Crystallization of purple nitrous oxide reductase from Pseudomonas stutzeri

International Nuclear Information System (INIS)

Pomowski, Anja; Zumft, Walter G.; Kroneck, Peter M. H.; Einsle, Oliver

2010-01-01

The physiologically active form of nitrous oxide reductase was isolated and crystallized under strict exclusion of dioxygen and diffraction data were collected from crystals belonging to two different space groups. Nitrous oxide reductase (N 2 OR) from Pseudomonas stutzeri catalyzes the final step in denitrification: the two-electron reduction of nitrous oxide to molecular dinitrogen. Crystals of the enzyme were grown under strict exclusion of dioxygen by sitting-drop vapour diffusion using 2R,3R-butanediol as a cryoprotectant. N 2 OR crystallized in either space group P1 or P6 5 . Interestingly, the key determinant for the resulting space group was the crystallization temperature. Crystals belonging to space group P1 contained four 130 kDa dimers in the asymmetric unit, while crystals belonging to space group P6 5 contained a single dimer in the asymmetric unit. Diffraction data were collected to resolutions better than 2 Å

Thermo-electric oxidization of iron in lithium niobate crystals

International Nuclear Information System (INIS)

Falk, Matthias

2007-01-01

Lithium niobate crystals (LiNbO 3 ) are a promising material for nonlinear-optical applications like frequency conversion to generate visible light, e.g., in laser displays, but their achievable output power is greatly limited by the ''optical damage'', i.e., light-induced refractive-index changes caused by excitation of electrons from iron impurities and the subsequent retrapping in unilluminated areas of the crystal. The resulting space-charge fields modify the refractive indices due to the electro-optic effect. By this ''photorefractive effect'' the phase-matching condition, i.e., the avoidance of destructive interference between light generated at different crystal positions due to the dispersion of the fundamental wave and the converted wave, is disturbed critically above a certain light intensity threshold. The influence of annealing treatments conducted in the presence of an externally applied electric field (''thermo-electric oxidization'') on the valence state of iron impurities and thereby on the optical damage is investigated. It is observed that for highly iron-doped LiNbO 3 crystals this treatment leads to a nearly complete oxidization from Fe 2+ to Fe 3+ indicated by the disappearance of the absorption caused by Fe 2+ . During the treatment an absorption front forms that moves through the crystal. The absorption in the visible as well as the electrical conductivity are decreased by up to five orders of magnitude due to this novel treatment. The ratio of the Fe 2+ concentration to the total iron concentration - a measure for the strength of the oxidization - is in the order of 10 -6 for oxidized crystals whereas it is about 10 -1 for untreated samples. Birefringence changes are observed at the absorption front that are explained by the removal of hydrogen and lithium ions from the crystal that compensate for the charges of the also removed electrons from Fe 2+ . A microscopic shock-wave model is developed that explains the observed absorption front by

Low temperature self-assembled growth of rutile TiO2/manganese oxide nanocrystalline films

Science.gov (United States)

Sun, Zhenya; Zhou, Daokun; Du, Jianhua; Xie, Yuxing

2017-10-01

We report formation of rutile TiO2 nanocrystal at low temperature range in the presence of α-MnO2 which self-assembled onto sulfanyl radical activated silicon oxide substrate. SEM, HRTEM, XPS and Raman spectroscopy were used to study the morphology and oxidation state of synthesised crystals. The results showed that when the α-MnO2 was reduced to Mn3O4, it induced the formation of rutile instead of anatase phase in the TiCl4-HCl aqueous system. The finding will promote the understanding of phase transformation mechanism when manganese oxide and titanium oxide co-exist in soil and water environment.

Thermal neutron detectors based on complex oxide crystals

CERN Document Server

Ryzhikov, V; Volkov, V; Chernikov, V; Zelenskaya, O

2002-01-01

The ways of improvement of spectrometric quality of CWO and GSO crystals have been investigated with the aim of their application in thermal neutron detectors based on radiation capture reactions. The efficiency of the neutron detection by these crystals was measured, and the obtained data were compared with the results for sup 6 LiI(Tl) crystals. It is shown that the use of complex oxide crystals and neutron-absorption filters for spectrometry of thermal and resonance neutrons could be a promising method in combination with computer data processing. Numerical calculations are reported for spectra of gamma-quanta due to radiation capture of the neutrons. To compensate for the gamma-background lines, we used a crystal pair of heavy complex oxides with different sensitivity to neutrons.

The Peak Pairs algorithm for strain mapping from HRTEM images

Energy Technology Data Exchange (ETDEWEB)

Galindo, Pedro L. [Departamento de Lenguajes y Sistemas Informaticos, CASEM, Universidad de Cadiz, Pol. Rio San Pedro s/n. 11510, Puerto Real, Cadiz (Spain)], E-mail: pedro.galindo@uca.es; Kret, Slawomir [Institute of Physics, PAS, AL. Lotnikow 32/46, 02-668 Warsaw (Poland); Sanchez, Ana M. [Departamento de Ciencia de los Materiales e Ing. Metalurgica y Q. Inorganica, Facultad de Ciencias, Universidad de Cadiz, Pol. Rio San Pedro s/n. 11510, Puerto Real, Cadiz (Spain); Laval, Jean-Yves [Laboratoire de Physique du Solide, UPR5 CNRS-ESPCI, Paris (France); Yanez, Andres; Pizarro, Joaquin; Guerrero, Elisa [Departamento de Lenguajes y Sistemas Informaticos, CASEM, Universidad de Cadiz, Pol. Rio San Pedro s/n. 11510, Puerto Real, Cadiz (Spain); Ben, Teresa; Molina, Sergio I. [Departamento de Ciencia de los Materiales e Ing. Metalurgica y Q. Inorganica, Facultad de Ciencias, Universidad de Cadiz, Pol. Rio San Pedro s/n. 11510, Puerto Real, Cadiz (Spain)

2007-11-15

Strain mapping is defined as a numerical image-processing technique that measures the local shifts of image details around a crystal defect with respect to the ideal, defect-free, positions in the bulk. Algorithms to map elastic strains from high-resolution transmission electron microscopy (HRTEM) images may be classified into two categories: those based on the detection of peaks of intensity in real space and the Geometric Phase approach, calculated in Fourier space. In this paper, we discuss both categories and propose an alternative real space algorithm (Peak Pairs) based on the detection of pairs of intensity maxima in an affine transformed space dependent on the reference area. In spite of the fact that it is a real space approach, the Peak Pairs algorithm exhibits good behaviour at heavily distorted defect cores, e.g. interfaces and dislocations. Quantitative results are reported from experiments to determine local strain in different types of semiconductor heterostructures.

Controlled synthesis of thorium and uranium oxide nano-crystals

International Nuclear Information System (INIS)

Hudry, Damien; Apostolidis, Christos; Walter, Olaf; Gouder, Thomas; Courtois, Eglantine; Kubel, Christian; Meyer, Daniel

2013-01-01

Very little is known about the size and shape effects on the properties of actinide compounds. As a consequence, the controlled synthesis of well-defined actinide-based nano-crystals constitutes a fundamental step before studying their corresponding properties. In this paper, we report on the non-aqueous surfactant-assisted synthesis of thorium and uranium oxide nano-crystals. The final characteristics of thorium and uranium oxide nano-crystals can be easily tuned by controlling a few experimental parameters such as the nature of the actinide precursor and the composition of the organic system (e.g., the chemical nature of the surfactants and their relative concentrations). Additionally, the influence of these parameters on the outcome of the synthesis is highly dependent on the nature of the actinide element (thorium versus uranium). By using optimised experimental conditions, monodisperse isotropic uranium oxide nano-crystals with different sizes (4.5 and 10.7 nm) as well as branched nano-crystals (overall size ca. 5 nm), nano-dots (ca. 4 nm) and nano-rods (with ultra-small diameters of 1 nm) of thorium oxide were synthesised. (authors)

HRTEM investigation of orthorhombic phase in Mg-PSZ

International Nuclear Information System (INIS)

Liu, Z.W.; Spargo, A.E.C.; Hannink, R.H.J.

1997-01-01

Tetragonal, orthorhombic and monoclinic phases are only slight distortions of the cubic structure. Due to minor differences in unit cell parameters it is difficult to distinguish these phases only by high resolution images. However, using high resolution transmission electron microscopy (HRTEM) observation in combination with image simulation and digital Fourier transformation of HRTEM images, it was found that one tetragonal precipitate can be transformed to several orthorhombic domains with different orientations in MgO-partially-stabilized zirconia (Mg-PSZ). The lattice correspondence between two adjacent orthorhombic domains is such that their b axes are parallel, while their a axes are perpendicular to each other. Also it was found that cubic ZrO 2 could be transformed to orthorhombic ZrO 2 . 8 refs., 1 tab., 4 figs

Zinc Oxide Nano crystals Synthesized by Quenching Technique

International Nuclear Information System (INIS)

Norhayati Abu Bakar; Akrajas Ali Umar; Muhamad Mat Salleh; Muhammad Yahya

2011-01-01

This paper reports an attempt to synthesize non toxic zinc oxide (ZnO) nano crystals using a simple quenching technique. The hot zinc oxide powder was quenched in hexane solution to obtain ZnO nano crystals. As the result, diameter size of the synthesized ZnO is 200 nm. It was also exhibited a good crystalline with wurtzite phase. The nano crystals properties of ZnO were revealed from good absorbance and green luminescence under UV exposure. This may be related with oxygen vacancy ionization during the annealing process. (author)

Revealing the nanostructure of calcium phosphate coatings using HRTEM/FIB techniques

International Nuclear Information System (INIS)

Solla, E.L.; Rodríguez-González, B.; Aguiar, H.; Rodríguez-Valencia, C.; Serra, J.; González, P.

2016-01-01

Herein, we report on the micro- and nanostructure of the calcium phosphate coating produced by pulsed laser deposition (PLD), using focused ion beam (FIB) lamella sample preparation and transmission electron microscopy (TEM) as the characterization technique. The initial selected area electron diffraction (SAED) data demonstrated the presence of hydroxyapatite (HA) over any other possible calcium phosphate crystalline structure and the polycrystalline nature of the coating. Moreover, the SAED analyses showed clear textured ring patterns coherent with the presence of a preferred orientation in the HA nano-crystal growth. The SAED data also indicated that the coating appears to be textured in the 〈002〉 crystalline direction. Dark-field images obtained using 002 as the working reflection showed a clear oriented crystal growth in columns, from bottom to top. These columns have a peculiar arrangement of nano-crystals since, in some cases, the preferred orientation appears to start at a certain distance from the substrate. Direct d-spacing measurements on high-resolution TEM images provided further proof of the presence of an HA nano-crystal structure. The reported data may be of interest in the future to adjust the microstructure of the HA coatings. - Highlights: •The FIB lift-out technique allows a very site-specific sample preparation method for HRTEM analysis. •It also permits a fast assessment of the HA coating thickness and elemental composition (EDS). •The coatings exhibit a nano-crystalline nature, with a texturing effect along the 002 planes. •PLD is suitable for the production of crystalline c-axis oriented hydroxyapatite coatings. •The crystalline HA phase in the PLD coating is very similar to the present in bone.

Revealing the nanostructure of calcium phosphate coatings using HRTEM/FIB techniques

Energy Technology Data Exchange (ETDEWEB)

Solla, E.L., E-mail: esolla@uvigo.es [Servicio de Microscopía Electrónica, CACTI, University of Vigo, Campus As Lagoas-Marcosende, 36310 Vigo (Spain); Rodríguez-González, B. [Servicio de Microscopía Electrónica, CACTI, University of Vigo, Campus As Lagoas-Marcosende, 36310 Vigo (Spain); Aguiar, H.; Rodríguez-Valencia, C.; Serra, J.; González, P. [Applied Physics Department, School of Industrial Engineering, University of Vigo, Campus As Lagoas-Marcosende, 36310 Vigo (Spain)

2016-12-15

Herein, we report on the micro- and nanostructure of the calcium phosphate coating produced by pulsed laser deposition (PLD), using focused ion beam (FIB) lamella sample preparation and transmission electron microscopy (TEM) as the characterization technique. The initial selected area electron diffraction (SAED) data demonstrated the presence of hydroxyapatite (HA) over any other possible calcium phosphate crystalline structure and the polycrystalline nature of the coating. Moreover, the SAED analyses showed clear textured ring patterns coherent with the presence of a preferred orientation in the HA nano-crystal growth. The SAED data also indicated that the coating appears to be textured in the 〈002〉 crystalline direction. Dark-field images obtained using 002 as the working reflection showed a clear oriented crystal growth in columns, from bottom to top. These columns have a peculiar arrangement of nano-crystals since, in some cases, the preferred orientation appears to start at a certain distance from the substrate. Direct d-spacing measurements on high-resolution TEM images provided further proof of the presence of an HA nano-crystal structure. The reported data may be of interest in the future to adjust the microstructure of the HA coatings. - Highlights: •The FIB lift-out technique allows a very site-specific sample preparation method for HRTEM analysis. •It also permits a fast assessment of the HA coating thickness and elemental composition (EDS). •The coatings exhibit a nano-crystalline nature, with a texturing effect along the 002 planes. •PLD is suitable for the production of crystalline c-axis oriented hydroxyapatite coatings. •The crystalline HA phase in the PLD coating is very similar to the present in bone.

Covalent modification and exfoliation of graphene oxide using ferrocene

Science.gov (United States)

Avinash, M. B.; Subrahmanyam, K. S.; Sundarayya, Y.; Govindaraju, T.

2010-09-01

Large scale preparation of single-layer graphene and graphene oxide is of great importance due to their potential applications. We report a simple room temperature method for the exfoliation of graphene oxide using covalent modification of graphene oxide with ferrocene to obtain single-layer graphene oxide sheets. The samples were characterized by FESEM, HRTEM, AFM, EDAX, FT-IR, Raman and Mössbauer spectroscopic studies. HRTEM micrograph of the covalently modified graphene oxide showed increased interlayer spacing of ~2.4 nm due to ferrocene intercalation. The presence of single-layer graphene oxide sheets were confirmed by AFM studies. The covalently modified ferrocene-graphene oxide composite showed interesting magnetic behavior.Large scale preparation of single-layer graphene and graphene oxide is of great importance due to their potential applications. We report a simple room temperature method for the exfoliation of graphene oxide using covalent modification of graphene oxide with ferrocene to obtain single-layer graphene oxide sheets. The samples were characterized by FESEM, HRTEM, AFM, EDAX, FT-IR, Raman and Mössbauer spectroscopic studies. HRTEM micrograph of the covalently modified graphene oxide showed increased interlayer spacing of ~2.4 nm due to ferrocene intercalation. The presence of single-layer graphene oxide sheets were confirmed by AFM studies. The covalently modified ferrocene-graphene oxide composite showed interesting magnetic behavior. Electronic supplementary information (ESI) available: Magnetic data; AFM images; TEM micrographs; and Mössbauer spectroscopic data. See DOI: 10.1039/c0nr00024h

Crystallization dynamics in glass-forming systems

Energy Technology Data Exchange (ETDEWEB)

Cullinan, Timothy Edward [Iowa State Univ., Ames, IA (United States)

2016-02-19

Crystallization under far-from-equilibrium conditions is investigated for two different scenarios: crystallization of the metallic glass alloy Cu₅₀Zr₅₀ and solidification of a transparent organic compound, o-terphenyl. For Cu₅₀Zr₅₀, crystallization kinetics are quanti ed through a new procedure that directly fits thermal analysis data to the commonly utilized JMAK model. The phase evolution during crystallization is quantified through in-situ measurements (HEXRD, DSC) and ex-situ microstructural analysis (TEM, HRTEM). The influence of chemical partitioning, diffusion, and crystallographic orientation on this sequence are examined. For o-terphenyl, the relationship between crystal growth velocity and interface undercooling is systematically studied via directional solidification.

Influence of total beam current on HRTEM image resolution in differentially pumped ETEM with nitrogen gas.

Science.gov (United States)

Bright, A N; Yoshida, K; Tanaka, N

2013-01-01

Environmental transmission electron microscopy (ETEM) enables the study of catalytic and other reaction processes as they occur with Angstrom-level resolution. The microscope used is a dedicated ETEM (Titan ETEM, FEI Company) with a differential pumping vacuum system and apertures, allowing aberration corrected high-resolution transmission electron microscopy (HRTEM) imaging to be performed with gas pressures up to 20 mbar in the sample area and with significant advantages over membrane-type E-cell holders. The effect on image resolution of varying the nitrogen gas pressure, electron beam current density and total beam current were measured using information limit (Young's fringes) on a standard cross grating sample and from silicon crystal lattice imaging. As expected, increasing gas pressure causes a decrease in HRTEM image resolution. However, the total electron beam current also causes big changes in the image resolution (lower beam current giving better resolution), whereas varying the beam current density has almost no effect on resolution, a result that has not been reported previously. This behavior is seen even with zero-loss filtered imaging, which we believe shows that the drop in resolution is caused by elastic scattering at gas ions created by the incident electron beam. Suitable conditions for acquiring high resolution images in a gas environment are discussed. Lattice images at nitrogen pressures up to 16 mbar are shown, with 0.12 nm information transfer at 4 mbar. Copyright © 2012 Elsevier B.V. All rights reserved.

Photocatalytic mechanism of high-activity anatase TiO2 with exposed (001) facets from molecular-atomic scale: HRTEM and Raman studies

Science.gov (United States)

Wu, Jun; Shi, Chentian; Zhang, Yupeng; Fu, Qiang; Pan, Chunxu

2017-12-01

Anatase TiO2 with a variant percentage of exposed (001) facets was prepared under hydrothermal processes by adjusting the volume of HF, and the photocatalytic mechanism was studied from atomic-molecular scale by HRTEM and Raman spectroscopy. It was revealed that: 1) From HRTEM observations, the surface of original TiO2 with exposed (001) facets was clean without impurity, and the crystal lattice was clear and completed; however, when mixed with methylene blue (MB) solution, there were many 1 nm molecular absorbed at the surface of TiO2; after the photocatalytic experiment, MB molecules disappeared and the TiO2 lattice image became fuzzy. 2) The broken path of the MB chemical bond was obtained by Raman spectroscopy, i.e., after the irradiation of the light, the vibrational mode of C-N-C disappeared due to the chemical bond breakage, and the groups containing C-N bond and carbon rings were gradually decomposed. Accordingly, we propose that the driving force for breaking the chemical bond and the disappearance of groups is from the surface lattice distortion of TiO2 during photocatalyzation.

Diagenetic Microcrystalline Opal Varieties from the Monterey Formation, CA: HRTEM Study of Structures and Phase Transformation Mechanisms

Science.gov (United States)

Cady, Sherry L.; Wenk, H.-R.; DeVincenzi, Don (Technical Monitor)

1994-01-01

Microcrystalline opal varieties form as intermediary precipitates during the diagenetic transformation of biogenically precipitated non-crystalline opal (opal-A) to microquartz. With regard to the Monterey Formation of California, X-ray powder diffraction studies have shown that a decrease in the primary d-spacing of opal-CT toward that of cristobalite occurs with increasing diagenesis. The initial timing of opal-CT/quartz formation and the value of the primary opal-CT d-spacing, are influenced by the sediment. lithology. Transmission electron microscopy methods (CTEM/HRTEM) were used to investigate the structure of the diagenetic phases and establish transformation mechanisms between the varieties of microcrystalline opals in charts and porcelanites from the Monterey Formation. HRTEM images revealed that the most common fibrous varieties of microcrystalline opals contain varying amounts of structural disorder. Finite lamellar units of cristobalite-and tridymite-type. layer sequences were found to be randomly stacked in a direction perpendicular to the fiber axis. Disordered and ordered fibers were found to have coprecipitated within the same radial fiber bundles that formed within the matrix of the Most siliceous samples. HRTEM images, which reveal that the fibers within radial and lepispheric fiber bundles branch non-crystallographically, support an earlier proposal that microspheres in chert grow via a spherulitic growth mechanism. A less common variety of opal-CT was found to be characterized by non-parallel (low-angle) stacking sequences that often contain twinned lamellae. Tabular-shaped crystals of orthorhombic tridymite (PO-2) were also identified in the porcelanite samples. A shift in the primary d-spacing of opal-CT has been interpreted as an indication of solid-state ordering g toward a predominantly cristobalite structure, (opal-C). Domains of opal-C were identified as topotactically-oriented overgrowths on discrete Sections of opal-CT fibers and as

Unveiling the chemical and morphological features of Sb:SnO2 nanocrystals by the combined use of HRTEM and Ab Initio surface energy calculations

International Nuclear Information System (INIS)

Stroppa, Daniel G.; Montoro, Luciano A.; Ramirez, Antonio J.; Beltran, Armando; Andres, Juan; Conti, Tiago G.; Silva, Rafael O. da; Longo, Elson; Leite, Edson R.

2009-01-01

Modeling of nanocrystals supported by advanced morphological and chemical characterization is a unique tool for the development of reliable nanostructured devices, which depends on the ability to synthesize and characterize material on the atomic scale. Among the most significant challenges in nanostructural characterization is the evaluation of crystal growth mechanisms and their dependence on the shape of nanoparticles and the distribution of doping elements. This work presents a new strategy to characterize nanocrystals, applied here to antimony-doped tin oxide (Sb-SnO 2 ) (ATO) by the combined use of experimental and simulated high-resolution transmission electron microscopy (HRTEM) images and surface energy ab initio calculations. The results show that the Wulff construction can not only describe the shape of nanocrystals as a function of surface energy distribution but also retrieve quantitative information on dopant distribution by the dimensional analysis of nanoparticle shapes. In addition, a novel three-dimensional evaluation of an oriented attachment growth mechanism is provided in the proposed methodology. This procedure is a useful approach for faceted nanocrystal shape modeling and indirect quantitative evaluation of dopant spatial distribution, which are difficult to evaluate by other techniques. (author)

N-Oxide-N-oxide interactions and Cl...Cl halogen bonds in pentachloropyridine N-oxide: the many-body approach to interactions in the crystal state.

Science.gov (United States)

Wzgarda-Raj, Kinga; Rybarczyk-Pirek, Agnieszka J; Wojtulewski, Sławomir; Palusiak, Marcin

2018-02-01

Pentachloropyridine N-oxide, C 5 Cl 5 NO, crystallizes in the monoclinic space group P2 1 /c. In the crystal structure, molecules are linked by C-Cl...Cl halogen bonds into infinite ribbons extending along the crystallographic [100] direction. These molecular aggregates are further stabilized by very short intermolecular N-oxide-N-oxide interactions into herringbone motifs. Computations based on quantum chemistry methods allowed for a more detailed description of the N-oxide-N-oxide interactions and Cl...Cl halogen bonds. For this purpose, Hirshfeld surface analysis and the many-body approach to interaction energy were applied.

On the influence of the electron dose rate on the HRTEM image contrast

Energy Technology Data Exchange (ETDEWEB)

Barthel, Juri, E-mail: ju.barthel@fz-juelich.de [RWTH Aachen University, Ahornstraße 55, 52074 Aachen (Germany); Ernst Ruska-Centre for Microscopy and Spectroscopy with Electrons, Forschungszentrum Jülich GmbH, 52425 Jülich (Germany); Lentzen, Markus; Thust, Andreas [Peter Grünberg Institute, Forschungszentrum Jülich GmbH, 52425 Jülich (Germany); Ernst Ruska-Centre for Microscopy and Spectroscopy with Electrons, Forschungszentrum Jülich GmbH, 52425 Jülich (Germany)

2017-05-15

We investigate a possible dependence between the applied electron dose-rate and the magnitude of the resulting image contrast in HRTEM of inorganic crystalline objects. The present study is focussed on the question whether electron irradiation can induce excessively strong atom vibrations or displacements, which in turn could significantly reduce the resulting image contrast. For this purpose, high-resolution images of MgO, Ge, and Au samples were acquired with varying dose rates using a C{sub S}-corrected FEI Titan 80–300 microscope operated at 300 kV accelerating voltage. This investigation shows that the magnitude of the signal contrast is independent from the dose rates occurring in conventional HRTEM experiments and that excessively strong vibrations or displacements of bulk atoms are not induced by the applied electron irradiation. - Highlights: • No dependence between electron dose rate and HRTEM image contrast is found. • This finding is in full accordance with established solid-state physics theory. • Object-related causes for the previous Stobbs-factor phenomenon are ruled out.

Oxide nano crystals for in vivo imaging

International Nuclear Information System (INIS)

Heinrich, E.

