temperatures and time of exposure, on NW size, shape, and composition. The crystal structure and optical properties individual NWs from selected substrates has been mapped using transmission Kikuchi diffraction and photoluminescence (PL) microscopy. NWs consistently exhibit a hexagonal structure, with growth along the c-axis. Strong PL peaks are observed between the expected bandgap emission from CdS and CdSe, confirming formation of CdSxSe1-x. PL peaks vary significantly with intensity along the long axis of the nanowire, suggesting that the NW surface is not uniformly passivated. These nanowires show promise for future investigation and manipulation of energy band gaps contain in CdS/CdSe. CREST.

Synthesis, structural characterization, thermal analysis, and DFT calculation of a novel zinc (II)-trifluoro-β-diketonate 3D supramolecular nano organic-inorganic compound with 1,3,5-triazine derivative

Energy Technology Data Exchange (ETDEWEB)

Mirtamizdoust, Babak, E-mail: babakm.tamizdoust@gmail.com [Department of Chemistry, Yasouj University, Yasouj, 75918-74831 (Iran, Islamic Republic of); Department of Chemistry, Faculty of Science, University of Qom, PO Box 37185-359, Qom, Islamic Republic of Iran (Iran, Islamic Republic of); Ghaedi, Mehrorang [Department of Chemistry, Yasouj University, Yasouj, 75918-74831 (Iran, Islamic Republic of); Hanifehpour, Younes, E-mail: y_hanifehpour@yu.ac.kr [School of Mechanical Engineering, WCU Nano Research Center, Yeungnam University, Gyongsan, 712-749 (Korea, Republic of); Mague, Joel T. [Department of Chemistry, Tulane University, New Orleans (United States); Joo, Sang Woo, E-mail: swjoo1@gmail.com [School of Mechanical Engineering, WCU Nano Research Center, Yeungnam University, Gyongsan, 712-749 (Korea, Republic of)

2016-10-01

A sonochemical method was used to synthesize a novel nano-structure of a zinc(II) organic-inorganic compound [Zn(dapt){sub 2}(ttfa){sub 2}] (1) [dapt = 2,4-diamino-6-phenyl-1,3,5-triazine and ttfa = 2-thenoyltrifluoroacetonate]. The new nanostructure was characterized by scanning electron microscopy, X-ray powder diffraction, elemental analysis, and thermal analysis. The single-crystal X-ray structure shows that 1 is a discrete coordination compound. Strong intra- and intermolecular hydrogen bonds are observed in the structure with the latter forming chains of molecules running parallel to (110). The chains are further extended into a three-dimensional supramolecular structure by intermolecular C−F⋯π interactions between trifluoromethyl and triazine moieties. The coordination number of the zinc(II) ion is six (ZnN{sub 2}O{sub 4}), and the coordination sphere is tetragonally elongated octahedral. The structure of the title complex was optimized by DFT calculations. - Highlights: • A new zinc(II) 3D coordination supramolecular compound was synthesized. • Ultrasound synthesis of nano coordination compound have been reported. • The X-ray crystal structure of the compound is reported.

Synthesis of second phase hybrid ceramics using two different bio-source and a comparative study on their morphological characterization

Science.gov (United States)

Karivaratharajan, Adhitya; Baskaran, Sidharth; Thillairajan, K.

2018-02-01

Ceramics are generally synthesized with various sources and methods. The most common method for synthesis of ceramics with reduced cost and energy is SOL-GEL method. Combustion synthesis is also a most widely used method for ceramic synthesis. In general, ceramics have enhanced hardness and dimensional stability even at elevated temperatures. For this reason, they are used in the production of refractories, thermal barrier coatings, chemical resistant coatings, wear resistant coatings, and also as reinforcement material to produce metal matrix composites and polymer matrix composites. This work concentrates on the comparison of morphological characterization of such reinforcement particles synthesized from different sources. The particles size range varying from 7 μm to 250 μm with flaky and spongy structures are observed in the ash of Vicia faba. However, the ash of Cocos nucífera resulted in fibrous structure with a diameter of 50 μm to length above 600 μm, particles size ranging from 10 μm to 70 μm micro tubes of diameter 3.6 μm to length of 150 μm. The EDX and XRD analysis of Vicia faba showed the presence of carbon as the major element with a few other elements.

Mesoporous silicas with covalently immobilized β-cyclodextrin moieties: synthesis, structure, and sorption properties

Science.gov (United States)

Roik, Nadiia V.; Belyakova, Lyudmila A.; Trofymchuk, Iryna M.; Dziazko, Marina O.; Oranska, Olena I.

2017-09-01

Mesoporous silicas with chemically attached macrocyclic moieties were successfully prepared by sol-gel condensation of tetraethyl orthosilicate and β-cyclodextrin-silane in the presence of a structure-directing agent. Introduction of β-cyclodextrin groups into the silica framework was confirmed by the results of IR spectral, thermogravimetric, and quantitative chemical analysis of surface compounds. The porous structure of the obtained materials was characterized by nitrogen adsorption-desorption measurements, powder X-ray diffraction, transmission electron microscopy, and dynamic light scattering. It was found that the composition of the reaction mixture used in β-cyclodextrin-silane synthesis significantly affects the structural parameters of the resulting silicas. The increase in (3-aminopropyl)triethoxysilane as well as the coupling agent content in relation to β-cyclodextrin leads ultimately to the lowering or complete loss of hexagonal arrangement of pore channels in the synthesized materials. Formation of hexagonally ordered mesoporous structure was observed at molar composition of the mixture 0.049 TEOS:0.001 β-CD-silane:0.007 CTMAB:0.27 NH4OH:7.2 H2O and equimolar ratio of components in β-CD-silane synthesis. The sorption of alizarin yellow on starting silica and synthesized materials with chemically attached β-cyclodextrin moieties was studied in phosphate buffer solutions with pH 7.0. Experimental results of the dye equilibrium sorption were analyzed using Langmuir, Freundlich, and Redlich-Peterson isotherm models. It was proved that the Redlich-Peterson isotherm model is the most appropriate for fitting the equilibrium sorption of alizarin yellow on parent silica with hexagonally arranged mesoporous structure as well as on modified one with chemically immobilized β-cyclodextrin groups. [Figure not available: see fulltext.

Synthesis and characterization of alumina-coated aluminum sponges manufactured by sintering and dissolution process as possible structured reactors

Energy Technology Data Exchange (ETDEWEB)

Méndez, Franklin J., E-mail: fmendez@ivic.gob.ve [Centro de Química, Instituto Venezolano de Investigaciones Científicas, Apartado Postal 21827, Caracas 1020-A (Venezuela, Bolivarian Republic of); Rivero-Prince, Sayidh [Centro de Química, Instituto Venezolano de Investigaciones Científicas, Apartado Postal 21827, Caracas 1020-A (Venezuela, Bolivarian Republic of); Facultad de Ingeniería, Universidad Central de Venezuela, Caracas (Venezuela, Bolivarian Republic of); Escalante, Yelisbeth; Villasana, Yanet [Centro de Química, Instituto Venezolano de Investigaciones Científicas, Apartado Postal 21827, Caracas 1020-A (Venezuela, Bolivarian Republic of); Brito, Joaquín L., E-mail: joabrito@ivic.gob.ve [Centro de Química, Instituto Venezolano de Investigaciones Científicas, Apartado Postal 21827, Caracas 1020-A (Venezuela, Bolivarian Republic of)

2016-03-01

Al{sub 2}O{sub 3}–Al sponges were manufactured by sintering and dissolution process with the aim of using these materials as structured catalytic reactors. For this purpose, several synthesis conditions were examined for the design of the cellular material, such as: particle size of NaCl, weight fraction of Al, compaction pressure, and sintering temperature or time. An alumina layers was grown on top of the aluminum surfaces during both: sintering and thermal treatment. The obtained results showed that the synthesized materials could be promising as structured reactors for endothermic or exothermic reactions. - Highlights: • An efficient method for manufactured of aluminum sponges is reported. • Methods for productions of superficial Al{sub 2}O{sub 3} are studied. • Al{sub 2}O{sub 3}–Al sponges could be used as structured reactors.

Structured synthesis of MEMS using evolutionary approaches

DEFF Research Database (Denmark)

Fan, Zhun; Wang, Jiachuan; Achiche, Sofiane

2008-01-01

In this paper, we discuss the hierarchy that is involved in a typical MEMS design and how evolutionary approaches can be used to automate the hierarchical synthesis process for MEMS. The paper first introduces the flow of a structured MEMS design process and emphasizes that system-level lumped...

Metal–organic coordination architectures of tetrazole heterocycle ligands bearing acetate groups: Synthesis, characterization and magnetic properties

International Nuclear Information System (INIS)

Hu, Bo-Wen; Zheng, Xiang-Yu; Ding, Cheng

2015-01-01

Two new coordination complexes with tetrazole heterocycle ligands bearing acetate groups, [Co(L) 2 ] n (1) and [Co 3 (L) 4 (N 3 ) 2 ·2MeOH] n (2) (L=tetrazole-1-acetate) have been synthesized and structurally characterized. Single crystal structure analysis shows that the cobalt-complex 1 has the 3D 3,6-connected (4 2 .6) 2 (4 4 .6 2 .8 8 .10)-ant topology. By introducing azide in this system, complex 2 forms the 2D network containing the [Co 3 ] units. And the magnetic properties of 1 and 2 have been studied. - Graphical abstract: The synthesis, crystal structure, and magnetic properties of the new coordination complexes with tetrazole heterocycle ligands bearing acetate groups are reported. - Highlights: • Two novel Cobalt(II) complexes with tetrazole acetate ligands were synthesized. • The magnetic properties of two complexes were studied. • Azide as co-ligand resulted in different structures and magnetic properties. • The new coordination mode of tetrazole acetate ligand was obtained.

Structural characterization of copper (II tetradecanoate with 2,2′-bipyridine and 4,4′-bipyridine to study magnetic properties

Directory of Open Access Journals (Sweden)

Noha Said Bedowr

2018-03-01

Full Text Available This paper presents synthesis, structural characterization and spintronic applications of copper (II tetradecanoate derived magnetic complexes. The complexes were prepared by a chemical reaction between [Cu2(CH3(CH212COO4](EtOH2 and 2,2′-bipyridine-4,4′-bipyridine ligands respectively. The complexes were further reacted between the product of the first reaction and 4,4′-bipyridine-2,2′-bipyridine respectively. The structural characterization techniques included elemental analysis, Fourier transformed infrared spectroscopy (FTIR, Ultra-violet–Visible (UV–Vis spectroscopy, polarized optical microscopy, magnetic moment and thermogravimetric analysis. The structural and characterization results suggested that the synthesized complexes were binuclear and mononuclear covalent complexes of copper(II with structural formulas [Cu2(η2-(OOCR4](4,4′-bpy2H2O] and [Cu(η1-(OOCR2(2,2′-bpy (4,4′-bpy] respectively.

Synthesis and structural features of resorcinol–formaldehyde resin chars containing nickel nanoparticles

International Nuclear Information System (INIS)

Galaburda, M.V.; Bogatyrov, V.M.; Skubiszewska-Zięba, J.; Oranska, O.I.; Sternik, D.; Gun’ko, V.M.

2016-01-01

Graphical abstract: - Highlights: • Facile synthesis of the Ni-doped carbon sorbents via carbonization of resorcinol–formaldehyde polymers/nickel(II) acetate mixtures in the inert atmosphere. • Effects of Ni content, as well as water volume and temperature treatment on the morphology and texture of the chars. • Ni/C composites are characterized by a core–shell structure with well-crystallized graphitic shells. • Ni content influences the structure of the carbon. • Nickel-doped carbon nanocomposites were used as a magnetically separable adsorbent. - Abstract: A series of meso- and microporous carbons containing magnetic Ni nanoparticles (Ni/C) with a variety of Ni loadings were synthesized by a simple one-pot procedure through carbonization of resorcinol–formaldehyde polymers containing various amounts of nickel(II) acetate. Such composite materials were characterized by N_2 sorption, Raman spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM) and Transmission electron microscope (TEM). The XRD patterns reveal peaks corresponding to face centered cubic nickel with the average size of crystallites of 17–18 nm. SEM and TEM results reveal that the formation of the nanoparticles took place mainly in the carbon spheres (1–2 μm in size) and on the outer surface as well. The as-prepared composites are characterized by a core–shell structure with well-crystallized graphitic shells about 8–15 nm in thickness. The Raman spectra show that Ni content influences the structure of the carbon. It was also shown that the morphology (particle shape and sizes) and porosity (pore volume and pore size distribution) of the chars are strongly dependent on water and nickel contents in the blends. One of the applications of Ni/C was demonstrated as a magnetically separable adsorbent.

Synthesis and characterization of tunable coumarin- linked glasses as new class of organic/inorganic phosphors

Energy Technology Data Exchange (ETDEWEB)

Luridiana, Alberto; Pretta, Gianluca; Secci, Francesco; Frongia, Angelo [Dipartimento di Scienze Chimiche e Geologiche, Università degli Studi di Cagliari, Complesso universitario di Monserrato, SS 554, bivio per Sestu, Monserrato (Canada) (Italy); Chiriu, Daniele; Carbonaro, Carlo Maria; Corpino, Riccardo [Dipartimento di Fisica, Università degli Studi di Cagliari, Complesso universitario di Monserrato, SS 554, bivio per Sestu, Monserrato (Canada) (Italy); Ricci, Pier Carlo, E-mail: carlo.ricci@dsf.unica.it [Dipartimento di Fisica, Universitá degli Studi di Cagliari, S.P. Monserrato-Sestu Km 0,700, 09042 Monserrato (Canada) (Italy)

2014-10-21

It is well known that stilbene with a trans conformation is highly fluorescent. From the viewpoint of molecular structure, coumarins bear a carbon-carbon double bond which is fixed as trans conformation as in trans-stilbene through a lactone structure. This can help to avoid the trans-cis transformation of the double bond under ultraviolet (UV) irradiation as observed in stilbene compounds and results in strong fluorescence and high fluorescence quantum yield and photostability in most of coumarin derivatives. Herein we report some preliminary results about the synthesis and spectroscopic characterization of tunable coumarins and the development of a new linkage protocol for the obtainment of monolayer coumarin-covalently linked glasses. The resulting organic/inorganic coumarin/silica based Self-Assembled Monolayer (SMA) film is proposed as new phosphors for the substituting of critical raw materials, like rare earths, in photonics applications.

Synthesis, purification and characterization of [3,5 - T] p-aminobenzoic acid

International Nuclear Information System (INIS)

Corol-Cucu, Delia-Irina; Chiper, Diana; Mihaila, V.; Negoita, N.

2000-01-01

This paper refers to the synthesis, purification and characterization of [3,5-T] p-aminobenzoic acid (PAB,H' vitamine). The p-aminobenzoic acid is used in the treatment of rheumatic arthritis and dermatological affections. The advantage of tritium labelling of p-aminobenzoic acid is that some biomedical important aspects of collagen's behaviour are made clear. The PAB stimulate the grow of intestinal bacteria so necessary to synthesis of some vitamins (bio tine, pantothenic acid). Tritium is the only radioactive isotope of hydrogen. Several steps have to be carried out in the synthesis of the final product as well as to study its biological behavior. For the labelling of PAB one prefers the substitution of bromine from PAB-3,5-Br with tritium because of simplicity of reaction and the easy synthesis of halogen compound. The first step in synthesis is the protection of NH 2 group through acetylation of PAB. After that PAB is bromated into the 3 and 5 position with elementary bromine. The raw compound is purified and recrystallized and characterized through thin layer chromatography.The tritium labelling is performed through substitution of bromine from bromate derivative, using Pd/C (10% Pd) as catalyst and low basic conditions for the neutralization of HBr resulting from reaction. After the separation of PAB-3,5-T through filtration, the catalyst remains on the filter paper and the labelled compound goes in aqueous solution. PAB-3,5-T is purified through thin layer chromatography with the solvent system n-BuOH:NH 4 OH(25%):H 2 O:EtOH (8:1:2:2,5, v/v) with silica gel GF 254 as support. The determination of activity is carried out with LSC (Liquid Scintillation Counter). A 98% purity was determined through TLC in the same conditions while determination of activity distribution was performed with a 2π Berthold scanner with gas running and without window. The chemical concentration has been measured through UV spectrophotometry and by comparing extinction with

Synthesis, characterization and mechanistic insights of mycogenic iron oxide nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Bhargava, Arpit; Jain, Navin; Manju Barathi L [Birla Institute of Technology and Science, Centre for Biotechnology, Department of Biological Sciences (India); Akhtar, Mohd Sayeed [Jimma University, Department of Applied Microbiology, College of Natural Sciences (Ethiopia); Yun, Yeoung-Sang [Chonbuk National University, Division of Environmental and Chemical Engineering (Korea, Republic of); Panwar, Jitendra, E-mail: drjitendrapanwar@yahoo.co.in [Birla Institute of Technology and Science, Centre for Biotechnology, Department of Biological Sciences (India)

2013-11-15

In the present study, extracellular synthesis of iron oxide nanoparticles (IONPs) was achieved using Aspergillus japonicus isolate AJP01. The isolate demonstrated its ability to hydrolyze the precursor salt solution, a mixture of iron cyanide complexes, under ambient conditions. Hydrolysis of these complexes released ferric and ferrous ions, which underwent protein-mediated coprecipitation and controlled nucleation resulting in the formation of IONPs. Transmission electron microscopy, selected area electron diffraction pattern, energy dispersive spectroscopy and grazing incidence X-ray diffraction analysis confirmed the mycosynthesis of IONPs. The synthesized particles were cubic in shape with a size range of 60–70 nm with crystal structure corresponding to magnetite. Scanning electron microscopy analysis revealed the absence of IONPs on fungal biomass surface, indicating the extracellular nature of synthesis. Fourier transform infrared spectroscopy confirmed the presence of proteins on as-synthesised IONPs, which may confer their stability. Preliminary investigation indicated the role of proteins in the synthesis and stabilization of IONPs. On the basis of present findings, a probable mechanism for synthesis of IONPs is suggested. The simplicity and versatility of the present approach can be utilized for the synthesis of other nanomaterials.

Controllable synthesis and characterization of novel copper-carbon core-shell structured nanoparticles

International Nuclear Information System (INIS)

Zhai, Jing; Tao, Xia; Pu, Yuan; Zeng, Xiao-Fei; Chen, Jian-Feng

2011-01-01

Highlights: → We reported a facile, green and cheap hydrothermal method to obtain novel copper-carbon core-shell nanoparticles. → The as-formed particles with controllable size and morphology are antioxidant. → The particles with organic-group-loaded surfaces and protective shells are expected to be applied in fields of medicine, electronics, sensors and lubricant. -- Abstract: A facile hydrothermal method was developed for preparing copper-carbon core-shell structured particles through a reaction at 160 o C in which glucose, copper sulfate pentahydrate and cetyltrimethylammonium bromide were used as starting materials. The original copper-carbon core-shell structured particles obtained were sized of 100-250 nm. The thickness of carbonaceous shells was controlled ranging from 25 to 100 nm by adjusting the hydrothermal duration time and the concentrations of glucose in the process. Products were characterized with transmission electron microscopy, X-ray diffraction, energy dispersive spectroscopy, Fourier transform infrared spectroscopy. Since no toxic materials were involved in the preparation, particles with stable carbonaceous framework and reactive surface also showed promising applications in medicine, electronics, sensors, lubricant, etc.

Controllable synthesis and characterization of novel copper-carbon core-shell structured nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Zhai, Jing [Sin-China Nano Technology Center, Key Lab for Nanomaterials, Ministry of Education, Beijing University of Chemical Technology, Beijing 100029 (China); Research Center of the Ministry of Education for High Gravity Engineering and Technology, Beijing University of Chemical Technology, No. 15 Beisanhuan Dong Lu, Beijing 100029 (China); Tao, Xia; Pu, Yuan; Zeng, Xiao-Fei [Sin-China Nano Technology Center, Key Lab for Nanomaterials, Ministry of Education, Beijing University of Chemical Technology, Beijing 100029 (China); Chen, Jian-Feng, E-mail: chenjf@mail.buct.edu.cn [Research Center of the Ministry of Education for High Gravity Engineering and Technology, Beijing University of Chemical Technology, No. 15 Beisanhuan Dong Lu, Beijing 100029 (China)

2011-06-15

Highlights: {yields} We reported a facile, green and cheap hydrothermal method to obtain novel copper-carbon core-shell nanoparticles. {yields} The as-formed particles with controllable size and morphology are antioxidant. {yields} The particles with organic-group-loaded surfaces and protective shells are expected to be applied in fields of medicine, electronics, sensors and lubricant. -- Abstract: A facile hydrothermal method was developed for preparing copper-carbon core-shell structured particles through a reaction at 160 {sup o}C in which glucose, copper sulfate pentahydrate and cetyltrimethylammonium bromide were used as starting materials. The original copper-carbon core-shell structured particles obtained were sized of 100-250 nm. The thickness of carbonaceous shells was controlled ranging from 25 to 100 nm by adjusting the hydrothermal duration time and the concentrations of glucose in the process. Products were characterized with transmission electron microscopy, X-ray diffraction, energy dispersive spectroscopy, Fourier transform infrared spectroscopy. Since no toxic materials were involved in the preparation, particles with stable carbonaceous framework and reactive surface also showed promising applications in medicine, electronics, sensors, lubricant, etc.