2005-01-01

For small animal, fluorescence imaging is complementary with other techniques such as nuclear imaging (PET, SPECT). In vivo imaging studies imply the development of new luminescent probes, with a better sensitivity and a better biological targeting. These markers must filled biological and optical conditions. Our goal is to study new doped lanthanides oxide nano-crystals, their properties, their functionalization and their ability to target biological molecules. Characterizations of Y 2 O 3 :Eu and Y 2 SiO 5 :Eu nano-crystals (light diffusion, spectrometry, microscopy) allowed the determination of their size, their fluorescence properties but also their photo-bleaching. Means of stabilization of the nanoparticles were also studied in order to decrease their aggregation. Gd 2 O 3 :Eu nano-crystals were as well excited by X rays. Nano-crystals of Y 2 SiO 5 :Eu were functionalized, and organic ligands grafting evidenced by fluorescence and NMR. The functionalized nano-crystals could then recognized biological targets (streptavidin-biotin) and be incubated in the presence of HeLa cells. This report deals with the properties of these nano-crystals and their ability to meet the optical and biological conditions required for the application of in vivo imaging. (author)

Unique Crystal Orientation of Poly(ethylene oxide) Thin Films by Crystallization Using a Thermal Gradient

DEFF Research Database (Denmark)

Gbabode, Gabin; Delvaux, Maxime; Schweicher, Guillaume

2017-01-01

Poly(ethylene oxide), (PEO), thin films of different thicknesses (220, 450, and 1500 nm) and molecular masses (4000, 8000, and 20000 g/mol) have been fabricated by spin-coating of methanol solutions onto glass substrates. All these samples have been recrystallized from the melt using a directional......, to significantly decrease the distribution of crystal orientation obtained after crystallization using the thermal gradient technique....

Statistical analysis of support thickness and particle size effects in HRTEM imaging of metal nanoparticles

International Nuclear Information System (INIS)

House, Stephen D.; Bonifacio, Cecile S.; Grieshaber, Ross V.; Li, Long; Zhang, Zhongfan; Ciston, Jim; Stach, Eric A.; Yang, Judith C.

2016-01-01

High-resolution transmission electron microscopy (HRTEM) examination of nanoparticles requires their placement on some manner of support – either TEM grid membranes or part of the material itself, as in many heterogeneous catalyst systems – but a systematic quantification of the practical imaging limits of this approach has been lacking. Here we address this issue through a statistical evaluation of how nanoparticle size and substrate thickness affects the ability to resolve structural features of interest in HRTEM images of metallic nanoparticles on common support membranes. The visibility of lattice fringes from crystalline Au nanoparticles on amorphous carbon and silicon supports of varying thickness was investigated with both conventional and aberration-corrected TEM. Over the 1–4 nm nanoparticle size range examined, the probability of successfully resolving lattice fringes differed significantly as a function both of nanoparticle size and support thickness. Statistical analysis was used to formulate guidelines for the selection of supports and to quantify the impact a given support would have on HRTEM imaging of crystalline structure. For nanoparticles ≥1 nm, aberration-correction was found to provide limited benefit for the purpose of visualizing lattice fringes; electron dose is more predictive of lattice fringe visibility than aberration correction. These results confirm that the ability to visualize lattice fringes is ultimately dependent on the signal-to-noise ratio of the HRTEM images, rather than the point-to-point resolving power of the microscope. This study provides a benchmark for HRTEM imaging of crystalline supported metal nanoparticles and is extensible to a wide variety of supports and nanostructures. - Highlights: • The impact of supports on imaging nanoparticle lattice structure is quantified. • Visualization probabilities given particle size and support thickness are estimated. • Aberration-correction provided limited benefit

Statistical analysis of support thickness and particle size effects in HRTEM imaging of metal nanoparticles

Energy Technology Data Exchange (ETDEWEB)

House, Stephen D., E-mail: sdh46@pitt.edu [Chemical and Petroleum Engineering, and Physics, University of Pittsburgh, Pittsburgh, PA 15261 (United States); Bonifacio, Cecile S.; Grieshaber, Ross V.; Li, Long; Zhang, Zhongfan [Chemical and Petroleum Engineering, and Physics, University of Pittsburgh, Pittsburgh, PA 15261 (United States); Ciston, Jim [National Center of Electron Microscopy, Molecular Foundry, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Stach, Eric A. [Center for Functional Nanomaterials, Brookhaven National Laboratory, Upton, NY 11973 (United States); Yang, Judith C. [Chemical and Petroleum Engineering, and Physics, University of Pittsburgh, Pittsburgh, PA 15261 (United States)

2016-10-15

High-resolution transmission electron microscopy (HRTEM) examination of nanoparticles requires their placement on some manner of support – either TEM grid membranes or part of the material itself, as in many heterogeneous catalyst systems – but a systematic quantification of the practical imaging limits of this approach has been lacking. Here we address this issue through a statistical evaluation of how nanoparticle size and substrate thickness affects the ability to resolve structural features of interest in HRTEM images of metallic nanoparticles on common support membranes. The visibility of lattice fringes from crystalline Au nanoparticles on amorphous carbon and silicon supports of varying thickness was investigated with both conventional and aberration-corrected TEM. Over the 1–4 nm nanoparticle size range examined, the probability of successfully resolving lattice fringes differed significantly as a function both of nanoparticle size and support thickness. Statistical analysis was used to formulate guidelines for the selection of supports and to quantify the impact a given support would have on HRTEM imaging of crystalline structure. For nanoparticles ≥1 nm, aberration-correction was found to provide limited benefit for the purpose of visualizing lattice fringes; electron dose is more predictive of lattice fringe visibility than aberration correction. These results confirm that the ability to visualize lattice fringes is ultimately dependent on the signal-to-noise ratio of the HRTEM images, rather than the point-to-point resolving power of the microscope. This study provides a benchmark for HRTEM imaging of crystalline supported metal nanoparticles and is extensible to a wide variety of supports and nanostructures. - Highlights: • The impact of supports on imaging nanoparticle lattice structure is quantified. • Visualization probabilities given particle size and support thickness are estimated. • Aberration-correction provided limited benefit

Eliminating Crystals in Non-Oxide Optical Fiber Preforms and Optical Fibers

Science.gov (United States)

Tucker, Dennis S.; LaPointe, Michael R.

2012-01-01

Non ]oxide fiber optics such as heavy metal fluoride and chalcogenide glasses are extensively used in infrared transmitting applications such as communication systems, chemical sensors, and laser fiber guides for cutting, welding and medical surgery. The addition of rare earths such as erbium, enable these materials to be used as fiber laser and amplifiers. Some of these glasses however are very susceptible to crystallization. Even small crystals can lead to light scatter and a high attenuation coefficient, limiting their usefulness. Previously two research teams found that microgravity suppressed crystallization in heavy metal fluoride glasses. Looking for a less expensive method to suppress crystallization, ground based research was performed utilizing an axial magnetic field. The experiments revealed identical results to those obtained via microgravity processing. This research then led to a patented process for eliminating crystals in optical fiber preforms and the resulting optical fibers. In this paper, the microgravity results will be reviewed as well as patents and papers relating to the use of magnetic fields in various material and glass processing applications. Finally our patent to eliminate crystals in non ]oxide glasses utilizing a magnetic field will be detailed.

The thickness of native oxides on aluminum alloys and single crystals

Energy Technology Data Exchange (ETDEWEB)

Evertsson, J., E-mail: jonas.evertsson@sljus.lu.se [Division of Synchrotron Radiation Research, Lund University, Box 118, 221 00 Lund (Sweden); Bertram, F. [Division of Synchrotron Radiation Research, Lund University, Box 118, 221 00 Lund (Sweden); Zhang, F. [KTH Royal Institute of Technology, Department of Chemistry, Division of Surface and Corrosion Science, Drottning Kristinas Vg 51, 100 44 Stockholm (Sweden); Rullik, L.; Merte, L.R.; Shipilin, M. [Division of Synchrotron Radiation Research, Lund University, Box 118, 221 00 Lund (Sweden); Soldemo, M.; Ahmadi, S. [KTH Royal Institute of Technology, ICT, Material Physics, 16440 Kista (Sweden); Vinogradov, N.; Carlà, F. [ESRF, B.P. 220, 38043 Grenoble (France); Weissenrieder, J.; Göthelid, M. [KTH Royal Institute of Technology, ICT, Material Physics, 16440 Kista (Sweden); Pan, J. [KTH Royal Institute of Technology, Department of Chemistry, Division of Surface and Corrosion Science, Drottning Kristinas Vg 51, 100 44 Stockholm (Sweden); Mikkelsen, A. [Division of Synchrotron Radiation Research, Lund University, Box 118, 221 00 Lund (Sweden); Nilsson, J.-O. [Sapa Technology, Kanalgatan 1, 612 31 Finspång (Sweden); Lundgren, E. [Division of Synchrotron Radiation Research, Lund University, Box 118, 221 00 Lund (Sweden)

2015-09-15

Highlights: • We have determined the native oxide film thickness on several Al samples. • The results obtained from XRR and XPS show excellent agreement. • The results obtained from EIS show consistently thinner oxide films. • The oxides on the alloys are thicker than the oxides on the single crystals. - Abstract: We present results from measurements of the native oxide film thickness on four different industrial aluminum alloys and three different aluminum single crystals. The thicknesses were determined using X-ray reflectivity, X-ray photoelectron spectroscopy, and electrochemical impedance spectroscopy. In addition, atomic force microscopy was used for micro-structural studies of the oxide surfaces. The reflectivity measurements were performed in ultra-high vacuum, vacuum, ambient, nitrogen and liquid water conditions. The results obtained using X-ray reflectivity and X-ray photoelectron spectroscopy demonstrate good agreement. However, the oxide thicknesses determined from the electrochemical impedance spectroscopy show a larger discrepancy from the above two methods. In the present contribution the reasons for this discrepancy are discussed. We also address the effect of the substrate type and the presence of water on the resultant oxide thickness.

Oxidation kinetics of crystal violet by potassium permanganate in acidic medium

Science.gov (United States)

Khan, Sameera Razi; Ashfaq, Maria; Mubashir; Masood, Summyia

2016-05-01

The oxidation kinetics of crystal violet (a triphenylmethane dye) by potassium permanganate was focused in an acidic medium by the spectrophotometric method at 584 nm. The oxidation reaction of crystal violet by potassium permanganate is carried out in an acidic medium at different temperatures ranging within 298-318 K. The kinetic study was carried out to investigate the effect of the concentration, ionic strength and temperature. The reaction followed first order kinetics with respect to potassium permanganate and crystal violet and the overall rate of the reaction was found to be second order. Thermodynamic activation parameters like the activation energy ( E a), enthalpy change (Δ H*), free energy change (Δ G*), and entropy change (Δ S*) have also been evaluated.

Synthesis of boron nitride nanotubes by an oxide-assisted chemical method

International Nuclear Information System (INIS)

Singhal, S. K.; Srivastava, A. K.; Gupta, Anil K.; Chen, Z. G.

2010-01-01

We report a new method for the synthesis of boron nitride (BN) nanotubes employing a two-step process in which some oxides have found to catalyze the growth of BN nanotubes. In the first step, a precursor containing B-N-O-Fe/Mg was prepared by ball milling a mixture of B, B 2 O 3 , Fe 2 O 3 and MgO (1:7:2:1 mass ratio) in NH 3 for 3 h. BN nanotubes (diameter: 20-100 nm) were grown in the second step from this precursor by isothermal annealing at 1,350 o C in NH 3 for about 4 h. XRD, SEM and HR-TEM studies elucidated the spindle-like morphology of these nanotubes of hexagonal crystal structure. The Raman spectrum showed the peak broadening and shifts to higher frequency. The present method showed that some oxides assisted the growth of BN nanotubes. A possible reaction mechanism on the formation of BN nanotubes in the presence of these oxides is discussed.

Numerical correction of anti-symmetric aberrations in single HRTEM images of weakly scattering 2D-objects

International Nuclear Information System (INIS)

Lehtinen, Ossi; Geiger, Dorin; Lee, Zhongbo; Whitwick, Michael Brian; Chen, Ming-Wei; Kis, Andras; Kaiser, Ute

2015-01-01

Here, we present a numerical post-processing method for removing the effect of anti-symmetric residual aberrations in high-resolution transmission electron microscopy (HRTEM) images of weakly scattering 2D-objects. The method is based on applying the same aberrations with the opposite phase to the Fourier transform of the recorded image intensity and subsequently inverting the Fourier transform. We present the theoretical justification of the method, and its verification based on simulated images in the case of low-order anti-symmetric aberrations. Ultimately the method is applied to experimental hardware aberration-corrected HRTEM images of single-layer graphene and MoSe 2 resulting in images with strongly reduced residual low-order aberrations, and consequently improved interpretability. Alternatively, this method can be used to estimate by trial and error the residual anti-symmetric aberrations in HRTEM images of weakly scattering objects

Multislice simulations for in-situ HRTEM studies of nanostructured magnesium hydride at ambient hydrogen pressure

International Nuclear Information System (INIS)

Surrey, Alexander; Schultz, Ludwig; Rellinghaus, Bernd

2017-01-01

Highlights: • Multislice HRTEM contrast simulations of a windowed environmental cell. • Study of Mg and MgH2 nanocrystals as model system in hydrogen at ambient pressure. • Investigation of spatial resolution and contrast depending on specimen thickness, defocus, and hydrogen pressure. • Atomic resolution is expected for specimens as thin as 5  nm. - Abstract: The use of transmission electron microscopy (TEM) for the structural characterization of many nanostructured hydrides, which are relevant for solid state hydrogen storage, is hindered due to a rapid decomposition of the specimen upon irradiation with the electron beam. Environmental TEM allows to stabilize the hydrides by applying a hydrogen back pressure of up to 4.5 bar in a windowed environmental cell. The feasibility of high-resolution TEM (HRTEM) investigations of light weight metals and metal hydrides in such a “nanoreactor” is studied theoretically by means of multislice HRTEM contrast simulations using Mg and its hydride phase, MgH_2, as model system. Such a setup provides the general opportunity to study dehydrogenation and hydrogenation reactions at the nanoscale under technological application conditions. We analyze the dependence of both the spatial resolution and the HRTEM image contrast on parameters such as the defocus, the metal/hydride thickness, and the hydrogen pressure in order to explore the possibilities and limitations of in-situ experiments with windowed environmental cells. Such simulations may be highly valuable to pre-evaluate future experimental studies.

Multislice simulations for in-situ HRTEM studies of nanostructured magnesium hydride at ambient hydrogen pressure

Energy Technology Data Exchange (ETDEWEB)

Surrey, Alexander, E-mail: a.surrey@ifw-dresden.de [IFW Dresden, Institute for Metallic Materials, P.O. Box 270116, D-01171 Dresden (Germany); Institut für Festkörperphysik, Technische Universität Dresden, D-01062 Dresden (Germany); Schultz, Ludwig [IFW Dresden, Institute for Metallic Materials, P.O. Box 270116, D-01171 Dresden (Germany); Institut für Festkörperphysik, Technische Universität Dresden, D-01062 Dresden (Germany); Rellinghaus, Bernd, E-mail: b.rellinghaus@ifw-dresden.de [IFW Dresden, Institute for Metallic Materials, P.O. Box 270116, D-01171 Dresden (Germany)

2017-04-15

Highlights: • Multislice HRTEM contrast simulations of a windowed environmental cell. • Study of Mg and MgH2 nanocrystals as model system in hydrogen at ambient pressure. • Investigation of spatial resolution and contrast depending on specimen thickness, defocus, and hydrogen pressure. • Atomic resolution is expected for specimens as thin as 5  nm. - Abstract: The use of transmission electron microscopy (TEM) for the structural characterization of many nanostructured hydrides, which are relevant for solid state hydrogen storage, is hindered due to a rapid decomposition of the specimen upon irradiation with the electron beam. Environmental TEM allows to stabilize the hydrides by applying a hydrogen back pressure of up to 4.5 bar in a windowed environmental cell. The feasibility of high-resolution TEM (HRTEM) investigations of light weight metals and metal hydrides in such a “nanoreactor” is studied theoretically by means of multislice HRTEM contrast simulations using Mg and its hydride phase, MgH{sub 2}, as model system. Such a setup provides the general opportunity to study dehydrogenation and hydrogenation reactions at the nanoscale under technological application conditions. We analyze the dependence of both the spatial resolution and the HRTEM image contrast on parameters such as the defocus, the metal/hydride thickness, and the hydrogen pressure in order to explore the possibilities and limitations of in-situ experiments with windowed environmental cells. Such simulations may be highly valuable to pre-evaluate future experimental studies.

Crystal size effect on the electrochemical oxidation of formate on carbon-supported palladium nanoparticles

International Nuclear Information System (INIS)

Santos, Rayana Marcela Izidoro da Silva; Nakazato, Roberto Zenhei; Ciapina, Eduardo Goncalves

2016-01-01

Full text: The electrochemical oxidation of formate in alkaline electrolytes has emerged an a promising anodic reaction in the Direct Formate Fuel Cells[1]. Although palladium is considered to be one of the best electro catalyst for the oxidation of formate, important structure-activity relationships are still not understood. In the present work, we investigated the effect of the size of the palladium crystals in the electrochemical oxidation of formate in 0.1 mol L -1 KOH. Carbon-supported palladium nanoparticles (Pd/C) were prepared by chemical reduction of palladium (II) chloride in aqueous media by sodium borohydride in the presence of varying quantities of sodium citrate in the reaction media to obtain metallic crystals with distinct sizes. Analysis of the X-ray diffraction profile revealed the presence of palladium crystals in the range of 6 to 19 nm. Potentiostatic oxidation of formate on the distinct Pd/C samples revealed a volcano-like dependence of the specific activity with the size of the palladium crystals, presenting the highest activity for crystals around 7.5 nm. Reference: [1] A.M. Bartrom, J.L. Haan, The direct formate fuel cell with an alkaline anion exchange membrane, J. Power Sources. 214 (2012) 68-74. (author)

The sorption of silver by poorly crystallized manganese oxides

Science.gov (United States)

Anderson, B.J.; Jenne, E.A.; Chao, T.T.

1973-01-01

The sorption of silver by poorly crystallized manganese oxides was studied using synthesized samples of three members of the manganous manganite (birnessite) group, of different chemical composition and crystallinity, and a poorly organized ??-MnO2. All four oxides sorbed significant quantities of silver. The manganous manganites showed the greatest sorption (up to 0.5 moles silver/mole MnOx at pH 7) while the ??-MnO2 showed the least (0.3 moles silver/ mole MnOx at pH 7). Sorption of silver was adequately described by the Langmuir equation over a considerable concentration range. The relationship failed at low pH values and high equilibrium silver concentrations. The sorption capacity showed a direct relationship with pH. However, the rate of increase of sorption capacity decreased at the higher pH values. Silver sorption maxima. were not directly related to surface area but appeared to vary with the amount of occluded sodium and potassium present in the manganese oxide. The important processes involved in the uptake of silver by the four poorly crystallized manganese oxides ara considered to be surface exchange for manganese, potassium and sodium as well as exchange for structural manganese, potassium and sodium. ?? 1973.

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

International Nuclear Information System (INIS)

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

2012-01-01

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

Synthesis and crystal kinetics of cerium oxide nanocrystallites prepared by co-precipitation process

International Nuclear Information System (INIS)

Shih, C.J.; Chen, Y.J.; Hon, M.H.

2010-01-01

Cerium oxide nanocrystallites were synthesized at a relatively low temperature using cerium nitrate as starting materials in a water solution by a co-precipitation process. Effect of calcination temperature on the crystallite growth of cerium oxide nano-powders was investigated by X-ray diffraction, transmission electron microscopy and electron diffraction. The crystallization temperature of the cerium oxide powders was estimated to be about 273 K by XRD analysis. When calcined from 473 to 1273 K, the crystallization of the face-centered cubic phase was observed by XRD. The crystallite size of the cerium oxide increased from 10.0 to 43.8 nm with calcining temperature increasing from 673 to 1273 K. The activation energy for growth of cerium oxide nanoparticles was found to be 16.0 kJ mol -1 .

Synthesis and crystal kinetics of cerium oxide nanocrystallites prepared by co-precipitation process

Energy Technology Data Exchange (ETDEWEB)

Shih, C.J., E-mail: cjshih@kmu.edu.tw [Department of Fragrance and Cosmetics Science, Kaohsiung Medical University, 100 Shi-Chuan 1st Road, Kaohsiung 807, Taiwan (China); Chen, Y.J. [Institute of Biomedical Sciences, National Sun Yat-Sen University, Kaohsiung 804, Taiwan (China); Hon, M.H. [Department of Materials Science and Engineering, National Cheng Kung University, Tainan 701, Taiwan (China)

2010-05-15

Cerium oxide nanocrystallites were synthesized at a relatively low temperature using cerium nitrate as starting materials in a water solution by a co-precipitation process. Effect of calcination temperature on the crystallite growth of cerium oxide nano-powders was investigated by X-ray diffraction, transmission electron microscopy and electron diffraction. The crystallization temperature of the cerium oxide powders was estimated to be about 273 K by XRD analysis. When calcined from 473 to 1273 K, the crystallization of the face-centered cubic phase was observed by XRD. The crystallite size of the cerium oxide increased from 10.0 to 43.8 nm with calcining temperature increasing from 673 to 1273 K. The activation energy for growth of cerium oxide nanoparticles was found to be 16.0 kJ mol{sup -1}.

Indium hydroxide to oxide decomposition observed in one nanocrystal during in situ transmission electron microscopy studies

International Nuclear Information System (INIS)

Miehe, Gerhard; Lauterbach, Stefan; Kleebe, Hans-Joachim; Gurlo, Aleksander

2013-01-01

The high-resolution transmission electron microscopy (HR-TEM) is used to study, in situ, spatially resolved decomposition in individual nanocrystals of metal hydroxides and oxyhydroxides. This case study reports on the decomposition of indium hydroxide (c-In(OH) 3 ) to bixbyite-type indium oxide (c-In 2 O 3 ). The electron beam is focused onto a single cube-shaped In(OH) 3 crystal of {100} morphology with ca. 35 nm edge length and a sequence of HR-TEM images was recorded during electron beam irradiation. The frame-by-frame analysis of video sequences allows for the in situ, time-resolved observation of the shape and orientation of the transformed crystals, which in turn enables the evaluation of the kinetics of c-In 2 O 3 crystallization. Supplementary material (video of the transformation) related to this article can be found online at (10.1016/j.jssc.2012.09.022). After irradiation the shape of the parent cube-shaped crystal is preserved, however, its linear dimension (edge) is reduced by the factor 1.20. The corresponding spotted selected area electron diffraction (SAED) pattern representing zone [001] of c-In(OH) 3 is transformed to a diffuse strongly textured ring-like pattern of c-In 2 O 3 that indicates the transformed cube is no longer a single crystal but is disintegrated into individual c-In 2 O 3 domains with the size of about 5–10 nm. The induction time of approximately 15 s is estimated from the time-resolved Fourier transforms. The volume fraction of the transformed phase (c-In 2 O 3 ), calculated from the shrinkage of the parent c-In(OH) 3 crystal in the recorded HR-TEM images, is used as a measure of the kinetics of c-In 2 O 3 crystallization within the framework of Avrami–Erofeev formalism. The Avrami exponent of ∼3 is characteristic for a reaction mechanism with fast nucleation at the beginning of the reaction and subsequent three-dimensional growth of nuclei with a constant growth rate. The structural transformation path in reconstructive

Influence of total beam current on HRTEM image resolution in differentially pumped ETEM with nitrogen gas

International Nuclear Information System (INIS)

Bright, A.N.; Yoshida, K.; Tanaka, N.

2013-01-01

Environmental transmission electron microscopy (ETEM) enables the study of catalytic and other reaction processes as they occur with Angstrom-level resolution. The microscope used is a dedicated ETEM (Titan ETEM, FEI Company) with a differential pumping vacuum system and apertures, allowing aberration corrected high-resolution transmission electron microscopy (HRTEM) imaging to be performed with gas pressures up to 20 mbar in the sample area and with significant advantages over membrane-type E-cell holders. The effect on image resolution of varying the nitrogen gas pressure, electron beam current density and total beam current were measured using information limit (Young's fringes) on a standard cross grating sample and from silicon crystal lattice imaging. As expected, increasing gas pressure causes a decrease in HRTEM image resolution. However, the total electron beam current also causes big changes in the image resolution (lower beam current giving better resolution), whereas varying the beam current density has almost no effect on resolution, a result that has not been reported previously. This behavior is seen even with zero-loss filtered imaging, which we believe shows that the drop in resolution is caused by elastic scattering at gas ions created by the incident electron beam. Suitable conditions for acquiring high resolution images in a gas environment are discussed. Lattice images at nitrogen pressures up to 16 mbar are shown, with 0.12 nm information transfer at 4 mbar. -- Highlights: ► ETEM images with point resolution of 0.12 nm in 4 mbar of nitrogen gas. ► Clear Si lattice imaging with 16 mbar of nitrogen gas. ► ETEM image resolution in gas can be much improved by decreasing total beam current. ► Beam current density (beam convergence) has no effect on the image resolution.

Spent oxide fuel regeneration by crystallization in molybdate melts

International Nuclear Information System (INIS)

Ustinov, O.A.; Sukhanov, L.P.; Yakunin, S.A.

2006-01-01

Paper describes a procedure to regenerate spent oxide fuel by its crystallization in molybdate melts. Paper presents the process procedures to regenerate spent fuel of both fast and thermal neutron reactors. One analyzes the advantages of the elaborated procedure [ru

Indium hydroxide to oxide decomposition observed in one nanocrystal during in situ transmission electron microscopy studies

Science.gov (United States)

Miehe, Gerhard; Lauterbach, Stefan; Kleebe, Hans-Joachim; Gurlo, Aleksander

2013-02-01

The high-resolution transmission electron microscopy (HR-TEM) is used to study, in situ, spatially resolved decomposition in individual nanocrystals of metal hydroxides and oxyhydroxides. This case study reports on the decomposition of indium hydroxide (c-In(OH)3) to bixbyite-type indium oxide (c-In2O3). The electron beam is focused onto a single cube-shaped In(OH)3 crystal of {100} morphology with ca. 35 nm edge length and a sequence of HR-TEM images was recorded during electron beam irradiation. The frame-by-frame analysis of video sequences allows for the in situ, time-resolved observation of the shape and orientation of the transformed crystals, which in turn enables the evaluation of the kinetics of c-In2O3 crystallization. Supplementary material (video of the transformation) related to this article can be found online at 10.1016/j.jssc.2012.09.022. After irradiation the shape of the parent cube-shaped crystal is preserved, however, its linear dimension (edge) is reduced by the factor 1.20. The corresponding spotted selected area electron diffraction (SAED) pattern representing zone [001] of c-In(OH)3 is transformed to a diffuse strongly textured ring-like pattern of c-In2O3 that indicates the transformed cube is no longer a single crystal but is disintegrated into individual c-In2O3 domains with the size of about 5-10 nm. The induction time of approximately 15 s is estimated from the time-resolved Fourier transforms. The volume fraction of the transformed phase (c-In2O3), calculated from the shrinkage of the parent c-In(OH)3 crystal in the recorded HR-TEM images, is used as a measure of the kinetics of c-In2O3 crystallization within the framework of Avrami-Erofeev formalism. The Avrami exponent of ˜3 is characteristic for a reaction mechanism with fast nucleation at the beginning of the reaction and subsequent three-dimensional growth of nuclei with a constant growth rate. The structural transformation path in reconstructive decomposition of c-In(OH)3 to c

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

Energy Technology Data Exchange (ETDEWEB)

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

2012-04-05

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

Crystallization process and magnetic properties of amorphous iron oxide nanoparticles

International Nuclear Information System (INIS)

Phu, N D; Luong, N H; Chau, N; Hai, N H; Ngo, D T; Hoang, L H

2011-01-01

This paper studied the crystallization process, phase transition and magnetic properties of amorphous iron oxide nanoparticles prepared by the microwave heating technique. Thermal analysis and magnetodynamics studies revealed many interesting aspects of the amorphous iron oxide nanoparticles. The as-prepared sample was amorphous. Crystallization of the maghemite γ-Fe 2 O 3 (with an activation energy of 0.71 eV) and the hematite α-Fe 2 O 3 (with an activation energy of 0.97 eV) phase occurred at around 300 deg. C and 350 deg. C, respectively. A transition from the maghemite to the hematite occurred at 500 deg. C with an activation energy of 1.32 eV. A study of the temperature dependence of magnetization supported the crystallization and the phase transformation. Raman shift at 660 cm -1 and absorption band in the infrared spectra at 690 cm -1 showed the presence of disorder in the hematite phase on the nanoscale which is supposed to be the origin of the ferromagnetic behaviour of that antiferromagnetic phase.

Thorium/uranium mixed oxide nano-crystals: Synthesis, structural characterization and magnetic properties

International Nuclear Information System (INIS)

Hudry, Damien; Griveau, Jean-Christophe; Apostolidis, Christos; Colineau, Eric; Rasmussen, Gert; Walter, Olaf; Wang, Di; Venkata Sai Kiran Chakravadhaluna; Courtois, Eglantine; Kubel, Christian

2014-01-01

One of the primary aims of the actinide community within nano-science is to develop a good understanding similar to what is currently the case for stable elements. As a consequence, efficient, reliable and versatile synthesis techniques dedicated to the formation of new actinide-based nano-objects (e.g., nano-crystals) are necessary. Hence, a 'library' dedicated to the preparation of various actinide based nano-scale building blocks is currently being developed. Nano-scale building blocks with tunable sizes, shapes and compositions are of prime importance. So far, the non-aqueous synthesis method in highly coordinating organic media is the only approach which has demonstrated the capability to provide size and shape control of actinide-based nano-crystals (both for thorium and uranium, and recently extended to neptunium and plutonium). In this paper, we demonstrate that the non-aqueous approach is also well adapted to control the chemical composition of the nano-crystals obtained when mixing two different actinides. Indeed, the controlled hot co-injection of thorium acetylacetonate and uranyl acetate (together with additional capping agents) into benzyl ether can be used to synthesize thorium/uranium mixed oxide nano-crystals covering the full compositional spectrum. Additionally, we found that both size and shape are modified as a function of the thorium/uranium ratio. Finally, the magnetic properties of the different thorium/uranium mixed oxide nano-crystals were investigated. Contrary to several reports, we did not observe any ferromagnetic behavior. As a consequence, ferromagnetism cannot be described as a universal feature of nano-crystals of non-magnetic oxides as recently claimed in the literature. (authors)

Crystal structure of the uranyl-oxide mineral rameauite

Czech Academy of Sciences Publication Activity Database

Plášil, Jakub; Škoda, R.; Čejka, J.; Bourgoin, V.; Boulliard, J.C.

2016-01-01

Roč. 28, č. 5 (2016), s. 959-967 ISSN 0935-1221 R&D Projects: GA MŠk LO1603 EU Projects: European Commission(XE) CZ.2.16/3.1.00/24510 Institutional support: RVO:68378271 Keywords : rameauite * uranyl-oxide hydroxy-hydrate * crystal structure * Raman spectrum Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.362, year: 2016

Kinetic studies on the degradation of crystal violet by the Fenton oxidation process.

Science.gov (United States)

Wu, H; Fan, M M; Li, C F; Peng, M; Sheng, L J; Pan, Q; Song, G W

2010-01-01

The degradation of dye crystal violet (CV) by Fenton oxidation process was investigated. The UV-Vis spectrogram has shown that CV can be degraded effectively by Fenton oxidation process. Different system variables namely initial H(2)O(2) concentration, initial Fe(2 + ) concentration and reaction temperature, which have effect on the degradation of CV by Fenton oxidation process, have been studied systematically. The degradation kinetics of CV was also elucidated based on the experimental data. The degradation of CV obeys the first-order reaction kinetics. The kinetic model can be described as k=1.5 exp(-(7.5)/(RT))[H(2)O(2)](0)(0.8718)[Fe(2+)](0)(0.5062). According to the IR spectrogram, it is concluded that the benzene ring of crystal violet has been destroyed by Fenton oxidation. The result will be useful in treating dyeing wastewater containing CV by Fenton oxidation process.

Short review of high-pressure crystal growth and magnetic and electrical properties of solid-state osmium oxides

Energy Technology Data Exchange (ETDEWEB)

Yamaura, Kazunari, E-mail: YAMAURA.Kazunari@nims.go.jp [Superconducting Properties Unit, National Institute for Materials Science, 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan); Graduate School of Chemical Sciences and Engineering, Hokkaido University, North 10 West 8, Kita-ku, Sapporo, Hokkaido 060-0810 (Japan)

2016-04-15

High-pressure crystal growth and synthesis of selected solid-state osmium oxides, many of which are perovskite-related types, are briefly reviewed, and their magnetic and electrical properties are introduced. Crystals of the osmium oxides, including NaOsO{sub 3}, LiOsO{sub 3}, and Na{sub 2}OsO{sub 4}, were successfully grown under high-pressure and high-temperature conditions at 6 GPa in the presence of an appropriate amount of flux in a belt-type apparatus. The unexpected discovery of a magnetic metal–insulator transition in NaOsO{sub 3}, a ferroelectric-like transition in LiOsO{sub 3}, and high-temperature ferrimagnetism driven by a local structural distortion in Ca{sub 2}FeOsO{sub 6} may represent unique features of the osmium oxides. The high-pressure and high-temperature synthesis and crystal growth has played a central role in the development of solid-state osmium oxides and the elucidation of their magnetic and electronic properties toward possible use in multifunctional devices. - Graphical Abstract: Flux-grown crystals of NaOsO{sub 3} under high-pressure and high-temperature conditions in a belt-type apparatus. The crystal shows a magnetically driven metal–insulator transition at a temperature of 410 K. - Highlights: • Short review of high-pressure crystal growth of solid-state osmium oxides. • Wide variety of magnetic properties of solid-state osmium oxides. • Perovskite and related dense structures stabilized at 3–17 GPa.

The interfacial orientation relationship of oxide nanoparticles in a hafnium-containing oxide dispersion-strengthened austenitic stainless steel

Energy Technology Data Exchange (ETDEWEB)

Miao, Yinbin, E-mail: miao2@illinois.edu [Department of Nuclear, Plasma and Radiological Engineering, University of Illinois at Urbana-Champaign, Urbana, IL 61801 (United States); Mo, Kun [Nuclear Engineering Division, Argonne National Laboratory, Lemont, IL 60493 (United States); Cui, Bai [Department of Mechanical and Materials Engineering, University of Nebraska-Lincoln, Lincoln, NE 68588 (United States); Department of Material Science and Engineering, University of Illinois at Urbana-Champaign, Urbana, IL 61801 (United States); Chen, Wei-Ying [Department of Nuclear, Plasma and Radiological Engineering, University of Illinois at Urbana-Champaign, Urbana, IL 61801 (United States); Miller, Michael K.; Powers, Kathy A. [Center for Nanophase Materials Sciences, Oak Ridge National Laboratory, Oak Ridge, TN 37830 (United States); McCreary, Virginia; Gross, David [Department of Material Science and Engineering, University of Illinois at Urbana-Champaign, Urbana, IL 61801 (United States); Almer, Jonathan [X-ray Science Division, Argonne National Laboratory, Lemont, IL 60493 (United States); Robertson, Ian M. [Department of Material Science and Engineering, University of Wisconsin-Madison, Madison, WA 53706 (United States); Department of Material Science and Engineering, University of Illinois at Urbana-Champaign, Urbana, IL 61801 (United States); Stubbins, James F. [Department of Nuclear, Plasma and Radiological Engineering, University of Illinois at Urbana-Champaign, Urbana, IL 61801 (United States)

2015-03-15

This work reports comprehensive investigations on the orientation relationship of the oxide nanoparticles in a hafnium-containing austenitic oxide dispersion-strengthened 316 stainless steel. The phases of the oxide nanoparticles were determined by a combination of scanning transmission electron microscopy–electron dispersive X-ray spectroscopy, atom probe tomography and synchrotron X-ray diffraction to be complex Y–Ti–Hf–O compounds with similar crystal structures, including bixbyite Y{sub 2}O{sub 3}, fluorite Y{sub 2}O{sub 3}–HfO{sub 2} solid solution and pyrochlore (or fluorite) Y{sub 2}(Ti,Hf){sub 2−x}O{sub 7−x}. High resolution transmission electron microscopy was used to characterize the particle–matrix interfaces. Two different coherency relationships along with one axis-parallel relation between the oxide nanoparticles and the steel matrix were found. The size of the nanoparticles significantly influences the orientation relationship. The results provide insight into the relationship of these nanoparticles with the matrix, which has implications for interpreting material properties as well as responses to radiation. - Highlights: • The oxide nanoparticles in a hafnium-containing austenitic ODS were characterized. • The nanoparticles are Y–Hf–Ti–O enriched phases according to APT and STEM–EDS. • Two coherency and an axis-parallel orientation relationships were found by HR-TEM. • Particle size has a prominent effect on the orientation relationship (OR). • Formation mechanism of the oxide nanoparticles was discussed based on the ORs.

Simulation of bonding effects in HRTEM images of light element materials

Directory of Open Access Journals (Sweden)

Simon Kurasch

2011-07-01

Full Text Available The accuracy of multislice high-resolution transmission electron microscopy (HRTEM simulation can be improved by calculating the scattering potential using density functional theory (DFT. This approach accounts for the fact that electrons in the specimen are redistributed according to their local chemical environment. This influences the scattering process and alters the absolute and relative contrast in the final image. For light element materials with well defined geometry, such as graphene and hexagonal boron nitride monolayers, the DFT based simulation scheme turned out to be necessary to prevent misinterpretation of weak signals, such as the identification of nitrogen substitutions in a graphene network. Furthermore, this implies that the HRTEM image does not only contain structural information (atom positions and atomic numbers. Instead, information on the electron charge distribution can be gained in addition.In order to produce meaningful results, the new input parameters need to be chosen carefully. Here we present details of the simulation process and discuss the influence of the main parameters on the final result. Furthermore we apply the simulation scheme to three model systems: A single atom boron and a single atom oxygen substitution in graphene and an oxygen adatom on graphene.

Transmission electron microscopy and Raman characterization of copper (I) oxide microspheres composed of nanoparticles

International Nuclear Information System (INIS)

Wang Wenzhong; Tu Ya; Wang Lijuan; Liang Yujie; Shi Honglong

2013-01-01

Highlights: ► Raman spectroscopy of copper (I) oxide microspheres were investigated. ► Infrared active mode is greatly activated in Raman scattering spectrum. ► Infrared active mode shows up in Raman spectrum of copper (I) oxide microspheres. ► The defects existed in spheres could be responsible for the observed Raman property. - Abstract: The high-resolution transmission electron microscope and Raman spectroscopy were used to investigate the microstructures and Raman scattering property of copper (I) oxide microspheres composed of nanoparticles. High-resolution transmission electron microscope images indicate that the copper (I) oxide microspheres are composed of nanoparticles with random growth direction, indicating that there are many defects in microspheres. The Raman spectrum shows that infrared active mode, which must be odd parity and is Raman forbidden for bulk crystal due to its inversion symmetry, is activated and shows up in Raman scattering spectrum. On the basis of investigations of the microstructure features of copper (I) oxide microspheres, we attribute the appearance of IR active mode in Raman scattering spectrum to the breakdown of the symmetry of the lattice due to the presence of defects in the prepared copper (I) oxide microspheres as observed in HRTEM images.

Flame synthesis of zinc oxide nanocrystals

Energy Technology Data Exchange (ETDEWEB)

Merchan-Merchan, Wilson, E-mail: wmerchan-merchan@ou.edu [School of Aerospace and Mechanical Engineering, University of Oklahoma, Norman, OK 73019 (United States); Farahani, Moien Farmahini [School of Aerospace and Mechanical Engineering, University of Oklahoma, Norman, OK 73019 (United States)

2013-02-01

Highlights: Black-Right-Pointing-Pointer We report a single-step flame method for the synthesis of Zn oxide nanocrystals. Black-Right-Pointing-Pointer Diverse flame positions lead to a variation of Zn oxide nanocrystal growth. Black-Right-Pointing-Pointer The synthesized crystals have polyhedral, pipet- and needle-like shape. Black-Right-Pointing-Pointer High length-to-diameter aspect-ratio crystals appear in a higher temperature flame. Black-Right-Pointing-Pointer The crystal growth mechanism corresponds to vapor-to-solid conversion. - Abstract: Distinctive zinc oxide (ZnO) nanocrystals were synthesized on the surface of Zn probes using a counter-flow flame medium formed by methane/acetylene and oxygen-enriched air streams. The source material, a zinc wire with a purity of {approx}99.99% and diameter of 1 mm, was introduced through a sleeve into the oxygen rich region of the flame. The position of the probe/sleeve was varied within the flame medium resulting in growth variation of ZnO nanocrystals on the surface of the probe. The shape and structural parameters of the grown crystals strongly depend on the flame position. Structural variations of the synthesized crystals include single-crystalline ZnO nanorods and microprisms (ZMPs) (the ZMPs have less than a few micrometers in length and several hundred nanometers in cross section) with a large number of facets and complex axial symmetry with a nanorod protruding from their tips. The protruding rods are less than 100 nm in diameter and lengths are less than 1 {mu}m. The protruding nanorods can be elongated several times by increasing the residence time of the probe/sleeve inside the oxygen-rich flame or by varying the flame position. At different flame heights, nanorods having higher length-to-diameter aspect-ratio can be synthesized. A lattice spacing of {approx}0.26 nm was measured for the synthesized nanorods, which can be closely correlated with the (0 0 2) interplanar spacing of hexagonal ZnO (Wurtzite) cells

Crystal orientation dependent thermoelectric properties of highly oriented aluminum-doped zinc oxide thin films

KAUST Repository

Abutaha, Anas I.; Sarath Kumar, S. R.; Alshareef, Husam N.

2013-01-01

We demonstrate that the thermoelectric properties of highly oriented Al-doped zinc oxide (AZO) thin films can be improved by controlling their crystal orientation. The crystal orientation of the AZO films was changed by changing the temperature

Crystallization of the NADH-oxidizing domain of the Na+-translocating NADH:ubiquinone oxidoreductase from Vibrio cholerae

International Nuclear Information System (INIS)

Tao, Minli; Türk, Karin; Diez, Joachim; Grütter, Markus G.; Fritz, Günter; Steuber, Julia

2006-01-01

The FAD domain of the NqrF subunit from the Na + -translocating NADH dehydrogenase from V. cholerae has been purified and crystallized. A complete data set was recorded at 3.1 Å. The Na + -translocating NADH:quinone oxidoreductase (Na + -NQR) from pathogenic and marine bacteria is a respiratory complex that couples the exergonic oxidation of NADH by quinone to the transport of Na + across the membrane. The NqrF subunit oxidizes NADH and transfers the electrons to other redox cofactors in the enzyme. The FAD-containing domain of NqrF has been expressed, purified and crystallized. The purified NqrF FAD domain exhibited high rates of NADH oxidation and contained stoichiometric amounts of the FAD cofactor. Initial crystallization of the flavin domain was achieved by the sitting-drop technique using a Cartesian MicroSys4000 robot. Optimization of the crystallization conditions yielded yellow hexagonal crystals with dimensions of 30 × 30 × 70 µm. The protein mainly crystallizes in long hexagonal needles with a diameter of up to 30 µm. Crystals diffract to 2.8 Å and belong to space group P622, with unit-cell parameters a = b = 145.3, c = 90.2 Å, α = β = 90, γ = 120°

Zinc oxide crystal whiskers as a novel sorbent for solid-phase extraction of flavonoids.

Science.gov (United States)

Wang, Licheng; Shangguan, Yangnan; Hou, Xiudan; Jia, Yong; Liu, Shujuan; Sun, Yingxin; Guo, Yong

2017-08-15

As a novel solid-phase extraction material, zinc oxide crystal whiskers were used to extract flavonoid compounds and showed good extraction abilities. X-ray diffraction, scanning electron microscopy with energy dispersive X-ray spectroscopy and surface area/pore volume characterized the sorbent. The zinc oxide was packed into a solid-phase extraction micro-column and its extraction ability was evaluated by four model flavonoid compounds. The sample loading and elution parameters were optimized and the zinc oxide based analytical method for flavonoids was established. It showed that the method has wide linearities from 1 to 150μg/L and low limits of detection at 0.25μg/L. The relative standard deviations of a single column repeatability and column to column reproducibility were less than 6.8% and 10.6%. Several real samples were analyzed by the established method and satisfactory results were obtained. The interactions between flavonoids and zinc oxide were calculated and proved to be from the Van der Waals' forces between the 4p and 5d orbitals from zinc atom and the neighboring π orbitals from flavonoid phenyl groups. Moreover, the zinc oxide crystal whiskers showed good stability and could be reused more than 50 times under the operation conditions. This work proves that the zinc oxide crystal whiskers are a good candidate for flavonoids enrichment. Copyright © 2017. Published by Elsevier B.V.

The effect of crystal textures on the anodic oxidization of zirconium in a boiling nitric acid solution

International Nuclear Information System (INIS)

Kato, Chiaki; Ishijima, Yasuhiro; Ueno, Fumiyoshi; Yamamoto, Masahiro

2016-01-01

The effects of crystal textures and the potentials in the anodic oxidation of zirconium in a boiling nitric acid solution were investigated to study the stress corrosion cracking of zirconium in nitric acid solutions. The test specimen was machined such that the specimen surface was parallel to the rolling surface, arranged with a (0002) crystal texture. The potentials applied for the anodic oxidation of zirconium were set at 1.2, 1.4, and 1.5 V against a saturated KCl–Ag/AgCl electrode (SSE) in boiling 6 M HNO_3. The growth of the zirconium oxide film dramatically changed depending on the applied potential at a closed depassivation potential (1.47 V vs. SSE in this study). At 1.5 V, the zirconium oxide film rapidly grows, and its growth exhibits cyclic oxidation kinetics in accordance with a nearly cubic rate law. The zirconium oxide film grows according to the quantity of electric charge and the growth rate does not depend on the crystal texture in the pretransition region before the cyclic oxidation kinetics. However, the growth and cracking under the thick oxide film depend on the crystal texture in the transition region. On the normal direction side, the oxide film thickness decreases on average since some areas of the thick oxide film are separated from the specimen surface owing to the cracks in the thick oxide. On the rolling direction (RD) side, no cracks in the thick oxide film are observed, but cracks are found under the thick oxide film, which deeply propagate in metal matrix along the RD without an external stress. The cracks under the thick oxide film propagate to the center of the oxide layer. The crystal orientation relationship between the oxide layer and the zirconium matrix is (0002)_Z_r//(111)_Z_r_O_2, and the cracks in the oxide layer propagate in the (0002)_Z_r plane in the zirconium matrix. The oxide layer consists of string-like zirconium oxide and zirconium hydride. The string-like zirconium oxide contains orthorhombic ZrO_2 in addition

Indium Gallium Zinc Oxide: Phase Formation and Crystallization Kinetics during Millisecond Laser Spike Annealing

Science.gov (United States)

Lynch, David Michael

Flat panel displays have become ubiquitous, enabling products from highresolution cell phones to ultra-large television panels. Amorphous silicon (a- Si) has been the industry workhorse as the active semiconductor in pixeladdressing transistors due to its uniformity and low production costs. However, a-Si can no longer support larger and higher-resolution displays, and new materials with higher electron mobilities are required. Amorphous indium gallium zinc oxide (a-IGZO), which retains the uniformity and low cost of amorphous films, has emerged as a viable candidate due to its enhanced transport properties. However, a-IGZO devices suffer from long-term instabilities--the origins of which are not yet fully understood--causing a drift in switching characteristics over time and affecting product lifetime. More recently, devices fabricated from textured nanocrystalline IGZO, termed c-axis aligned crystalline (CAAC), have demonstrated superior stability. Unfortunately, little is known regarding the phase formation and crystallization kinetics of either the CAAC structure or in the broader ternary IGZO system. Crystallinity and texture of CAAC IGZO films deposited by RF reactive sputtering were studied and characterized over a wide range of deposition conditions. The characteristic CAAC (0 0 9) peak at 2theta = 30° was observed by X-ray diffraction, and nanocrystalline domain texture was determined using a general area detector diffraction system (GADDS). Highly ordered CAAC films were obtained near the InGaZnO4 composition at a substrate temperature of 310 °C and in a 10%O2/90% Ar sputtering ambient. High-resolution transmission electron microscopy (HRTEM) confirmed the formation of CAAC and identified 2-3 nm domains coherently aligned over large ranges extending beyond the field of view (15 nm x 15 nm). Cross-section HRTEM of the CAAC/substrate interface shows formation of an initially disordered IGZO layer prior to CAAC formation, suggesting a nucleation mechanism

Preparation and properties of crystals of mixed refractory oxides with perovskite structure

Energy Technology Data Exchange (ETDEWEB)

Melekh, B T; Andreev, A A; Kartenko, N F; Pevtsov, A B; Trepakov, V A; Filin, Yu N [AN SSSR, Moscow. Fiziko-Tekhnicheskij Inst.