Synthesis and characterization of inverse spinels, intercalation materials for Li-ion batteries

NARCIS (Netherlands)

Van Landschoot, N.

2006-01-01

Chapter 2 describes the solid-state synthesis of LiNiVO4 and LiCoVO4. The materials are prepared at 800C and are phase pure, as shown by X-ray diffraction and have the inverse spinel structure. Due to the solid-state synthesis the particle size is quite large and the particle size distribution is

Synthesis and structure of two-dimensional transition-metal dichalcogenides

KAUST Repository

Shi, Yumeng; Zhang, Hua; Chang, Wen-Hao; Shin, Hyeon Suk; Li, Lain-Jong

2015-01-01

Two-dimensional (2D) transition-metal dichalcogenides (TMDCs) exhibit unique electrical, optical, thermal, and mechanical properties, which enable them to be used as building blocks in compact and lightweight integrated electronic systems. The controllable and reliable synthesis of atomically thin TMDCs is essential for their practical application. Recent progress in large-area synthesis of monolayer TMDCs paves the way for practical production of various 2D TMDC layers. The intrinsic optical and electrical properties of monolayer TMDCs can be defined by stoichiometry during synthesis. By manipulating the lattice structure or layer stacking manner, it is possible to create atomically thin van der Waals materials with unique and unexplored physical properties. In this article, we review recent developments in the synthesis of TMDC monolayers, alloys, and heterostructures, which shine light on the design of novel TMDCs with desired functional properties.

Synthesis and structure of two-dimensional transition-metal dichalcogenides

KAUST Repository

Shi, Yumeng

2015-07-13

Two-dimensional (2D) transition-metal dichalcogenides (TMDCs) exhibit unique electrical, optical, thermal, and mechanical properties, which enable them to be used as building blocks in compact and lightweight integrated electronic systems. The controllable and reliable synthesis of atomically thin TMDCs is essential for their practical application. Recent progress in large-area synthesis of monolayer TMDCs paves the way for practical production of various 2D TMDC layers. The intrinsic optical and electrical properties of monolayer TMDCs can be defined by stoichiometry during synthesis. By manipulating the lattice structure or layer stacking manner, it is possible to create atomically thin van der Waals materials with unique and unexplored physical properties. In this article, we review recent developments in the synthesis of TMDC monolayers, alloys, and heterostructures, which shine light on the design of novel TMDCs with desired functional properties.

Sol – Gel synthesis and characterization of magnesium peroxide nanoparticles

International Nuclear Information System (INIS)

Jaison, J; Chan, Y S; Ashok raja, C; Balakumar, S

2015-01-01

Magnesium peroxide is an excellent source of oxygen in agriculture applications, for instance it is used in waste management as a material for soil bioremediation to remove contaminants from polluted underground water, biological wastes treatment to break down hydrocarbon, etc. In the present study, sol-gel synthesis of magnesium peroxide (MgO 2 ) nanoparticles is reported. Magnesium peroxide is odourless; fine peroxide which releases oxygen when reacts with water. During the sol-gel synthesis, the magnesium malonate intermediate is formed which was then calcinated to obtain MgO 2 nanoparticles. The synthesized nanoparticles were characterized using Thermo gravimetric -Differential Thermal Analysis (TG- DTA), X-Ray Diffraction studies (XRD) and High Resolution Transmission Electron Microscope (HRTEM). Our study provides a clear insight that the formation of magnesium malonate during the synthesis was due to the reaction between magnesium acetate, oxalic acid and ethanol. In our study, we can conclude that the calcination temperature has a strong influence on particle size, morphology, monodispersity and the chemistry of the particles. (paper)

Niobium-Doped Hydroxyapatite Bioceramics: Synthesis, Characterization and In Vitro Cytocompatibility

Directory of Open Access Journals (Sweden)

Nádia S. V. Capanema

2015-07-01

Full Text Available Doping calcium phosphates with ionic species can play an important role in biological responses promoting alkaline phosphatase activity, and, therefore inducing the generation of new bone. Thus, in this study, the synthesis of niobium-doped hydroxyapatite (Nb-HA nanosize particles obtained by the precipitation process in aqueous media followed by thermal treatment is presented. The bioceramics were extensively characterized by X-ray diffraction, wavelength dispersive X-ray fluorescence spectrometry, Fourier transform infrared spectroscopy, scanning electron microscopy/energy dispersive X-ray spectroscopy analysis, transmission electron microscopy, atomic force microscopy and thermal analysis regarding their chemical composition, structure and morphology. The results showed that the precipitate dried at 110 °C was composed of amorphous calcium phosphate and HA, with polidisperse particles ranging from micro to nano dimensions. After the thermal treatment at 900 °C, the bioceramic system evolved predominantly to HA crystalline phase, with evident features of particle sintering and reduction of surface area. Moreover, the addition of 10 mol% of niobium salt precursor during the synthesis indicated the complete incorporation of the Nb(V species in the HA crystals with detectable changes in the original lattice parameters. Furthermore, the incorporation of Nb ions caused a significant refinement on the average particle size of HA. Finally, the preliminary cytocompatibility response of the biomaterials was accessed by human osteoblast cell culture using MTT and resazurin assays, which demonstrated no cytotoxicity of the Nb-alloyed hydroxyapatite. Thus, these findings seem promising for developing innovative Nb-doped calcium phosphates as artificial biomaterials for potential use in bone replacements and repair.

Synthesis, structural characterization of nano ZnTiO3 ceramic: An effective azo dye adsorbent and antibacterial agent

Directory of Open Access Journals (Sweden)

R.S. Raveendra

2014-12-01

Full Text Available Nanocrystalline meta-zinc titanate (ZnTiO3 ceramic was prepared using a self-propagating solution combustion synthesis (SCS for the first time using urea as fuel. The product was calcined at 800 °C for 2 h to improve the crystallinity. Powder X-ray diffraction (PXRD, Fourier transform infrared spectroscopy (FTIR, scanning electron microscopy (SEM, energy-dispersive X-ray spectroscopy (EDAX, high resolution transmission electron microscopy (HR-TEM and UV–vis absorption spectroscopy were used to characterize the final product. PXRD results show that the ilmenite type rhombohedral structure was formed when the sample was calcined at 800 °C for 2 h. Adsorption experiments were performed with cationic malachite green (MG dye. ∼96% dye was adsorbed onto nanocrystalline ZnTiO3 ceramic at pH 9 for 30 min of the contact time. The optimum adsorbent dose was found to be 0.45 g/L of dye. Langmuir–Hinshelwood model was used to study adsorption kinetics and first order kinetic model best describes the MG adsorption on ZnTiO3. Antibacterial activity was investigated against gram negative Klebsiella aerogenes, Pseudomonas desmolyticum, Escherichia coli, and gram positive Staphylococcus aureus bacteria by agar well diffusion method. Nanocrystalline ZnTiO3 ceramic showed significant effect on all the four bacterial strains at the concentration of 1000 and 1500 μg per well.

Synthesis and structural characterization of coaxial nano tubes intercalated of molybdenum disulfide with carbon; Sintesis y caracterizacion estructural de nanotubos coaxiales intercalados de disulfuro de molibdeno con carbono

Energy Technology Data Exchange (ETDEWEB)

Reza San German, C M

2005-07-01

In this work the study of some fundamental aspects in the growth of unidimensional systems of coaxial nano tubes from the mold method is approached. This method is an inclusion technique of a precursor reagent into oxide nano porous alumina film (mold), and later applying some processes of synthesis it is gotten to obtain the wished material. The synthesized structures are identified later because they take place by means of the initial formation of nano tubes of MoS{sub 2}, enclosing to carbon nano tubes by the same method, with propylene flow which generates a graphitization process that 'copy' the mold through as it flows. Binary phase MoS{sub 2} + C nano tubes were synthesized by propylene pyrolysis inside MoS{sub 2} nano tubes prepared by template assisted technique. The large coaxial nano tubes constituted of graphite sheets inserted between the MoS{sub 2} layers forming the outer part, and coaxial multi wall carbon nano tubes (MWCNT) intercalated with MoS{sub 2} inside. High resolution electron microscopy (HRTEM), electron energy loss spectroscopy (EELS), high angle annular dark field (HAADF), gatan image filter (GIF), nano beam electron diffraction patterns (NBEDP), along with molecular dynamics simulation and quantum mechanical calculations were used to characterize the samples. The one-dimensional structures exhibit diverse morphologies such as long straight and twisted nano tubes with several structural irregularities. The inter-planar spacing between MoS{sub 2} layers was found to increase from 6.3 to 7.4 A due to intercalation with carbon. Simulated HREM images revealed the presence of these twisted nano structures, with mechanical stretch into intercalate carbon between MoS{sub 2} layers. Our results open up the possibility of using MoS{sub 2} nano tubes as templates for the synthesis of new one- dimensional binary phase systems. (Author)

Synthesis and structural characterization of coaxial nano tubes intercalated of molybdenum disulfide with carbon; Sintesis y caracterizacion estructural de nanotubos coaxiales intercalados de disulfuro de molibdeno con carbono

Energy Technology Data Exchange (ETDEWEB)

Reza San German, C.M

2005-07-01

In this work the study of some fundamental aspects in the growth of unidimensional systems of coaxial nano tubes from the mold method is approached. This method is an inclusion technique of a precursor reagent into oxide nano porous alumina film (mold), and later applying some processes of synthesis it is gotten to obtain the wished material. The synthesized structures are identified later because they take place by means of the initial formation of nano tubes of MoS{sub 2}, enclosing to carbon nano tubes by the same method, with propylene flow which generates a graphitization process that 'copy' the mold through as it flows. Binary phase MoS{sub 2} + C nano tubes were synthesized by propylene pyrolysis inside MoS{sub 2} nano tubes prepared by template assisted technique. The large coaxial nano tubes constituted of graphite sheets inserted between the MoS{sub 2} layers forming the outer part, and coaxial multi wall carbon nano tubes (MWCNT) intercalated with MoS{sub 2} inside. High resolution electron microscopy (HRTEM), electron energy loss spectroscopy (EELS), high angle annular dark field (HAADF), gatan image filter (GIF), nano beam electron diffraction patterns (NBEDP), along with molecular dynamics simulation and quantum mechanical calculations were used to characterize the samples. The one-dimensional structures exhibit diverse morphologies such as long straight and twisted nano tubes with several structural irregularities. The inter-planar spacing between MoS{sub 2} layers was found to increase from 6.3 to 7.4 A due to intercalation with carbon. Simulated HREM images revealed the presence of these twisted nano structures, with mechanical stretch into intercalate carbon between MoS{sub 2} layers. Our results open up the possibility of using MoS{sub 2} nano tubes as templates for the synthesis of new one- dimensional binary phase systems. (Author)

The synthesis, characterization, crystal structure and theoretical calculations of a new meso-BOBIPY substituted phthalonitrile

International Nuclear Information System (INIS)

Sen, Pinar; Yildiz, S. Zeki; Atalay, Yusuf; Dege, Necmi; Demirtas, Günes

2014-01-01

A novel 4-(2-meso-BOBIPY-phenoxy)phthalonitrile (6) derivative has been synthesized starting from BF 3 –OEt 2 complex and 4-(2-meso-dipyrromethene-phenoxy)phthalonitrile (5) which was prepared by the oxidation of 4-(2-meso-dipyrromethane-phenoxy)phthalonitrile (4). The final product exhibit noticeable spectroscopic properties which were examined by its absorption and fluorescence emission spectra. The original compounds prepared in the reaction pathway were characterized by the combination of FT-IR, 1 H and 13 C NMR, UV–vis, MS and HRMS spectral data. The final product (6) was obtained as single crystal which crystallized in the triclinic space group P-1 with a=7.9411 (6) Å, b=9.0150 (6) Å, c=14.419 (1) Å, α=74.917 (5)°, β=86.824 (6)°, γ=84.109 (5)° and Z=2. The crystal structure has intermolecular C–H···F–B and C–H···N interactions. These interactions construct bifurcated hydrogen bonds in the crystal structure. In this study, It has been calculated; molecular structure, vibrational frequencies, 1 H and 13 C NMR chemical shifts and HOMO and LUMO energies of the title compound by using B3LYP method with 6–311++G(dp) basis set, and the electronic spectral characterization was investigated for the target product, as well. - Highlights: • A novel 4-(2-meso-BOBIPY-phenoxy)phthalonitrile derivative has been synthesized. • The title product exhibit noticeable spectroscopic properties which were examined by its absorption and fluorescence emission spectra. • The final product (6) was obtained as single crystal which crystallized in the triclinic space group. • Molecular structure, vibrational frequencies, 1 H and 13 C NMR chemical shifts and HOMO and LUMO energies of the title compound were calculated theoretically. • The electronic spectral characterization was investigated, as well. • The title compound is also open to prepare further BODIPY substituted oligomeric molecules via on it

Synthesis and Characterization of Block Copolymers with Unique Chemical Functionalities and Entropically-Hindering Moieties

Science.gov (United States)

2017-08-14

methanol as a function of chemistry , morphology and hydration levels. Accomplishments: This section is included in the "upload" section. Training...Copolymer Blend Membranes.” In Press, Polymer Engineering and Science, DOI: 10.1002 /pen.24508, 2017. 5. M. Pérez-Pérez and D. Suleiman. “Synthesis and...Synthesis and Characterization of Sulfonated Amine Block Copolymers for Energy Efficient Applications". Chemical Engineering Symposium, University of

Ionothermal synthesis, crystal structure, and magnetic study of Co2PO4OH isostructural with caminite.

Science.gov (United States)

Wang, Guangmei; Valldor, Martin; Spielberg, Eike T; Mudring, Anja-Verena

2014-03-17

A new framework cobalt(II) hydroxyl phosphate, Co2PO4OH, was prepared by ionothermal synthesis using 1-butyl-4-methyl-pyridinium hexafluorophosphate as the ionic liquid. As the formation of Co2PO4F competes in the synthesis, the synthesis conditions have to be judiciously chosen to obtain well-crystallized, single phase Co2PO4OH. Single-crystal X-ray diffraction analyses reveal Co2PO4OH crystallizes with space group I41/amd (a = b = 5.2713(7) Å, c = 12.907(3) Å, V = 358.63(10) Å(3), and Z = 4). Astonishingly, it does not crystallize isotypically with Co2PO4F but rather isotypically with the hydroxyl minerals caminite Mg1.33[SO4(OH)0.66(H2O)0.33] and lipscombite Fe(2–y)PO4(OH) (0 ≤ y ≤ 2/3). Phosphate tetrahedra groups interconnect four rod-packed face-sharing ∞(1){CoO(6/2)} octahedra chains to form a three-dimensional framework structure. The compound Co2PO4OH was further characterized by powder X-ray diffraction, Fourier transform–infrared, and ultraviolet–visible spectroscopy, confirming the discussed structure. The magnetic measurement reveals that Co2PO4OH undergoes a magnetic transition and presents at low temperatures a canted antiferromagnetic spin order in the ground state.

Synthesis, structural characterization and cytotoxic activity of two new organoruthenium(II complexes

Directory of Open Access Journals (Sweden)

SANJA GRGURIC-SIPKA

2008-06-01

Full Text Available Two new p-cymene ruthenium(II complexes containing as additional ligands N-methylpiperazine ([(η6-p-cymeneRuCl2(CH3NH(CH24NH]PF6, complex 1 or vitamin K3-thiosemicarbazone ([(η6-p-cymeneRuCl2(K3tsc], complex 2 were synthesized starting from [(η6-p-cymene2RuCl2]2 and the corresponding ligand. The complexes were characterized by elemental analysis, IR, electronic absorption and NMR spectroscopy. The X-ray crystal structure determination of complex 1 revealed “piano-stool” geometry. The differences in the cytotoxic activity of the two complexes are discussed in terms of the ligand present.

Synthesis, characterization and magnetic properties of highly monodispersed PtNi nanoparticles

International Nuclear Information System (INIS)

Du, Juan-Juan; Yang, Yi; Zhang, Rong-Hua; Zhou, Xin-Wen

2015-01-01

In this paper, we report the controlled-synthesis of PtNi nanoparticles through galvanic displacement reaction and chemical reduction. The size, composition and morphology of the products are characterized by transmission electron microscopy (TEM), powder X-ray diffraction (XRD), energy dispersed X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS) analyses. The structure and composition of the PtNi nanoparticles can be controlled by adjusting the synthetic conditions. The possible formation mechanism is obtained from the academic analysis and experimental studies. The results of the magnetic measurement illustrate that the PtNi nanoparticles show a superparamagnetic behavior with a blocking temperature (T B ) about 8.0 K. - Highlights: • Highly monodispersed PtNi nanoparticles were synthesized by galvanic displacement reaction. • The formation of Pt nanocrystals was the foremost step because of its self-catalysis effect. • The PtNi nanoparticles show a superparamagnetic behavior with a T B about 8.0 K

Synthesis of CdS hollow/solid nanospheres and their chain-structures by membrane technique

International Nuclear Information System (INIS)

Duan Shumin; Wu Qingsheng; Jia Runping; Liu Xinbo

2008-01-01

CdS hollow/solid nanospheres and their chain-structures were successfully synthesized through supporting liquid membrane (SLM) system with bio-membrane. X-ray powder diffraction (XRD), transmission electron microscopy (TEM), UV-Vis spectroscopy, and photoluminescence (PL) spectroscopy have been used for the characterization of the products. The average diameters of CdS solid/hollow spheres are about 10, 40 nm, respectively. The wall of the hollow spheres is about 5 nm. CdS products are all cubic face-centered structure with the cell constant a = 5.830 A. We also explore the morphology, structure and possible synthesis mechanism. A possible template mechanism has been proposed for the production of the hollow CdS nanocrystals, that is, CdS nanoparticles grow along the non-soakage interface between CHCl3 and reactant solution. During this process, the organic functional groups were crucial to the control of crystal morphologies

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

Science.gov (United States)

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

2018-01-01

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

Synthesis and characterization of polyglycerols dendrimers for applications in tissue engineering biological

Energy Technology Data Exchange (ETDEWEB)

Passos, E.D.; Queiroz, A.A.A. de [Universidade Federal de Itajuba (UNIFEI), MG (Brazil)

2014-07-01

Full text: Introduction: Over the last twenty years is the growing development in the manufacture of synthetic scaffold in tissue engineering applications. These new materials are based on polyglycerol dendrimers (PGLD's). PGLD's are highly functional polymers with hydroxymethyl side groups, fulfill all structural prerequisites to replace poly(ethylene glycol)s in medical applications. Furthermore, since these materials are based on naturally occurring compounds that degrades over time in the body and can be safely excreted. The objective of this work was the synthesis, physicochemical, biological characterization of HPGL's with potential use as scaffolds in tissue engineering. HPGL's with oligomeric cores, of diglycerol triglycerol and tetraglycerol was used. Theoretical and Experimental Simulation Details: The synthesis of PGLD procedures involves the etherification of glycerol through anionic polymerization of glycidol. The PGLD's were characterized by chromatographic techniques (SEC and HPLC), spectroscopic (FTIR, 1H-NMR and 13C - NMR) electrochemical (zeta potential) and thermal analysis (DSC and TGA) techniques. The structure- activity relationships (SAR's) of compound prototype and its analogs were studied to determine the generation number (G) of the molecule responsible for the biological activity on the adhesion and cell proliferation process. A detailed study of the structure of PGLD's of G=0-4 was performed using the Hyperchem 7. 5 and Gromacs 4 software packages. The biocompatibility studies were studied by scanning electron microscopy (SEM) and fluorescence microscopy (EPF) technique after PGLD (G=0-4) blood contact. The overall electro-negativity/total charge density, dipole moment, frontier orbital's (HOMO - LUMO) and electrostatic potential maps (EPM) were calculated. The most stable form of the resulting compounds was determined by estimating the hydration energy and energy conformation. Results and

Synthesis and characterization of polyaniline–Fe@C magnetic nanocomposite powder

Energy Technology Data Exchange (ETDEWEB)

Fleaca, C.T., E-mail: claudiufleaca@yahoo.com [National Institute for Lasers, Plasma and Radiation Physics (NILPRP), Atomistilor 409, R-077125 Magurele (Romania); “Politehnica” University of Bucharest, Faculty of Applied Sciences, Physics Department, Independentei 313, Bucharest (Romania); Dumitrache, F. [National Institute for Lasers, Plasma and Radiation Physics (NILPRP), Atomistilor 409, R-077125 Magurele (Romania); “Politehnica” University of Bucharest, Faculty of Applied Sciences, Physics Department, Independentei 313, Bucharest (Romania); Morjan, I.; Niculescu, A.-M.; Sandu, I. [National Institute for Lasers, Plasma and Radiation Physics (NILPRP), Atomistilor 409, R-077125 Magurele (Romania); Ilie, A. [National Institute for Lasers, Plasma and Radiation Physics (NILPRP), Atomistilor 409, R-077125 Magurele (Romania); University of Bucharest, Physics Faculty, Atomistilor 405, Magurele (Romania); Stamatin, I.; Iordache, A. [3NanoSAE Research Center, University of Bucharest, Atomistilor 405, Magurele (Romania); Vasile, E. [“Politehnica” University of Bucharest, Faculty of Applied Chemistry and Materials Science, Gh. Polizu. 1-7, Bucharest (Romania); Prodan, G. [“Ovidius” University, Nanotechnology and Alternative Energy Sources Institute, Mamaia 124, Constanta (Romania)

2016-06-30

Highlights: • Carbon-encapsulated Fe–Fe{sub x}C nanoparticles were synthesized by laser pyrolysis. • Fe–C@PANI was obtained by redox polymerization in aqueous acid suspension. • The composite show low coercivity and 6 emu/g saturation magnetization. • Electric and redox behavior of Fe–C@PANI is similar with those of pure PANI. - Abstract: We report the synthesis of novel magnetic nanocomposite based on polyaniline (PANI) matrix and Fe–C nanoparticles. These hydrophobic Fe–Fe{sub x}C@C nanoparticles (having diameters under 20 nm) were synthesized by laser pyrolysis from Fe(CO){sub 5} and C{sub 2}H{sub 4}/H{sub 2} and dispersed in water using sodium carboxymethylcellulose, followed by the PANI coating using ultrasonication-assisted oxidative polymerization of aniline hydrochloride. The structure of the resulted composite was characterized by Transmission Electron Microscopy, X-ray diffraction and also by Raman and Infrared spectroscopy. The composite powder shows ferromagnetic behavior with low coercivity and 6.4 emu/g saturation magnetization, having also electric and electrochemical behavior similar with pure PANI reference.