1982-10-01

Peculiar features of crystal growth of some complex refractory oxides with perovskite structure using the method of direct high-frequency melting in a cold container are studied. Melting, synthesis and directed crystallization have been conducted in the air. X-ray diffraction investigations of the prepared SrTiO/sub 3/, CaZrO/sub 3/, BaZrO/sub 3/, BaHFO/sub 3/, LaCrO/sub 3/, YCrO/sub 3/, ErCrO/sub 3/, La/sub 2/Ti/sub 2/O/sub 7/, LaTaO/sub 3/ and other oxides are conducted, lattice parameters are given. Optical spectra of absorption, photo- and thermoluminescence and thermostimulated currents are studied.

Fano resonance in anodic aluminum oxide based photonic crystals.

Science.gov (United States)

Shang, Guo Liang; Fei, Guang Tao; Zhang, Yao; Yan, Peng; Xu, Shao Hui; Ouyang, Hao Miao; Zhang, Li De

2014-01-08

Anodic aluminum oxide based photonic crystals with periodic porous structure have been prepared using voltage compensation method. The as-prepared sample showed an ultra-narrow photonic bandgap. Asymmetric line-shape profiles of the photonic bandgaps have been observed, which is attributed to Fano resonance between the photonic bandgap state of photonic crystal and continuum scattering state of porous structure. And the exhibited Fano resonance shows more clearly when the sample is saturated ethanol gas than air-filled. Further theoretical analysis by transfer matrix method verified these results. These findings provide a better understanding on the nature of photonic bandgaps of photonic crystals made up of porous materials, in which the porous structures not only exist as layers of effective-refractive-index material providing Bragg scattering, but also provide a continuum light scattering state to interact with Bragg scattering state to show an asymmetric line-shape profile.

Cobalt oxides from crystal chemistry to physics

CERN Document Server

Raveau, Bernard

2012-01-01

Unparalleled in the breadth and depth of its coverage of all important aspects, this book systematically treats the electronic and magnetic properties of stoichiometric and non-stoichiometric cobaltites in both ordered and disordered phases. Authored by a pioneer and a rising star in the field, the monograph summarizes, organizes and streamlines the otherwise difficult-to-obtain information on this topic. An introductory chapter sets forth the crystal chemistry of cobalt oxides to lay the groundwork for an understanding of the complex phenomena observed in this materials class. Special emphasis is placed on a comprehensive discussion of cobaltite physical properties in different structural families. Providing a thorough introduction to cobalt oxides from a chemical and physical viewpoint as a basis for understanding their intricacies, this is a must-have for both experienced researchers as well as entrants to the field.

Zirconium oxide crystal phase: The role of the pH and time to attain the final pH for precipitation of the hydrous oxide

International Nuclear Information System (INIS)

Srinivasan, R.; Harris, M.B.; Simpson, S.F.; De Angelis, R.J.; Davis, B.H.

1988-01-01

Precipitated hydrous zirconium oxide can be calcined to produce either a monoclinic or tetragonal product. It has been observed that the time taken to attain the final pH of the solution in contact with the precipitate plays a dominant role in determining the crystal structure of the zirconium oxide after calcination at 500 0 C. The dependence of crystal structure on the rate of precipitation is observed only in the pH range 7--11. Rapid precipitation in this pH range yields predominately monoclinic zirconia, whereas slow (8 h) precipitation produces the tetragonal phase. At pH of approximately 13.0, only the tetragonal phase is formed from both slowly and rapidly precipitated hydrous oxide. The present results, together with earlier results, show that both the pH of the supernatant liquid and the time taken to attain this pH play dominant roles in determining the crystal structure of zirconia that is formed after calcination of the hydrous oxide. The factors that determine the crystal phase are therefore imparted in a mechanism of precipitation that depends upon the pH, and it is inferred that it is the hydroxyl concentration that is the dominant factor

Fruit peel extract mediated green synthesis of zinc oxide nanoparticles

Science.gov (United States)

Nava, O. J.; Soto-Robles, C. A.; Gómez-Gutiérrez, C. M.; Vilchis-Nestor, A. R.; Castro-Beltrán, A.; Olivas, A.; Luque, P. A.

2017-11-01

This work presents a study of the effects on the photocatalytic capabilities of zinc oxide nanoparticles when prepared via green synthesis using different fruit peel extracts as reducing agents. Zinc nitrate was used as a source of the zinc ions, while Lycopersicon esculentum (tomato), Citrus sinensis (orange), Citrus paradisi (grapefruit) and Citrus aurantifolia (lemon) contributed their peels for extracts. The Synthesized Samples were studied and characterized through Fourier Transform Infrared Spectroscopy (FTIR), X-Ray Diffraction (XRD), and High Resolution Transmission Electron Microscopy (HRTEM). All samples presented a band at 618 cm-1, indicating the presence of the Znsbnd O bond. The different samples all presented the same hexagonal crystal growth in their structure, the Wurtzite phase. The surface morphology of the nanoparticles showed that, depending on the extract used, the samples vary in size and shape distribution due to the chemical composition of the extracts. The photocatalytic properties of the zinc oxide samples were tested through UV light aided degradation of methylene blue. Most samples exhibited degradation rates at 180 min of around 97%, a major improvement when compared to chemically synthesized commercially available zinc oxide nanoparticles.

Oxidation and crystal field effects in uranium

Energy Technology Data Exchange (ETDEWEB)

Tobin, J. G. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Booth, C. H. [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Shuh, D. K. [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); van der Laan, G. [Diamond Light Source, Didcot (United Kingdom); Sokaras, D. [Stanford Synchrotron Radiation Lightsource, Stanford, CA (United States); Weng, T. -C. [Stanford Synchrotron Radiation Lightsource, Stanford, CA (United States); Yu, S. W. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Bagus, P. S. [Univ. of North Texas, Denton, TX (United States); Tyliszczak, T. [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Nordlund, D. [Stanford Synchrotron Radiation Lightsource, Stanford, CA (United States)

2015-07-06

An extensive investigation of oxidation in uranium has been pursued. This includes the utilization of soft x-ray absorption spectroscopy, hard x-ray absorption near-edge structure, resonant (hard) x-ray emission spectroscopy, cluster calculations, and a branching ratio analysis founded on atomic theory. The samples utilized were uranium dioxide (UO₂), uranium trioxide (UO₃), and uranium tetrafluoride (UF₄). As a result, a discussion of the role of non-spherical perturbations, i.e., crystal or ligand field effects, will be presented.

Crystal-phase intergradation in InAs nanostructures grown by van der Waals heteroepitaxy on graphene

Science.gov (United States)

Choi, Ji Eun; Yoo, Jinkyoung; Lee, Donghwa; Hong, Young Joon; Fukui, Takashi

2018-04-01

This study demonstrates the crystal-phase intergradation of InAs nanostructures grown on graphene via van der Waals epitaxy. InAs nanostructures with diverse diameters are yielded on graphene. High-resolution transmission electron microscopy (HR-TEM) reveals two crystallographic features of (i) wurtzite (WZ)-to-zinc blende (ZB) intergradation along the growth direction of InAs nanostructures and (ii) an increased mean fraction of ZB according to diameter increment. Based on the HR-TEM observations, a crystal-phase intergradation diagram is depicted. We discuss how the formation of a WZ-rich phase during the initial growth stage is an effective way of releasing heterointerfacial stress endowed by the lattice mismatch of InAs/graphene for energy minimization in terms of less in-plane lattice mismatching between WZ-InAs and graphene. The WZ-to-ZB evolution is responsible for the attenuation of the bottom-to-top surface charge interaction as growth proceeds.

Gas Sensors Based on Tin Oxide Nanoparticles Synthesized from a Mini-Arc Plasma Source

Directory of Open Access Journals (Sweden)

Ganhua Lu

2006-01-01

Full Text Available Miniaturized gas sensors or electronic noses to rapidly detect and differentiate trace amount of chemical agents are extremely attractive. In this paper, we report on the fabrication and characterization of a functional tin oxide nanoparticle gas sensor. Tin oxide nanoparticles are first synthesized using a convenient and low-cost mini-arc plasma source. The nanoparticle size distribution is measured online using a scanning electrical mobility spectrometer (SEMS. The product nanoparticles are analyzed ex-situ by high resolution transmission electron microscopy (HRTEM for morphology and defects, energy dispersive X-ray (EDX spectroscopy for elemental composition, electron diffraction for crystal structure, and X-ray photoelectron spectroscopy (XPS for surface composition. Nonagglomerated rutile tin oxide (SnO2 nanoparticles as small as a few nm have been produced. Larger particles bear a core-shell structure with a metallic core and an oxide shell. The nanoparticles are then assembled onto an e-beam lithographically patterned interdigitated electrode using electrostatic force to fabricate the gas sensor. The nanoparticle sensor exhibits a fast response and a good sensitivity when exposed to 100 ppm ethanol vapor in air.

Correlation of electrolyte-derived inclusions to crystallization in the early stage of anodic oxide film growth on titanium

Energy Technology Data Exchange (ETDEWEB)

Jaeggi, C., E-mail: christian.jaeggi@empa.ch [Empa, Swiss Federal Laboratories for Materials Testing and Research, Advanced Materials Processing Laboratory, Feuerwerkerstrasse 39, CH-3602 Thun (Switzerland); Parlinska-Wojtan, M., E-mail: magdalena.parlinska@empa.ch [Empa, Swiss Federal Laboratories for Materials Testing and Research, Center for Electron Microscopy, Ueberlandstrasse 129, CH-8600 Duebendorf (Switzerland); Kern, P., E-mail: Philippe.Kern@neopac.ch [Empa, Swiss Federal Laboratories for Materials Testing and Research, Laboratory for Mechanics of Materials and Nanostructures, Feuerwerkerstrasse 39, CH-3602 Thun (Switzerland)

2012-01-01

Pure titanium has been subjected to anodization in sulfuric and phosphoric acid. For a better understanding of the oxide growth and properties of the final film, with a particular interest focused on the solution anions in the early stage of crystallization, microstructural analyses (Raman, Transmission Electron Microscopy [TEM]) of the oxide films were correlated to chemical depth profiling by glow discharge optical emission spectroscopy (GDOES). Raman spectroscopy shows that crystallization of the oxide films starts at potentials as low as 10-20 V. The onset of crystallization and the ongoing increase in crystallinity with increasing anodization potentials had already earlier been correlated to ac-impedance measurements [Jaeggi et al., Surf. Interface Anal. 38 (2006) 182]. TEM observations show a clear difference in the early phase of crystallization between oxides grown in 1 M sulfuric acid compared to 1 M phosphoric acid. Moreover, independent of electrolyte type, nano-sized pores from oxygen bubbles formation were revealed in the central part of the films. Until now, oxygen bubbles inside an anodically grown oxide have not been observed before without the presence of crystalline regions nearby. A growth model is proposed, in which the different starting locations of crystallization inside the films are correlated to the presence of the acid anions as residues in the film, as found by GDOES chemical depth-profiling.

Selective tuning of high-Q silicon photonic crystal nanocavities via laser-assisted local oxidation.

Science.gov (United States)

Chen, Charlton J; Zheng, Jiangjun; Gu, Tingyi; McMillan, James F; Yu, Mingbin; Lo, Guo-Qiang; Kwong, Dim-Lee; Wong, Chee Wei

2011-06-20

We examine the cavity resonance tuning of high-Q silicon photonic crystal heterostructures by localized laser-assisted thermal oxidation using a 532 nm continuous wave laser focused to a 2.5 μm radius spot-size. The total shift is consistent with the parabolic rate law. A tuning range of up to 8.7 nm is achieved with ∼ 30 mW laser powers. Over this tuning range, the cavity Qs decreases from 3.2×10(5) to 1.2×10(5). Numerical simulations model the temperature distributions in the silicon photonic crystal membrane and the cavity resonance shift from oxidation.

Platinum single crystal electrodes for the electrocatalysis of methane oxidation

Directory of Open Access Journals (Sweden)

Mayara Munaretto

2011-03-01

Full Text Available The main objective of this paper is to characterize the voltammetric profiles of platinum single crystals of low Miller indexes Pt(100 and Pt(110 and study their catalytic activities on the oxidation of methane. In this way, it was developed a metallic surface modified by presence of other metal oxide, which presents catalytic activity for this reaction. It is well known that the electrooxidation of methane (CH4 leads mainly to the formation of CO2 and H2O, however, the oxidation can also lead to the formation of CO, a reaction intermediate that has strong interaction with metal surfaces, such as platinum. This molecule tends to accumulate on the platinum surface and to passive it, due to the self-poisoning, decreasing its catalytic activity. Therefore, the main aim of this work was the development of a platinum electrode modified by deposition of titanium oxide, which presented electrocatalytic properties for the oxidation of methane.

Ni-Si oxide as an inducing crystallization source for making poly-Si

Energy Technology Data Exchange (ETDEWEB)

Meng, Zhiguo; Liu, Zhaojun; Li, Juan; Wu, Chunya; Xiong, Shaozhen [Institute of Photo-electronics, Nankai University, Tianjin (China); Zhao, Shuyun; Wong, Man; Kwok, Hoi Sing [Department of Electronic and Computer Engineering, Hong Kong University of Science and Technology, Kowloon, Hong Kong (China)

2010-04-15

Nickel silicon oxide mixture was sputtered on a-Si with Ni-Si alloy target with Ni:Si weight ratio of 1:9 and used as a new inducing source for metal induced lateral crystallization (MILC). The characteristics of the resulted poly-Si materials induced by Ni-Si oxide with different thickness were nearly the same. This means the metal induced crystallization with this new inducing source has wide processing tolerance to make MILC poly-Si. Besides, it reduced the residual Ni content in the resulted poly-Si film. The transfer characteristic curve of poly-Si TFT and a TFT-OLED display demo made with this kind of new inducing source were also presented in this paper. (copyright 2010 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

Rapid synthesis and catalytic performance of {alpha}-Mn{sub 2}O{sub 3} single-crystal nanowires

Energy Technology Data Exchange (ETDEWEB)

Yuan, Xinsong; Hu, Xingming; Zhu, Jinmiao; Dong, Huaze; Wang, Yanping [Department of Chemistry and Chemical Engineering, Hefei Normal University, Hefei 230061 (China); Yang, Baojun [Anhui Key Laboratory of Controllable Chemistry Reaction and Material Chemical Engineering, School of Chemical Engineering, Hefei University of Technology, Hefei 230009 (China); Hao, Jianwen [Department of Chemical Engineering, Anhui Vocational and Technical College, Hefei 230051 (China)

2011-12-15

Single-crystal {alpha}-Mn{sub 2}O{sub 3} nanowires were prepared via a ''self-sacrificing template'' route, simply by calcining the prepared {alpha}-MnO{sub 2} nanowire precursors at 550 C for 1.5 h. XRD, TEM, SEM and HRTEM characterizations show that the as-prepared {alpha}-Mn{sub 2}O{sub 3} samples are all phase pure and the nanowires have uniform diameters of approximately 15-30 nm and lengths up to several micrometers. The catalytic performances of the prepared {alpha}-Mn{sub 2}O{sub 3} nanowires were studied in the degradation of coking wastewater with H{sub 2}O{sub 2} as the oxidant, and the technological conditions were optimized by single-factor and orthogonal experiments. (copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

Crystal habit dependent quantum confined photoluminescence of zinc oxide nanostructures

International Nuclear Information System (INIS)

Arellano, Ian Harvey J.; Payawan, Leon Jr. M.; Sarmago, Roland V.

2008-01-01

Diverse zinc oxide crystal habits namely wire, rods, tubes, whiskers and tetrapods were synthesized via hydrothermal and carbothermal reduction routes. A vapor current induced regionalization in the carbothermal synthesis lead to the isolation of these crystal habits for characterization. The surface morphology of the nanostructures was analyzed via field emission scanning electron microscopy (FESEM). The morphology and crystallinity of the as-synthesized nanostructure architectural motifs were related to their photoluminescence (PL). The photoluminescence at 157 nm was taken using F2 excimer laser and a crystal habit dependent response was observed. X-ray diffraction (XRD) analyses were conducted to deduce the degree of crystallinity showing results consistent with the excitonic emission at the band edge and visible emission at the electron-hole recombination sites. The presence of minimal crystal defects which gave the green emission was supported by energy dispersive spectroscopy (EDS) data. Transmission spectroscopy for the tetrapods exhibited an interesting PL reduction associated with high-energy deep traps in the nanostructures. Furthermore, some intensity dependent characteristics were deduced indicating quantum confined properties of these nano structures. (author)

One-step green synthesis of cuprous oxide crystals with truncated octahedra shapes via a high pressure flux approach

International Nuclear Information System (INIS)

Li Benxian; Wang Xiaofeng; Xia Dandan; Chu Qingxin; Liu Xiaoyang; Lu Fengguo; Zhao Xudong

2011-01-01

Cuprous oxide (Cu 2 O) was synthesized via reactions between cupric oxide (CuO) and copper metal (Cu) at a low temperature of 300 deg. C. This progress is green, environmentally friendly and energy efficient. Cu 2 O crystals with truncated octahedra morphology were grown under high pressure using sodium hydroxide (NaOH) and potassium hydroxide (KOH) with a molar ratio of 1:1 as a flux. The growth mechanism of Cu 2 O polyhedral microcrystals are proposed and discussed. - Graphical Abstract: The Cu 2 O crystals with truncated octahedral shape were one-step synthesized in high yield via high pressure flux method for the first time, which is green and environmentally friendly. The mechanisms of synthesis and crystal growth were discussed in this paper. Highlights: → Cuprous oxide was one-step green synthesized by high pressure flux method. → The approach was based on the reverse dismutation reactions between cupric oxide and copper metal. → This progress is green, environmentally friendly and energy efficient. → The synthesized Cu2O crystals were of truncated octahedra morphology.

DSC and HRTEM investigation of the precipitates in Al-1.0%Mg{sub 2} Si-0.5%Ag alloy

Energy Technology Data Exchange (ETDEWEB)

Gaber, A.; Ali, A.M.; Zou, Y. [Toyama University (Japan). Venture Business Laboratory; Matsuda, K.; Ikeno, S. [Toyama University (Japan). Faculty of Engineering

2004-12-15

The understanding and control of nanoscale precipitation in an Al-1.0 wt-%Mg{sub 2} Si-0.5 wt-% Ag alloy during artificial aging is critical for achieving optimum mechanical properties. To achieve this objective, both differential scanning calorimetry (DSC) and high resolution transmission electron microscopy (HRTEM) have been utilised. The non-isothermal DSC thermograms exhibited eight reaction peaks; six are exothermic (precipitation) and two are endothermic (dissolution) reactions. The activation energies associated with the individual precipitates are determined. With the aid of HRTEM, the evolved precipitates have been characterised. (author)

Synthesis and Characterization of K-Ta Mixed Oxides for Hydrogen Generation in Photocatalysis

Directory of Open Access Journals (Sweden)

Beata Zielińska

2012-01-01

Full Text Available K-Ta mixed oxides photocatalysts have been prepared by impregnation followed by calcination. The influence of the reaction temperature (450°C–900°C on the phase formation, crystal morphology, and photocatalytic activity in hydrogen generation of the produced materials was investigated. The detailed analysis has revealed that all products exhibit high crystallinity and irregular structure. Moreover, two different crystal structures of potassium tantalates such as KTaO3 and K2Ta4O11 were obtained. It was also found that the sample composed of KTaO3 and traces of unreacted Ta2O5 (annealed at 600°C exhibits the highest activity in the reaction of photocatalytic hydrogen generation. The crystallographic phases, optical and vibronic properties were examined by X-ray diffraction (XRD and diffuse reflectance (DR UV-vis and resonance Raman spectroscopic methods, respectively. Morphology and chemical composition of the produced samples were studied using a high-resolution transmission electron microscope (HR-TEM and an energy dispersive X-ray spectrometer (EDX as its mode.

Analysis of thermal treatment effects upon optico-luminescent and scintillation characteristics of oxide and chalcogenide crystals

International Nuclear Information System (INIS)

Ryzhikov, Vladimir D.; Grinyov, Boris V.; Pirogov, Evgeniy N.; Galkin, Sergey N.; Nagornaya, Lyudmila L.; Bondar, Vladimir G.; Babiychuk, Inna P.; Krivoshein, Vadim I.; Silin, Vitaliy I.; Lalayants, Alexandr I.; Voronkin, Evgeniy F.; Katrunov, Konstantin A.; Onishchenko, Gennadiy M.; Vostretsov, Yuriy Ya.; Malyi, Pavel Yu.; Lisetskaya, Elena K.; Lisetskii, Longin N.

2005-01-01

This work has been aimed at analyzing the effects of various thermal treatment factors upon optical-luminescent, scintillation and other functional characteristics of complex oxide and chalcogenide crystals. The crystals considered in this work are scintillators with intrinsic (PWO, CWO, BGO), activator (GSO:Ce) or complex-defect ZnSe(Te) type of luminescence. Important factors of thermal treatment are not only the temperature and its variation with time, but also the chemical composition of the annealing medium, its oxidation-reduction properties

The crystal structure of tris(thenoyltrifluoroacetonato)bis(triphenylphosphine oxide)neodymium(III)

International Nuclear Information System (INIS)

Leipoldt, J.G.; Bok, L.D.C.; Laubscher, A.E.; Basson, S.S.

1975-01-01

The crystal structure of tris(thenoyltrifluoroacetonato)bis= x (triphenylphosphine oxide)neodymium(III), (Nd(TTa) 3 .2TPPO), has been determined by single crystal X-ray diffraction. A total number of 5505 independent reflections was used for the structure determination. The complex crystallized in the triclinic space group P 1 - with two molecules in the unit cell. The cell dimensions are a = 23.64 A, b Z= 12.15 A, C 11.19 A, α = 109.4 0 , β = 104.2 0 , γ = 90.8 0 . The final calculated R vale is 8.4%. The molecule is monomeric and the neodymium atom is coordinated to eight oxygen atoms (six from the three thenoyltrifluoroacetone groups and two from the two triphenylphosphine groups) which form a dodecahedron. The average neodymium-oxygen bond length is 2.44 A. (author)

High-pressure phases in the system W-O. Pt. 2

International Nuclear Information System (INIS)

Barabanenkov, Yu.A.; Zakharov, N.D.; Zibrov, I.P.; Filonenko, V.P.; Werner, P.; Popov, A.I.; Valkovskii, M.D.

1993-01-01

A new type of tungsten oxide has been synthesized from a mixture of W and WO 3 by a solid-phase sintering method under high-pressure conditions. The crystal structure of the new oxide was investigated by HRTEM, selected-area electron diffraction and X-ray powder diffraction. The structure belongs to space group Pbam or P2 1 2 1 2 and has the following unit-cell parameters: a=21.431(9), b=17.766(7), c=3.783(2) A, V=1440 A 3 , Z=32, D x =8.33 g cm -3 . The structural model and W-cation positions were determined by HRTEM and image processing. X-ray powder analysis and the SHELX computer program were used to prove the proposed structural model: N=158, R=0.075, U iso (W)=0.019(3), U iso (O)=0.055(12) A 2 . The investigated crystal structure is, in fact, similar to WO 2.72 and is formed by W-O octahedra and pentagonal bipyramids. (orig.)

Crystallization and unusual rheological behavior in poly(ethylene oxide)–clay nanocomposites

KAUST Repository

Kelarakis, Antonios; Giannelis, Emmanuel P.