Synthesis, characterization, and cytotoxicity evaluation of high-magnetization multifunctional nanoclusters

Energy Technology Data Exchange (ETDEWEB)

Petran, Anca; Radu, Teodora; Nan, Alexandrina [National Institute for Research and Development of Isotopic and Molecular Technologies (Romania); Olteanu, Diana; Filip, Adriana, E-mail: adrianafilip33@yahoo.com; Clichici, Simona; Baldea, Ioana [Iuliu Hatieganu University of Medicine and Pharmacy, Department of Physiology (Romania); Suciu, Maria; Turcu, Rodica, E-mail: rodica.turcu@itim-cj.ro [National Institute for Research and Development of Isotopic and Molecular Technologies (Romania)

2017-01-15

The paper presents the synthesis, characterization, and in vitro cytotoxicity tests of Fe{sub 3}O{sub 4} magnetic nanoclusters coated with ethylenediaminetetraacetic acid disodium salt (EDTA). Electron microscopy analysis (SEM) evidences that magnetite nanoparticles are closely packed into the clusters stabilized with EDTA with well-defined near spherical shapes and sizes in the range 100–200 nm. From XRD measurements, we determined the mean size of the crystallites inside the magnetic cluster about 36 nm. The saturation magnetization determined for the magnetic clusters stabilized with EDTA has high value, about 81.7 emu/g at 300 K. X-ray photoelectron spectroscopy has been used to determine both the elemental and chemical structure of the magnetic cluster surface. In vitro studies have shown that the magnetic clusters at low doses did not induce toxicity on human umbilical vein endothelial cells or lesions of the cell membrane. In contrast, at high doses, the magnetic clusters increased the lipid peroxidation and reduced the leakage of a cytoplasmic enzyme, lactate dehydrogenase (LDH), in parallel with increasing the antioxidant defense.

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

Directory of Open Access Journals (Sweden)

Wenyuan Wu

2017-05-01

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

Synthesis, properties, structure and thermochemistry of hexa-aqua-tris (N,N-dimethylformamide) lanthanide tri fluoro methane sulfonates

International Nuclear Information System (INIS)

Araujo Melo, D.M. de.

1989-01-01

Addition compounds between several lanthanide salts and dimethylformamide (DMF) have been described in the literature. This thesis reports the synthesis and characterization of the compounds of general composition Ln (C H 3 SO 3 ) 3 . 3 DMF.6 H 3 O) (Ln = La - Ho) and Ln (C H 3 SO 3 ) 3 DMF.6 H 2 O (Ln = Er - Lu). The structure of the neodymium compound, isomorphous with the series, is also described. The enthalpy variations were determined by solution calorimetry. (author)

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.

Palladium(II)-Stabilized Pyridine-2-Diazotates: Synthesis, Structural Characterization, and Cytotoxicity Studies.

Science.gov (United States)

Tskhovrebov, Alexander G; Vasileva, Anna A; Goddard, Richard; Riedel, Tina; Dyson, Paul J; Mikhaylov, Vladimir N; Serebryanskaya, Tatiyana V; Sorokoumov, Viktor N; Haukka, Matti

2018-02-05

Well-defined diazotates are scarce. Here we report the synthesis of unprecedented homoleptic palladium(II) diazotate complexes. The palladium(II)-mediated nitrosylation of 2-aminopyridines with NaNO 2 results in the formation of metal-stabilized diazotates, which were found to be cytotoxic to human ovarian cancer cells.

Synthesis and characterization of metal soaps of lanthanides (III)

International Nuclear Information System (INIS)

Payolla, Filipe Boccato; Ribeiro, Sidney Jose Lima; Massbni, Antonio Carlos

2015-01-01

The present study describes synthesis and partial characterization of Eu"3"+, Nd"3"+, Dy"3"+, Tb"3"+ and Yb"3"+ behenate complexes. The compounds were analyzed using IR-Spectroscopy, TG-DTG, DSC, elemental analysis, XRD, luminescence and SEM. The results show the purity of the compounds. The XRD analysis and the SEM images show the high crystallinity of the complexes. TG-DTG and DSC analyses do not show a liquid crystal behavior, as occurs with other lanthanide metallic soaps. The mass loses until 1000° C show that the compounds lose ligand fragments at specific temperatures. XRD of the residues are compatible with the respective lanthanide oxides. The luminescence analysis shows that the Eu"3"+, Nd"3"+ and Tb"3"+ complexes presents appreciable emission. The Judd-Ofelt parameters obtained are compatible with the values found in the literature. It was not possible to obtain the complexes in a glass-form because it is difficult to prevent the crystallization of the complexes even using liquid nitrogen. The XDR data indicate that one of the complexes axis has 52 Å of length, agreeing with a structure containing behenate-lanthanide ion-behenate. The structures of the complexes were not fully elucidated and more analyses are necessary. The complexes presented a molar ratio of 3:1 (L:M) and were formulated as Bh_3Eu, Bh_3Nd, Bh_3Dy, Bh_3Tb e Bh_3Yb (Bh = behenate anion). (author)

Mechanical synthesis of copper-carbon nanocomposites: Structural changes, strengthening and thermal stabilization

International Nuclear Information System (INIS)

Nunes, D.; Livramento, V.; Mateus, R.; Correia, J.B.; Alves, L.C.; Vilarigues, M.; Carvalho, P.A.

2011-01-01

Highlights: → The study characterized Cu-nanodiamond (Cu-nD) and Cu-graphite (Cu-G) composites. → Preservation of nD crystalline structure during high-energy milling was demonstrated. → Higher refinement of matrix in Cu-nD comparing to Cu-G is due to a milling mechanism. → Remarkable thermal stability and microhardness have been achieved in Cu-nD and Cu-G. → Strengthening resulted mainly from grain refinement and second-phase reinforcement. - Abstract: Processing of copper-carbon nanocomposites by mechanical synthesis poses specific challenges as carbon phases are prone to amorphization and exhibit an intrinsically difficult bonding with copper. The present work investigates Cu-nanodiamond (Cu-nD) and Cu-graphite (Cu-G) composites produced by mechanical synthesis and subsequent heat treatments. Transmission electron microscopy observations showed homogeneous particle distributions and intimate bonding between the metallic matrix and the carbon phases. Ring diffraction patterns of chemically extracted carbon phases demonstrated that milled nanodiamond preserved crystallinity, while an essentially amorphous nature could be inferred for milled graphite. Raman spectra confirmed that nanodiamond particles remained essentially unaffected by the mechanical synthesis, whereas the bands of milled graphite were significantly changed into the typical amorphous carbon fingerprint. Particle-induced X-ray emission spectroscopy showed that the total contamination originating from the milling media remained below 0.7 wt.%. The Cu-nanodiamond composite exhibited remarkable microhardness and microstructural thermal stability when compared with pure nanostructured copper.

Mechanical synthesis of copper-carbon nanocomposites: Structural changes, strengthening and thermal stabilization

Energy Technology Data Exchange (ETDEWEB)

Nunes, D., E-mail: daniela.nunes@ist.utl.pt [Associacao Euratom/IST, Instituto de Plasmas e Fusao Nuclear - Laboratorio Associado, Instituto Superior Tecnico, Av. Rovisco Pais, 1049-001 Lisboa (Portugal); LNEG, Estrada do Paco do Lumiar, 1649-038 Lisboa (Portugal); ICEMS, Instituto Superior Tecnico, Av. Rovisco Pais, 1049-001 Lisboa (Portugal); Livramento, V. [Associacao Euratom/IST, Instituto de Plasmas e Fusao Nuclear - Laboratorio Associado, Instituto Superior Tecnico, Av. Rovisco Pais, 1049-001 Lisboa (Portugal); LNEG, Estrada do Paco do Lumiar, 1649-038 Lisboa (Portugal); Mateus, R. [Associacao Euratom/IST, Instituto de Plasmas e Fusao Nuclear - Laboratorio Associado, Instituto Superior Tecnico, Av. Rovisco Pais, 1049-001 Lisboa (Portugal); Correia, J.B. [LNEG, Estrada do Paco do Lumiar, 1649-038 Lisboa (Portugal); Alves, L.C. [ITN, Instituto Tecnologico e Nuclear, Estrada Nacional 10, 2686-953 Sacavem (Portugal); Vilarigues, M. [Departamento de Conservacao e Restauro e R and D Unit Vidro e da Ceramica Para as Artes, FCT-UNL, Quinta da Torre, 2829-516 Caparica (Portugal); Carvalho, P.A. [ICEMS, Instituto Superior Tecnico, Av. Rovisco Pais, 1049-001 Lisboa (Portugal); Departamento de Bioengenharia, Instituto Superior Tecnico, Av. Rovisco Pais, 1049-001 Lisboa (Portugal)

2011-11-15

Highlights: {yields} The study characterized Cu-nanodiamond (Cu-nD) and Cu-graphite (Cu-G) composites. {yields} Preservation of nD crystalline structure during high-energy milling was demonstrated. {yields} Higher refinement of matrix in Cu-nD comparing to Cu-G is due to a milling mechanism. {yields} Remarkable thermal stability and microhardness have been achieved in Cu-nD and Cu-G. {yields} Strengthening resulted mainly from grain refinement and second-phase reinforcement. - Abstract: Processing of copper-carbon nanocomposites by mechanical synthesis poses specific challenges as carbon phases are prone to amorphization and exhibit an intrinsically difficult bonding with copper. The present work investigates Cu-nanodiamond (Cu-nD) and Cu-graphite (Cu-G) composites produced by mechanical synthesis and subsequent heat treatments. Transmission electron microscopy observations showed homogeneous particle distributions and intimate bonding between the metallic matrix and the carbon phases. Ring diffraction patterns of chemically extracted carbon phases demonstrated that milled nanodiamond preserved crystallinity, while an essentially amorphous nature could be inferred for milled graphite. Raman spectra confirmed that nanodiamond particles remained essentially unaffected by the mechanical synthesis, whereas the bands of milled graphite were significantly changed into the typical amorphous carbon fingerprint. Particle-induced X-ray emission spectroscopy showed that the total contamination originating from the milling media remained below 0.7 wt.%. The Cu-nanodiamond composite exhibited remarkable microhardness and microstructural thermal stability when compared with pure nanostructured copper.

Synthesis and characterization of carbon nano fibers for its application in the adsorption of toxic gases

International Nuclear Information System (INIS)

Juanico L, J.A.

2004-01-01

The production of carbon nano fibers (CNF's) by diverse techniques as the electric arc, laser ablation, or chemical deposition in vapor phase, among other, they have been so far used from final of the 90's. However, the synthesis method by discharge Glow arc of alternating current and high frequency developed by Pacheco and collaborators, is a once alternative for its obtaining. In the plasma Application Laboratory (LAP) of the National Institute of Nuclear Research (INlN) it was designed and manufactured a reactor of alternating current and high frequency that produces a Glow arc able to synthesize carbon nano fibers. Its were carried out nano fibers synthesis with different catalysts to different proportions and with distinct conditions of vacuum pressure and methane flow until obtaining the best nano fibers samples and for it, this nano structures were characterized by Scanning and Transmission Electron Microscopy, X-ray Diffraction, Raman spectrometry and EDS spectrometry. Once found the optimal conditions for the nano fibers production its were contaminated with NO 2 toxic gas and it was determined if they present adsorption, for it was used the thermal gravimetric analysis technique. This work is divided in three parts, in the first one, conformed by the chapters 1, at the 3, they are considered the foundations of the carbon nano fibers, their history, their characteristics, growth mechanisms, synthesis techniques, the thermal gravimetric analysis principles and the adsorption properties of the nano fibers. In the second part, consistent of the chapters 4 and 5, the methodology of synthesis and characterization of the nano fibers is provided. Finally, in third part its were carried out the activation energy calculation, the adsorption of the CNF's is analyzed and the conclusions are carried out. The present study evaluates the adsorption of environmental gas pollutants as the nitrogen oxides on carbon nano fibers at environmental or near conditions. Also

Synthesis and characterization of anisotropic magnetic hydrogels

Energy Technology Data Exchange (ETDEWEB)

Hinrichs, Stephan, E-mail: stephan.hinrichs@chemie.uni-hamburg.de; Nun, Nils; Fischer, Birgit, E-mail: birgit.fischer@chemie.uni-hamburg.de

2017-06-01

Multiresponsive hydrogels are an interesting new class of materials. They offer the advantage, that they respond to different stimuli like temperature, pH and magnetic fields. By this they can change their properties which makes the hydrogels ideal candidates for many applications in the technical as well as medical field. Here we present the synthesis and characterization of hydrogels - micro- as well as macrogels - which consist of an iron oxide core, varying in phase and morphology, embedded in a thermoresponsive polymer, consisting of poly N-isopropylacrylamide. By using dynamic light scattering we investigated the thermoresponsive properties. In addition we were able to follow the formation of the macrogel by monitoring the shear viscosity.

One-Dimensional SnO2 Nano structures: Synthesis and Applications

International Nuclear Information System (INIS)

Pan, J.; Shen, H.; Mathur, S.; Pan, J.

2012-01-01

Nano scale semiconducting materials such as quantum dots (0-dimensional) and one-dimensional (1D) structures, like nano wires, nano belts, and nano tubes, have gained tremendous attention within the past decade. Among the variety of 1D nano structures, tin oxide (SnO 2 ) semiconducting nano structures are particularly interesting because of their promising applications in optoelectronic and electronic devices due to both good conductivity and transparence in the visible region. This article provides a comprehensive review of the recent research activities that focus on the rational synthesis and unique applications of 1D SnO 2 nano structures and their optical and electrical properties. We begin with the rational design and synthesis of 1D SnO 2 nano structures, such as nano tubes, nano wires, nano belts, and some heterogeneous nano structures, and then highlight a range of applications (e.g., gas sensor, lithium-ion batteries, and nano photonics) associated with them. Finally, the review is concluded with some perspectives with respect to future research on 1D SnO 2 nano structures

Superheavy Element Synthesis and Nuclear Structure

International Nuclear Information System (INIS)

Ackermann, D.

2009-01-01

The search for the next closed proton and neutron shells beyond 2 08P b has yielded a number of exciting results in terms of the synthesis of new elements [1,2,3]. The superheavy elements (SHE), however, are a nuclear structure phenomenon. They owe their existence to the quantum mechanical origin of shell correction energies without which they would not be bound. In recent years the development of efficient experimental set-ups including separators and advanced particle and photon detection arrangements allowed for more and more detailed nuclear structure studies for nuclei at and beyond Z=100. A review of those recent achievements is given in ref. [4]. Among the most interesting features is the observation of K-isomeric states. Experimentally about 14 cases have been identified in the region of Z>96 as shown in Fig. 1. K-isomers or indications of their existence have been found for almost all even-Z elements in the region Z=100 to 110. We could recently establish and/or confirm such states in the even-even isotopes 2 52,254N o [5]. The heaviest nucleus where such a state was found is 2 70D s with Z=110 as we reported in 2001 [6]. Those nuclear structure studies lay out the grounds for a detailed understanding of these heavy and high-Z nuclear systems, and contribute at the same time valuable information to preparation of strategies to successfully continue the hunt for the localisation of the next spherical proton and neutron shells after 2 08P b. The recent activities for both SHE synthesis and nuclear structure investigations at GSI will be reported.(author)

Large area synthesis, characterization, and anisotropic etching of two dimensional tungsten disulfide films

International Nuclear Information System (INIS)

Mutlu, Zafer; Ozkan, Mihrimah; Ozkan, Cengiz S.

2016-01-01

Emergent properties of tungsten disulfide at the quantum confinement limit hold promise for electronic and optoelectronic applications. Here we report on the large area synthesis of atomically thin tungsten disulfide films with strong photoluminescence properties via sulfurization of the pre-deposited tungsten films. Detailed characterization of the pre-deposited tungsten films and tungsten disulfide films are performed using microscopy and spectroscopy methods. By directly heating tungsten disulfide films in air, we have shown that the films tend to be etched into a series of triangular shaped pits with the same orientations, revealing the anisotropic etching behavior of tungsten disulfide edges. Moreover, the dimensions of the triangular pits increase with the number of layers, suggesting a thickness dependent behavior of etching in tungsten disulfide films. This method offers a promising new avenue for engineering the edge structures of tungsten disulfide films. - Highlights: • Large-scale synthesis of WS_2 films is achieved via sulfurization of W films. • Annealing of W films leads to a substantial improvement in the quality of WS_2 films. • WS_2 films show laser power dependent photoluminescence characteristics. • WS_2 films are etched with well-oriented triangular pits upon annealing in air. • Anisotropic oxidative etching is greatly affected by the thickness of WS_2 films.

A novel LaFeO3−XNX oxynitride. Synthesis and characterization

International Nuclear Information System (INIS)

Sierra Gallego, G.; Marín Alzate, N.; Arnache, O.

2013-01-01

Highlights: ► LaFeO 3 perovskite synthesized by auto combustion method. ► LaFeO 3−X N X oxynitride produced by ammonolysis reaction. ► Oxynitride characterized by XRD, Rietveld, SEM, EDX, BET, Raman, TGA and FTIR. ► Partial replacement of oxygen by nitrogen increases slightly the cell parameters. ► TGA shows that oxynitride start to decompose in air above 550 °C. Evolution of N 2 and NO was detected. - Abstract: A perovskite LaFeO 3 was synthesized by auto combustion method and then LaFeO 3−X N X oxynitride was produced by ammonolysis reaction. The synthesized LaFeO 3−X N X oxynitride was characterized by X-ray diffraction (XRD), Rietveld refinement, scanning electron microscopy (SEM), energy dispersive X-ray (EDX), Brunauer–Emmett–Teller (BET) nitrogen adsorption, particle size distribution, Raman spectroscopy, thermogravimetric analysis (TGA) and Fourier transform infrared spectroscopy (FTIR). Nitrogen effect into the perovskite structure was confirmed by DRX. The structure refinement using the Rietveld method indicates that partial replacement of oxygen by nitrogen increases slightly the cell parameters of the LaFeO 3 perovskite. FTIR analysis show that bands at 995 and 1070 cm −1 in the oxynitrides spectra could be assigned to the stretching vibration modes of Fe–N bonds in the FeO 6−X N X octahedral. Thermogravimetric analysis (TGA) showed that LaFeO 3−X N X oxynitride series start to decompose in air above 550 °C. During the decomposition it was found that some amount of nitrogen stays retained in the structure forming intermediate compounds. MS analysis of the gaseous products reveals the evolution of N 2 and NO, suggesting a complex reaction mechanism. To our knowledge, there are no reports on the synthesis and characterization of the LaFeO 3−X N X oxynitrides.

Octalithium plumbate as breeding blanket ceramic: Neutronic performances, synthesis and partial characterization

International Nuclear Information System (INIS)

Colominas, S.; Palermo, I.; Abellà, J.; Gómez-Ros, J.M.; Sanz, J.; Sedano, L.

2012-01-01

Highlights: ► Definition of a suitable configuration for the Li 8 PbO 6 breeding blanket design. ► Demonstration of the feasibility of Li 8 PbO 6 as a breeding material. ► Synthesis optimization in the Li 8 PbO 6 production. ► Characterization of Li 8 PbO 6 by X-ray phase analysis is discussed. - Abstract: A neutronic assessment of the performances of a helium-cooled Li 8 PbO 6 breeding blanket (BB) for the conceptual design of a DEMO fusion reactor is given. Different BB configurations have been considered in order to minimize the amount of beryllium required for neutron multiplication, including the use of graphite as reflector material. The calculated neutronic responses: tritium breeding ratio (TBR), power deposition in TF coils and power amplification factor, indicate the feasibility of Li 8 PbO 6 as breeding material. Furthermore, the synthesis and characterization of Li 8 PbO 6 by X-ray phase analysis are also discussed.