2011-01-01

We report a systematic study of the crystallization and rheological behavior of poly(ethylene oxide) (PEO)-clay nanocomposites. To that end a series of nanocomposites based on PEOs of different molecular weight (103 < MW < 105 g/mol) and clay

Physical and electrochemical study of cobalt oxide nano- and microparticles

Energy Technology Data Exchange (ETDEWEB)

Alburquenque, D. [Dpto. de Química de los Materiales, USACh, Av. L.B.O.‘Higgins 3363, 9170022 Santiago (Chile); Dpto. de Metalurgia, USACh, Av. Ecuador 3469, 9170124, Santiago (Chile); Vargas, E. [Dpto. de Física, USACh and CEDENNA, Av. Ecuador 3493, 9170124 Santiago (Chile); Dpto. de Metalurgia, USACh, Av. Ecuador 3469, 9170124, Santiago (Chile); Denardin, J.C.; Escrig, J. [Dpto. de Física, USACh and CEDENNA, Av. Ecuador 3493, 9170124 Santiago (Chile); Marco, J.F. [Instituto de Química Física “Rocasolano”, CSIC, c/Serrano 119, 28006 Madrid (Spain); Ortiz, J. [Dpto. de Química de los Materiales, USACh, Av. L.B.O.‘Higgins 3363, 9170022 Santiago (Chile); Gautier, J.L., E-mail: juan.gautier@usach.cl [Dpto. de Química de los Materiales, USACh, Av. L.B.O.‘Higgins 3363, 9170022 Santiago (Chile)

2014-07-01

Cobalt oxide nanocrystals of size 17–21 nm were synthesized by a simple reaction between cobalt acetate (II) and dodecylamine. On the other hand, micrometric Co{sub 3}O{sub 4} was prepared using the ceramic method. The structural examination of these materials was performed using powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and transmission electron microscopy (TEM and HRTEM). XRD studies showed that the oxides were pure, well-crystallized, spinel cubic phases with a-cell parameter of 0.8049 nm and 0.8069 nm for the nano and micro-oxide, respectively. The average particle size was 19 nm (nano-oxide) and 1250 μm (micro-oxide). Morphological studies carried out by SEM and TEM analyses have shown the presence of octahedral particles in both cases. Bulk and surface properties investigated by X-ray photoelectron spectroscopy (XPS), point zero charge (pzc), FTIR and cyclic voltammetry indicated that there were no significant differences in the composition on both materials. The magnetic behavior of the samples was determined using a vibrating sample magnetometer. The compounds showed paramagnetic character and no coercivity and remanence in all cases. Galvanostatic measurements of electrodes formed with nanocrystals showed better performance than those built with micrometric particles. - Highlights: • Spinel Co{sub 3}O{sub 4} nanoparticles and microparticles with same structure but with different cell parameters, particle size and surface area were synthesized. • Oxide nanoparticles showed better electrochemical behavior than micrometric ones due to area effect.

Chemical inhomogeneity in InxGa1-xN and ZnO. A HRTEM study on atomic scale clustering

International Nuclear Information System (INIS)

Bartel, T.P.

2008-01-01

Nanostructuration as well as the nucleation and growth of nanoparticles pervades the development of modern materials and devices. Quantitative high resolution transmission electron microscopy (HRTEM) is currently being developed for a structural and chemical analysis at an atomic scale. It is used in this thesis to study the chemical inhomogeneity and clustering in In x Ga 1-x N, InN and ZnO. A methodology for reliable quantitative HRTEM is rst de ned: it necessitates a damage free sample, the avoidance of electron beam damage and the control of microscope instabilities. With these conditions satis ed, the reliability of quantitative HRTEM is demonstrated by an accurate measurement of lattice relaxation in a thin TEM sample. Clustering in an alloy can then be distinguished from a random distribution of atoms. In In x Ga 1-x N for instance, clustering is detected for concentrations x>0.1. The sensitivity is insufficient to determine whether clustering is present for lower concentrations. HRTEM allows to identify the amplitude and the spatial distribution of the decomposition which is attributed to a spinodal decomposition. In InN, nanometer scale metallic indium inclusions are detected. With decreasing size of the metallic clusters, the photoluminescence of the sample shifts towards the infrared. This indicates that the inclusions may be responsible for the infrared activity of InN. Finally, ZnO grown homoepitaxially on zinc-face and oxygen-face substrates is studied. The O-face epilayer is strained whereas the Zn-face epilayer is almost strain free and has a higher crystalline quality. Quantitative analysis of exit wave phases is in good agreement with simulations, but the signal to noise ratio needs to be improved for the detection of single point defects. (orig.)

Microstructure imaging of the YBCO thin film/MgO substrate interface: HRTEM and Fourier analysis of the Moire fringe pattern

International Nuclear Information System (INIS)

Auzary, S.; Pailloux, F.; Denanot, M.F.; Gaboriaud, R.J.

1998-01-01

Detailed microstructural aspects of the interface between YBaCuO thin films and MgO substrate are studied by means of a Fourier analysis of Moire fringe pattern obtained from HRTEM investigations of plan view samples. The main features of the observations are large, well oriented crystallographic domains surrounded by wide boundaries. HRTEM investigations together with the Fourier analysis show evidence of both orthorhombic and pseudo-tetragonal structure in the YBaCuO film. An accommodation mechanism is suggested from the Fourier analysis of the Moire fringe pattern. (orig.)

Crystallization and deuterium permeation behaviors of yttrium oxide coating prepared by metal organic decomposition

Directory of Open Access Journals (Sweden)

Takumi Chikada

2016-12-01

Full Text Available Yttrium oxide coatings were fabricated on reduced activation ferritic/martensitic steels by metal organic decomposition with a dip-coating technique, and their deuterium permeation behaviors were investigated. The microstructure of the coatings varied with heat-treatment temperature: amorphous at 670ºC (amorphous coating and crystallized at 700ºC (crystallized coating. Deuterium permeation flux of the amorphous coating was lower than the uncoated steel by a factor of 5 at 500ºC, while that of the crystallized coating was lower by a factor of around 100 at 400‒550ºC. The permeation fluxes of both coatings were drastically decreased during the measurements at higher temperatures by a factor of up to 790 for the amorphous coating and 1000 for the crystallized one, indicating a microstructure modification occurred by an effect of test temperature with hydrogen flux. Temperature dependence of deuterium diffusivity in the coatings suggests that the decrease of the permeation flux has been derived from a decrease of the diffusivity. Characteristic permeation behaviors were observed with different annealing conditions; however, they can be interpreted using the permeation mechanism clarified in the previous erbium oxide coating studies.

HR-TEM and FT-Raman dataset of the caffeine interacted Phe–Phe peptide nanotube for possible sensing applications

Directory of Open Access Journals (Sweden)

A. Lakshmi Narayanan

2018-02-01

Full Text Available Sensing ability of caffeine interaction with Phe-Phe annotates (PNTs, is presented (Govindhan et al., 2017; Karthikeyan et al., 2014; Tavagnacco et al., 2013; Kennedy et al., 2011; Wang et al., 2017 [1–5] in this data set. Investigation of synthesized caffeine carrying peptide nanotubes are carried out by FT-Raman spectral analysis and high resolution transmission electron microscopy (HR-TEM. Particle size of the caffeine loaded PNTs is < 40 nm. The FT-Raman spectrum signals are enhanced in the region of 400–1700 cm−1. These data are ideal tool for the applications like biosensing and drug delivery research (DDS. Keywords: Caffeine, PNTs, Sensing, HR-TEM, FT-Raman data

Rapid hydrothermal route to synthesize cubic-phase gadolinium oxide nanorods

International Nuclear Information System (INIS)

Hazarika, Samiran; Paul, Nibedita; Mohanta, Dambarudhar

2014-01-01

An inexpensive fabrication route and growth mechanism is being reported for obtaining quality gadolinium oxide ( Gd 2 O 3 ) nanoscale rods. The elongated nanoscale systems, as produced via a hydrothermal process, were characterized by X-ray diffraction (XRD), high resolution transmission electron microscopy (HRTEM), optical absorption spectroscopy, photoluminescence (PL) spectroscopy, Raman spectroscopy and magnetic hysteresis measurements. XRD patterns of the nanorods, as-prepared from independent precursors of different pH, depict a cubic crystal phase and an average crystallite size of 5-6.5 nm. As revealed from HRTEM micrographs, diameter of the nanorods prepared at pH = 13.3 (∼7 nm) was much smaller than the rods prepared at pH = 10.8 (∼19 nm). However, the aspect ratio was more than double in the former case than the latter case. PL response was found to be dominated by defect mediated emissions, whereas Raman spectrum of a given specimen (pH = 10.8) has revealed characteristic F g + A g modes of cubic phase of Gd 2 O 3 nanorods, apart from other independent modes. Furthermore, M ∼ H plot of the nanorod system (pH = 10.8) exhibited slight departure from the ideal superparamagnetic behaviour, with low remanence and coercive field values. The exploitation of one-dimensional Gd 2 O 3 nanorods have immense potential in the production of advanced contrast agents, smart drives and also in making novel ferrofluids of technological relevance. (author)

Spectroscopy of photonic band gaps in mesoporous one-dimensional photonic crystals based on aluminum oxide

International Nuclear Information System (INIS)

Gorelik, V.S.; Voinov, Yu.P.; Shchavlev, V.V.; Bi, Dongxue; Shang, Guo Liang; Fei, Guang Tao

2017-01-01

Mesoporous one-dimensional photonic crystals based on aluminum oxide have been synthesized by electrochemical etching method. Reflection spectra of the obtained mesoporous samples in a wide spectral range that covers several band gaps are presented. Microscopic parameters of photonic crystals are calculated and corresponding reflection spectra for the first six band gaps are presented.

Ion-induced crystal damage during plasma-assisted MBE growth of GaN layers

Science.gov (United States)

Kirchner, V.; Heinke, H.; Birkle, U.; Einfeldt, S.; Hommel, D.; Selke, H.; Ryder, P. L.

1998-12-01

Gallium nitride layers were grown by plasma-assisted molecular-beam epitaxy on (0001)-oriented sapphire substrates using an electron cyclotron resonance (ECR) and a radio frequency (rf) plasma source. An applied substrate bias was varied from -200 to +250 V, resulting in a change of the density and energy of nitrogen ions impinging the growth surface. The layers were investigated by high-resolution x-ray diffractometry and high-resolution transmission electron microscopy (HRTEM). Applying a negative bias during growth has a marked detrimental effect on the crystal perfection of the layers grown with an ECR plasma source. This is indicated by a change in shape and width of (0002) and (202¯5) reciprocal lattice points as monitored by triple axis x-ray measurements. In HRTEM images, isolated basal plane stacking faults were found, which probably result from precipitation of interstitial atoms. The crystal damage in layers grown with a highly negative substrate bias is comparable to that observed for ion implantation processes at orders of magnitude larger ion energies. This is attributed to the impact of ions on the growing surface. None of the described phenomena was observed for the samples grown with the rf plasma source.

Study of phase separation and crystallization phenomena in soda-lime borosilicate glass enriched in MoO3

International Nuclear Information System (INIS)

Magnin, M.

2009-09-01

Molybdenum oxide immobilization (MoO 3 , as fission product) is one of the major challenges in the nuclear glass formulation issues for high level waste solutions conditioning since many years, these solutions arising from spent nuclear fuel reprocessing. Phase separation and crystallisation processes may arise in molten glass when the MoO 3 content is higher than its solubility limit that may depend on glass composition. Molybdenum combined with other elements such as alkali and alkaline-earth may form crystalline molybdates, known as 'yellow phases' in nuclear glasses which may decrease the glass durability. In order to confine high level wastes (HLW) such as the fission product solutions arising from the reprocessing of high burn-up UOX-type nuclear spent fuels, a new glass composition (HLW glass) is being optimized. This work is devoted to the study of the origin and the mechanism of phase separation and crystallization phenomena induced by molybdenum oxide incorporation in the HLW glass. From microstructural and structural point of view, the molybdenum oxide behavior was studied in glass compositions belonging to the SiO 2 -B 2 O 3 - Na 2 O-CaO simplified system which constituted basis for the HLW glass formulation. The structural role of molybdenum oxide in borosilicate network explaining the phase separation and crystallization tendency was studied through the coupling of structural ( 95 Mo, 29 Si, 11 B, 23 Na MAS NMR, XRD) and microstructural (SEM, HRTEM) analysis techniques. The determination of phase separation (critical temperature) and crystallization (liquidus temperature) appearance temperatures by in situ viscosimetry and Raman spectroscopy experiments allowed us to propose a transformation scenario during melt cooling. These processes and the nature of the crystalline phases formed (CaMoO 4 , Na 2 MoO 4 ) that depend on the evolution of MoO 3 , CaO and B 2 O 3 contents were correlated with changes of sodium and calcium cations proportions in the

Clustered atom-replaced structure in single-crystal-like metal oxide

Science.gov (United States)

Araki, Takeshi; Hayashi, Mariko; Ishii, Hirotaka; Yokoe, Daisaku; Yoshida, Ryuji; Kato, Takeharu; Nishijima, Gen; Matsumoto, Akiyoshi

2018-06-01

By means of metal organic deposition using trifluoroacetates (TFA-MOD), we replaced and localized two or more atoms in a single-crystalline structure having almost perfect orientation. Thus, we created a new functional structure, namely, clustered atom-replaced structure (CARS), having single-crystal-like metal oxide. We replaced metals in the oxide with Sm and Lu and localized them. Energy dispersive x-ray spectroscopy results, where the Sm signal increases with the Lu signal in the single-crystalline structure, confirm evidence of CARS. We also form other CARS with three additional metals, including Pr. The valence number of Pr might change from 3+ to approximately 4+, thereby reducing the Pr–Ba distance. We directly observed the structure by a high-angle annular dark-field image, which provided further evidence of CARS. The key to establishing CARS is an equilibrium chemical reaction and a combination of additional larger and smaller unit cells to matrix cells. We made a new functional metal oxide with CARS and expect to realize CARS in other metal oxide structures in the future by using the above-mentioned process.

CTAB assisted synthesis of tungsten oxide nanoplates as an efficient low temperature NOX sensor

Science.gov (United States)

Mehta, Swati S.; Tamboli, Mohaseen S.; Mulla, Imtiaz S.; Suryavanshi, Sharad S.

2018-02-01

Tungsten oxide nanoplates with porous morphology were effectively prepared by acidification using CTAB (HexadeCetyltrimethyl ammonium bromide) as a surfactant. For characterization, the synthesized materials were subjected to X-Ray powder diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), UV-Visible spectroscopy (UV-Vis) and surface area (BET) measurements. The morphology and size of the particles were controlled by solution acidity. The BET results confirmed that the materials are well crystallized and mesoporous in nature. The nanocrystalline powder was used to prepare thick films by screen printing on alumina substrate for the investigation of gas sensing properties. The gas response measurements revealed that the samples acidified using 10 M H2SO4 exhibits highest response of 91% towards NOX at optimum temperature of 200 °C for 100 ppm, and it also exhibits 35% response at room temperature.

Oxygen Barrier Properties and Melt Crystallization Behavior of Poly(ethylene terephthalate/Graphene Oxide Nanocomposites

Directory of Open Access Journals (Sweden)

Anna Szymczyk

2015-01-01

Full Text Available Poly(ethylene terephthalate nanocomposites with low loading (0.1–0.5 wt% of graphene oxide (GO have been prepared by using in situ polymerization method. TEM study of nanocomposites morphology has shown uniform distribution of highly exfoliated graphene oxide nanoplatelets in PET matrix. Investigations of oxygen permeability of amorphous films of nanocomposites showed that the nanocomposites had better oxygen barrier properties than the neat PET. The improvement of oxygen permeability for PET nanocomposite films over the neat PET is approximately factors of 2–3.3. DSC study on the nonisothermal crystallization behaviors proves that GO acts as a nucleating agent to accelerate the crystallization of PET matrix. The evolution of the lamellar nanostructure of nanocomposite and neat PET was monitored by SAXS during nonisothermal crystallization from the melt. It was found that unfilled PET and nanocomposite with the highest concentration of GO (0.5 wt% showed almost similar values of the long period (L=11.4 nm for neat PET and L=11.5 nm for PET/0.5GO.

Ligand mediated synthesis of AgInSe2 nanoparticles with tetragonal/orthorhombic crystal phases

International Nuclear Information System (INIS)

Abazović, Nadica D.; Čomor, Mirjana I.; Mitrić, Miodrag N.; Piscopiello, Emanuela; Radetić, Tamara; Janković, Ivana A.; Nedeljković, Jovan M.

2012-01-01

Nanosized AgInSe 2 particles (d ∼ 7–25 nm) were synthesized using colloidal chemistry method at 270 °C. As solvents/surface ligands 1-octadecene, trioctylphosphine, and oleylamine were used. It was shown that choice of ligand has crucial impact not only on final crystal phase of nanoparticles, but also at mechanism of crystal growth. X-ray diffraction and TEM/HRTEM techniques were used to identify obtained crystal phases and to measure average size and shape of nanoparticles. UV/Vis data were used to estimate band-gap energies of obtained samples. It was shown that presented routes can provide synthesis of nanoparticles with desired crystal phase (tetragonal and/or orthorhombic), with band-gap energies in the range from 1.25 to 1.53 eV.

Growth of cadmium oxide whiskers on cadmium sulphide single crystals with copper as growth activator

Energy Technology Data Exchange (ETDEWEB)

Koparanova, N.; Simov, S. (Bylgarska Akademiya na Naukite, Sofia. Inst. po Fizika na Tvyrdoto Tyalo); Genchev, D. (Bylgarska Akademiya na Naukite, Sofia. Inst. za Yadrena Izsledvaniya i Yadrena Energetika); Metchenov, G. (Research Inst. of Criminalistics and Criminology, Sofia (Bulgaria))

1985-02-01

Some results on the growth and morphology of cadmium oxide whiskers, obtained on cadmium sulphide single crystals with copper as a growth activator, are presented in this work. Cadmium oxide whiskers have been obtained on brace 112-bar0 brace faces of cadmium sulphide plates with a copper layer deposited in advance. The whiskers grew during the annealing of the plates in a weak stream of technically pure argon at temperatures 670 to 730 deg C for 15 min to 3.5 h. Details about the procedure have been given elsewhere. The composition and morphology of the whiskers have been studied by an X-ray microanalyser JEOL 35 DDS and a scanning electron microscope JEOL, JSM 35. The optical microscopic observations have shown that after annealing, a gray-black granular layer is formed on the cadmium sulphide single crystals and this layer can easily be separated from the crystal substrate. Under the granular layer the crystal is heavily damaged. The whiskers grow on the granular layer and they are coloured yellow-brown or red-brown. The maximum whisker length attains several hundreds of micrometres and in some cases up to 1 mm or more.

Growth of cadmium oxide whiskers on cadmium sulphide single crystals with copper as growth activator

International Nuclear Information System (INIS)

Koparanova, N.; Simov, S.

1985-01-01

Some results on the growth and morphology of cadmium oxide whiskers, obtained on cadmium sulphide single crystals with copper as a growth activator, are presented in this work. Cadmium oxide whiskers have been obtained on brace 112-bar0 brace faces of cadmium sulphide plates with a copper layer deposited in advance. The whiskers grew during the annealing of the plates in a weak stream of technically pure argon at temperatures 670 to 730 deg C for 15 min to 3.5 h. Details about the procedure have been given elsewhere. The composition and morphology of the whiskers have been studied by an X-ray microanalyser JEOL 35 DDS and a scanning electron microscope JEOL, JSM 35. The optical microscopic observations have shown that after annealing, a gray-black granular layer is formed on the cadmium sulphide single crystals and this layer can easily be separated from the crystal substrate. Under the granular layer the crystal is heavily damaged. The whiskers grow on the granular layer and they are coloured yellow-brown or red-brown. The maximum whisker length attains several hundreds of micrometres and in some cases up to 1 mm or more. (author)

Synthesis of cerium oxide (CeO{sub 2}) nanoparticles using simple CO-precipitation method

Energy Technology Data Exchange (ETDEWEB)

Farahmandjou, M.; Zarinkamar, M.; Firoozabadi, T. P., E-mail: farahamndjou@iauvaramin.ac.ir [Islamis Azad University, Varamin-Phisva Branch, Department of Physics, Varamin (Iran, Islamic Republic of)

2016-11-01

Synthesis of cerium oxide (CeO{sub 2}) nanoparticles was studied by new and simple co-precipitation method. The cerium oxide nanoparticles were synthesized using cerium nitrate and potassium carbonate precursors. Their physicochemical properties were characterized by high resolution transmission electron microscopy (HRTEM), scanning electron microscopy (Sem), X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (Ftir) and UV-Vis spectrophotometer. XRD pattern showed the cubic structure of the cerium oxide nanoparticles. The average particle size of CeO{sub 2} was around 20 nm as estimated by XRD technique and direct HRTEM observations. The surface morphological studies from Sem and Tem depicted spherical particles with formation of clusters. The sharp peaks in Ftir spectrum determined the existence of CeO{sub 2} stretching mode and the absorbance peak of UV-Vis spectrum showed the bandgap energy of 3.26 eV. (Author)

Crystal growth and scintillation properties of multi-component oxide single crystals: Ce:GGAG and Ce:La-GPS

Energy Technology Data Exchange (ETDEWEB)

Yoshikawa, A., E-mail: yoshikawa@imr.tohoku.ac.jp [Institute for Materials Research (IMR), Tohoku University, Sendai 980-8577 (Japan); New Industry Creation Hatchery Center (NICHe), Tohoku University, Sendai 980-8579 (Japan); C& A Corporation, 6-6-40 Aramaki Aza Aoba, Aoba-ku, Sendai 980-8579 (Japan); Kamada, K. [New Industry Creation Hatchery Center (NICHe), Tohoku University, Sendai 980-8579 (Japan); C& A Corporation, 6-6-40 Aramaki Aza Aoba, Aoba-ku, Sendai 980-8579 (Japan); Kurosawa, S. [Institute for Materials Research (IMR), Tohoku University, Sendai 980-8577 (Japan); New Industry Creation Hatchery Center (NICHe), Tohoku University, Sendai 980-8579 (Japan); Shoji, Y. [Institute for Materials Research (IMR), Tohoku University, Sendai 980-8577 (Japan); C& A Corporation, 6-6-40 Aramaki Aza Aoba, Aoba-ku, Sendai 980-8579 (Japan); Yokota, Y. [New Industry Creation Hatchery Center (NICHe), Tohoku University, Sendai 980-8579 (Japan); Chani, V.I. [Institute for Materials Research (IMR), Tohoku University, Sendai 980-8577 (Japan); Nikl, M. [Institute of Physics, AS CR, Cukrovarnická 10, 162 53 Prague (Czech Republic)

2016-01-15

Crystal growth by micro-pulling-down, Czochralski, and floating zone methods and scintillation properties of Ce:Gd{sub 3}(Ga,Al){sub 5}O{sub 12} (Ce:GGAG) multi-component oxide garnets, and Ce:Gd{sub 2}Si{sub 2}O{sub 7} (Ce:GPS) or Ce:(La,Gd){sub 2}Si{sub 2}O{sub 7} (Ce:La-GPS) pyro-silicates are reviewed. GGAG crystals demonstrated practically linear dependences of some of the parameters including lattice constant, emission wavelength, and band gap on Ga content. However, emission intensity, light yield and energy resolution showed maxima for intermediate compositions. GGAG crystals had the highest light yield of 56,000 photon/MeV for Ga content of 2.7 atoms per garnet formula unit. Similarly the light yield and energy resolution of La-GPS showed the highest values of 40,000 photon/MeV and 4.4%@662 keV, respectively, for La-GPS containing 10% of La. Moreover, La-GPS demonstrated stable scintillation performance up to 200 °C.

Silver nanoparticles anchored reduced graphene oxide for enhanced electrocatalytic activity towards methanol oxidation

Science.gov (United States)

Kumar, Sanjeev; Mahajan, Mani; Singh, Rajinder; Mahajan, Aman

2018-02-01

In this report, silver nanoparticles (Ag NPs) anchored reduced graphene oxide (rGO) sheets (rGO/Ag) nanohybrid has been explored as anode material in direct methanol fuel cells (DMFCs). The synthesized rGO/Ag nanohybrid is characterized by XRD, XPS, FTIR spectroscopy and HRTEM techniques. Cyclic voltammograms demonstrate that the rGO/Ag nanohybrid exhibits higher electrocatalytic activity in comparison to rGO sheets for methanol oxidation reaction (MOR). This enhancement is attributed to the synergetic effect produced by the presence of more active sites provided by Ag NPs anchored on a conducting network of large surface area rGO sheets.

The Mobility Enhancement of Indium Gallium Zinc Oxide Transistors via Low-temperature Crystallization using a Tantalum Catalytic Layer

OpenAIRE

Shin, Yeonwoo; Kim, Sang Tae; Kim, Kuntae; Kim, Mi Young; Oh, Saeroonter; Jeong, Jae Kyeong

2017-01-01

High-mobility indium gallium zinc oxide (IGZO) thin-film transistors (TFTs) are achieved through low-temperature crystallization enabled via a reaction with a transition metal catalytic layer. For conventional amorphous IGZO TFTs, the active layer crystallizes at thermal annealing temperatures of 600??C or higher, which is not suitable for displays using a glass substrate. The crystallization temperature is reduced when in contact with a Ta layer, where partial crystallization at the IGZO bac...

Investigation of the nanoscale two-component ZnS-ZnO heterostructures by means of HR-TEM and X-ray based analysis

Science.gov (United States)

Pankin, I. A.; Polozhentsev, O. E.; Soldatov, M. A.; Bugaev, A. L.; Tsaturyan, A.; Lomachenko, K. A.; Guda, A. A.; Budnyk, A. P.; Lamberti, C.; Soldatov, A. V.

2018-06-01

This article is devoted to the spectroscopic characterization of ZnS-ZnO nanoscale heterostructures synthesized by the microwave-assisted solvothermal method. The synthesized samples were investigated by means of X-ray powder diffraction (XRPD), high energy resolution fluorescence detected X-ray absorption near-edge-structure (HERFD-XANES) spectroscopy, valence-to-core X-ray emission spectroscopy (VtC-XES) and high resolution transmission electron microscopy (HR-TEM) as well as energy dispersive X-ray spectroscopy (EDX). The average crystallite size estimated by the broadening of XRPD peaks increases from 2.7 nm to 3.7 nm in the temperature range from 100 °C to 150 °C. HR-TEM images show that nanoparticles are arranged in aggregates with the 60-200 nm size. Theoretical estimation shows that the systems synthesized at higher temperatures more prone to the agglomeration. The full profile Reitveld analysis of XRPD data reveals the formation of hexagonal zinc sulfide structure, whereas electron diffraction data reveal also the formation of cubic zinc sulfide and claim the polymorphous character of the system. High energy resolution Zn K-edge XANES data unambiguously demonstrate the presence of a certain amount of the zinc oxide which is likely to have an amorphous structure and could not be detected by XRPD. Qualitative analysis of XANES data allows deriving ZnS/ZnO ratio as a function of synthesis temperature. EDX analysis depicts homogeneous distribution of ZnS and amorphous ZnO phases across the conglomerates. A complementary element-selective valence to core X-ray emission spectroscopy evidences formation of two-component system and confirms estimations of ZnS/ZnO fractions obtained by linear combination fit of XANES data.

Wet etching mechanism and crystallization of indium-tin oxide layer for application in light-emitting diodes

Science.gov (United States)

Su, Shui-Hsiang; Kong, Hsieng-Jen; Tseng, Chun-Lung; Chen, Guan-Yu

2018-01-01

In the article, we describe the etching mechanism of indium-tin oxide (ITO) film, which was wet-etched using a solution of hydrochloric acid (HCl) and ferric chloride (FeCl3). The etching mechanism is analyzed at various etching durations of ITO films by scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM), and selective area diffraction (SAD) analysis. In comparison with the crystalline phase of SnO2, the In2O3 phase can be more easily transformed to In3+ and can form an inverted conical structure during the etching process. By adjusting the etching duration, the residual ITO is completely removed to show a designed pattern. This is attributed to the negative Gibbs energy of In2O3 transformed to In3+. The result also corresponds to the finding of energy-dispersive X-ray spectroscopy (EDS) analysis that the Sn/In ratio increases with increasing etching duration.

Studies on oxidation and deuterium permeation behavior of a low temperature α-Al_2O_3-forming Fe−Cr−Al ferritic steel

International Nuclear Information System (INIS)

Xu, Yu-Ping; Zhao, Si-Xiang; Liu, Feng; Li, Xiao-Chun; Zhao, Ming-Zhong; Wang, Jing; Lu, Tao; Hong, Suk-Ho; Zhou, Hai-Shan; Luo, Guang-Nan

2016-01-01

To evaluate the capability of Fe−Cr−Al ferritic steels as tritium permeation barrier in fusion systems, the oxidation behavior together with the permeation behavior of a Fe−Cr−Al steel was investigated. Gas driven permeation experiments were performed. The permeability of the oxidized Fe−Cr−Al steel was obtained and a reduced activation ferritic/martensitic steel CLF-1 was used as a comparison. In order to characterize the oxide layer, SEM, XPS, TEM, HRTEM were used. Al_2O_3 was detected in the oxide film by XPS, and HRTEM showed that Al_2O_3 in the α phase was found. The formation of α-Al_2O_3 layer at a relatively low temperature may result from the formation of Cr_2O_3 nuclei.

Crystal and molecular structure of dichlorodioxobis (triphenylphosphine oxide)uranium(VI)

Energy Technology Data Exchange (ETDEWEB)

Bombieri, G; Forsellini, E [Consiglio Nazionale delle Ricerche, Padua (Italy). Lab. di Chimica e Tecnologia dei Radioelementi; Day, J P; Azeez, W I

1978-01-01

The crystal structure of (UO/sub 2/Cl/sub 2/(PPh/sub 3/O)/sub 2/) has been determined from three-dimensional X-ray diffraction data. Crystals are triclinic, space group P1, with a = 10.0101(6), b = 10.2589(9), c = 9.2347(8) A, ..cap alpha.. = 110.093(6). ..beta.. = 92.129(6), and ..gamma.. = 78.384(6), and Z = 1. The structure has been solved by the heavy-atom method from counter data, and refined by least squares to a final R of 0.054. The coordination polyhedron around uranium is a distorted octahedron, with a linear uranyl group (U-O 1.764A) perpendicular to a plane in which the two chloride and two oxide ions trans to each other occupy the corners of a rectangle (U-O 2.300; U-Cl 2.645 A).

The early stages of oxidation of magnesium single crystal surfaces

International Nuclear Information System (INIS)

Hayden, B.E.; Schweizer, E.; Koetz, R.; Bradshaw, A.M.

1981-01-01

The early stages of oxidation of Mg(001) and Mg(100) single crystal surfaces at 300 K have been investigated by LEED, ELS, work function and ellipsometric measurements. A sharp decrease in work function on both surfaces during the first 12 L exposure indicates the incorporation of oxygen in the earliest stages of the interaction. The incorporated oxygen on Mg(001) gives rise to a broadening of the integral order LEED spots for an exposure 3 L. (orig.)

Thin films of metal oxides on metal single crystals: Structure and growth by scanning tunneling microscopy

International Nuclear Information System (INIS)

Galloway, H.C.

1995-12-01

Detailed studies of the growth and structure of thin films of metal oxides grown on metal single crystal surfaces using Scanning Tunneling Microscopy (STM) are presented. The oxide overlayer systems studied are iron oxide and titanium oxide on the Pt(III) surface. The complexity of the metal oxides and large lattice mismatches often lead to surface structures with large unit cells. These are particularly suited to a local real space technique such as scanning tunneling microscopy. In particular, the symmetry that is directly observed with the STM elucidates the relationship of the oxide overlayers to the substrate as well as distinguishing, the structures of different oxides

Crystal Growth Technology

Science.gov (United States)

Scheel, Hans J.; Fukuda, Tsuguo

2004-06-01

This volume deals with the technologies of crystal fabrication, of crystal machining, and of epilayer production and is the first book on industrial and scientific aspects of crystal and layer production. The major industrial crystals are treated: Si, GaAs, GaP, InP, CdTe, sapphire, oxide and halide scintillator crystals, crystals for optical, piezoelectric and microwave applications and more. Contains 29 contributions from leading crystal technologists covering the following topics: General aspects of crystal growth technology Silicon Compound semiconductors Oxides and halides Crystal machining Epitaxy and layer deposition Scientific and technological problems of production and machining of industrial crystals are discussed by top experts, most of them from the major growth industries and crystal growth centers. In addition, it will be useful for the users of crystals, for teachers and graduate students in materials sciences, in electronic and other functional materials, chemical and metallurgical engineering, micro-and optoelectronics including nanotechnology, mechanical engineering and precision-machining, microtechnology, and in solid-state sciences.

Physical model construction for electrical anisotropy of single crystal zinc oxide micro/nanobelt using finite element method

International Nuclear Information System (INIS)

Yu, Guangbin; Tang, Chaolong; Song, Jinhui; Lu, Wenqiang

2014-01-01

Based on conductivity characterization of single crystal zinc oxide (ZnO) micro/nanobelt (MB/NB), we further investigate the physical mechanism of nonlinear intrinsic resistance-length characteristic using finite element method. By taking the same parameters used in experiment, a model of nonlinear anisotropic resistance change with single crystal MB/NB has been deduced, which matched the experiment characterization well. The nonlinear resistance-length comes from the different electron moving speed in various crystal planes. As the direct outcome, crystallography of the anisotropic semiconducting MB/NB has been identified, which could serve as a simple but effective method to identify crystal growth direction of single crystal semiconducting or conductive nanomaterial

Physiochemical Characterization of Iodine (V Oxide Part II: Morphology and Crystal Structure of Particulate Films

Directory of Open Access Journals (Sweden)

Brian K. Little

2015-11-01

Full Text Available In this study, the production of particulate films of iodine (V oxides is investigated. The influence that sonication and solvation of suspended particles in various alcohol/ketone/ester solvents have on the physical structure of spin or drop cast films is examined in detail with electron microscopy, powder x-ray diffraction, and UV-visible absorption spectroscopy. Results indicate that sonicating iodine oxides in alcohol mixtures containing trace amounts of water decreases deposited particle sizes and produces a more uniform film morphology. UV-visible spectra of the pre-cast suspensions reveal that for some solvents, the iodine oxide oxidizes the solvent, producing I2 and lowering the pH of the suspension. Characterizing the crystals within the cast films reveal their composition to be primarily HI3O8, their orientations to exhibit a preferential orientation, and their growth to be primarily along the ac-plane of the crystal, enhanced at higher spin rates. Spin-coating at lower spin rates produces laminate-like particulate films versus higher density, one-piece films of stacked particles produced by drop casting. The particle morphology in these films consists of a combination of rods, plates, cubes, and rhombohedra structure.

Facile crystal-structure-controlled synthesis of iron oxides for adsorbents and anode materials of lithium batteries

International Nuclear Information System (INIS)

Luo, Yao; Liu, Lihu; Qiao, Wencan; Liu, Fan; Zhang, Yashan; Tan, Wenfeng; Qiu, Guohong

2016-01-01

Iron oxides exhibit excellent physicochemical properties as functional materials because of the diversity of crystal structure. Nano-sized iron oxides, including akaganite (β-FeOOH), maghemite (γ-Fe_2O_3), ferrihydrite (Fe_5HO_8∙4H_2O) and hematite (α-Fe_2O_3), were prepared by a facile reflux treatment of iron powder in NaClO solution at 50 °C for 12 h. The crystal structures were controlled by adjusting the pH values of reaction systems. Akaganite, maghemite, ferrihydrite, and hematite were formed when pHs were adjusted to 2–4, 6, 8, and 10, respectively. They showed excellent adsorption performance for As(III), and the adsorption capacity was affected by crystal structure as well as specific surface area. The maximum adsorption capacity for akaganite, maghemite, ferrihydrite, and hematite reached 89.8, 79.1, 78.4, and 63.4 mg g"−"1, respectively. Hematite showed lithium storage capacity of 2043 mAh g"−"1 for the first cycle and then kept stable after twenty cycles at a current density of 100 mA g"−"1. The discharge specific capacity stabilized at 639 mAh g"−"1 after 100 cycles. The as-prepared iron oxides might be applied as potential adsorbents and anode materials for rechargeable lithium-ion battery. - Highlights: • Nano-sized ferric oxides were fabricated by refluxing iron powder in NaClO solutions. • Crystal structures were controlled by adjusting pHs from 2.0 to 10.0 in systems. • Akaganite exhibited the largest As(III) adsorption capacity of 89.8 mg g"−"1. • Hematite had lithium storage capacity of 639 mAh g"−"1 after 100 cycles.

Facile crystal-structure-controlled synthesis of iron oxides for adsorbents and anode materials of lithium batteries

Energy Technology Data Exchange (ETDEWEB)

Luo, Yao; Liu, Lihu; Qiao, Wencan; Liu, Fan [College of Resources and Environment, Huazhong Agricultural University, Wuhan, 430070 (China); Zhang, Yashan [Department of Chemistry, University of Connecticut, Storrs, 55 North Eagleville Road, Storrs, CT, 06269 (United States); Tan, Wenfeng [College of Resources and Environment, Huazhong Agricultural University, Wuhan, 430070 (China); Qiu, Guohong, E-mail: qiugh@mail.hzau.edu.cn [College of Resources and Environment, Huazhong Agricultural University, Wuhan, 430070 (China)

2016-02-15

Iron oxides exhibit excellent physicochemical properties as functional materials because of the diversity of crystal structure. Nano-sized iron oxides, including akaganite (β-FeOOH), maghemite (γ-Fe{sub 2}O{sub 3}), ferrihydrite (Fe{sub 5}HO{sub 8}∙4H{sub 2}O) and hematite (α-Fe{sub 2}O{sub 3}), were prepared by a facile reflux treatment of iron powder in NaClO solution at 50 °C for 12 h. The crystal structures were controlled by adjusting the pH values of reaction systems. Akaganite, maghemite, ferrihydrite, and hematite were formed when pHs were adjusted to 2–4, 6, 8, and 10, respectively. They showed excellent adsorption performance for As(III), and the adsorption capacity was affected by crystal structure as well as specific surface area. The maximum adsorption capacity for akaganite, maghemite, ferrihydrite, and hematite reached 89.8, 79.1, 78.4, and 63.4 mg g{sup −1}, respectively. Hematite showed lithium storage capacity of 2043 mAh g{sup −1} for the first cycle and then kept stable after twenty cycles at a current density of 100 mA g{sup −1}. The discharge specific capacity stabilized at 639 mAh g{sup −1} after 100 cycles. The as-prepared iron oxides might be applied as potential adsorbents and anode materials for rechargeable lithium-ion battery. - Highlights: • Nano-sized ferric oxides were fabricated by refluxing iron powder in NaClO solutions. • Crystal structures were controlled by adjusting pHs from 2.0 to 10.0 in systems. • Akaganite exhibited the largest As(III) adsorption capacity of 89.8 mg g{sup −1}. • Hematite had lithium storage capacity of 639 mAh g{sup −1} after 100 cycles.

Comparison Study on the Microstructure of Nanocrystalline TiO2 in Different Ti-Si Binary Oxides

Institute of Scientific and Technical Information of China (English)

无

2007-01-01

Three different Ti-Si oxide structuares, silica supported titania, silica coated titania and intimately mixed silicatitania, containing 10%-40% SiO2, were made by sol-gel process. The variations of microstructure parameters of nanocrystalline (nc) TiO2-anatase in the three kirds of binary oxides, including in-plane spacing d, cell constants (a0, CQ), cell volume V, cell axial ratio c0/a0 and crystal grain size, were comparatively investigated by high resolution transmission electron microscopy (HRTEM) and X-ray diffraction (XRD). It is found that the microstructure parameters vary remarkably with increasing SiO2 content and annealing temperature. Different structured Ti-Si binary oxides lead to different variation tendencies of microstructure parameters. The more SiO2 the binary oxide contains, the more lattice defects of nc TiO2-anatase appear; diffusion or migration of Si cations could be an important influential factor in the variations of microstructure. The grain size of nc TiO2 in the three kinds of binary oxides not only depends on SiO2 content and annealing temperature but also on the degree of lattice microstrain and distortion of nc TiO2-anatase. Both grain size and phase transformation of nc TiO2-anatase are effectively inhibited with increasing SiOa content.

Ceramic/metal nanocomposites by lyophilization: Processing and HRTEM study

International Nuclear Information System (INIS)

Gutierrez-Gonzalez, C.F.; Agouram, S.; Torrecillas, R.; Moya, J.S.; Lopez-Esteban, S.

2012-01-01

Highlights: ► A cryogenic route has been used to obtain ceramic/metal nanostructured powders. ► The powders present good homogeneity and dispersion of metal. ► The metal nanoparticle size distributions are centred in 17–35 nm. ► Both phases, ceramic and metal, present a high degree of crystallinity. ► Good metal/ceramic interfaces due to epitaxial growth, studied by HRTEM. -- Abstract: This work describes a wet-processing route based on spray-freezing and subsequent lyophilization designed to obtain nanostructured ceramic/metal powders. Starting from the ceramic powder and the corresponding metal salt, a water-based suspension is sprayed on liquid nitrogen. The frozen powders are subsequently freeze-dried, calcined and reduced. The material was analyzed using X-ray diffraction analysis at all stages. High resolution transmission electron microscopy studies showed a uniform distribution of metal nanoparticles on the ceramic grain surfaces, good interfaces and high crystallinity, with an average metal particle size in the nanometric range.

Hydrothermal deposition and characterization of silicon oxide nanospheres

International Nuclear Information System (INIS)

Pei, L.Z.

2008-01-01

Silicon oxide nanospheres with the average diameter of about 100 nm have been synthesized by hydrothermal deposition process using silicon and silica as the starting materials. The silicon oxide nanospheres were characterized by field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectrum (EDS), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and photoluminescence (PL) spectrum, respectively. The results show that large scale silicon oxide nanospheres with the uniform size are composed of Si and O showing the amorphous structure. Strong PL peak at 435 nm is observed demonstrating the good blue light emission property

DT fusion neutron irradiation of ORNL magnesium oxide crystals and BNL--LASL superconductor wires

International Nuclear Information System (INIS)

MacLean, S.C.

1978-01-01

The DT fusion neutron irradiation of two ORNL magnesium oxide crystals and eleven BNL-LASL superconductor wires is described. The sample position and neutron dose record are given. The maximum neutron fluence on any sample was 2.16 x 10 16 neutrons/cm 2

Chemical inhomogeneity in In{sub x}Ga{sub 1-x}N and ZnO. A HRTEM study on atomic scale clustering

Energy Technology Data Exchange (ETDEWEB)

Bartel, T.P.

2008-10-08

Nanostructuration as well as the nucleation and growth of nanoparticles pervades the development of modern materials and devices. Quantitative high resolution transmission electron microscopy (HRTEM) is currently being developed for a structural and chemical analysis at an atomic scale. It is used in this thesis to study the chemical inhomogeneity and clustering in In{sub x}Ga{sub 1-x}N, InN and ZnO. A methodology for reliable quantitative HRTEM is rst de ned: it necessitates a damage free sample, the avoidance of electron beam damage and the control of microscope instabilities. With these conditions satis ed, the reliability of quantitative HRTEM is demonstrated by an accurate measurement of lattice relaxation in a thin TEM sample. Clustering in an alloy can then be distinguished from a random distribution of atoms. In In{sub x}Ga{sub 1-x}N for instance, clustering is detected for concentrations x>0.1. The sensitivity is insufficient to determine whether clustering is present for lower concentrations. HRTEM allows to identify the amplitude and the spatial distribution of the decomposition which is attributed to a spinodal decomposition. In InN, nanometer scale metallic indium inclusions are detected. With decreasing size of the metallic clusters, the photoluminescence of the sample shifts towards the infrared. This indicates that the inclusions may be responsible for the infrared activity of InN. Finally, ZnO grown homoepitaxially on zinc-face and oxygen-face substrates is studied. The O-face epilayer is strained whereas the Zn-face epilayer is almost strain free and has a higher crystalline quality. Quantitative analysis of exit wave phases is in good agreement with simulations, but the signal to noise ratio needs to be improved for the detection of single point defects. (orig.)

Reversible conversion of valence-tautomeric copper metal-organic frameworks dependent single-crystal-to-single-crystal oxidation/reduction: a redox-switchable catalyst for C-H bonds activation reaction.

Science.gov (United States)

Huang, Chao; Wu, Jie; Song, Chuanjun; Ding, Ran; Qiao, Yan; Hou, Hongwei; Chang, Junbiao; Fan, Yaoting

2015-06-28

Upon single-crystal-to-single-crystal (SCSC) oxidation/reduction, reversible structural transformations take place between the anionic porous zeolite-like Cu(I) framework and a topologically equivalent neutral Cu(I)Cu(II) mixed-valent framework. The unique conversion behavior of the Cu(I) framework endowed it as a redox-switchable catalyst for the direct arylation of heterocycle C-H bonds.

Growth and time dependent alignment of KCl crystals in Hemoglobin LB monolayer

International Nuclear Information System (INIS)

Mahato, Mrityunjoy; Pal, Prabir; Tah, Bidisha; Kamilya, Tapanendu; Talapatra, G.B.

2012-01-01

Nature and organism often use the biomineralization technique to build up various highly regular structures such as bone, teeth, kidney stone etc., and recently this becomes the strategy to design and synthesis of novel biocomposite materials. We report here the controlled crystallization of KCl in Langmuir and Langmuir Blodgett (LB) monolayer of Hemoglobin (Hb) at ambient condition. The nucleation and growth of KCl crystals in Hb monolayer has temporal and KCl concentration dependency. The growth of KCl crystals in LB film of Hb has distinct behavior in the alignment of crystals from linear to fractal like structures depending on growth time. The crystallographic identity of the biomineralized KCl crystal is confirmed from HR-TEM, XRD, and from powder diffraction simulation. Our results substantiated that the template of Langmuir monolayer of proteins plays a crucial role in biomineralization as well as in designing and synthesizing of novel biocomposite materials. Highlights: ► Biomineralization of KCl crystal has been studied in Hemoglobin LB film. ► KCl crystal growth is time and concentration of KCl dependent. ► The alignment of KCl crystal growth is fractal nature with time. ► The unfolding of Hb and evaporation factor has some role in crystallization and fractal growth.

A study of magnetoplumbite-type (M-type) cobalt-titanium-substituted barium ferrite, BaCoxTixFe12-2xO19 (x = 1-6)

International Nuclear Information System (INIS)

Teh, G.B.; Saravanan, N.; Jefferson, D.A.

2007-01-01

Cobalt(II)-titanium(IV)-substituted barium ferrite forming the chemical formula of BaCo x Ti x Fe 12-2x O 19 (x = 1-6) have been investigated using X-ray diffraction spectroscopy (XRD), Superconducting Quantum Interference Device (SQUID) and high-resolution transmission electron microscopy (HRTEM). The specimen of magnetoplumbite (M-type) Co-Ti-substituted BaFe 12 O 19 were synthesised via sol-gel method using ethylene glycol as precursor. Significant increase in line broadening of the XRD patterns were observed indicating the decrease of particle sizes due to the Co(II)-Ti(IV) substitution. BaCo 3 Ti 3 Fe 6 O 19 showed the highest coercivity but moderate saturation and remnant magnetisations. HRTEM imaging showed that Co(II)-Ti(IV) substitution in the system of BaCo x Ti x Fe 12-2x O 19 (x = 1-6) produced no drastic change in the structure of the M-type ferrites. Most of the M-types crystals examined by HRTEM displayed a long axis perpendicular to the c-axis of the M-type structure. Disordered crystals showing the intergrowth between Co-Ti-substituted barium ferrite and the spinel-structured iron oxide were detected

Indium-tin oxide surface treatments: Effects on the performance of liquid crystal devices

International Nuclear Information System (INIS)

Abderrahmen, A.; Romdhane, F.F.; Ben Ouada, H.; Gharbi, A.

2006-01-01

In this work, we investigate the effect of indium tin oxide (ITO) substrate cleaning on the surface properties. Wettability technique was used to measure the contact angle and the surface energy of the different treated ITO substrates. It is found that treatment with the methanol without dehydration gives the lowest water contact angle (most hydrophilic surface) and the highest surface energy compared to other solvents. This result was confirmed by impedance measurements performed on nematic liquid crystal cells with ITO electrodes. Indeed, we check the decrease of ionic entities in the interface ITO/liquid crystal. The polarity and dielectric parameters of the used solvents explain the obtained results

Indium-tin oxide surface treatments: Effects on the performance of liquid crystal devices

Energy Technology Data Exchange (ETDEWEB)

Abderrahmen, A. [Laboratoire de physique et chimie des interfaces, Faculte des sciences, 5000, Monastir (Tunisia)]. E-mail: asma_abderrahmen@yahoo.fr; Romdhane, F.F. [Laboratoire de la matiere molle, Faculte des sciences, Tunis (Tunisia); Ben Ouada, H. [Laboratoire de physique et chimie des interfaces, Faculte des sciences, 5000, Monastir (Tunisia); Gharbi, A. [Laboratoire de la matiere molle, Faculte des sciences, Tunis (Tunisia)

2006-03-15

In this work, we investigate the effect of indium tin oxide (ITO) substrate cleaning on the surface properties. Wettability technique was used to measure the contact angle and the surface energy of the different treated ITO substrates. It is found that treatment with the methanol without dehydration gives the lowest water contact angle (most hydrophilic surface) and the highest surface energy compared to other solvents. This result was confirmed by impedance measurements performed on nematic liquid crystal cells with ITO electrodes. Indeed, we check the decrease of ionic entities in the interface ITO/liquid crystal. The polarity and dielectric parameters of the used solvents explain the obtained results.