Cu(II AND Zn(II COMPLEX COMPOUNDS WITH BIGUANIDES AROMATIC DERIVATIVES. SYNTHESIS, CHARACTERIZATION, BIOLOGICAL ACTIVITY

Directory of Open Access Journals (Sweden)

Ticuţa Negreanu-Pîrjol

2011-05-01

Full Text Available In this paper we report the synthesis, physical-chemical characterization and antimicrobial activity of some new complex compounds of hetero-aromatic biguanides ligands, chlorhexidine base (CHX and chlorhexidine diacetate (CHXac2 with metallic ions Cu(II and Zn(II, in different molar ratio. The synthesized complexes were characterized by elemental chemical analysis and differential thermal analysis. The stereochemistry of the metallic ions was determined by infrared spectra, UV-Vis, EPR spectroscopy and magnetic susceptibility in the aim to establish the complexes structures. The biological activity of the new complex compounds was identified in solid technique by measuring minimum inhibition diameter of bacterial and fungal culture, against three standard pathogen strains, Escherichia coli ATCC 25922, Staphilococcus aureus ATCC 25923 and Candida albicans ATCC 10231. The results show an increased specific antimicrobial activity for the complexes chlorhexidine:Cu(II 1:1 and 1:2 compared with the one of the Zn(II complexes.

Synthesis and characterization of solvent-free ionic molybdenum disulphide (MoS2) nanofluids

International Nuclear Information System (INIS)

Gu, Shu-Ying; Gao, Xie-Feng; Zhang, Yi-Han

2015-01-01

A development of the novel and stable solvent-free ionic MoS 2 nanofluids by a facile and scalable hydrothermal method is presented. The nanofluids were synthesized by surface functionalizing nanoscale MoS 2 from hydrothermal synthesis with a charged corona, and ionically tethering with oligomeric chains as a canopy. The structures and properties of the nanofluids were characterized by Fourier transform infrared (FTIR), nuclear magnetic resonance (NMR, 1 H), differential scanning calorimeter (DSC), thermogravimetric analysis (TGA) and ARES rheometer. The obtained solvent-free nanofluids are homogeneous, stable amber-like fluids with no evidence of phase separation. The nanofluids could be easily dispersed in both aqueous and organic solvents to form transparent and stable liquids due to the ionic nature and the presence of oligomeric polymer chains. It was found that the solvent-free nanofluids with up to 32 wt% inorganic content show Newtonian rheological behaviors due to the high graft density and uniform dispersion of inorganic cores, indicating that the nanofluids would have a stable lubricating performance. As reported in our previous communication, the nanofluids showing lower, more stable friction coefficients of less than 0.1 with self-healing lubricating behaviors. For deeper understanding of the nanofluids, the details of synthesis, chemical structures, rheological behaviors and molecular dynamics of the nanofluids were investigated in details. The rheological behaviors can be tailored by varying the grafting density of the canopy. Dynamic results of the canopy of the MoS 2 nanofluids show that inorganic MoS 2 cores have hindrance effect on the canopy segmental motions above 253 K due to their effect to the mobility of anions and the departing-recombining motions between the paired cations and anions. - Highlights: • A development of the novel synthesis of solvent-free MoS 2 nanofluids is presented. • The rheological behaviors can be tailored by

Synthesis, Structure, Stability and Redispersion of Gold-based Nanoparticles

Science.gov (United States)

Tiruvalam, Ram Chandra

Nanoscale gold has been shown to possess an intriguing combination of unexpected optical, photochemical and catalytic properties. The ability to control the size, shape, morphology, composition and dispersion of gold-based nanostructures is key to optimizing their performance for nanotechnology applications. The advanced electron microscopy studies described in this thesis analyze three important aspects of gold and gold-palladium alloy nanoparticles: namely, (i) the ability to synthesize gold nanoparticles of controlled size and shape in an aqueous medium; (ii) the colloidal preparation of designer gold-palladium alloys for selective oxidation catalysis; and (iii) the ability to disperse gold as finely and homogeneously as possible on a metal oxide or carbon support. The ability to exploit the nanoscale properties of gold for various engineering applications often depends on our ability to control size and shape of the nanoscale entity by careful manipulation of the synthesis parameters. We have explored an aqueous based synthesis route, using oleylamine as both a reductant and surfactant, for preparing gold nanostructures. By systematically varying synthesis parameters such as oleylamine concentration, reaction temperature, and aging time it is possible to identify processing regimens that generate Au nanostructures having either pseudo-spherical, faceted polyhedral, nanostar or wire shaped morphologies. Furthermore, by quenching the reaction partway through it is possible to create a class of metastable Au-containing structures such as nanocubes, nanoboxes and nanowires. Possible formation mechanisms for these gold based nano-objects are discussed. There is a growing interest in using supported bimetallic AuPd alloy nanoparticles for selective oxidation reactions. In this study, a systematic series of size controlled AuPd bimetallic particles have been prepared by colloidal synthesis methods. Particles having random alloy structures, as well as `designer

Novel metallomesogenic polyurethanes: Synthesis, characterization and properties

International Nuclear Information System (INIS)

Senthilkumar, Natarajan; Narasimhaswamy, Tanneru; Kim, Il-Jin

2012-01-01

A series of tetradentate Schiff base metallomesogenic diols were synthesized from two simple dihydroxy benzenes. The metallomesogenic diol was constructed from three ring containing mesogen linked through ester and azomethine with terminal hydroxy group. This upon complexation with copper(II) formed metallomesogenic diol with varying terminal chain length. A series of metallomesogenic polyurethanes were synthesized using these metallomesogenic diols as chain extenders for the prepolymers based on polytetramethylene glycol (PTMG) of varying molecular weight (M n = 650, 2000) and 2,4-toluene diisocyanate (TDI), or 4,4′-methylene bis(phenyl isocyanate) (MDI). The molar ratio of metallomesogenic diol and PTMG were varied in the polyurethane to find their role in liquid crystalline and mechanical properties. Extensive characterization of all metallomesogenic compounds and intermediates were carried out by FT-IR, 1 H and 13 C NMR, EPR, VSM, Mass (EI and FAB) and UV–visible spectroscopy. Hot stage polarizing microscope and differential scanning calorimetry were used to ensure the phase characteristics such as nature of phase, melting and clearing temperatures and phase range. The appearance of enantiotropic smectic A phases indicated high molecular polarizability of the core due to the metal ion. - Highlights: ► Design and synthesis of metallomesogenic diols. ► Metallomesogenic polyurethanes were prepared using these diols as chain extenders. ► Liquid crystalline and mechanical properties were studied. ► A square pyramidal structure for the copper(II) complexes have been proposed. ► Polyurethanes exhibited enantiotropic smectic A phases.

MWW-type titanosilicate synthesis, structural modification and catalytic applications to green oxidations

CERN Document Server

Wu, Peng; Xu, Le; Liu, Yueming; He, Mingyuan

2013-01-01

This book provides a comprehensive review of a new generation of selective oxidation titanosilicate catalysts with the MWW topology (Ti-MWW) based on the research achievements of the past 12 years. It gives an overview of the synthesis, structure modification and catalytic properties of Ti-MWW. Ti-MWW can readily be prepared by means of direct hydrothermal synthesis with crystallization-supporting agents, using dual-structure-directing agents and a dry-gel conversion technique. It also can be post-synthesized through unique reversible structure transformation and liquid-phase isomorphous subst

Novel acridone-modified MCM-41 type silica: Synthesis, characterization and fluorescence tuning

Directory of Open Access Journals (Sweden)

Maximilian Hemgesberg

2011-06-01

Full Text Available A Mobil Composition of Matter (MCM-41 type mesoporous silica material containing N-propylacridone groups has been successfully prepared by co-condensation of an appropriate organic precursor with tetraethyl orthosilicate (TEOS under alkaline sol–gel conditions. The resulting material was fully characterized by means of X-ray diffraction (XRD, N2-adsorption–desorption, transmission electron microscopy (TEM, IR and UV–vis spectroscopy, as well as 29Si and 13C CP-MAS NMR techniques. The material features a high inner surface area and a highly ordered two-dimensional hexagonal pore structure. The fluorescence properties of the organic chromophore can be tuned via complexation of its carbonyl group with scandium triflate, which makes the material a good candidate for solid state sensors and optics. The successful synthesis of highly ordered MCM materials through co-condensation was found to be dependent on the chemical interaction of the different precursors.

Synthesis and characterization of cobaltite nanotubes for solid-oxide fuel cell cathodes

Energy Technology Data Exchange (ETDEWEB)

Napolitano, F; Baque, L; Troiani, H; Granada, M; Serquis, A, E-mail: aserquis@cab.cnea.gov.a [Instituto Balseiro-Centro Atomico Bariloche and CONICET, San Carlos de Bariloche (Argentina)

2009-05-01

La{sub 1-x}Sr{sub x}Co{sub 1-y}FeyO{sub 3-d}elta oxides are good candidates for solid oxide fuel cell (SOFC) cathodes because these materials present high ionic and electronic conductivity, and compatibility with Cerium Gadolinium Oxide (CGO) electrolytes allowing a lower operation temperature. In this work, we report the synthesis of La{sub 0.4}Sr{sub 0.6}Co{sub 0.8}Fe{sub 0.2}O{sub 3-d}elta (LSCF) nanotubes prepared by a porous polycarbonate membrane approach, obtaining different microstructures depending on sintering conditions. The structure and morphology of the nanotubes and deposited films were characterized by X-ray diffraction, transmission and scanning microscopy. Finally, we obtained nanostructured films of vertically aligned LSCF tubes deposited over the whole surface of CGO pellets with diameter up to 2.5cm in a direct and single step process.

Characterization of the system MoS2 + C, HAADF vs Tem conventional

International Nuclear Information System (INIS)

Reza, C.; Cruz, G.; Santiago, P.; Rendon, L.

2004-01-01

A study is presented about the synthesis and characterization of unidimensional nano systems composed of MoS 2 and C with potential use as solid lubricant. The synthesis process was developed for the mold method, via thermal decomposition, which uses a film of nano porous aluminium oxide. Such systems were characterized by two analysis methods that involve Transmission Electron Microscopy, HRTEM (Conventional TEM) and HAADF (Z Contrast). The results obtained in the structural and morphological characterization were supplemented to determine the structure type obtained in the unidimensional systems. (Author)

Colloidal synthesis and characterization of Bi2S3 nanoparticles for photovoltaic applications

International Nuclear Information System (INIS)

Piras, R; Aresti, M; Saba, M; Marongiu, D; Mula, G; Quochi, F; Mura, A; Bongiovanni, G; Cannas, C; Mureddu, M; Ardu, A; Ennas, G; Musinu, A; Calzia, V; Mattoni, A

2014-01-01

Bismuth sulfide is a promising n-type semiconductor for solar energy conversion. We have explored the colloidal synthesis of Bi 2 S 3 nanocrystals, with the aim of employing them in the fabrication of solution-processable solar cells and to replace toxic heavy metals chalcogenides like PbS or CdS, that are currently employed in such devices. We compare different methods to obtain Bi 2 S 3 colloidal quantum dots, including the use of environmentally benign reactants, through organometallic synthesis. Different sizes and shapes were obtained according to the synthesis parameters and the growth process has been rationalized by comparing the predicted morphology with systematic physical-chemistry characterization of nanocrystals by X-ray diffraction, FT-IR spectroscopy, Transmission Electron Microscopy (TEM)

Sulfaguanidine cocrystals: Synthesis, structural characterization and their antibacterial and hemolytic analysis.

Science.gov (United States)

Abidi, Syed Sibte Asghar; Azim, Yasser; Khan, Shahper Nazeer; Khan, Asad U

2018-02-05

Sulfaguanidine (SG), belongs to the class of sulfonamide drug used as an effective antibiotic. In the present work, using crystal engineering approach two novel cocrystals of SG were synthesized (SG-TBA and SG-PT) with thiobarbutaric acid (TBA) and 1,10-phenanthroline (PT), characterized by solid state techniques viz., powder X-ray diffraction (PXRD), fourier transform infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC) and the crystal structures were determined by single crystal X-ray diffraction studies. A comparative antibacterial activity and hemolytic potential was done on SG drug, coformers and their cocrystals. The tested cocrystals formulations showed almost two fold higher antibacterial activity against the tested strains of bacteria Gram-positive bacteria (S. mutans and E. faecalis) and Gram-negative bacteria (E. coli, K. pneumonia and E. clocae) over SG alone and their coformers. Cocrystal SG-TBA showed better antibacterial activity and reduced hemolysis, thereby, reduced cytotoxicity than SG-PT. Copyright © 2017 Elsevier B.V. All rights reserved.

Synthesis and characterization of polypyrrole and its application for solar cell

Science.gov (United States)

Almuntaser, Faisal M. A.; Majumder, Sutripto; Baviskar, Prashant K.; Sali, Jaydeep V.; Sankapal, B. R.

2017-08-01

In this report, the fabrication of a solar cell device with the structures FTO/PPy/PTh/ZnO/Al was performed using wet chemical synthesis methods in open environment. The cost-effective methods like CBD, SILAR, and spin coating have been used for the synthesis. The effect of thickness of PPy active layer on the device performance is investigated. Features such as structural, morphological, and chemical bonding of the layers have been investigated using X-ray diffraction, field emission scanning electron microscopy, and Fourier transform infrared spectroscopy and are discussed herein. Effects of PPy thickness on current-voltage characteristics have been studied under dark and illumination at 1 Sun (100 mW/cm2, AM 1.5 G) condition to study the solar cell performance.

Synthesis and characterization of M-type barium hexferrite by ultrasonic inter-dispersion of chemical precipitate

International Nuclear Information System (INIS)

Garcia Junior, E.S.; Gomes Junior, G.G.; Ogasawara, T.

2010-01-01

This work is concerned with the study the synthesis and characterization of M-type barium hexaferrite powder by chemical precipitation type and ultrasonic interdispersion of precursor materials Fe(OH) 3 and Ba(OH) 2 ,separately and ultrasonic inter-dispersion, followed by drying and calcining. In order to guide the experimental work was carried out a preliminary thermodynamic analysis of the system Ba-Fe-H 2 O at 25 deg C. The study shows that the phase formation of M-type barium hexaferrite is obtained at a calcination at 1000 deg C, characterized by X-ray diffraction, the grain growth of the final product of synthesis depending on the calcination temperature is visible by SEM. The synthesis method developed in this research is an option to achieve the results that would be obtained if the co-precipitation of ferric and barium hydroxide was thermodynamically possible, where you can get crystallization of barium hexaferrite in a calcination at 1000 deg C. (author)

Carboranyl tetrahydroisoquinolines. Synthesis and the X-ray structural study of 1-(o-Carboran-1-ylmethyl)-1,2,3,4-Tetrahydroisoquinolines

Energy Technology Data Exchange (ETDEWEB)

Lee, Jong Dae; Kang, Sang Ook [Korea University, Dept. of Chemistry, Chung-nam (Korea); Lee, Chai-Ho [Wonkwang Univ., Dept. of Chemistry, Jeonbuk (Korea); Lee, Seung-Hoon [National Cancer Center, Kyungi-do (Korea); Lim, Sang-Moo [Korea Cancer Center Hospital, Seoul (Korea); Cho, Sungil [Seoul City Univ., Dept. of Chemical Engineering, Seoul (Korea)

2001-11-01

Synthesis of the first fully characterized boronated tetrahydroisoquinolines is reported. Thus, tetrahydroisoquinolines containing 1-(0-carboran-1-ylmethyl)-1,2,3,4-tetrahydroisoquinolines have been synthesized from the corresponding arylethylamines to provide carboranes attached to functional group capable of being covalently incorporated into structures of potential use in boron neutron capture therapy (BNCT). The carboranyl functionalities were attached at the 1-position of the tetrahydroisoquinoline molecule. Experimental details and analytical data leading to the identification of the reported compounds are provided. Additionally, the X-ray diffraction structure of 9b is reported. (author)

Synthesis, characterization, and catalytic properties of stable mesoporous molecular sieve MCM-41 prepared from zeolite mordenite

International Nuclear Information System (INIS)

Wang Shan; Dou Tao; Li Yuping; Zhang Ying; Li Xiaofeng; Yan Zichun

2004-01-01

Mesoporous molecular sieves (denoted as M-MCM-41) with ordered hexagonal structure have been successfully synthesized from the assembly of precursors from preformed zeolite Mordenite with CTAB surfactant micelle in alkaline media. The samples were characterized by XRD, N 2 adsorption, IR and DTG. The materials exhibit highly hydrothermal stability, as compared with conventional MCM-41. Characterization results indicate that the mesoporous walls of M-MCM-41 contain the secondary building units similar to those in microporous crystal of zeolite Mordenite. In catalytic dealkylation of C10 + aromatic hydrocarbon, M-MCM-41 shows higher activities in comparison with Mordenite and MCM-41, which would be ascribed to the combination of advantages of both MCM-41 (large pores) and Mordenite (strong acidity). Furthermore, this synthesis strategy could be used as a new general method for the preparation of hydrothermally stable mesoporous aluminosilicate materials under alkaline conditions

Synthesis, structural and surface morphological characterizations of ...

African Journals Online (AJOL)

Sulfated zirconia (SZ) nanoparticles (NPs) were successfully synthesized and deposited via chemical route called sol-gel technique. The structural, morphological, and optical properties the samples were investigated by X-ray diffraction (XRD), Energy Dispersive X-ray Spectrometry (EDX), Scanning Electron Microscopy ...

Transition metal borides. Synthesis, characterization and superconducting properties

International Nuclear Information System (INIS)

Kayhan, Mehmet

2013-01-01

A systematic study was done on the synthesis and superconducting properties of metal rich transition metal borides. Five different binary systems were investigated including the boride systems of niobium, tantalum, molybdenum, tungsten and rhenium. High temperature solid state methods were used in order to synthesize samples of different transition metal borides of the composition M 2 B, MB, M 3 B 2 , MB 2 , and M 2 B 4 . The reactions were carried out in three different furnaces with different sample containers: the electric arc (copper crucible), the high frequency induction furnace (boron nitride, tantalum or glassy carbon crucibles), and the conventional tube furnace (sealed evacuated quartz ampoules). The products obtained were characterized with X-ray powder diffractometry, scanning electron microscopy and energy-dispersive X-ray spectroscopy. Phase analyses and crystal structure refinements using the Rietveld method and based on structure models known from literature were performed. A neutron diffraction measurement was done for W 2 B 4 to allow for a complete crystal structure determination, because of the presence of a heavy element like tungsten and a light element like boron that made it difficult to determine the accurate determination of the boron atom positions and occupancies from X-ray data. A new structure model for W 2 B 4 was proposed. Magnetic measurements in a SQUID magnetometer down to temperatures as low as 1.8 K were performed to several of the products in order to see if the transition metal borides become superconducting at low temperatures, and the results were compared with data from literature. Superconducting properties were found for the following compounds: NbB 2 (T C = 3.5 K), β-MoB (T C = 2.4 K), β-WB (T C = 2.0 K), α-WB (T C = 4.3 K), W 2 B 4 (T C = 5.4 K), Re 7 B 3 (T C = 2.4 K). A relationship between the superconducting properties and the compositional and structural features was discussed for metal diborides. Also it was

Synthesis and characterization of boehmites obtained from gibbsite in presence of different environments

Energy Technology Data Exchange (ETDEWEB)

Denigres Filho, Ricardo Wilson Nastari; Rocha, Gisele de Araujo; Vieira-Coelho, Antonio Carlos, E-mail: acvcoelh@usp.br [Universidade de Sao Paulo (LPSS/EP/USP), SP (Brazil). Departamento de Engenharia Metalurgica e de Materiais. Laboratorio de Materias-Primas Particuladas; Montes, Celia Regina [Centro de Energia Nuclear na Agricultura (NUPEGEL/CENA/USP), Piracicaba, SP (Brazil). Nucleo de Pesquisas Geoquimicas e Geofisicas da Listosfera

2016-05-15

In this study, results related to boehmite synthesis by hydrothermal processes starting from a Bayer commercial gibbsite are reported. The processes have been conducted from aqueous suspensions with initial acidic or alkaline pH, without or with acetate ion, at 160 deg C for 72h to 168h. The final materials were characterized by X-ray diffraction (XRD), thermal methods (DTA and TGA) and scanning electron microscopy (SEM). The influence of the synthesis conditions on the morphology of the boehmite crystals obtained from the gibbsite at different hydrothermal processes are discussed. (author)

Synthesis and Characterization of Mg-doped ZnO Nanorods for Biomedical Applications

Science.gov (United States)

Gemar, H.; Das, N. C.; Wanekaya, A.; Delong, R.; Ghosh, K.

2013-03-01

Nanomaterials research has become a major attraction in the field of advanced materials research in the area of Physics, Chemistry, and Materials Science. Bio-compatible and chemically stable metal nanoparticles have biomedical applications that includes drug delivery, cell and DNA separation, gene cloning, magnetic resonance imaging (MRI). This research is aimed at the fabrication and characterization of Mg-doped ZnO nanorods. Hydrothermal synthesis of undoped ZnO and Mg-doped ZnO nanorods is carried out using aqueous solutions of Zn(NO3)2 .6H2O, MgSO4, and using NH4OH as hydrolytic catalyst. Nanomaterials of different sizes and shapes were synthesized by varying the process parameters such as molarity (0.15M, 0.3M, 0.5M) and pH (8-11) of the precursors, growth temperature (130°C), and annealing time during the hydrothermal Process. Structural, morphological, and optical properties are studied using various techniques such as XRD, SEM, UV-vis and PL spectroscopy. Detailed structural, and optical properties will be discussed in this presentation. This work is partially supported by National Cancer Institute (1 R15 CA139390-01).

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

Science.gov (United States)

Song, Shaokun; Huang, Qiwei; Zhu, Wanting

2017-10-01

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

Marine Nucleosides: Structure, Bioactivity, Synthesis and Biosynthesis

Directory of Open Access Journals (Sweden)

Ri-Ming Huang

2014-12-01

Full Text Available Nucleosides are glycosylamines that structurally form part of nucleotide molecules, the building block of DNA and RNA. Both nucleosides and nucleotides are vital components of all living cells and involved in several key biological processes. Some of these nucleosides have been obtained from a variety of marine resources. Because of the biological importance of these compounds, this review covers 68 marine originated nucleosides and their synthetic analogs published up to June 2014. The review will focus on the structures, bioactivities, synthesis and biosynthetic processes of these compounds.

Synthesis and characterization of carbon fibers obtained through plasma techniques

International Nuclear Information System (INIS)

Valdivia B, M.

2005-01-01

The study of carbon, particularly the nano technology is a recent field, the one which has important implications in the science of new materials. It investigation is of great interest for industries producers of ceramic, metallurgy, electronic, energy storage, biomedicine, among others. The diverse application fields are a reason at national as international level, so that many works are focused in the production of nano fibers of carbon. The Thermal plasma applications laboratory (LAPT) of the National Institute of Nuclear Research (ININ), it is carrying out works about carbon nano technology. The present work has as purpose to carry out the synthesis and characterization of the carbon nano fibers which are obtained by electric arch of alternating current (CA) to high frequencies and by a plasma gun of non transferred arch, where are used hydrocarbons like benzene, methane, acetylene like carbon source and ferrocene, nickel, yttrium and cerium oxide like catalysts. For both techniques its were thought about a relationship among hydrocarbon-catalyst that it favored to the nano fibers production. The obtained product of each experiment outlined it was analyzed by transmission electron microscopy (TEM), scanning electron microscopy (SEM) and X-ray diffraction (XRD), analysis with those were obtained pictures and diffraction graphs, which were observed to arrive to one conclusion on the operation conditions, same analysis with those were characterized the tests carried out according to the nano structures formation of carbon. (Author)

Low-temperature synthesis and characterization of anatase TiO2 nanoparticles by an acid assisted sol–gel method

International Nuclear Information System (INIS)

Leyva-Porras, C.; Toxqui-Teran, A.; Vega-Becerra, O.; Miki-Yoshida, M.; Rojas-Villalobos, M.; García-Guaderrama, M.

2015-01-01

The synthesis of anatase TiO 2 nanoparticles by an acid-assisted sol–gel method at 25 and 80 °C is described. Specifically, acetic acid (AA) was used and the evolution of the anatase phase with the amount of AA was observed. The results of X-ray diffraction (XRD) and transmission electron microscopy (TEM) both showed that a pure anatase phase was obtained with particle size smaller than 5 nm. Structural refinements and quantitative determination of phase composition was achieved by using the Rietveld method. The particle size distribution became slightly narrower as the amount of AA was increased. Raman spectroscopy showed that when the amount of AA was increased a small amount of brookite was present at the contamination level. The anatase phase was studied by differential thermal analysis (DTA), providing phase stability up to 600 °C. These and other results were discussed in terms of particle size and structure. Likewise, the formation of the anatase phase under these synthesis conditions was explained. - Highlights: • Synthesis of anatase TiO 2 nanoparticles by an acid assisted sol–gel method at mild conditions. • Microstructure characterization by XRD, TEM and Raman spectroscopy. • Observation of the formation and evolution of the anatase phase as acetic acid was increased. • Anatase thermal stability up to 600 °C and band gap range between 3.2 and 3.5 eV. • A simplified method which can be considered as a green chemistry process

Synthesis, characterization and crystal structure of [Cu2(LH2]•(ClO42. Influence of the weak Cu•••O(perchlorate interaction on the structure of Cu2N2O2 metallocycle

Directory of Open Access Journals (Sweden)

Mirković Marija

2014-01-01

Full Text Available The diimine-dioxime ligand, 4,9-diaza-3,10-diethyl-3,9-dodecadiene-2,11-dione bisoxime (LH2, containing a N4 donor set was prepared by Schiff base condensation of 2-hydroxyimino-3-pentanone and 1,4-diaminobutane in two ways: in protic and in aprotic solvent. Higher yield of (LH2 imine was obtained when the synthesis was carried out using protic solvent (C2H5OH instead of aprotic benzene (78% and 30%, respectively. Cu(II metal complex of diimine-dioxime was synthesized in CH3OH from metal salt and LH2 in mole ratio 1:1. The isolated complex was characterized by the elemental analysis, IR spectroscopy and cyclic voltammetry. The structure of [Cu2(LH2]•(ClO42 was determined by the single-crystal X-ray diffraction analysis. Comparison with the structurally related diimine-dioxime Cu(II complexes revealed the influence of the weak Cu•••O(perchlorate interaction on the geometry of the metallocycle. [Projekat Ministarstva nauke Republike Srbije, br. 45015, br. 172013, br. 172065 i br. 172014

Synthesis and characterization of NiO nanoparticles by thermal decomposition of nickel linoleate and their optical properties

Energy Technology Data Exchange (ETDEWEB)

Kalam, Abul, E-mail: abul_k33@yahoo.com [Department of Chemistry, Faculty of Science, King Khalid University, Abha 61413, P.O. Box 9004 (Saudi Arabia); Al-Sehemi, Abdullah G.; Al-Shihri, Ayed S. [Department of Chemistry, Faculty of Science, King Khalid University, Abha 61413, P.O. Box 9004 (Saudi Arabia); Du Gaohui [Zhejiang Key Laboratory for Reactive Chemistry on Solid Surfaces, Institute of Physical Chemistry, Zhejiang Normal University, Jinhua 321004 (China); Ahmad, Tokeer [Nanochemistry Laboratory, Department of Chemistry, Jamia Millia Islamia, New Delhi 110025 (India)

2012-06-15

Well dispersed nickel oxide nanoparticles have been synthesized successfully by direct calcination of nickel linoleate. The structure, morphology and properties of the nanoparticles were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, high-resolution transmission electron microscopy and ultraviolet-visible spectroscopy. Transmission electron microscopic studies show that nickel oxide nanoparticles are uniform with an average size of 14-20 nm. The optical band gap of 3.8 eV is obtained using UV-Visible spectroscopy which exhibits the red shift compared with the bulk counterpart. - Highlights: Black-Right-Pointing-Pointer Synthesis of metal oxide nanoparticles by using metal complexes as precursors. Black-Right-Pointing-Pointer Characterization of isolated nanoparticles using XRD, FTIR, SEM, TEM and HRTEM data. Black-Right-Pointing-Pointer The expected optical properties of these nanoparticles are clarified.

Subsurface synthesis and characterization of Ag nanoparticles embedded in MgO

Science.gov (United States)

Vilayurganapathy, S.; Devaraj, A.; Colby, R.; Pandey, A.; Varga, T.; Shutthanandan, V.; Manandhar, S.; El-Khoury, P. Z.; Kayani, Asghar; Hess, W. P.; Thevuthasan, S.

2013-03-01

Metal nanoparticles exhibit a localized surface plasmon resonance (LSPR) which is very sensitive to the size and shape of the nanoparticle and the surrounding dielectric medium. The coupling between the electromagnetic radiation and the localized surface plasmon in metallic nanoparticles results in a sizable enhancement of the incident fields, making them possible candidates for plasmonic applications. In particular, partially exposed metallic nanoparticles distributed in a dielectric matrix can provide prime locations for LSPR spectroscopy and sensing. We report the synthesis and characterization of a plasmonic substrate consisting of Ag nanoparticles partially buried in MgO. Ag nanoparticles of different shapes and size distributions were synthesized below the surface of MgO by implanting 200 keV Ag+ ions followed by annealing at 1000 °C for 10 and 30 h. A detailed optical and structural characterization was carried out to understand the evolution of the Ag nanoparticle and size distribution inside the MgO matrix. Micro x-ray diffraction (Micro-XRD) was employed to investigate the structural properties and estimate the crystallite size. The nanoparticles evolved from a spherical to a faceted morphology with annealing time, assuming an octahedral shape truncated at the (001) planes, as visualized from aberration-corrected transmission electron microscopy (TEM) images. The nanoparticles embedded in MgO were shown to be pure metallic Ag using atom probe tomography (APT). The nanoparticles were partially exposed to the surface by employing plasma etch techniques to remove the overlaying MgO. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) were employed to study the surface morphology and obtain a height distribution for the partially exposed nanoparticles.

Subsurface synthesis and characterization of Ag nanoparticles embedded in MgO

International Nuclear Information System (INIS)

Vilayurganapathy, S; Devaraj, A; Colby, R; Pandey, A; Varga, T; Shutthanandan, V; Manandhar, S; Thevuthasan, S; El-Khoury, P Z; Hess, W P; Kayani, Asghar

2013-01-01

Metal nanoparticles exhibit a localized surface plasmon resonance (LSPR) which is very sensitive to the size and shape of the nanoparticle and the surrounding dielectric medium. The coupling between the electromagnetic radiation and the localized surface plasmon in metallic nanoparticles results in a sizable enhancement of the incident fields, making them possible candidates for plasmonic applications. In particular, partially exposed metallic nanoparticles distributed in a dielectric matrix can provide prime locations for LSPR spectroscopy and sensing. We report the synthesis and characterization of a plasmonic substrate consisting of Ag nanoparticles partially buried in MgO. Ag nanoparticles of different shapes and size distributions were synthesized below the surface of MgO by implanting 200 keV Ag + ions followed by annealing at 1000 °C for 10 and 30 h. A detailed optical and structural characterization was carried out to understand the evolution of the Ag nanoparticle and size distribution inside the MgO matrix. Micro x-ray diffraction (Micro-XRD) was employed to investigate the structural properties and estimate the crystallite size. The nanoparticles evolved from a spherical to a faceted morphology with annealing time, assuming an octahedral shape truncated at the (001) planes, as visualized from aberration-corrected transmission electron microscopy (TEM) images. The nanoparticles embedded in MgO were shown to be pure metallic Ag using atom probe tomography (APT). The nanoparticles were partially exposed to the surface by employing plasma etch techniques to remove the overlaying MgO. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) were employed to study the surface morphology and obtain a height distribution for the partially exposed nanoparticles. (paper)

Localized synthesis, assembly and integration of silicon nanowires

Science.gov (United States)

Englander, Ongi

Localized synthesis, assembly and integration of one-dimensional silicon nanowires with MEMS structures is demonstrated and characterized in terms of local synthesis processes, electric-field assisted self-assembly, and a proof-of-concept nanoelectromechanical system (HEMS) demonstration. Emphasis is placed on the ease of integration, process control strategies, characterization techniques and the pursuit of integrated devices. A top-down followed by a bottom-up integration approach is utilized. Simple MEMS heater structures are utilized as the microscale platforms for the localized, bottom-up synthesis of one-dimensional nanostructures. Localized heating confines the high temperature region permitting only localized nanostructure synthesis and allowing the surroundings to remain at room temperature thus enabling CMOS compatible post-processing. The vapor-liquid-solid (VLS) process in the presence of a catalytic nanoparticle, a vapor phase reactant, and a specific temperature environment is successfully employed locally. Experimentally, a 5nm thick gold-palladium layer is used as the catalyst while silane is the vapor phase reactant. The current-voltage behavior of the MEMS structures can be correlated to the approximate temperature range required for the VLS reaction to take place. Silicon nanowires averaging 45nm in diameter and up to 29mum in length synthesized at growth rates of up to 1.5mum/min result. By placing two MEMS structures in close proximity, 4--10mum apart, localized silicon nanowire growth can be used to link together MEMS structures to yield a two-terminal, self-assembled micro-to-nano system. Here, one MEMS structure is designated as the hot growth structure while a nearby structure is designated as the cold secondary structure, whose role is to provide a natural stopping point for the VLS reaction. The application of a localized electric-field, 5 to 13V/mum in strength, during the synthesis process, has been shown to improve nanowire

Synthesis and characterization of covalent diphenylalanine nanotube-folic acid conjugates

DEFF Research Database (Denmark)

León, John Jairo Castillo; Rindzevicius, Tomas; Wu, Kaiyu

2014-01-01

Herein, we describe the synthesis and characterization of a covalent nanoscale assembly formed between diphenylalanine micro/nanotubes (PNT) and folic acid (FA). The conjugate was obtained via chemical functionalization through coupling of amine groups of PNTs and carboxylic groups of FA. The sur...... for applications in the detection and diagnosis of cancer or tropical diseases such as leishmaniasis and as a carrier nanosystem delivering drugs to malignant tumors that overexpress folate receptors....

Synthesis of lever-blade dampers with enhanced mechanical structure

Directory of Open Access Journals (Sweden)

Igor I. Sydorenko

2015-03-01

Full Text Available Since the torsion bar represents just an elastic element, the energy dissipation in suspensions problem is highly relevant for its application. Currently in quality of a dissipation device in torsion suspension are used the hydraulic dampers with movable members reciprocating translational motion respectively to the housing or lever-type hydraulic shock absorbers of piston and vane types, with the movable member’s rotational movement respectively to the housing. These dampers are implementing only throttle-valve performance type, associated with these devices’ functional capacities and depending on design constraints. The paper presents a synthesis of innovative lever-blade dampers, whose performance is not related to the value of working chambers inner pressure. Their essential peculiarity relates to the mechanical control loop presence in the structure that determines a close relationship between the performance and the value of the shock absorber movable element displacement relatively to the body. In the process of synthesis carried out tested are the appropriate methods, built on the basis of technical systems’ modeling with modified kinematic graphs. The synthesis results are shown in the form of two structurally implemented samples. Performed is a comparative analysis of the samples with their basic performance determining.

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

International Nuclear Information System (INIS)

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

2009-01-01

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

Synthesis and characterization of hydroxyapatite crystals: a review study on the analytical methods

NARCIS (Netherlands)

Koutsopoulos, S.

2002-01-01

For the synthesis of hydroxyapatite crystals from aqueous solutions three preparation methods were employed. From the experimental processes and the characterization of the crystals it was concluded that aging and precipitation kinetics are critical for the purity of the product and its

Synthesis, characterization and applications of graphene architectures

Science.gov (United States)

Thomas, Abhay Varghese

Graphene, a two--dimensional sheet of sp2 hybridized carbon atoms arranged in a honeycomb lattice structure, has garnered tremendous interest from the scientific community for its unique combination of properties. It has interesting electrical, thermal, optical and mechanical properties that scientists and engineers are trying to understand and harness to improve current products as well as focus on disruptive technologies that can be made possible by this next generation material. In this thesis the synthesis, characterization and applications of various graphene architectures were explored from the context of a bottom--up and top--down synthesis approach. The work is divided into three main chapters and each one deals with a unique architecture of graphene as well as its properties and an application to a real world problem. In Chapter 2, we focus on bottom--up synthesis of graphene sheets by chemical vapor deposition. We then studied the wetting properties of graphene coated surfaces. More specifically the wetting properties of single and multilayer graphene films on flat and nanoscale rough surfaces are explored and the insights gained are used in improving heat transfer performance of copper surfaces. Single layer graphene, on certain flat surfaces, was shown to exhibit `wetting transparency' as a result of its sheer thinness and this property is of interest in various wetting related applications. Surface protection from corrosion and/or oxidation without change in wetting properties is tremendously useful in multiple fields and we looked to apply this property to dehumidification of copper surfaces. The short time scales results demonstrated that graphene indeed served to prevent oxidation of the surface which in turn promoted increased heat transfer co--efficients with respect to the oxidized copper surfaces. Closer inspection of the surface over long time scales however revealed that the oxide layer changed the wetting properties and this was detrimental

Synthesis, fabrication and characterization of magnetic and dielectric nanoparticles and nanocomposite films

Science.gov (United States)

Liu, Xiaohua

Materials science is an interdisciplinary field investigating the structure-property relationship in solid-state materials scientifically and technologically. Nanoscience is concerned with the distinctive properties that matter exhibits when confined to physical dimensions on the order of 10-9 meters. At these length scales, behaviors of particles or elaborate structures are often governed by the rules of quantum mechanics in addition to the physical properties associated with the bulk material. The work reported here seeks to employ nanocystals, binary nanocomposites and thin films of materials, to build versatile, functional systems and devices. With a focus on dielectric, ferroelectric, and magnetoelectric performance, a series of materials has been synthesized and different types of nanocomposites have been built. Barium strontium titannate particles at various sizes was developed, aiming at high dielectric constant and low loss at high frequency range. Cobalt ferrite-polymer nanocomposite was fabricated with potential magnetoelectric coupling. Along with synthesis, advanced electron microscopies (TEM, SEM, STEM, EELS) at atomic resolution were employed to thoroughly investigate the crystallinity, morphology and composition. By means of spin-coating and printing techniques, single and multiple layered capacitors featuring improved dielectric performance (high k, low loss, high breakdown voltage, etc.) were developed through a) electrode deposition, b) dielectric layer deposition, and c) parylene evaporation. Such capacitors are further incorporated into electric power converters for LED lighting. Hopefully in the future we can make electronic devices more efficient, sustainable, smaller and cheaper. By advancing our knowledge of nanomaterials, especially those with potential of multifunction, energy efficiency and sustainability, we have strived to push the limits of synthesis, characterization, fabrication and property analysis of nanostructures towards new

Synthesis, Structural Characterization and Catalytic Activity of A Cu(II Coordination Polymer Constructed from 1,4-Phenylenediacetic Acid and 2,2’-Bipyridine

Directory of Open Access Journals (Sweden)

Wang Li-Hua

2017-04-01

Full Text Available In order to study the catalytic activity of Cu(II coordination polymer material, a novel 1D chained Cu(II coordination polymer material, [CuL(bipy(H2O5]n (A1 (H2L = 1,4-phenylenediacetic acid, bipy = 2,2’-bipyridine, has been prepared by the reaction of 1,4-phenylenediacetic acid, 2,2’-bipyridine, Cu(CH3COO2·H2O and NaOH. The composition of A1 was determined by elemental analysis, IR spectra and single crystal X-ray diffraction. The results of characterization show that each Cu(II atom adopts six-coordination and forms a distorted octahedral configuration. The catalytic activity and reusability of A1 catalyst for A3 coupling reaction of benzaldehyde, piperidine, and phenylacetylene have been investigated. And the results show that the Cu(II complex catalyst has good catalytic activity with a maximum yield of 54.3% and stability. Copyright © 2017 BCREC GROUP. All rights reserved Received: 21st October 2016; Revised: 17th November 2016; Accepted: 22nd November 2016 How to Cite: Li-Hua, W., Lei, L., Xin, W. (2017. Synthesis, Structural Characterization and Catalytic Activity of A Cu(II Coordination Polymer Constructed from 1,4-Phenylenediacetic Acid and 2,2’-Bipyridine. Bulletin of Chemical Reaction Engineering & Catalysis, 12 (1: 113-118 (doi:10.9767/bcrec.12.1.735.113-118 Permalink/DOI: http://dx.doi.org/10.9767/bcrec.12.1.735.113-118

Synthesis and structural characterization of carboxyethylpyrrole-modified proteins: mediators of age-related macular degeneration.

Science.gov (United States)

Lu, Liang; Gu, Xiaorong; Hong, Li; Laird, James; Jaffe, Keeve; Choi, Jaewoo; Crabb, John; Salomon, Robert G

2009-11-01

Protein modifications in which the epsilon-amino group of lysyl residues is incorporated into a 2-(omega-carboxyethyl)pyrrole (CEP) are mediators of age-related macular degeneration (AMD). They promote both angiogenesis into the retina ('wet AMD') and geographic retinal atrophy ('dry AMD'). Blood levels of CEPs are biomarkers for clinical prognosis of the disease. To enable mechanistic studies of their role in promoting AMD, for example, through the activation of B- and T-cells, interaction with receptors, or binding with complement proteins, we developed an efficient synthesis of CEP derivatives, that is especially effective for proteins. The structures of tryptic peptides derived from CEP-modified proteins were also determined. A key finding is that 4,7-dioxoheptanoic acid 9-fluorenylmethyl ester reacts with primary amines to provide 9-fluorenylmethyl esters of CEP-modified proteins that can be deprotected in situ with 1,8-diazabicyclo[5.4.0]undec-7-ene without causing protein denaturation. The introduction of multiple CEP-modifications with a wide variety of CEP:protein ratios is readily achieved using this strategy.

High temperature bismuth cuprate superconductors synthesis and characterization

International Nuclear Information System (INIS)

Mansori, M.; Satre, P.; Breandon, C.; Roubin, M.; Sebaoun, A.