Enhanced oxidation stability of quasi core-shell alloyed CdSeS quantum dots prepared through aqueous microwave synthesis technique.

Science.gov (United States)

Zhan, Hong-Ju; Zhou, Pei-Jiang; Ma, Rong; Liu, Xi-Jing; He, Yu-Ning; Zhou, Chuan-Yun

2014-01-01

Quasi core shell alloyed CdSeS quantum dots (QDs) have been prepared through a facile aqueous-phase route employing microwave irradiation technique. The optical spectroscopy and structure characterization evidenced the quasi core shell alloyed structures of CdSeS QDs. The X-ray diffraction patterns of the obtained CdSeS QDs displayed peak positions very close to those of bulk cubic CdS crystal structures and the result of X-ray photoelectron spectroscopy data re-confirmed the thick CdS shell on the CdSe core. The TEM images and HRTEM images of the CdSeS QDs ascertained the well-defined spherical particles and a relatively narrow size distribution. On the basis, the stability of the obtained QDs in an oxidative environment was also discussed using etching reaction by H2O2. The experiments result showed the as-prepared QDs present high tolerance towards H2O2, obviously superior to the commonly used CdTe QDs and core-shell CdTe/CdS QDs, which was attributed to the unique quasi core-shell CdSeS crystal structure and the small lattice mismatch between CdSe and CdS semiconductor materials. This assay provided insight to obtain high stable crystal structured semiconductor nanocrystals in the design and synthesis process.

Single crystalline Co3O4 nanocrystals exposed with different crystal planes for Li-O2 batteries.

Science.gov (United States)

Su, Dawei; Dou, Shixue; Wang, Guoxiu

2014-08-29

Single crystalline Co3O4 nanocrystals exposed with different crystal planes were synthesised, including cubic Co3O4 nanocrystals enclosed by {100} crystal planes, pseudo octahedral Co3O4 enclosed by {100} and {110} crystal planes, Co3O4 nanosheets exposed by {110} crystal planes, hexagonal Co3O4 nanoplatelets exposed with {111} crystal planes, and Co3O4 nanolaminar exposed with {112} crystal planes. Well single crystalline features of these Co3O4 nanocrystals were confirmed by FESEM and HRTEM analyses. The electrochemical performance for Li-O2 batteries shows that Co3O4 nanocrystals can significantly reduce the discharge-charge over-potential via the effect on the oxygen evolution reaction (OER). From the comparison on their catalytic performances, we found that the essential factor to promote the oxygen evolution reactions is the surface crystal planes of Co3O4 nanocrystals, namely, crystal planes-dependent process. The correlation between different Co3O4 crystal planes and their effect on reducing charge-discharge over-potential was established: {100} < {110} < {112} < {111}.

Inductive crystal field control in layered metal oxides with correlated electrons

International Nuclear Information System (INIS)

Balachandran, P. V.; Cammarata, A.; Rondinelli, J. M.; Nelson-Cheeseman, B. B.; Bhattacharya, A.

2014-01-01

We show that the NiO 6 crystal field energies can be tailored indirectly via heterovalent A cation ordering in layered (La,A)NiO 4 Ruddlesden–Popper (RP) oxides, where A = Sr, Ca, or Ba, using density functional calculations. We leverage as a driving force the electrostatic interactions between charged [LaO] 1+ and neutral [AO] 0 planes to inductively tune the Ni–O bond distortions, without intentional doping or epitaxial strain, altering the correlated d-orbital energies. We use this strategy to design cation ordered LaCaNiO 4 and LaBaNiO 4 with distortions favoring enhanced Ni e g orbital polarization, and find local electronic structure signatures analogous to those in RP La-cuprates, i.e., parent phases of the high-temperature superconducting oxides

The crystal chemistry and structural analysis of uranium oxide hydrates. Final report, May 15, 1995--December 31, 1997

International Nuclear Information System (INIS)

Miller, M.L.; Ewing, R.C.

1998-01-01

The purpose of this research program was to develop a thorough understanding of the crystal-chemical and crystal-structural systematics of uranyl oxide hydrates which are the initial corrosion products of the UO 2 in spent nuclear fuel and the principal phases in which actinides occur in the near surface environment. The scope of this program has been expanded to include all inorganic phases in which U 6+ plays a significant structural role; currently 183 phases with known crystal structures

Strengthening mechanisms of Fe nanoparticles for single crystal Cu–Fe alloy

International Nuclear Information System (INIS)

Shi, Guodong; Chen, Xiaohua; Jiang, Han; Wang, Zidong; Tang, Hao; Fan, Yongquan

2015-01-01

A single crystal Cu–Fe alloy with finely dispersed precipitate Fe nanoparticles was fabricated in this study. The interface relationship of iron nanoparticle and copper matrix was analyzed with a high-resolution transmission electron microscope (HRTEM), and the effect of Fe nanoparticles on mechanical properties of single crystal Cu–Fe alloy was discussed. Results show that, the finely dispersed Fe nanoparticles can be obtained under the directional solidification condition, with the size of 5–50 nm and the coherent interface between the iron nanoparticle and the copper matrix. Single crystal Cu–Fe alloy possesses improved tensile strength of 194.64 MPa, and total elongation of 44.72%, respectively, at room temperature, in contrast to pure Cu sample. Nanoparticles which have coherent interface with matrix can improve the dislocation motion state. Some dislocations can slip through the nanoparticle along the coherent interface and some dislocations can enter into the nanoparticles. Thus to improve the tensile strength of single crystal Cu–Fe alloy without sacrificing the ductility simultaneously. Based on the above analyses, strengthening mechanisms of Fe nanoparticles for single crystal Cu–Fe alloy was described

Controlled reduction and oxidation of La0.85Sr0.15MnO3 single crystals

International Nuclear Information System (INIS)

De Leon-Guevara, A.M.; Berthet, P.; Berthon, J.; Millot, F.; Revcolevschi, A.

1997-01-01

La 0.85 Sr 0.15 MnO 3 single crystals were grown by the floating zone method. They can be reversibly reduced under controlled oxygen partial pressure. Their defect chemistry is investigated together with the evolution of their cell parameters and that of their electric conductivity which is very sensitive to their oxygen content. On the other hand, stoichiometric crystals can be oxidized with a slow kinetics making possible the preparation of diphasic materials. (orig.)

Crystallization and unusual rheological behavior in poly(ethylene oxide)–clay nanocomposites

KAUST Repository

Kelarakis, Antonios

2011-05-01

We report a systematic study of the crystallization and rheological behavior of poly(ethylene oxide) (PEO)-clay nanocomposites. To that end a series of nanocomposites based on PEOs of different molecular weight (103 < MW < 105 g/mol) and clay surface modifier was synthesized and characterized. Incorporation of organoclays with polar (MMT-OH) or aromatic groups (MMT-Ar) suppresses the crystallization of polymer chains in low MW PEO, but does not significantly affect the crystallization of high MW matrices. In addition, the relative complex viscosity of the nanocomposites based on low MW PEO increases significantly, but the effect is less pronounced at higher MWs. The viscosity increases in the series MMT-Alk < MMT-OH < MMT-Ar. In contrast to the neat PEO which exhibits a monotonic decrease of viscosity with temperature, all nanocomposites show an increase after a certain temperature. This is the first report of such dramatic enhancements in the viscoelasticity of nanocomposites, which are reversible, are based on a simple polymer matrix and are true in a wide temperature range. © 2011 Elsevier Ltd. All rights reserved.

Far from the equilibrium crystallization of oxide quantum dots in dried inorganic gels

Science.gov (United States)

Costille, B.; Dumoulin, M.; Ntsame Abagha, A. M.; Thune, E.; Guinebretière, R.

2018-06-01

We synthesized, through the sol-gel process, far from the equilibrium amorphous materials in which heterogeneous crystallization allowed the formation of oxide quantum dots. The isothermal evolutions of the mean size of the nanocrystals and the crystallinity of the materials were determined through x-ray diffraction experiments. The heterogeneous crystallization is characterized by a kinetic behavior that is far from that expected, according to the classical nucleation theory. We demonstrate that the evolution of the crystallinity is characterized by an Avrami exponent largely smaller than 1. Finally, nanocrystals exhibiting a size significantly below their Bohr radius are obtained and the number of these nanocrystals increases during isothermal treatment, whereas their mean size remains quasi-constant.

Growth Stresses in Thermally Grown Oxides on Nickel-Based Single-Crystal Alloys

Science.gov (United States)

Rettberg, Luke H.; Laux, Britta; He, Ming Y.; Hovis, David; Heuer, Arthur H.; Pollock, Tresa M.

2016-03-01

Growth stresses that develop in α-Al2O3 scale that form during isothermal oxidation of three Ni-based single crystal alloys have been studied to elucidate their role in coating and substrate degradation at elevated temperatures. Piezospectroscopy measurements at room temperature indicate large room temperature compressive stresses in the oxides formed at 1255 K or 1366 K (982 °C or 1093 °C) on the alloys, ranging from a high of 4.8 GPa for René N4 at 1366 K (1093 °C) to a low of 3.8 GPa for René N5 at 1255 K (982 °C). Finite element modeling of each of these systems to account for differences in coefficients of thermal expansion of the oxide and substrate indicates growth strains in the range from 0.21 to 0.44 pct at the oxidation temperature, which is an order of magnitude higher than the growth strains measured in the oxides on intermetallic coatings that are typically applied to these superalloys. The magnitudes of the growth strains do not scale with the parabolic oxidation rate constants measured for the alloys. Significant spatial inhomogeneities in the growth stresses were observed, due to (i) the presence of dendritic segregation and (ii) large carbides in the material that locally disrupts the structure of the oxide scale. The implications of these observations for failure during cyclic oxidation, fatigue cycling, and alloy design are considered.

High temperature oxidation behavior of aluminide on a Ni-based single crystal superalloy in different surface orientations

Institute of Scientific and Technical Information of China (English)

Fahamsyah H.Latief; Koji Kakehi; El-Sayed M.Sherif

2014-01-01

An investigation on oxidation behavior of coated Ni-based single crystal superalloy in different surface orientations has been carried out at 1100 1C. It has been found that the {100} surface shows a better oxidation resistance than the {110} one, which is attributed that the {110}surface had a slightly higher oxidation rate when compared to the {100} surface. The experimental results also indicated that the anisotropic oxidation behavior took place even with a very small difference in the oxidation rates that was found between the two surfaces. The differences of the topologically close packed phase amount and its penetration depth between the two surfaces, including the ratio of α-Al2O3 after 500 h oxidation, were responsible for the oxidation anisotropy.

Hysteresis losses in iron oxide nanoparticles prepared by glass crystallization or wet chemical precipitation

International Nuclear Information System (INIS)

Mueller, Robert; Dutz, Silvio; Hergt, Rudolf; Schmidt, Christopher; Steinmetz, Hanna; Zeisberger, Matthias; Gawalek, Wolfgang

2007-01-01

Ferrofluids were prepared from glass crystallized as well as wet precipitated iron oxide particles. Comparing hysteresis losses versus applied field amplitude from particles in immobilized state (powder) and in fluid state (ferrofluid) shows in some cases anomalous large losses at low magnetic fields. The influence of texture on the losses was investigated

Behavior of aluminum oxide, intermetallics and voids in Cu-Al wire bonds

International Nuclear Information System (INIS)

Xu, H.; Liu, C.; Silberschmidt, V.V.; Pramana, S.S.; White, T.J.; Chen, Z.; Acoff, V.L.

2011-01-01

Nanoscale interfacial evolution in Cu-Al wire bonds during isothermal annealing from 175 deg. C to 250 deg. C was investigated by high resolution transmission electron microscopy (HRTEM). The native aluminum oxide film (∼5 nm thick) of the Al pad migrates towards the Cu ball during annealing. The formation of intermetallic compounds (IMC) is controlled by Cu diffusion, where the kinetics obey a parabolic growth law until complete consumption of the Al pad. The activation energies to initiate crystallization of CuAl 2 and Cu 9 Al 4 are 60.66 kJ mol -1 and 75.61 kJ mol -1 , respectively. During IMC development, Cu 9 Al 4 emerges as a second layer and grows together with the initial CuAl 2 . When Al is completely consumed, CuAl 2 transforms to Cu 9 Al 4 , which is the terminal product. Unlike the excessive void growth in Au-Al bonds, only a few voids nucleate in Cu-Al bonds after long-term annealing at high temperatures (e.g., 250 o C for 25 h), and their diameters are usually in the range of tens of nanometers. This is due to the lower oxidation rate and volumetric shrinkage of Cu-Al IMC compared with Au-Al IMC.

Combined HRTEM and PEELS analysis of nanoporous and amorphous carbon

International Nuclear Information System (INIS)

Peng, J.L.; Fan, X. D.; Bursill, L.A.

1997-01-01

Both the mass density (1.37 kgm/m 3 ) and sp 2 +sp 3 bonding fraction (0.15) were determined for an unusual nanoporous amorphous carbon consisting of curved single graphitic sheets. A combination of high-resolution transmission electron microscopy (HRTEM) and parallel electron energy loss spectroscopy (PEELS) was used. The values of these two parameters provide important constraints for the determination of the structure of this relatively low density variety of nanoporous carbon. The results are relevant also in the search for negatively-curved Schwarzite-related carbon structures. New date are also presented for highly-oriented pyrollytic graphite (HOPG), chemically vapour deposited (CVD) diamond, C 60 , glassy carbon (GC) and evaporated amorphous carbon (EAC); these are compared with the results for NAC. Kramers-Kronig analysis (KKA) of the low-loss PEELS data shows that the band gaps of both NAC and EAC are collapsed relative to that of CVD diamond. 18 refs., 2 tabs., 3 figs

Combined HRTEM and PEELS analysis of nanoporous and amorphous carbon

Energy Technology Data Exchange (ETDEWEB)

Peng, J.L.; Fan, X. D.; Bursill, L.A.

1997-06-01

Both the mass density (1.37 kgm/m{sup 3}) and sp{sup 2}+sp{sup 3} bonding fraction (0.15) were determined for an unusual nanoporous amorphous carbon consisting of curved single graphitic sheets. A combination of high-resolution transmission electron microscopy (HRTEM) and parallel electron energy loss spectroscopy (PEELS) was used. The values of these two parameters provide important constraints for the determination of the structure of this relatively low density variety of nanoporous carbon. The results are relevant also in the search for negatively-curved Schwarzite-related carbon structures. New date are also presented for highly-oriented pyrollytic graphite (HOPG), chemically vapour deposited (CVD) diamond, C{sub 60}, glassy carbon (GC) and evaporated amorphous carbon (EAC); these are compared with the results for NAC. Kramers-Kronig analysis (KKA) of the low-loss PEELS data shows that the band gaps of both NAC and EAC are collapsed relative to that of CVD diamond. 18 refs., 2 tabs., 3 figs.

Inductive crystal field control in layered metal oxides with correlated electrons

Energy Technology Data Exchange (ETDEWEB)

Balachandran, P. V.; Cammarata, A.; Rondinelli, J. M., E-mail: jrondinelli@nortwestern.edu [Department of Materials Science and Engineering, Drexel University, Philadelphia, Pennsylvania 19104 (United States); Nelson-Cheeseman, B. B. [School of Engineering, University of St. Thomas, St. Paul, Minnesota 55105 (United States); Materials Science Division, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Bhattacharya, A. [Materials Science Division, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Center for Nanoscale Materials, Argonne National Laboratory, Argonne, Illinois 60439 (United States)

2014-07-01

We show that the NiO{sub 6} crystal field energies can be tailored indirectly via heterovalent A cation ordering in layered (La,A)NiO{sub 4} Ruddlesden–Popper (RP) oxides, where A = Sr, Ca, or Ba, using density functional calculations. We leverage as a driving force the electrostatic interactions between charged [LaO]{sup 1+} and neutral [AO]{sup 0} planes to inductively tune the Ni–O bond distortions, without intentional doping or epitaxial strain, altering the correlated d-orbital energies. We use this strategy to design cation ordered LaCaNiO{sub 4} and LaBaNiO{sub 4} with distortions favoring enhanced Ni e{sub g} orbital polarization, and find local electronic structure signatures analogous to those in RP La-cuprates, i.e., parent phases of the high-temperature superconducting oxides.

Coherent diffractive imaging of solid state reactions in zinc oxide crystals

Science.gov (United States)

Leake, Steven J.; Harder, Ross; Robinson, Ian K.

2011-11-01

We investigated the doping of zinc oxide (ZnO) microcrystals with iron and nickel via in situ coherent x-ray diffractive imaging (CXDI) in vacuum. Evaporated thin metal films were deposited onto the ZnO microcrystals. A single crystal was selected and tracked through annealing cycles. A solid state reaction was observed in both iron and nickel experiments using CXDI. A combination of the shrink wrap and guided hybrid-input-output phasing methods were applied to retrieve the electron density. The resolution was 33 nm (half order) determined via the phase retrieval transfer function. The resulting images are nevertheless sensitive to sub-angstrom displacements. The exterior of the microcrystal was found to degrade dramatically. The annealing of ZnO microcrystals coated with metal thin films proved an unsuitable doping method. In addition the observed defect structure of one crystal was attributed to the presence of an array of defects and was found to change upon annealing.

Ultrasonic-assisted synthesis and magnetic studies of iron oxide/MCM-41 nanocomposite

International Nuclear Information System (INIS)

Ursachi, Irina; Vasile, Aurelia; Ianculescu, Adelina; Vasile, Eugeniu; Stancu, Alexandru

2011-01-01

Highlights: → A quick and facile route for the synthesis of iron oxide/MCM-41 nanocomposite. → Magnetic nanoparticles were stabilized inside the pores of mesoporous silica MCM-41. → The pore size of MCM-41 dictates the properties of iron oxide nanoparticles. → The procedure provides a narrow size distribution of magnetic nanoparticles. - Abstract: Iron oxide nanoparticles were stabilized within the pores of mesoporous silica MCM-41 amino-functionalized by a sonochemical method. Formation of iron oxide nanoparticles inside the mesoporous channels of amino-functionalized MCM-41 was realized by wet impregnation using iron nitrate, followed by calcinations at 550 deg. C in air. The effect of functionalization level on structural and magnetic properties of obtained nanocomposites was studied. The resulting materials were characterized by powder X-ray diffraction (XRD), high-resolution transmission electron microscopy and selected area electron diffraction (HRTEM and SAED), vibrating sample and superconducting quantum interface magnetometers (VSM and SQUID) and nitrogen adsorption-desorption isotherms measurements. The HRTEM images reveal that the most of the iron oxide nanoparticles were dispersed inside the mesopores of silica matrix and the pore diameter of the amino-functionalized MCM-41 matrix dictates the particle size of iron oxide nanoparticles. The obtained material possesses mesoporous structure and interesting magnetic properties. Saturation magnetization value of magnetic iron oxide nanopatricles stabilized in MCM-41 amino-functionalized by in situ sonochemical synthesis was 1.84 emu g -1 . An important finding is that obtained magnetic nanocomposite materials exhibit enhanced magnetic properties than those of iron oxide/MCM-41 nanocomposite obtained by conventional method. The described method is providing a rather short preparation time and a narrow size distribution of iron oxide nanoparticles.

Synthesis and magnetic characterizations of uniform iron oxide nanoparticles

International Nuclear Information System (INIS)

Jiang, FuYi; Li, XiaoYi; Zhu, Yuan; Tang, ZiKang

2014-01-01

Uniform iron oxide nanoparticles with a cubic shape were prepared by the decomposition of homemade iron oleate in 1-octadecene with the presence of oleic acid. The particle shape and size uniformity are sensitive to the quantity of oleic acid. XRD, HRTEM and SAED results indicated that the main phase content of as-prepared iron oxide nanoparticles is Fe 3 O 4 with an inverse spinel structure. Magnetic measurements revealed that the as-prepared iron oxide nanoparticles display a ferromagnetic behavior with a blocking temperature of 295 K. At low temperatures the magnetic anisotropy of the aligned nanoparticles caused the appearance of a hysteresis loop.

Tungsten Oxide Photonic Crystals as Optical Transducer for Gas Sensing.

Science.gov (United States)

Amrehn, Sabrina; Wu, Xia; Wagner, Thorsten

2018-01-26

Some metal oxide semiconductors, such as tungsten trioxide or tin dioxide, are well-known as resistive transducers for gas sensing and offer high sensitivities down to the part per billion level. Electrical signal read-out, however, limits the information obtained on the electronic properties of metal oxides to a certain frequency range and its application because of the required electrical contacts. Therefore, a novel approach for building an optical transducer for gas reactions utilizing metal oxide photonic crystals is presented here. By the rational design of the structure and composition it is possible to synthesize a functional material which allows one to obtain insight into its electronic properties in the optical frequency range with simple experimental measures. The concept is demonstrated by tungsten trioxide inverse opal structure as optical transducer material for hydrogen sensing. The sensing behavior is analyzed in a temperature range from room temperature to 500 °C and in a wide hydrogen concentration range (3000 ppm to 10%). The sensing mechanism is mainly the refractive index change resulting from hydrogen intercalation in tungsten trioxide, but the back reaction has also impact on the optical properties of this system. Detailed chemical reaction studies provide suggestions for specific sensing conditions.

Solid solutions of gadolinium doped zinc oxide nanorods by combined microwave-ultrasonic irradiation assisted crystallization

Science.gov (United States)

Kiani, Armin; Dastafkan, Kamran; Obeydavi, Ali; Rahimi, Mohammad

2017-12-01

Nanocrystalline solid solutions consisting of un-doped and gadolinium doped zinc oxide nanorods were fabricated by a modified sol-gel process utilizing combined ultrasonic-microwave irradiations. Polyvinylpyrrolidone, diethylene glycol, and triethylenetetramine respectively as capping, structure directing, and complexing agents were used under ultrasound dynamic aging and microwave heating to obtain crystalline nanorods. Crystalline phase monitoring, lattice parameters and variation, morphology and shape, elemental analysis, functional groups, reducibility, and the oxidation state of emerged species were examined by PXRD, FESEM, TEM, EDX, FTIR, micro Raman, H2-TPR, and EPR techniques. Results have verified that irradiation mechanism of gelation and crystallization reduces the reaction time, augments the crystal quality, and formation of hexagonal close pack structure of Wurtzite morphology. Besides, dissolution of gadolinium within host lattice involves lattice deformation, unit cell distortion, and angular position variation. Structure related shape and growth along with compositional purity were observed through microscopic and spectroscopic surveys. Furthermore, TPR and EPR studies elucidated more detailed behavior upon exposure to the exerted irradiations and subsequent air-annealing including the formed oxidation states and electron trapping centers, presence of gadolinium, zinc, and oxygen disarrays and defects, as well as alteration in the host unit cell via gadolinium addition.

Morphological Development of Melt Crystallized Poly(propylene oxide) by In Situ AFM: Formation of Banded Spherulites

NARCIS (Netherlands)

Beekmans, L.G.M.; Hempenius, Mark A.; Vancso, Gyula J.

2004-01-01

The morphology of poly(propylene oxide) (PPO) crystals grown from the melt was investigated. The spherulites of the optically pure S polymers displayed a regular pattern of concentric rings as observed by polarizing optical microscopy, while the stereocopolymer developed irregularly banded, or

Crystallization Behavior of Poly(ethylene oxide) in Vertically Aligned Carbon Nanotube Array.

Science.gov (United States)

Sheng, Jiadong; Zhou, Shenglin; Yang, Zhaohui; Zhang, Xiaohua

2018-03-27

We investigate the effect of the presence of vertically aligned multiwalled carbon nanotubes (CNTs) on the orientation of poly(ethylene oxide) (PEO) lamellae and PEO crystallinity. The high alignment of carbon nanotubes acting as templates probably governs the orientation of PEO lamellae. This templating effect might result in the lamella planes of PEO crystals oriented along a direction parallel to the long axis of the nanotubes. The presence of aligned carbon nanotubes also gives rise to the decreases in PEO crystallinity, crystallization temperature, and melting temperature due to the perturbation of carbon nanotubes to the crystallization of PEO. These effects have significant implications for controlling the orientation of PEO lamellae and decreasing the crystallinity of PEO and thickness of PEO lamellae, which have significant impacts on ion transport in PEO/CNT composite and the capacitive performance of PEO/CNT composite. Both the decreased PEO crystallinity and the orientation of PEO lamellae along the long axes of vertically aligned CNTs give rise to the decrease in the charge transfer resistance, which is associated with the improvements in the ion transport and capacitive performance of PEO/CNT composite.