1993-01-01

High temperature superconductor phases synthesis by coprecipitation in alkaline solution is reported. (Bi 1.6 Pb 0.4 )Sr 2 Ca 1 Cu 2 O 8+x and (Bi 1.6 Pb 0.4 )Sr 2 Ca 2 Cu 3 O 10+y noted (2212) and (2223) have been prepared and studied. From aqueous nitrate solutions of Bi, Pb, Sr, Ca and Cu and oxalic acid aqueous solution as well as ethylene glycol, using an organic base (the triethylamine), the pH was increased up to the path of the precipitation zone (pH = 10.5-11.2). This method assures a good granulometric homogeneity of powders. Thermal analysis and characterization of the different components produced during the synthesis have been studied by DTA (differential thermal analysis)- TGA (thermogravimetric analysis), X-ray diffraction at different temperatures and by Infrared spectroscopy with a Fourier transformation. The measurements of magnetic susceptibility for the 2212 (with and without lead) and 2223 (with lead) phases have permitted us to observe the critical temperatures of 84 K, 87 K and 114 K. (author). 29 refs., 2 figs., 4 tabs

Synthesis, structural characterization and selectively catalytic properties of metal-organic frameworks with nano-sized channels: A modular design strategy

International Nuclear Information System (INIS)

Qiu Lingguang; Gu Lina; Hu Gang; Zhang Lide

2009-01-01

Modular design method for designing and synthesizing microporous metal-organic frameworks (MOFs) with selective catalytical activity was described. MOFs with both nano-sized channels and potential catalytic activities could be obtained through self-assembly of a framework unit and a catalyst unit. By selecting hexaaquo metal complexes and the ligand BTC (BTC=1,3,5-benzenetricarboxylate) as framework-building blocks and using the metal complex [M(phen) 2 (H 2 O) 2 ] 2+ (phen=1,10-phenanthroline) as a catalyst unit, a series of supramolecular MOFs 1-7 with three-dimensional nano-sized channels, i.e. [M 1 (H 2 O) 6 ].[M 2 (phen) 2 (H 2 O) 2 ] 2 .2(BTC).xH 2 O (M 1 , M 2 =Co(II), Ni(II), Cu(II), Zn(II), or Mn(II), phen=1,10-phenanthroline, BTC=1,3,5-benzenetricarboxylate, x=22-24), were synthesized through self-assembly, and their structures were characterized by IR, elemental analysis, and single-crystal X-ray diffraction. These supramolecular microporous MOFs showed significant size and shape selectivity in the catalyzed oxidation of phenols, which is due to catalytic reactions taking place in the channels of the framework. Design strategy, synthesis, and self-assembly mechanism for the construction of these porous MOFs were discussed. - Grapical abstract: A modular design strategy has been developed to synthesize microporous metal-organic frameworks with potential catalytic activity by self-assembly of the framework-building blocks and the catalyst unit

Synthesis, Structural Characterization, Antimicrobial Activity, and In Vitro Biocompatibility of New Unsaturated Carboxylate Complexes with 2,2′-Bipyridine

Directory of Open Access Journals (Sweden)

Gina Vasile Scăețeanu

2018-01-01

Full Text Available The synthesis, structural characterization, cytotoxicity, and antimicrobial properties of four new complexes formed by employing acrylate anion and 2,2′-bipyridine are reported herein. X-ray crystallography revealed the trinuclear nature of [Mn3(2,2′-bipy2(C3H3O26] (1, meanwhile complexes with general formula [M(2,2′-bipy(C3H3O22(H2Ox]∙yH2O ((2 M: Ni, x = 1, y = 0; (3 M: Cu, x = 1, y = 0; (4 M: Zn, x = 0, y = 1; 2,2′-bipy: 2,2′-bipyridine; C3H3O2: acrylate anion were shown to be mononuclear. The lowest minimum inhibitory concentration (MIC of 128 μg mL−1 was recorded for all four tested complexes against Candida albicans, for complex (3 against Escherichia coli, and for complex (4 against Staphylocococcus aureus. Compounds (3 and (4 were also potent efflux pumps activity inhibitors (EPI, proving their potential for use in synergistic combinations with antibiotics. Complexes (1–(4 revealed that they were not cytotoxic to HCT-8 cells. They also proved to interfere with the cellular cycle of tumour HCT-8 cells by increasing the number of cells found in the S and G2/M phases. Taken together, these results demonstrate the potential of zinc and copper complexes for use in the development of novel antimicrobial and anti-proliferative agents.

Synthesis, structural characterization, and catalytic properties of tungsten-exchanged H-ZSM5

International Nuclear Information System (INIS)

Ding, Weiping; Meitzner, George D.; Marler, David O.; Iglesia, Enrique

2001-01-01

W-exchanged H-ZSM5 was prepared by sublimation of WCl6 at 673 K followed by hydrolysis of exchanged WClx species at 523 K. D2 exchange with residual OH groups showed that each W initially replaced about two zeolitic protons for W/Al ratios of 0.29 and 0.44, consistent with the formation of (WO2)2+ containing W6+ species bridging two cation exchange sites. As temperatures reached973 K during D2-OH exchange, these species reduced to (WO2)+ with the concurrent formation of one OD group. CH4 conversion turnover rates (per W) and C2-C1 2 selectivities are very similar to those observed on a Mo/H-ZSM5 sample with similar cation exchange level. As in the case of Mo/H-ZSM5, WOx/H-ZSM5 precursors are initially inactive in CH4 reactions, but they activate during induction with the concurrent evolution of CO, H2O, and an excess amount of H2. The reduction and carburization processes occurring during CH4 reactions and the structure of the exchanged WOx precursors was probed using in situ X-ray absorption spectroscopy (XAS). XAS studies confirmed the isolated initial nature of the exchanged WOx precursors after hydrolysis and dehydration and the formation of WCx clusters 0.6 nm in diameter during CH4 reactions at 973 K. The structural and catalytic resemblance between W- and Mo-exchanged H-ZSM5 is not unexpected, in view of chemical similarities between oxides or carbides of Mo and W. The synthesis of exchanged WOx precursors and their subsequent carburization during CH4 reactions, however, are more difficult than the corresponding processes for the MoOx counterparts. This may account for previous reports of lower CH4 reaction rates and aromatics selectivities on W/H-ZSM5 compared with those observed on Mo/H-ZSM5 and with those reported here for rigorously exchanged W/H-ZSM5

Synthesis and characterization of fluorine compounds

International Nuclear Information System (INIS)

Martinez Carrillo, M.

1991-01-01

The ( 18 F) D-glucose, 2-deoxy fluorine ( 18 FDG) is a radio pharmaceutic that is used in nuclear medicine it is utilized mainly in the glucose metabolism. It allows recently to observe the tumors accumulation and growing. The obtention of this radio pharmaceutic can realize by a nucleophilic or electrophilic process through the use of different fluorinated agents obtained as intermediates for introducing the 18 F radionuclide in a final step of synthesis. The first methods already has been studied in the National Institute of Nuclear Research. The second one which is based this work and it was realized through the reaction of acetyl hypo fluorite (CH 3 COOF) with tri acetyl glucal (TAG) in turn they require the obtention of several fluorated compounds that they serve as intermediates for their obtention so that objective of this work was to find the adequate technique for the obtention of anhydride hydrofluoric acid (HF), KF.2 HF and elemental fluorine so as the design and construction of the systems and equipment used for carry out each one of the reactions. Moreover it was designed the system that will be used for the obtention of acetyl hypo fluoride and the synthesis of composite tetraacetilide 3,4,6 tri-D-glucopyranosil fluoride (TAG-F) for that finally by hydrolysis it was obtained the 2-deoxy fluoride-D-glucose (TAG) in inactive. In this system were realized several preliminary tests. The results are showed in the content of this work also the techniques for compounds characterization were given. (Author)

Synthesis characterization, and properties of rubber lattices; a review

International Nuclear Information System (INIS)

Khan, S.M.; Chughtai, A.; Sattar, A.

2008-01-01

Latex is a stable dispersion of polymeric material in an aqueous medium. Lattices are present in natural as well as in synthetic forms. The range of applications of latex is extensive in carpet underlay, fabric back-coating, paper and paints coatings, adhesive, binder, leather finish, floor polish, waterproof clothing, bounded fiber, pigment printing, latex thread, cement and asphalt, foam scraps binders, can closure, thickeners, box toes and shoes counters, sealant and mastics, modifiers, protein reduction, enzyme treatment and peroxide vulcanization. In this review we are presenting synthesis, characterization, properties, manufacturing and processing of latex. (author)

Synthesis and Characterization of Biscoumarin and Benzopyrano Dicoumarin Derivatives

International Nuclear Information System (INIS)

Nik Khairunissa' Nik Abdullah Zawawi; Muhammad Taha; Norizan Ahmat; Nor Hadiani Ismail; Nik Khairunissa' Nik Abdullah Zawawi; Muhammad Taha; Norizan Ahmat; Nor Hadiani Ismail

2016-01-01

The wide-ranging biological activities of 4-hydroxycoumarin have stimulated considerable interest in this class of compounds, and various biscoumarin derivatives have been synthesized. Recently, a number of methods have been reported for the synthesis of biscoumarin by the reaction of 4-hydroxycoumarin and various aldehydes in the presence of catalysts. In the present study, a new series of biscoumarin and benzopyrano dicoumarin were synthesized and physically characterized by nuclear magnetic resonane ( 1 H and 13 C NMR), fourier transform infrared spectroscopy (FTIR), mass spectrometry (MS) and melting point. (author)

Synthesis and crystal structure of the quaternary compound AgFe{sub 2}GaTe{sub 4}

Energy Technology Data Exchange (ETDEWEB)

Delgado, Gerzon E., E-mail: gerzon@ula.ve [Laboratorio de Cristalografía, Departamento de Química, Facultad de Ciencias, Universidad de Los Andes, Mérida 5101 (Venezuela, Bolivarian Republic of); Quintero, Eugenio; Tovar, Rafael; Grima-Gallardo, Pedro; Quintero, Miguel [Centro de Estudio de Semiconductores, Departamento de Física, Facultad de Ciencias, Universidad de Los Andes, Mérida 5101 (Venezuela, Bolivarian Republic of)

2014-11-15

Highlights: • New quaternary compound. • Synthesis from solid state reaction. • Crystal structure. • Rietveld refinement. - Abstract: The crystal structure of the quaternary compound AgFe{sub 2}GaTe{sub 4}, belonging to the system I–II{sub 2}–III–VI{sub 4}, was characterized by Rietveld refinement using X-ray powder diffraction data. The powder pattern was composed by 84.5% of the principal phase AgFe{sub 2}GaTe{sub 4} and 15.5% of the secondary phase FeTe. This material crystallizes with stannite structure in the tetragonal space group I-42m (N° 121), Z = 2, unit cell parameters a = 6.3409(2) Å, c = 12.0233(4) Å, V = 483.42(3) Å{sup 3}, and is isostructural with CuFe{sub 2}InSe{sub 4}.

Synthesis, characterization and crystal structure of a ...

African Journals Online (AJOL)

The Mo atom in the complex is in octahedral coordination. Thermal stability of the complex has also been studied. KEY WORDS: Molybdenum complex, Hydrazone ligand, Crystal structure, X-ray diffraction, Thermal property. Bull. Chem. Soc. Ethiop. 2014, 28(3), 409-414. DOI: http://dx.doi.org/10.4314/bcse.v28i3.10 ...

Technetium cyanide chemistry: synthesis and characterization of technetium(III) and -(V) cyanide complexes

International Nuclear Information System (INIS)

Trop, H.S.; Jones, A.G.; Davison, A.

1980-01-01

Several new technetium cyanide complexes have been prepared and characterized. The reaction of ammonium hexaiodotechnetate(IV) with potassium cyanide in refluxing aqueous methanol under nitrogen yields potassium heptacyanotechnetate(III) dihydrate, K 4 Tc(CN) 7 .2H 2 O (1). Infrared and Raman measurements indicate that 1 has a pentagonal bipyramidal structure (D/sub 5h/) in both solid and solution. Aqueous solutions of 1 are air sensitive, decomposing to potassium oxopentacyanotechnetate(V) tetrahydrate, K 2 TcO(CN) 5 .4H 2 O (2). This species can also be prepared from the reaction of TcO 2 .xH 2 O with hot aqueous potassium cyanide solutions. Hydrolysis of 2 in water yields potassium trans-dioxo-tetracyanotechnetate(V), K 3 TcO 2 (CN) 4 (3). Preparation of 3 can also be achieved from the treatment of [TcO 2 (Py) 4 ]ClO 4 .2H 2 O with aqueous potassium cyanide. Infrared and Raman measurements on 3 are consistent with the proposed trans-dioxo (D/sub 4h/) structure. Reaction of the oxotetrachlorotechnetate(V) anion, TcOCl 4 , with potassium cyanide in methanol produces trans-oxomethoxytetracyanotechnetate(V). [TcO(OMe)(CN) 4 ] (4). The full details of the synthesis and characterization of these interesting technetium(III) and -(V) complexes, as well as observations on the infrared and Raman spectra of trans-dioxo metal complexes and the hydrolysis of species 2, are presented

Synthesis and characterization of multicolour fluorescent ...

Indian Academy of Sciences (India)

... of latent fingerprints. The optical and structural characterization of the nanoparticles was carried .... by absorption of phonons from the host matrix [13], the exchange of energy in ... impressions based on the fluorescent properties exhibited by.

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

International Nuclear Information System (INIS)

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

2015-01-01

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

Synthesis and Characterization of Nanocrystalline Aluminophosphate AlPO4-5 Molecular Sieve

Directory of Open Access Journals (Sweden)

Asir Alnaama

2018-03-01

Full Text Available Nanocrystalline aluminophosphate AlPO4-5 molecular sieves were synthesized by hydrothermal method (HTS. Synthesis parameters like time and temperature of crystallization were investigated. Type of template (R and ratio of R/P2O5 were studied also. Characterization of the synthesized AlPO4-5 were done by powder X-ray diffraction (XRD, scanning electron microscopy (SEM/EDX, Fourier transform infrared (FTIR, differential scanning calorimetry-thermogravimetry analysis (DSC-TGA, and N2 adsorption-desorption BET analysis. XRD patterns results showed excellent crystallinity for two types of templates, di-n-propylamine (DPA and tetrapropyl ammonium hydroxide (TPAOH for alumminophosphate five (AFI structure. Nano-level for particle size of 66 nm was revealed by AFM test. Good thermal stability was obtained in DSC-TGA results. Best time and temperature of crystallization of 24h and 190 O C were got. Optimum R/P2O5 for two kind of template was established.

Electrochemical synthesis and characterization of copper (I oxide

Directory of Open Access Journals (Sweden)

Bugarinović Sanja J.

2009-01-01

Full Text Available The quest and need for clean and economical energy sources have increased interest in the development of thin film cells technologies. Electrochemical deposition is an attractive method for synthesis of thin films. It offers the advantages of low synthesis temperature, low cost and high purity. Copper (I oxide or cuprous oxide is an oxide semiconductor which is used as the anodic material in the form of thin film in lithium batteries and solar cells. The cathodic process of synthesis of cuprous oxide thin film is carried out in a potentiostatic mode from the organic electrolyte. The process parameters are chosen in that way to accomplish maximum difference between the potentials at which Cu2O and CuO are obtained. The electrochemical characterization was carried out by cyclic voltammetry. The electrodeposition techniques are particularly well suited for the deposition of single elements but it is also possible to carry out simultaneous depositions of several elements and syntheses of well-defined alternating layers of metals and oxides with thicknesses down to a few nm. Nanomaterials exhibit novel physical properties and play an important role in fundamental research. In addition, cuprous oxide is commonly used as a pigment, a fungicide, and an antifouling agent for marine paints. It is insoluble in water and organic solvents. This work presents the examinations of the influence of bath, temperature, pH and current density on the characteristics of electrochemically synthesized cuprous oxide. In the 'classic' process of synthesis, which is carried out under galvanostatic conditions on the anode, the grain size of the powder decreases with the increase in current density while the grain colour becomes lighter. The best commercial quality of the Cu2O (grain size, colour, content of choride was obtained at the temperature of 80°C, concentration of NaCl of 3 mol/dm3 and current density of 400 A/m2.

Synthesis and X-ray structure of the dysprosium(III) complex derived ...

African Journals Online (AJOL)

Synthesis and X-ray structure of the dysprosium(III) complex derived from the ligand 5-chloro-1 ... Bulletin of the Chemical Society of Ethiopia ... synthesized and its crystal structure determined by single X-ray diffraction at room temperature.

Collagen-chitosan scaffold modified with Au and Ag nanoparticles: Synthesis and structure

International Nuclear Information System (INIS)

Rubina, M.S.; Kamitov, E.E.; Zubavichus, Ya. V.; Peters, G.S.; Naumkin, A.V.; Suzer, S.; Vasil’kov, A.Yu.

2016-01-01

Graphical abstract: - Highlights: • Biocompatible collagen-chitosan scaffolds were modified by Au and Ag nanoparticles via the metal-vapor synthesis. • Structural and morphological parameters of the nanocomposites were assessed using a set of modern instrumental techniques, including electron microscopy, X-ray diffraction, small-angle X-ray scattering, EXAFS, XPS. • Potential application of the nanocomposites are envisaged. - Abstract: Nowadays, the dermal biomimetic scaffolds are widely used in regenerative medicine. Collagen-chitosan scaffold one of these materials possesses antibacterial activity, good compatibility with living tissues and has been already used as a wound-healing material. In this article, collagen-chitosan scaffolds modified with Ag and Au nanoparticles have been synthesized using novel method - the metal-vapor synthesis. The nanocomposite materials are characterized by XPS, TEM, SEM and synchrotron radiation-based X-ray techniques. According to XRD data, the mean size of the nanoparticles (NPs) is 10.5 nm and 20.2 nm in Au-Collagen-Chitosan (Au-CollCh) and Ag-Collagen-Chitosan (Ag-CollCh) scaffolds, respectively in fair agreement with the TEM data. SAXS analysis of the composites reveals an asymmetric size distribution peaked at 10 nm for Au-CollCh and 25 nm for Ag-CollCh indicative of particle's aggregation. According to SEM data, the metal-carrying scaffolds have layered structure and the nanoparticles are rather uniformly distributed on the surface material. XPS data indicate that the metallic nanoparticles are in their unoxidized/neutral states and dominantly stabilized within the chitosan-rich domains.

Collagen-chitosan scaffold modified with Au and Ag nanoparticles: Synthesis and structure

Energy Technology Data Exchange (ETDEWEB)

Rubina, M.S.; Kamitov, E.E. [A.N. Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences, Moscow, 119991 Russian Federation (Russian Federation); Zubavichus, Ya. V.; Peters, G.S. [National Research center «Kurchatov Institute», Moscow, 123182 Russian Federation (Russian Federation); Naumkin, A.V. [A.N. Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences, Moscow, 119991 Russian Federation (Russian Federation); Suzer, S. [Department of Chemistry, Bilkent University, Ankara, 06800 Turkey (Turkey); Vasil’kov, A.Yu., E-mail: alexandervasilkov@yandex.ru [A.N. Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences, Moscow, 119991 Russian Federation (Russian Federation)

2016-03-15

Graphical abstract: - Highlights: • Biocompatible collagen-chitosan scaffolds were modified by Au and Ag nanoparticles via the metal-vapor synthesis. • Structural and morphological parameters of the nanocomposites were assessed using a set of modern instrumental techniques, including electron microscopy, X-ray diffraction, small-angle X-ray scattering, EXAFS, XPS. • Potential application of the nanocomposites are envisaged. - Abstract: Nowadays, the dermal biomimetic scaffolds are widely used in regenerative medicine. Collagen-chitosan scaffold one of these materials possesses antibacterial activity, good compatibility with living tissues and has been already used as a wound-healing material. In this article, collagen-chitosan scaffolds modified with Ag and Au nanoparticles have been synthesized using novel method - the metal-vapor synthesis. The nanocomposite materials are characterized by XPS, TEM, SEM and synchrotron radiation-based X-ray techniques. According to XRD data, the mean size of the nanoparticles (NPs) is 10.5 nm and 20.2 nm in Au-Collagen-Chitosan (Au-CollCh) and Ag-Collagen-Chitosan (Ag-CollCh) scaffolds, respectively in fair agreement with the TEM data. SAXS analysis of the composites reveals an asymmetric size distribution peaked at 10 nm for Au-CollCh and 25 nm for Ag-CollCh indicative of particle's aggregation. According to SEM data, the metal-carrying scaffolds have layered structure and the nanoparticles are rather uniformly distributed on the surface material. XPS data indicate that the metallic nanoparticles are in their unoxidized/neutral states and dominantly stabilized within the chitosan-rich domains.

Green synthesis of gold nanoparticles using Stevia rebaudiana leaf extracts: Characterization and their stability.

Science.gov (United States)

Sadeghi, Babak; Mohammadzadeh, M; Babakhani, B

2015-07-01

Various methods invented and developed for the synthesis of gold nanoparticles that increases daily consumed. According to this method, including potential environmental pollution problems and the complexity of the synthesis, in this study, the feasibility of using the leaves extract of Stevia rebaudiana (SR) for the reduction of gold ions to nanoparticles form have been studied. Stevia leaves were used to prepare the aqueous extract for this study. Gold nanoparticles were characterized with different techniques such as UV-vis spectroscopy, FT-IR spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Transmission electron microscopy experiments showed that these nanoparticles are spherical and uniformly distributed and its size is from 5 to 20 nm. FT-IR spectroscopy revealed that gold nanoparticles were functionalized with biomolecules that have primary amine group (NH2), carbonyl group, OH groups and other stabilizing functional groups. X-ray diffraction pattern showed high purity and face centered cubic structure of gold nanoparticles with size of 17 nm. The scanning electron microscopy (SEM) implies the right of forming gold nanoparticles. The results, confirm that gold nanoparticles have synthesized by the leaves extract of S. rebaudiana (SR). Copyright © 2015 Elsevier B.V. All rights reserved.

Silver nanostructures with well-controlled shapes: synthesis, characterization and growth mechanisms

International Nuclear Information System (INIS)

Kan Caixia; Zhu Jiejun; Zhu Xiaoguang

2008-01-01

This paper describes a poly(vinylpyrollidone)-directed polyol synthesis method for the fabrication of silver (Ag) nanostructures with well-controlled shapes (such as nanorods and nanocubes) by adjusting the synthesizing parameters. The structure characterizations suggest that the Ag nanorods grow from the five-fold twinned decahedral crystal nuclei. The nature of the {1 1 1} planes of Ag crystal and the highly selective poly(vinylpyrollidone) adsorption on the {100} planes of Ag crystal nuclei are favourable for the formation of Ag nanorods and Ag nanowires. The single crystalline Ag nanocubes obtained at optimum conditions are perfect in shape and are enclosed by the {1 0 0} facets. The optical properties of the Ag nanostructures show an attractive plasma resonance, displaying a considerable dependence on the shape and size. The formation of the Ag nanostructures with well-defined shapes is probably due to the fact that the nanostructures are controlled thermodynamically and kinetically. The ability to generate shape-controlled Ag nanostructures also provides an opportunity to experimentally and systematically study the relationship between their properties and geometric shapes

Silver nanostructures with well-controlled shapes: synthesis, characterization and growth mechanisms

Science.gov (United States)

Kan, Cai-Xia; Zhu, Jie-Jun; Zhu, Xiao-Guang

2008-08-01

This paper describes a poly(vinylpyrollidone)-directed polyol synthesis method for the fabrication of silver (Ag) nanostructures with well-controlled shapes (such as nanorods and nanocubes) by adjusting the synthesizing parameters. The structure characterizations suggest that the Ag nanorods grow from the five-fold twinned decahedral crystal nuclei. The nature of the {1 1 1} planes of Ag crystal and the highly selective poly(vinylpyrollidone) adsorption on the {100} planes of Ag crystal nuclei are favourable for the formation of Ag nanorods and Ag nanowires. The single crystalline Ag nanocubes obtained at optimum conditions are perfect in shape and are enclosed by the {1 0 0} facets. The optical properties of the Ag nanostructures show an attractive plasma resonance, displaying a considerable dependence on the shape and size. The formation of the Ag nanostructures with well-defined shapes is probably due to the fact that the nanostructures are controlled thermodynamically and kinetically. The ability to generate shape-controlled Ag nanostructures also provides an opportunity to experimentally and systematically study the relationship between their properties and geometric shapes.

Synthesis of nano-structured materials by laser-ablation and their application to sensors

International Nuclear Information System (INIS)

Okada, T.; Suehiro, J.

2007-01-01

We describe the synthesis of nano-structured materials of ZnO and Pd by laser ablation and their applications to sensors. The synthesis of ZnO nano-wires was performed by nano-particle assisted deposition (NPAD) where nano-crystals were grown with nano-particles generated by laser-ablating a ZnO sintered target in an Ar background gas. The synthesized ZnO nano-wires were characterized with a scanning electron microscopy and the photoluminescent characteristics were examined under an excitation with the third harmonics of a Nd:YAG laser. The nano-wires with a diameter in the range from 50 to 150 nm and a length of up to 5 μm were taken out of the substrate by laser blow-off technique and/or sonication. It was confirmed that the nano-wires showed the stimulated emission under optical pumping, indicating a high quality of the crystalinity. Pd nano-particles were generated by laser-ablating a Pd plate in pure water. The transmission electron microscope observation revealed that Pd nano-particles with a diameter in the range from 3 nm to several tens of nanometers were produced. Using these nano-structured materials, we successfully fabricated sensors by the dielectrophoresis techniques. In the case of the ultraviolet photosensor, a detection sensitivity of 10 nW/cm 2 was achieved and in the case of hydrogen sensing, the response time of less than 10 s has been demonstrated with Pd nano-particles

Green Synthesis, Characterization and Application of Proanthocyanidins-Functionalized Gold Nanoparticles

Directory of Open Access Journals (Sweden)

Linhai Biao

2018-01-01

Full Text Available Green synthesis of gold nanoparticles using plant extracts is one of the more promising approaches for obtaining environmentally friendly nanomaterials for biological applications and environmental remediation. In this study, proanthocyanidins-functionalized gold nanoparticles were synthesized via a hydrothermal method. The obtained gold nanoparticles were characterized by ultraviolet and visible spectrophotometry (UV-Vis, Fourier transform infrared spectroscopy (FTIR, transmission electron microscopy (TEM and X-ray diffraction (XRD measurements. UV-Vis and FTIR results indicated that the obtained products were mainly spherical in shape, and that the phenolic hydroxyl of proanthocyanidins had strong interactions with the gold surface. TEM and XRD determination revealed that the synthesized gold nanoparticles had a highly crystalline structure and good monodispersity. The application of proanthocyanidins-functionalized gold nanoparticles for the removal of dyes and heavy metal ions Ni2+, Cu2+, Cd2+ and Pb2+ in an aqueous solution was investigated. The primary results indicate that proanthocyanidins-functionalized gold nanoparticles had high removal rates for the heavy metal ions and dye, which implies that they have potential applications as a new kind of adsorbent for the removal of contaminants in aqueous solution.

Synthesis and Characterization of Smart Block Copolymers for Biomineralization and Biomedical Applications

Energy Technology Data Exchange (ETDEWEB)

Kanapathipillai, Mathumai [Iowa State Univ., Ames, IA (United States)

2008-01-01

Self-assembly is a powerful tool in forming structures with nanoscale dimensions. Self-assembly of macromolecules provides an efficient and rapid pathway for the formation of structures from the nanometer to micrometer range that are difficult, if not impossible to obtain by conventional lithographic techniques [1]. Depending on the morphologies obtained (size, shape, periodicity, etc.) these self-assembled systems have already been applied or shown to be useful for a number of applications in nanotechnology [2], biomineralization [3, 4], drug delivery [5, 6] and gene therapy [7]. In this respect, amphiphilic block copolymers that self-organize in solution have been found to be very versatile [1]. In recent years, polymer-micellar systems have been designed that are adaptable to their environment and able to respond in a controlled manner to external stimuli. In short, synthesis of 'nanoscale objects' that exhibit 'stimulus-responsive' properties is a topic gathering momentum, because their behavior is reminiscent of that exhibited by proteins [8]. By integrating environmentally sensitive homopolymers into amphiphilic block copolymers, smart block copolymers with self assembled supramolecular structures that exhibit stimuli or environmentally responsive properties can be obtained [1]. Several synthetic polymers are known to have environmentally responsive properties. Changes in the physical, chemical or biochemical environment of these polymers results in modulation of the solubility or chain conformation of the polymer [9]. There are many common schemes of engineering stimuli responsive properties into materials [8, 9]. Polymers exhibiting lower critical solution temperature (LCST) are soluble in solvent below a specific temperature and phase separate from solvent above that temperature while polymers exhibiting upper critical solution temperatures (UCST) phase separate below a certain temperature. The solubility of polymers with ionizable

Synthesis and characterization of magnetic Co nanoparticles: A comparison study of three different capping surfactants

International Nuclear Information System (INIS)

Lu Yu; Lu Xianmao; Mayers, Brian T.; Herricks, Thurston; Xia Younan

2008-01-01

This paper compares the performance of three long-chain acids-oleic and elaidic (both olefinic) and stearic (aliphatic)-as a capping agent in the synthesis of magnetic Co nanoparticles. The particles were formed through thermal decomposition of dicobalt octacarbonyl in toluene in the presence of the long-chain acid, and characterized by TEM, high-resolution TEM, and SQUID measurements. Infrared spectra revealed that some of the added olefinic acid was transformed from cis- to trans-configuration (for oleic acid) or from trans- to cis- (for elaidic acid) to facilitate the formation of a densely packed monolayer on the surface of Co nanoparticles. As compared to aliphatic acids, olefinic acids are advantageous for dense packing on small particles with high surface curvatures due to a bent shape of the cis-isomer. The presence of an olefinic acid is able to control particle growth, stabilize the colloidal suspension, and prevent the final product from oxidation by air. Our results indicate that oleic acid, elaidic acid, and a mixture of oleic/stearic acids or elaidic/stearic acids have roughly the same performance in serving as a capping agent for the synthesis of Co nanoparticles with a spherical shape and narrow size distribution. - Graphical abstract: Magnetic Co nanoparticles were synthesized in the presence of different capping agents and the effect of their molecular structures on the morphology of Co nanoparticles was analyzed. The transformation between cis- and trans-isomers of olefinic acids was critical to the formation of a densely packed monolayer on the surface of small nanoparticles characterized by high curvatures

Structural and compositional characterization of the adhesive produced by reef building oysters.

Science.gov (United States)

Alberts, Erik M; Taylor, Stephen D; Edwards, Stephanie L; Sherman, Debra M; Huang, Chia-Ping; Kenny, Paul; Wilker, Jonathan J

2015-04-29

Oysters have an impressive ability to overcome difficulties of life within the stressful intertidal zone. These shellfish produce an adhesive for attaching to each other and building protective reef communities. With their reefs often exceeding kilometers in length, oysters play a major role in balancing the health of coastal marine ecosystems. Few details are available to describe oyster adhesive composition or structure. Here several characterization methods were applied to describe the nature of this material. Microscopy studies indicated that the glue is comprised of organic fiber-like and sheet-like structures surrounded by an inorganic matrix. Phospholipids, cross-linking chemistry, and conjugated organics were found to differentiate this adhesive from the shell. Symbiosis in material synthesis could also be present, with oysters incorporating bacterial polysaccharides into their adhesive. Oyster glue shows that an organic-inorganic composite material can provide adhesion, a property especially important when constructing a marine ecosystem.

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

Energy Technology Data Exchange (ETDEWEB)

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

2009-07-01

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

Synthesis and Structural Characterization of a CHA-type AlPO4 Molecular Sieve with Penta-Coordinated Framework Aluminum Atoms.

Science.gov (United States)

Park, Gi Tae; Jo, Donghui; Ahn, Nak Ho; Cho, Jung; Hong, Suk Bong

2017-07-17

The structure-directing effects of a series of polymethylimidazolium cations with different numbers of methyl groups as organic structure-directing agents (OSDAs) in the synthesis of aluminophosphate (AlPO 4 )-based molecular sieves in both fluoride and hydroxide media are investigated. On the one hand, among the OSDAs studied here, the smallest 1,3-dimethylimidazolium and the largest 1,2,3,4,5-pentamethylimidazolium cations were found to direct the synthesis of a new variant of the triclinic chabazite (CHA)-type AlPO 4 material, designated AlPO 4 -34(t) V , and the one-dimensional small-pore silicoaluminophosphate (SAPO) molecular sieve STA-6 in hydroxide media, respectively. On the other hand, the intermediate-sized 1,2,3,4-tetramethylimidazolium cation gave SSZ-51, a two-dimensional large-pore SAPO material, in fluoride media. Synchrotron powder X-ray diffraction and Rietveld analyses reveal that as-made AlPO 4 -34(t) V contains penta-coordinated framework Al species connected by hydroxyl groups, as well as tetrahedral framework Al, which contrasts with the distortions arising from the two F - or OH - bridges between octahedral Al atoms in all already known AlPO 4 -34 materials. The presence of Al-OH-Al linkages in this triclinic AlPO 4 -34 molecular sieve has been further corroborated by thermal analysis, variable-temperature IR,27Al magic-angle spinning NMR, and dispersion-corrected density functional theory calculations.

New Dilated LMI Characterization for the Multiobjective Full-Order Dynamic Output Feedback Synthesis Problem

Directory of Open Access Journals (Sweden)

Zrida Jalel

2010-01-01

Full Text Available This paper introduces new dilated LMI conditions for continuous-time linear systems which not only characterize stability and performance specifications, but also, performance specifications. These new conditions offer, in addition to new analysis tools, synthesis procedures that have the advantages of keeping the controller parameters independent of the Lyapunov matrix and offering supplementary degrees of freedom. The impact of such advantages is great on the multiobjective full-order dynamic output feedback control problem as the obtained dilated LMI conditions always encompass the standard ones. It follows that much less conservatism is possible in comparison to the currently used standard LMI based synthesis procedures. A numerical simulation, based on an empirically abridged search procedure, is presented and shows the advantage of the proposed synthesis methods.

Synthesis and properties of ZnFe2O4 replica with biological hierarchical structure

International Nuclear Information System (INIS)

Liu, Hongyan; Guo, Yiping; Zhang, Yangyang; Wu, Fen; Liu, Yun; Zhang, Di

2013-01-01

Highlights: • ZFO replica with hierarchical structure was synthesized from butterfly wings. • Biotemplate has a significant impact on the properties of ZFO material. • Our method opens up new avenues for the synthesis of spinel ferrites. -- Abstract: ZnFe 2 O 4 replica with biological hierarchical structure was synthesized from Papilio paris by a sol–gel method followed by calcination. The crystallographic structure and morphology of the obtained samples were characterized by X-ray diffraction, field-emission scanning electron microscope, and transmittance electron microscope. The results showed that the hierarchical structures were retained in the ZFO replica of spinel structure. The magnetic behavior of such novel products was measured by a vibrating sample magnetometer. A superparamagnetism-like behavior was observed due to nanostructuration size effects. In addition, the ZFO replica with “quasi-honeycomb-like structure” showed a much higher specific capacitance of 279.4 F g −1 at 10 mV s −1 in comparison with ZFO powder of 137.3 F g −1 , attributing to the significantly increased surface area. These results demonstrated that ZFO replica is a promising candidate for novel magnetic devices and supercapacitors

Low-temperature synthesis and characterization of anatase TiO{sub 2} nanoparticles by an acid assisted sol–gel method

Energy Technology Data Exchange (ETDEWEB)

Leyva-Porras, C. [Centro de Investigación en Materiales DIP-CUCEI, Universidad de Guadalajara, Av. Revolución # 1500, Col. Olímpica, C.P. 44430, Guadalajara (Mexico); Centro de Investigación en Materiales Avanzados, S.C. (CIMAV), Alianza Norte No. 202, Parque de Investigación e Innovación Tecnológica (PIIT), Carretera Aeropuerto km. 10, C.P. 66600, Apodaca, N.L. (Mexico); Toxqui-Teran, A.; Vega-Becerra, O. [Centro de Investigación en Materiales Avanzados, S.C. (CIMAV), Alianza Norte No. 202, Parque de Investigación e Innovación Tecnológica (PIIT), Carretera Aeropuerto km. 10, C.P. 66600, Apodaca, N.L. (Mexico); Miki-Yoshida, M. [Centro de Investigación en Materiales Avanzados, S.C. (CIMAV), Miguel de Cervantes No. 120, Parque Industrial Chihuahua, C.P. 31109, Chihuahua (Mexico); Rojas-Villalobos, M.; García-Guaderrama, M. [Centro de Investigación en Materiales DIP-CUCEI, Universidad de Guadalajara, Av. Revolución # 1500, Col. Olímpica, C.P. 44430, Guadalajara (Mexico); and others

2015-10-25

The synthesis of anatase TiO{sub 2} nanoparticles by an acid-assisted sol–gel method at 25 and 80 °C is described. Specifically, acetic acid (AA) was used and the evolution of the anatase phase with the amount of AA was observed. The results of X-ray diffraction (XRD) and transmission electron microscopy (TEM) both showed that a pure anatase phase was obtained with particle size smaller than 5 nm. Structural refinements and quantitative determination of phase composition was achieved by using the Rietveld method. The particle size distribution became slightly narrower as the amount of AA was increased. Raman spectroscopy showed that when the amount of AA was increased a small amount of brookite was present at the contamination level. The anatase phase was studied by differential thermal analysis (DTA), providing phase stability up to 600 °C. These and other results were discussed in terms of particle size and structure. Likewise, the formation of the anatase phase under these synthesis conditions was explained. - Highlights: • Synthesis of anatase TiO{sub 2} nanoparticles by an acid assisted sol–gel method at mild conditions. • Microstructure characterization by XRD, TEM and Raman spectroscopy. • Observation of the formation and evolution of the anatase phase as acetic acid was increased. • Anatase thermal stability up to 600 °C and band gap range between 3.2 and 3.5 eV. • A simplified method which can be considered as a green chemistry process.

Synthesis and characterization of boron nitrides nanotubes

International Nuclear Information System (INIS)

Ferreira, T.H.; Sousa, E.M.B.

2010-01-01

This paper presents a new synthesis for the production of boron nitride nanotubes (BNNT) from boron powder, ammonium nitrate and hematite tube furnace CVD method. The samples were subjected to some characterization techniques as infrared spectroscopy, thermal analysis, X-ray diffraction and scanning electron microscopy and transmission. By analyzing the results can explain the chemical reactions involved in the process and confirm the formation of BNNT with several layers and about 30 nanometers in diameter. Due to excellent mechanical properties and its chemical and thermal stability this material is promising for various applications. However, BNNT has received much less attention than carbon nanotubes, it is because of great difficulty to synthesize appreciable quantities from the techniques currently known, and this is one of the main reasons this work.(author)

Synthesis of [3H] Zolpidem

International Nuclear Information System (INIS)

Allen, J.; Parent, G.; Tizot, A.

1986-01-01

Zolpidem is a novel hypnotic agent possessing a substituted imidazo [1,2-a] pyridine structure. The synthesis of the tritium labelled compound with a specific activity of 60.5 Ci/mmol is described. This new radioligand was initially used to establish and characterize the binding properties of Zolpidem in the rat brain. (author)

Controlling Magnetic and Ferroelectric Order Through Geometry: Synthesis, Ab Initio Theory, Characterization of New Multi-Ferric Fluoride Materials

Energy Technology Data Exchange (ETDEWEB)

Halasyamani, Shiv [Univ. of Houston, TX (United States); Fennie, Craig [Cornell Univ., Ithaca, NY (United States)

2016-11-03

We have focused on the synthesis, characterization, and ab initio theory on multi-functional mixed-metal fluorides. With funding from the DOE, we have successfully synthesized and characterized a variety of mixed metal fluoride materials.

Physical and structural characterization of oxides

International Nuclear Information System (INIS)

Hussain, A.

2012-01-01

Objective of this thesis was the synthesis of the nano whiskers of aluminum ammonium carbonate hydroxide (AACH) from the mixture of aluminum nitrate and urea with different content levels of urea by hydrothermal process. The AACH precursor of nano alumina whiskers is added into zirconia powder along with CTAB and ethanol to obtain fine precipitates ready for calcining at 650 C. Fine powder of zirconia with alumina whiskers is compacted to form pellets of 5 mm diameter. Sintering of pellets has been performed at 1500 C in open atmosphere. Fabrication of sintered pellets is being done by using uniaxial press under 5 ton loads. The addition of alumina whiskers resulted better mechanical properties like compactness, hardness and flexural strength etc. The influence of urea composition upon the growth of alumina whisker has been revealed by FE-SEM. Low content of urea at 6 gm. to 8 gm. formed urchin like morphology of AACH whiskers, while at higher level 12 gm. of urea independent whiskers obtained. In second stage the varying amount of urea in aluminum nitrate was performed and calcined at different temperatures 80, 100, 200, 300, 400 degree C to reveal the effect on the pure AACH whiskers morphologies. Different characterization like SEM is used for structure morphologies, XRD used for determining of type of structure, FTIR technique used for the study of nature of functional groups, and impedance spectroscopy applied for electrical properties measurements. XRD pattern show the presence of a-alumina, FTIR tells about the missing peaks and absence of functional group due to increases in the temperature and SEM analysis of fractured surface of sintered pellets done for revealing structure morphology. Fracture study of nuclear fuel has also done by SEM analysis in this work to study cause of peeling off flakes at the outer edge of sintered UO 2 pellets. (author)

Synthesis and characterization of iron-cobalt (FeCo) alloy nanoparticles supported on carbon

DEFF Research Database (Denmark)

Koutsopoulos, Sotiris; Barfod, Rasmus; Eriksen, Kim Michael

2017-01-01

of the alloy nanoparticles differed depending on the preparation method. When the wet impregnation technique of acetate precursor salts of Fe and Co were used for the synthesis, the size of FeCo alloy nanoparticles was approximately 13 nm. FeCo alloy nanoparticles were characterized by crystallography (XRD...

Synthesis, purification and physico-chemical characterization of the deuterized chloroform

International Nuclear Information System (INIS)

Mihaila, Vasile; Chiper, Diana

1999-01-01

This work refers to deuterized chloroform synthesis and purification methods. Three preparation methods of deuterized chloroform are presented. In the first method the direct chlorination of methane (CH 4 + 3Cl 2 ) in the presence of light and in an oxygen-free atmosphere results in CHCl 3 + 3HCl. The method's drawback is that the resulting product is impure, being obtained also secondary chlorinated compounds, such as CHCl, CH 2 Cl 2 and CCl 4 . The second method consists in chlorination of acetaldehyde or acetone, in basic catalysis and in halogen excess (α substitution with direct synthesis of trihalogen compound), followed by a haloform reaction (hydrolytic splitting) in the presence of chlorinated lime. This method makes use of decarbolyzing of trichlor acetate acid (as a sodium salt), what results in CL 3 CH + NaHCO 3 . This method is the most suitable for the deuterized chloroform synthesis, since the reaction takes place in absence of other hydrogen atoms (protons) and in deuterized water of 99.87% purity, according to the following reaction: Cl 3 C-COONa → (D 2 O) → Cl 2 CD + NaDCO 3 . Another advantage is that this method avoids the synthesis of secondary products, which could entail additional purifications (distillations, rectification, a.s.o.). The deuterized chloroform is separated from the deuterized sodium bicarbonate aqueous solution by washing with deuterized water, in a liquid to liquid separating funnel. After separation, deuterized chloroform is dried in nitrogen atmosphere. The characterization of the final product is carried out by nuclear magnetic resonance spectrometry. (authors)

Chemical synthesis, characterization and evaluation of antimicrobial properties of Cu and its oxide nanoparticles

CSIR Research Space (South Africa)

Motlatle, Abesach M

2016-10-01

Full Text Available of Nanoparticle Research, vol. 18: DOI: 10.1007/s11051-016-3614-8 Chemical synthesis, characterization and evaluation of antimicrobial properties of Cu and its oxide nanoparticles Motlatle AM Kesevan Pillai S Scriba MR Ray SS ABSTRACT: Cu...

Synthesis, characterization and nano-structuration of poly-thiophene derivatives for organic photovoltaic solar cells

International Nuclear Information System (INIS)

Berson, S.

2007-10-01

This work is devoted to the synthesis of poly-thiophene derivatives with low bandgap and preserving high oxidation potential. Disubstituted thiophenes and 'Donor-Acceptor' bi-thiophenes were synthesized and then polymerized. The side chains of these polymers, donor or acceptor, were modified in order to tune the properties of material as well from the optical point of view as electrochemical. These polymers were also tested in blend with PCBM in bulk-heterojunction photovoltaic cells. Voc delivered by the devices showed a linear dependence according to the potential of oxidation of the polymers. Copolymers containing cyano-thiophene and alkyl- or alkoxy-thiophene showed values of 0.8 V. However, in spite of power conversion efficiency of 1 %, these performances remain lower than the one obtained with the P3HT. Optimizations in terms of morphology are certainly necessary. Indeed, the morphology of the active layer plays a key role in obtaining high power conversion efficiency. An original technique of nano-structuration of the polymer on a nano-metric scale was developed during this work, leading to the development of fibrillar P3HT. These nano-structures, presenting an important degree of order, are formed spontaneously in solution. Their rate compared to amorphous material is perfectly controllable and adjustable in solution and in solid state. Measurements of mobilities show a strong improvement of the transport of load within these fibrillar layers compared to a traditional film of P3HT obtained without annealing. Power conversion efficiencies of 3.6% on glass and 3.3 % on plastic were reached without annealing. (author)

Synthesis, characterization and nano-structuration of poly-thiophene derivatives for organic photovoltaic solar cells

International Nuclear Information System (INIS)

Berson, S.

2007-10-01

This work is devoted to the synthesis of poly-thiophene derivatives with low bandgap and preserving high oxidation potential. Di-substituted thiophenes and 'Donor-Acceptor' bi-thiophenes were synthesized and then polymerized. The side chains of these polymers, donor or acceptor, were modified in order to tune the properties of material as well from the optical point of view as electrochemical. These polymers were also tested in blend with PCBM in bulk-heterojunction photovoltaic cells. Voc delivered by the devices showed a linear dependence according to the potential of oxidation of the polymers. Copolymers containing cyano-thiophene and alkyl- or alkoxy-thiophene showed values of 0.8 V. However, in spite of power conversion efficiency of 1 %, these performances remain lower than the one obtained with the P3HT. Optimizations in terms of morphology are certainly necessary. Indeed, the morphology of the active layer plays a key role in obtaining high power conversion efficiency. An original technique of nano-structuration of the polymer on a nano-metric scale was developed during this work, leading to the development of fibrillary P3HT. These nano-structures, presenting an important degree of order, are formed spontaneously in solution. Their rate compared to amorphous material is perfectly controllable and adjustable in solution and in solid state. Measurements of mobilities show a strong improvement of the transport of load within these fibrillary layers compared to a traditional film of P3HT obtained without annealing. Power conversion efficiencies of 3.6 % on glass and 3.3 % on plastic were reached without annealing. (author)

Characterization of Nanocarbon Copper Composites Manufactured in Metallurgical Synthesis Process

Science.gov (United States)

Knych, Tadeusz; Kwaśniewski, Paweł; Kiesiewicz, Grzegorz; Mamala, Andrzej; Kawecki, Artur; Smyrak, Beata

2014-08-01

Currently, there is a worldwide search for new forms of materials with properties that are significantly improved in comparison to materials currently in use. One promising research direction lies in the synthesis of metals containing modern carbon materials ( e.g., graphene, nanotubes). In this article, the research results of metallurgical synthesis of a mixture of copper and two different kinds of carbon (activated carbon and multiwall carbon nanotubes) are shown. Samples of copper-carbon nanocomposite were synthesized by simultaneously exposing molten copper to an electrical current while vigorously stirring and adding carbon while under an inert gas atmosphere. The article contains research results of density, hardness, electrical conductivity, structure (TEM), and carbon decomposition (SIMS method) for the obtained materials.

Synthesis of silver nanoparticles by chemical reduction at various fraction of MSA and their structure characterization

Energy Technology Data Exchange (ETDEWEB)

Diantoro, Markus, E-mail: m-diantoror@yahoo.com; Fitrianingsih, Rina, E-mail: m-diantoror@yahoo.com; Mufti, Nandang, E-mail: m-diantoror@yahoo.com; Fuad, Abdulloh, E-mail: m-diantoror@yahoo.com [Department of Physics, Faculty of Mathematics and Natural Sciences, Universitas Negeri Malang (UM), Jl. Semarang No. 5 Malang 65145 (Indonesia)

2014-03-24

Nanosilver is currently one of the most common engineered nanomaterials and is used in many applications that lead to the release of silver nanoparticles and silver ions into aqueous systems. Nanosilver also possesses enhanced antimicrobial activity and bioavailability that may less environmental risk compared with other manufactured nanomaterials. Described in this research are the synthesis of silver nanoparticle produced by chemical reduction from silver nitrate (AgNO{sub 3}) solution. As a reducing agent, Sodium Borohydride (NaBH{sub 4}) was used and mercaptosuccinic Acid (MSA) as stabilizer to prevent the nanoparticle from aglomerating. It was also used two kinds of solvent, they are water and methanol. In typical experiment MSA was dissolve in methanol with a number of variation of molarity i.e. 0,03 M, 0,06 M, 0,12 M, 0,15 M, and the mixture was kept under vigorous stirring in an ice bath. A solution of silver nitrate of 340 mg in 6,792 ml water was added. A freshly prepared aqueous solution of sodium borohydride (756,6 mL in 100 mL of water) was added drop wisely. The solution was kept for half an hour for stirring and were allowed to settle down in methanol. The obtained samples then characterized by means of x-ray diffractometer, and scanning electron microscopy, as well as transmission electron microscopy to obtain their structures of silver nanoparticles, morphology, and sizes. It is shown that diameter of silver nanoparticle sized about 24.3 nm (Ag@MSA 0.03 M), 20.4 nm (Ag@MSA 0.06 M), 16.8 nm (Ag@MSA 0.12 M), 16.9 nm (Ag@MSA 0.15 M) which was calculated by Scherrer formula by taking the FWHM from fitting to Gaussian. The phases and lattice parameter showed that there is no significant change in its volume by increasing molarity of stabilizer. In contrast, the size of particles is decreasing.

Synthesis and characterization of new polyamino-cyclodextrin materials.

Science.gov (United States)

Lo Meo, Paolo; D'Anna, Francesca; Gruttadauria, Michelangelo; Riela, Serena; Noto, Renato

2012-01-10

With the aim of the synthesis of chemically modified cyclodextrins bearing polyamine pendant groups, potentially useful as capping agents for the preparation of nanosized metal systems or as auxiliaries for gene transfection, the reaction between the heptakis-(6-iodo)-(6-deoxy)-β-cyclodextrin and various polyamines has been explored. This synthetic approach allows obtaining materials constituted by mixtures of cyclodextrins, having different degrees of substitution, which were satisfactorily characterized by means of various complementary techniques (ESI-MS, NMR, potentiometric titration). The products obtained were successfully subjected to preliminary tests for their binding abilities towards suitable organic guests and as capping agents for the preparation of stable silver nanoparticles. Copyright © 2011 Elsevier Ltd. All rights reserved.

Synthesis, X-ray crystal structure, DNA binding and Nuclease activity ...

Indian Academy of Sciences (India)

s12039-016-1125-x. Synthesis, X-ray crystal structure, DNA binding and Nuclease activity of lanthanide(III) complexes of 2-benzoylpyridine acetylhydrazone. KARREDDULA RAJA, AKKILI SUSEELAMMA and KATREDDI HUSSAIN REDDY. ∗.

Synthesis and cyclic force characterization of helical polypyrrole actuators for artificial facial muscles

International Nuclear Information System (INIS)

Tadesse, Yonas; Grange, Robert W; Priya, Shashank

2009-01-01

This study focuses on the synthesis and characterization of thick and thin film polypyrrole (PPy)–metal composite actuators for application as artificial muscles in facial robotics. The fabrication method consists of three steps based upon the approach proposed by Ding et al (2003 Synth. Met. 138 391–8): (i) winding the conductive spiral structure around the platinum (Pt) wire core, (ii) deposition of PPy film on the Pt wire core, and (iii) removal of the Pt wire core. This approach yielded good performance from the synthesized actuators, but was complex to implement due to the difficulty in implementing the third step. To overcome the problem of mechanical damage occurring during withdrawal of the Pt wire, the core was replaced with a dispensable gold coated polylactide fiber that could be etched at the end of deposition step. Experimental results indicate that thin film actuators perform better in terms of response time and blocking force. A unique muscle-like structure with smoothly varying cross-section was grown by combining layer by layer deposition with changes in position and orientation of the counter electrode in reference to the working electrode

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)

Metal Oxide Nano structures: Synthesis, Properties, and Applications

International Nuclear Information System (INIS)

Xu, L. H.; Patil, D. S.; Yang, J.; Xiao, J.

2015-01-01

In recent years, nano structured materials have attracted wide attention due to their fascinating optical and electrical properties, which make these materials potentially suitable for applications in electronics, optics, photonics, and sensors. Some metal oxides show a wide variety of morphologies such as nano wires, nano rods, nano tubes, nano rings, and nano belts. Synthesis and investigation of these metal-oxide nano structures are beneficial not only for understanding the fundamental phenomena in low dimensional systems, but also for developing new-generation nano devices with high performance.

New bismuth calcium oxysilicate with apatite structure: Synthesis and structural characterization

International Nuclear Information System (INIS)

Uvarov, Vladimir; Shenawi-Khalil, Sanaa; Popov, Inna

2010-01-01

New bismuth calcium silicon oxide Ca 4 Bi 4.3 (SiO 4 )(HSiO 4 ) 5 O 0.95 , with apatite structure has been synthesized. The structure was refined from powder X-ray diffraction data. The refinement revealed that the phase has P6 3 /m (176) space group with unit cell parameters a=b=9.6090(7) A, c=7.0521(7) A, V=563.9 A 3 and c/a=0.734. The R wp factor at Rietveld refinement was equal to 0.082. The synthesized phase has an unusual quantity of cation vacancies in a crystal lattice. Mechanisms of compensation of the excess charge of a lattice are considered and checked experimentally using the FT-IR spectroscopy, the thermal analysis and the XPS analysis. - Graphical abstract: The fragment Ca 4 Bi 4.3 (SiO 4 )(HSiO 4 ) 5 O 0.95 structure along c-axis in polygonal mode.

Core/shell structured ZnO/SiO2 nanoparticles: Preparation, characterization and photocatalytic property

International Nuclear Information System (INIS)

Zhai Jing; Tao Xia; Pu Yuan; Zeng Xiaofei; Chen Jianfeng

2010-01-01

ZnO nanoparticles were prepared by a simple chemical synthesis route. Subsequently, SiO 2 layers were successfully coated onto the surface of ZnO nanoparticles to modify the photocatalytic activity in acidic or alkaline solutions. The obtained particles were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), transmission electron microscopy (TEM), energy dispersive spectrometry (EDS) and zeta potential. It was found that ultrafine core/shell structured ZnO/SiO 2 nanoparticles were successfully obtained. The photocatalytic performance of ZnO/SiO 2 core/shell structured nanoparticles in Rhodamine B aqueous solution at varied pH value were also investigated. Compared with uncoated ZnO nanoparticles, core/shell structured ZnO/SiO 2 nanoparticles with thinner SiO 2 shell possess improved stability and relatively better photocatalytic activity in acidic or alkaline solutions, which would broaden its potential application in pollutant treatment.

Synthesis and characterization of N-t-BOC protected pyrrole-sulfur oligomers and polymers

NARCIS (Netherlands)

Groenendaal, L.; Pieterse, K.; Vekemans, J.A.J.M.; Meijer, E.W.

1997-01-01

The synthesis and characterization of a new class of pyrrole-sulfur compounds is described. These compounds are designed to be precursors for an organic analogue of poly(sulfur nitride). Poly(N-t-BOC-2.5-pyrrolyl sulfide) was prepared from N-t-BOC-2,5-dibromopyrrole by first lithiating this compound

Transition metal borides. Synthesis, characterization and superconducting properties

Energy Technology Data Exchange (ETDEWEB)

Kayhan, Mehmet

2013-07-12

A systematic study was done on the synthesis and superconducting properties of metal rich transition metal borides. Five different binary systems were investigated including the boride systems of niobium, tantalum, molybdenum, tungsten and rhenium. High temperature solid state methods were used in order to synthesize samples of different transition metal borides of the composition M{sub 2}B, MB, M{sub 3}B{sub 2}, MB{sub 2}, and M{sub 2}B{sub 4}. The reactions were carried out in three different furnaces with different sample containers: the electric arc (copper crucible), the high frequency induction furnace (boron nitride, tantalum or glassy carbon crucibles), and the conventional tube furnace (sealed evacuated quartz ampoules). The products obtained were characterized with X-ray powder diffractometry, scanning electron microscopy and energy-dispersive X-ray spectroscopy. Phase analyses and crystal structure refinements using the Rietveld method and based on structure models known from literature were performed. A neutron diffraction measurement was done for W{sub 2}B{sub 4} to allow for a complete crystal structure determination, because of the presence of a heavy element like tungsten and a light element like boron that made it difficult to determine the accurate determination of the boron atom positions and occupancies from X-ray data. A new structure model for W{sub 2}B{sub 4} was proposed. Magnetic measurements in a SQUID magnetometer down to temperatures as low as 1.8 K were performed to several of the products in order to see if the transition metal borides become superconducting at low temperatures, and the results were compared with data from literature. Superconducting properties were found for the following compounds: NbB{sub 2} (T{sub C} = 3.5 K), β-MoB (T{sub C} = 2.4 K), β-WB (T{sub C} = 2.0 K), α-WB (T{sub C} = 4.3 K), W{sub 2}B{sub 4} (T{sub C} = 5.4 K), Re{sub 7}B{sub 3} (T{sub C} = 2.4 K). A relationship between the superconducting properties

Total synthesis, structure, and oral absorption of a thiazole cyclic peptide, sanguinamide A

DEFF Research Database (Denmark)

Nielsen, Daniel S; Hoang, Huy N; Lohman, Rink-Jan

2012-01-01

The first total synthesis and three-dimensional solution structure are reported for sanguinamide A, a thiazole-containing cyclic peptide from the sea slug H. sanguineus. Solution phase fragment synthesis, solid phase fragment assembly, and solution macrocyclization were combined to give (1) in 10......% yield. Spectral properties were identical for the natural product, requiring revision of its structure from (2) to (1). Intramolecular transannular hydrogen bonds help to bury polar atoms, which enables oral absorption from the gut....

Synthesis and structure of bis(β-dibenzoyl methanato -O,O') (aquo-O ...

Indian Academy of Sciences (India)

Synthesis and structure of bis(β-dibenzoyl methanato -O,O') (aquo-O) dioxouranium (VI) compound ... Keywords. β-diketonates; uranyl ion; adduct compound; crystal structure; hydrogen bonding. 1. Introduction. Structural studies on uranyl ... crystalline product obtained was filtered, washed with ether and dried. The crystal ...

The ethylene glycol template assisted hydrothermal synthesis of Co3O4 nanowires; structural characterization and their application as glucose non-enzymatic sensor

International Nuclear Information System (INIS)

Khun, K.; Ibupoto, Z.H.; Liu, X.; Beni, V.; Willander, M.

2015-01-01

Highlights: • Ethylene glycol assisted Co 3 O 4 nanowires were synthesized by hydrothermal method. • The grown Co 3 O 4 nanowires were used for sensitive non-enzymatic glucose sensor. • The proposed glucose sensor shows a wide linear range with fast response. • The Co 3 O 4 modified electrode is a highly specific enzyme-less glucose sensor. - Abstract: In the work reported herein the ethylene glycol template assisted hydrothermal synthesis, onto Au substrate, of thin and highly dense cobalt oxide (Co 3 O 4 ) nanowires and their characterization and their application for non-enzymatic glucose sensing are reported. The structure and composition of Co 3 O 4 nanowires have been fully characterized using scanning electron microscopy, X-ray diffraction, high resolution transmission electron microscopy and X-ray photoelectron spectroscopy. The synthesized Co 3 O 4 nanowires resulted to have high purity and showed diameter of approximately 10 nm. The prepared Co 3 O 4 nanowires coated gold electrodes were applied to the non-enzymatic detection of glucose. The developed sensor showed high sensitivity (4.58 × 10 1 μA mM −1 cm −2 ), a wide linear range of concentration (1.00 × 10 −4 –1.2 × 10 1 mM) and a detection limit of 2.65 × 10 −5 mM. The developed glucose sensor has also shown to be very stable and selective over interferents such as uric acid and ascorbic acid. Furthermore, the proposed fabrication process was shown to be highly reproducible response (over nine electrodes)

The synthesis and characterization of polymer-coated FeAu multifunctional nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Liu Hongling; Hou Peng; Zhang Wengxing [Institute of Molecular and Crystal Engineering, School of Chemistry and Chemical Engineering, Henan University, Kaifeng 475001, Henan (China); Kim, Young Keun [Department of Materials Science and Engineering, Korea University, Seoul 136-713 (Korea, Republic of); Wu Junhua, E-mail: feitianshenhu@yahoo.com [Research Institute of Engineering and Technology, Korea University, Seoul 136-713 (Korea, Republic of)

2010-08-20

We report the one-pot nanoemulsion synthesis of FeAu magnetic-optical multifunctional nanoparticles coated by the biocompatible triblock copolymer, poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol) (PEO-PPO-PEO). The FTIR study confirms the PEO-PPO-PEO molecules on the surface of the resulting nanoparticles. The structural characterization identifies the crystallographic parameter 4.072 A of the cubic phase and the morphology analysis gives the nanoparticle shape, size and size distribution, showing the high crystallinity of the FeAu nanoparticles and an average particle size of {approx} 6.5 nm. In addition there is direct confirmation of the alloying by elemental point probing of an individual nanoparticle. Following the visual demonstration of a rapid, efficient and reversible dispersion-collection process of the nanoparticles in solution, the magnetic measurement manifests a soft ferromagnetic behavior of the nanoparticles with a small coercivity of {approx} 60 Oe at room temperature. The corresponding magnetic hysteresis curves were effectively assessed by modified bi-phase Langevin equations, which were satisfactorily explained in terms of a bimodal particle size distribution. The UV-vis studies display the broadband absorption of the PEO-PPO-PEO-coated nanoparticles with the maximum surface plasmon resonance around 585 nm. The characterization and analysis, therefore, shows the unification of iron and gold into one alloy nanostructure entity covered by the biocompatible triblock copolymer thin film, preserving the optical and magnetic properties of the individual constituents. This gives the prospect of enhanced performance in applications.

The synthesis and characterization of polymer-coated FeAu multifunctional nanoparticles

International Nuclear Information System (INIS)

Liu Hongling; Hou Peng; Zhang Wengxing; Kim, Young Keun; Wu Junhua

2010-01-01

We report the one-pot nanoemulsion synthesis of FeAu magnetic-optical multifunctional nanoparticles coated by the biocompatible triblock copolymer, poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol) (PEO-PPO-PEO). The FTIR study confirms the PEO-PPO-PEO molecules on the surface of the resulting nanoparticles. The structural characterization identifies the crystallographic parameter 4.072 A of the cubic phase and the morphology analysis gives the nanoparticle shape, size and size distribution, showing the high crystallinity of the FeAu nanoparticles and an average particle size of ∼ 6.5 nm. In addition there is direct confirmation of the alloying by elemental point probing of an individual nanoparticle. Following the visual demonstration of a rapid, efficient and reversible dispersion-collection process of the nanoparticles in solution, the magnetic measurement manifests a soft ferromagnetic behavior of the nanoparticles with a small coercivity of ∼ 60 Oe at room temperature. The corresponding magnetic hysteresis curves were effectively assessed by modified bi-phase Langevin equations, which were satisfactorily explained in terms of a bimodal particle size distribution. The UV-vis studies display the broadband absorption of the PEO-PPO-PEO-coated nanoparticles with the maximum surface plasmon resonance around 585 nm. The characterization and analysis, therefore, shows the unification of iron and gold into one alloy nanostructure entity covered by the biocompatible triblock copolymer thin film, preserving the optical and magnetic properties of the individual constituents. This gives the prospect of enhanced performance in applications.

Synthesis and characterization of ZSM-5 and calcined kaolin evaluation using the content of structure-directing