Surface conductivity of the single crystal aluminum oxide in vacuum and caesium vapors

International Nuclear Information System (INIS)

Vasilchenko, A.V.; Izhvanov, O.L.

1996-01-01

Results of measurements of surface conductivity of single-crystal aluminum oxide samples in vacuum and cesium vapors at T=620 endash 830 K and P Cs =0.13 endash 2 Pa are shown in the paper. Analysis of caesium vapor influence is carried out and ultimate characteristics of samples conductivity under operation conditions in thermionic nuclear power system (NPP) TFE are estimated. copyright 1996 American Institute of Physics

Photonic Crystals: Tunable Design of Structural Colors Produced by Pseudo-1D Photonic Crystals of Graphene Oxide (Small 25/2016).

Science.gov (United States)

Tong, Liping; Qi, Wei; Wang, Mengfan; Huang, Renliang; Su, Rongxin; He, Zhimin

2016-07-01

The production of structural colors based on graphene oxide (GO) pseudo-one-dimensional photonic crystals (p1D-PhCs) in the visible spectrum is reported on page 3433 by W. Qi and co-workers. The structural colors could be tuned by simply changing either the volume or concentration of the aqueous GO dispersion. Moreover, GO p1D-PhCs exhibit visible and rapid responsiveness to humidity. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Thermal oxidative degradation behaviours of flame-retardant thermotropic liquid crystal copolyester/PET blends

International Nuclear Information System (INIS)

Du Xiaohua; Zhao Chengshou; Wang Yuzhong; Zhou Qian; Deng Yi; Qu Minghai; Yang Bing

2006-01-01

The flame retardancy and the thermal oxidative degradation behaviors of the blend of poly(ethylene terephthalate) (PET) with a kind of phosphorus-containing thermotropic liquid crystal copolyester (TLCP) with high flame retardancy (limited oxygen index, 70%) have been investigated by oxygen index test (LOI), UL-94 rating and thermogravimetric analysis (TGA) in air. The results show that TLCP can dramatically improve the flame retardancy and the melt dripping behavior of PET. Moreover, the apparent activation energies of thermal oxidative degradation of the blends were evaluated using Kissinger and Flynn-Wall-Ozawa methods. It is found that addition of TLCP improve thermal stability and restrain thermal decomposition of PET in air, especially at the primary degradation stage. Py-GC/MS analysis shows that there are remarkable changes in the pyrolysis products when TLCP are blended into PET. The interaction between TLCP and PET has changed their thermal oxidative degradation mechanism

A study of magnetoplumbite-type (M-type) cobalt-titanium-substituted barium ferrite, BaCo{sub x}Ti{sub x}Fe{sub 12-2x}O{sub 19} (x = 1-6)

Energy Technology Data Exchange (ETDEWEB)

Teh, G.B. [Department of Bioscience and Chemistry, Faculty of Engineering and Science, Universiti Tunku Abdul Rahman, 53300 Kuala Lumpur (Malaysia)], E-mail: tehgb@mail.utar.edu.my; Saravanan, N. [Department of Bioscience and Chemistry, Faculty of Engineering and Science, Universiti Tunku Abdul Rahman, 53300 Kuala Lumpur (Malaysia); Jefferson, D.A. [Department of Chemistry, University of Cambridge, Lensfield Road, Cambridge CB2 1EW (United Kingdom)

2007-10-15

Cobalt(II)-titanium(IV)-substituted barium ferrite forming the chemical formula of BaCo{sub x}Ti{sub x}Fe{sub 12-2x}O{sub 19} (x = 1-6) have been investigated using X-ray diffraction spectroscopy (XRD), Superconducting Quantum Interference Device (SQUID) and high-resolution transmission electron microscopy (HRTEM). The specimen of magnetoplumbite (M-type) Co-Ti-substituted BaFe{sub 12}O{sub 19} were synthesised via sol-gel method using ethylene glycol as precursor. Significant increase in line broadening of the XRD patterns were observed indicating the decrease of particle sizes due to the Co(II)-Ti(IV) substitution. BaCo{sub 3}Ti{sub 3}Fe{sub 6}O{sub 19} showed the highest coercivity but moderate saturation and remnant magnetisations. HRTEM imaging showed that Co(II)-Ti(IV) substitution in the system of BaCo{sub x}Ti{sub x}Fe{sub 12-2x}O{sub 19} (x = 1-6) produced no drastic change in the structure of the M-type ferrites. Most of the M-types crystals examined by HRTEM displayed a long axis perpendicular to the c-axis of the M-type structure. Disordered crystals showing the intergrowth between Co-Ti-substituted barium ferrite and the spinel-structured iron oxide were detected.

Crystal orientation dependent thermoelectric properties of highly oriented aluminum-doped zinc oxide thin films

KAUST Repository

Abutaha, Anas I.

2013-02-06

We demonstrate that the thermoelectric properties of highly oriented Al-doped zinc oxide (AZO) thin films can be improved by controlling their crystal orientation. The crystal orientation of the AZO films was changed by changing the temperature of the laser deposition process on LaAlO3 (100) substrates. The change in surface termination of the LaAlO3 substrate with temperature induces a change in AZO film orientation. The anisotropic nature of electrical conductivity and Seebeck coefficient of the AZO films showed a favored thermoelectric performance in c-axis oriented films. These films gave the highest power factor of 0.26 W m−1 K−1 at 740 K.

Characterization of Anodic Aluminum Oxide Membrane with Variation of Crystallizing Temperature for pH Sensor.

Science.gov (United States)

Yeo, Jin-Ho; Lee, Sung-Gap; Jo, Ye-Won; Jung, Hye-Rin

2015-11-01

We fabricated electrolyte-dielectric-metal (EDM) device incorporating a high-k Al2O3 sensing membrane from a porous anodic aluminum oxide (AAO) using a two step anodizing process for pH sensors. In order to change the properties of the AAO template, the crystallizing temperature was varied from 400 degrees C to 700 degrees C over 2 hours. The structural properties were observed by field emission scanning electron microscopy (FE-SEM). The pH sensitivity increased with an increase in the crystallizing temperature from 400 degrees C to 600 degrees C. However at 700 degrees C, deformation occurred. The porous AAO sensor with a crystallizing temperature of 600 degrees C displayed the good sensitivity and long-term stability and the values were 55.7 mV/pH and 0.16 mV/h, respectively.

The new ternary pnictides Er12Ni30P21 and Er13Ni25As19: Crystal structures and magnetic properties

International Nuclear Information System (INIS)

Oryshchyn, Stepan; Babizhetskyy, Volodymyr; Zhak, Olga; Zelinska, Mariya; Pivan, Jean-Yves; Duppel, Viola; Simon, Arndt; Kienle, Lorenz

2010-01-01

The new ternary pnictides Er 12 Ni 30 P 21 and Er 13 Ni 25 As 19 have been synthesized from the elements. They crystallize with hexagonal structures determined from single-crystal X-ray data for Er 12 Ni 30 P 21 (space group P6 3 /m, a=1.63900(3) nm, c=0.37573(1) nm, Z=1, R F =0.062 for 1574 F-values and 74 variable parameters), and for Er 13 Ni 25 As 19 (Tm 13 Ni 25 As 19 -type structure, space group P6-bar , a=1.6208(1) nm, c=0.38847(2) nm, Z=1, R F =0.026 for 1549 F-values and 116 variable parameters). These compounds belong to a large family of hexagonal structures with a metal-metalloid ratio of 2:1. HRTEM investigations were conducted to probe for local ordering of the disordered structure at the nanoscale. The magnetic properties of the phosphide Er 12 Ni 30 P 21 have been studied in the temperature of range 2 eff =9.59 μ B corresponds to the theoretical value of Er 3+ . - Graphical abstract: The new ternary pnictides Er 12 Ni 30 P 21 and Er 13 Ni 25 As 19 have been synthesized from the elements. They crystallize with hexagonal structures determined from single-crystal X-ray data. The compounds belong to a large family of structures with a metal-metalloid ratio of 2:1. HRTEM investigations were conducted to probe for local ordering of the disordered structure at the nanoscale. Display Omitted

Mechanism of ruthenium dioxide crystallization during high level waste vitrification

International Nuclear Information System (INIS)

Boucetta, H.

2012-01-01

Ruthenium, arising from the reprocessing of spent uranium oxide fuel, has a low solubility in glass melt. It crystallizes in the form of particles of RuO 2 of acicular or polyhedral morphology dispersed in fission product and actinides waste containment glass. Since the morphology of these particles strongly influences the physico-chemical properties, the knowledge and the control of their mechanism of formation are of major importance. The goal of this work is to determine the chemical reactions responsible for the formation of RuO 2 particles of acicular or polyhedral shape during glass synthesis. Using a simplification approach, the reactions between RuO 2 -NaNO 3 , and more complex calcine RuO 2 -Al 2 O 3 -Na 2 O and a sodium borosilicate glass are studied. In situ scanning electron microscopy and XANES at increasing temperatures are used to follow changes in composition, speciation and morphology of the ruthenium intermediate species. Those compounds are thoroughly characterised by SEM, XRD, HRTEM, and ruthenium K-edge X-ray absorption spectroscopy. This combined approach allows us to show that the ruthenium speciation modification during vitrification is the key of control of the morphology of RuO 2 particles in the glass. In particular, the formation of a specific intermediate compound (Na 3 RuO 4 ) is one of the main steps that lead to the precipitation of needle-shaped RuO 2 particles in the melt. The formation of polyhedral particles, on the contrary, results from the direct incorporation of RuO 2 crystals in the melt followed by an Ostwald ripening mechanism. (author) [fr

Crystallization of oxidized, moderately hydrous arc basalt at mid-to-lower crustal pressures

Science.gov (United States)

Blatter, D. L.; Sisson, T. W.; Hankins, W. B.

2012-12-01

Decades of experimental work show that dry, reduced, subalkaline basalts differentiate to produce tholeiitic (high Fe/Mg) daughter liquids, however the influences of H2O and oxidation on differentiation paths are not well established. Accordingly, we performed crystallization experiments on a relatively magnesian basalt (8.7 wt% MgO) typical of mafic lavas erupted in the Cascades magmatic arc near Mount Rainier, Washington. Starting material was synthesized with 3 wt% H2O and run in 2.54 cm piston-cylinder vessels at 900, 700, and 400 MPa and 1200 to 925 degrees C. Samples were contained in Au75Pd25 capsules pre-saturated with Fe by reaction with magnetite at controlled fO2. Oxygen fugacity was controlled during high-pressure syntheses by the double capsule method using Re-ReO2 plus H2O-CO2 vapor in the outer capsule, mixed to match the expected fH2O of the vapor-undersaturated sample. Crystallization was similar at all pressures with a high temperature interval consisting of augite + olivine + orthopyroxene + Cr-spinel (in decreasing abundance). With decreasing temperature, plagioclase crystallizes, FeTi-oxides replace spinel, olivine dissolves, and finally amphibole appears. Liquids at 900 MPa track along Miyashiro's (1974) tholeiitic vs. calc-alkaline boundary, whereas those at 700 and 400 MPa become calc-alkaline by ~57 wt% SiO2 and greater. Although these evolved liquids are similar in most respects to common calc-alkaline andesites, they differ in having low-CaO due to early and abundant crystallization of augite prior to plagioclase, with the result that they become peraluminous (ASI: Al/(Na+K+Ca)>1) by ~55 wt% SiO2, similar to liquids reported in other studies of the high-pressure crystallization of hydrous basalts (Müntener and Ulmer, 2006 and references therein). A compilation of >7000 analyses of volcanic and intrusive rocks from the Cascades and the Sierra Nevada batholith shows that ASI in arc magmas increases continuously and linearly with SiO2 from

Effects of surface crystallization and oxidation in nanocrystalline FeNbCuSiB(P) ribbons

Energy Technology Data Exchange (ETDEWEB)

Butvinová, B., E-mail: beata.butvinova@savba.sk [Institute of Physics SAS, Dúbravská cesta 9, 845 11 Bratislava (Slovakia); Butvin, P. [Institute of Physics SAS, Dúbravská cesta 9, 845 11 Bratislava (Slovakia); Brzózka, K. [Department of Physics, University of Technology and Humanities in Radom, Krasickiego 54, 26-600 Radom (Poland); Kuzminski, M. [Institute of Physics PAS, Al. Lotnikow 36/42, 02-668 Warsaw (Poland); Maťko, I.; Švec Sr, P. [Institute of Physics SAS, Dúbravská cesta 9, 845 11 Bratislava (Slovakia); Chromčíková, M. [Institute of Inorg. Chem. SAS, Centrum VILA, Študentská 2, 911 50 Trenčín (Slovakia)

2017-02-15

Si-poor Fe{sub 74}Nb{sub 3}Cu{sub 1}Si{sub 8}B{sub 14−x}P{sub x}, (x=0, 3) nanocrystalline ribbon-form alloys often form surfaces, which exert in-plane force on underlying ribbon interior when nanocrystallized in even modest presence of oxygen. Mostly unwanted hard-ribbon-axis magnetic anisotropy is standard result. Essential sources of the surface-caused stress have been sought and influence of P instead of B substitution on this effect was studied too. Preferred surface crystallization (PSC) was found to be the major reason. However P substitution suppresses PSC and promotes Fe-oxide formation, which eases the stress, softens the surfaces and provides different annealing evolution of surface properties. - Highlights: • Ar anneal of low-Si FeNbCuBSi ribbons produce surfaces that stress ribbon interior. • The stress comes mainly from preferred crystallization of surfaces. • Partial substitution of B by P changes annealing evolution of surface properties. • Without P, more crystalline surfaces significantly reduce ribbon's elasticity. • P suppresses surface crystallinity, promotes oxides and reduces mutual stress.

Polycaprolactone-templated reduced-graphene oxide liquid crystal nanofibers towards biomedical applications

DEFF Research Database (Denmark)

Jalili-Firoozinezhad, Sasan; Hasan Mohamadzadeh Moghadam, Mohamad; Ghanian, Mohammad Hossein

2017-01-01

Here, we report a facile method to generate electrically conductive nanofibers by coating and subsequently chemically reducing graphene oxide (GO) liquid crystals on a polycaprolactone (PCL) mat. Ultra large GO sheets obtained are in favor of charge carrier mobility and oriented morphology...... of the GO coating. We showed that coating the reduced GO (rGO) not only retains the three-dimensional topography, fiber orientation and size of the template PCL, but also makes it electroconductive. Our preliminary in vitro assessments using mesenchymal stem cells revealed no induced cytotoxicity yet...... increased cellular metabolism on PCL-templated rGO fibers....

Crystal structure of the uranyl-oxide mineral rameauite

Energy Technology Data Exchange (ETDEWEB)

Plasil, Jakub [ASCR, Prague (Czech Republic). Inst. of Physics; Skoda, Radek [Masaryk Univ., Brno (Czech Republic). Dept. of Geological Sciences; Cejka, Jiri [National Museum, Prague (Czech Republic). Dept. of Mineralogy and Petrology; Bourgoin, Vincent; Boulliard, Jean-Claude [Pierre et Marie Curie Univ., Paris (France). Association Jean Wyart, Collection des Mineraux de Jussieu

2016-12-15

Rameauite is a rare supergene uranyl-oxide hydroxy-hydrate mineral that forms during hydration-oxidation weathering of uraninite. On the basis of single-crystal X-ray diffraction data collected on a microfocus source, rameauite is monoclinic, space group Cc, with a = 13.9458(19), b = 14.3105(19), c = 13.8959(18) Aa, β = 118.477(14) , V = 2437.7(6) Aa{sup 3} and Z = 4, with D{sub calc} = 5.467 g cm{sup -3}. The structure of rameauite (R = 0.060 for 1698 unique observed reflections) contains sheets of the β-U{sub 3}O{sub 8} topology, with both UO{sub 6} and UO{sub 7} bipyramids, which is similar to the sheets found in spriggite, ianthinite and wyartite. The sheets alternate with the interlayer, which contains K{sup +}, Ca{sup 2+} and H{sub 2}O molecules. Interstitial cations are linked into infinite chains that extend along [10-1]. Adjacent sheets are linked through K-O, Ca-O and H-bonds. The structural formula of rameauite is K{sub 2} Ca(H{sub 2}{sup [3]}O){sub 1}(H{sub 2}{sup [5]}O){sub 4}[(UO{sub 2}) {sub 6}O{sub 6}(OH){sub 4}](H{sub 2}{sup [4]}O){sub 1}. The empirical formula obtained from the average of eight electron-microprobe analyses is (on the basi s of 6 U p.f.u.) K{sub 1.87}(Ca{sub 1.10}Sr{sub 0.04}){sub Σ1.14}[(UO 2){sub 6}O{sub 6}(OH){sub 4.15}].6H{sub 2}O. The Raman spectrum is dominate d by U.O and O.H vibrations. A discussion of related uranyl-oxide minerals is given.

Crystallization and electrical resistivity of Cu2O and CuO obtained by thermal oxidation of Cu thin films on SiO2/Si substrates

International Nuclear Information System (INIS)

De Los Santos Valladares, L.; Salinas, D. Hurtado; Dominguez, A. Bustamante; Najarro, D. Acosta; Khondaker, S.I.; Mitrelias, T.; Barnes, C.H.W.; Aguiar, J. Albino; Majima, Y.

2012-01-01

In this work, we study the crystallization and electrical resistivity of the formed oxides in a Cu/SiO 2 /Si thin film after thermal oxidation by ex-situ annealing at different temperatures up to 1000 °C. Upon increasing the annealing temperature, from the X ray diffractogram the phase evolution Cu → Cu + Cu 2 O → Cu 2 O → Cu 2 O + CuO → CuO was detected. Pure Cu 2 O films are obtained at 200 °C, whereas uniform CuO films without structural surface defects such as terraces, kinks, porosity or cracks are obtained in the temperature range 300–550 °C. In both oxides, crystallization improves with annealing temperature. A resistivity phase diagram, which is obtained from the current–voltage response, is presented here. The resistivity was expected to increase linearly as a function of the annealing temperature due to evolution of oxides. However, anomalous decreases are observed at different temperatures ranges, this may be related to the improvement of the crystallization and crystallite size when the temperature increases. - Highlights: ► The crystallization and electrical resistivity of oxides in a Cu films are studied. ► In annealing Cu films, the phase evolution Cu + Cu 2 O → Cu 2 O → Cu 2 O + CuO → CuO occurs. ► A resistivity phase diagram, obtained from the current–voltage response, is presented. ► Some decreases in the resistivity may be related to the crystallization.

The facile and low temperature synthesis of nanophase hydroxyapatite crystals using wet chemistry

International Nuclear Information System (INIS)

Dhand, Vivek; Rhee, K.Y.; Park, Soo-Jin

2014-01-01

A simple and facile wet chemistry route was used to synthesize nanophase hydroxyapatite (HaP) crystals at low temperature. The synthesis was carried out at a pH of 11.0 and at a temperature of 37 °C. The resulting samples were washed several times and subjected to further analysis. XRD studies revealed that the HaP crystals were polycrystalline in nature with a crystallite size of ∼ 15–60 ± 5 nm. SEM-EDXA images confirmed the presence of calcium (Ca), phosphorous (P), and oxygen (O) peaks. Likewise, FTIR confirmed the presence of characteristic phosphate and hydroxyl peaks in samples. Lastly, HRTEM images clearly showed distinctive lattice fringes positioned in the 100 and 002 planes. TGA analysis shows that HaP crystals can withstand higher calcination temperatures and are thermally stable. - Highlights: • Facile and low temperature nanophase HaP crystals synthesized at pH 11 and 37 °C • Electron microscopy image of HaP shows characteristic rice grain like morphology. • FTIR results show the characteristic and fingerprint functional groups of HaP. • Thermal stability of HaP crystals up to 500 °C • Growth of Hap crystals occur parallel to c-axis and a possible mechanism proposed

Investigation of distribution microhomogeneity of doped elements in oxide single crystals by means of LMA-AES

International Nuclear Information System (INIS)

Nikolova, L.; Krasnobaeva, N.; Manuilov, N.

1989-01-01

The distribution of V and Ti in oxide single crystals Al 2 O 3 :V 3+ , Y 3 Al 5 O 12 :V 3+ , Al 2 O 3 :Ti 3+ , Y 3 Al 5 O 12 :Ti 3+ is investigated by laser emission microspectral analysis with photographic registration of spectra. Single crystals have been grown by the method of vertical directed crystallization (method of Bridgman-Stockbarger). For evaluation of microhomogeneity of the investigated elements distribution the following statistical methods are applied: one-way variance analysis, two-way variance analysis, regression models and gradient method. A PC programme package is developed allowing to process photoregistration data, to choose the internal standard line by scatter diagrams, to perform all statistical analysis and to plot the distribution diagrams of the elements in the samples. 2 refs. (author)

Desorption of Furfural from Bimetallic Pt-Fe Oxides/Alumina Catalysts

OpenAIRE

Gloria Lourdes Dimas-Rivera; Javier Rivera de la Rosa; Carlos J. Lucio-Ortiz; José Antonio De los Reyes Heredia; Virgilio González González; Tomás Hernández

2014-01-01

In this work, the desorption of furfural, which is a competitive intermediate during the production of biofuel and valuable aromatic compounds, was studied using pure alumina, as well as alumina impregnated with iron and platinum oxides both individually and in combination, using thermogravimetric analysis (TGA). The bimetallic sample exhibited the lowest desorption percentage for furfural. High-resolution transmission electron microscopy (HRTEM) imaging revealed the intimate connection betwe...

Positron annihilation study of defects in electron-irradiated single crystal zinc oxide

Science.gov (United States)

To, C. K.; Yang, B.; Beling, C. D.; Fung, S.; Ling, C. C.; Gong, M.

2011-01-01

Pressurized melt grown zinc oxide (ZnO) single crystals purchased from Cermet Inc. were irradiated by 2MeV electrons with fluence of 6x1017cm-2. Isochronal annealing from 100°C-800°C was performed on the crystals under argon and air ambience. Variable Energy Doppler Broadening Spectroscopy (VEDBS) was carried out on both the as-grown and the irradiated samples at each annealing step. The migration, agglomeration and annealing of grown-in and irradiated-introduced defects were studied. It was observed that the grown-in vacancy-type defects concentration decreased at 300°C and 600 °C. For the irradiated sample annealed in argon, the positron trapping vacancy-type defect concentration decreased at 300°C and 600°C. Further annealing the as-grown and irradiated samples in argon increased the S parameter further. For the irradiated sample annealed in air, the vacancy-type defect concentration decreases at 300°C and 700°C.

Positron annihilation study of defects in electron-irradiated single crystal zinc oxide

Energy Technology Data Exchange (ETDEWEB)

To, C K; Yang, B; Beling, C D; Fung, S; Ling, C C [Department of Physics, University of Hong Kong (Hong Kong); Gong, M, E-mail: sfung@hkucc.hku.h, E-mail: edwardto04@yahoo.com.h [Department of Physics, Sichuan University, Chengdu (China)

2011-01-01

Pressurized melt grown zinc oxide (ZnO) single crystals purchased from Cermet Inc. were irradiated by 2 MeV electrons with fluence of 6x10{sup 17}cm{sup -2}. Isochronal annealing from 100 deg. C - 800 deg. C was performed on the crystals under argon and air ambience. Variable Energy Doppler Broadening Spectroscopy (VEDBS) was carried out on both the as-grown and the irradiated samples at each annealing step. The migration, agglomeration and annealing of grown-in and irradiated-introduced defects were studied. It was observed that the grown-in vacancy-type defects concentration decreased at 300 deg. C and 600 deg. C. For the irradiated sample annealed in argon, the positron trapping vacancy-type defect concentration decreased at 300 deg. C and 600 deg. C. Further annealing the as-grown and irradiated samples in argon increased the S parameter further. For the irradiated sample annealed in air, the vacancy-type defect concentration decreases at 300 deg. C and 700 deg. C.

Positron annihilation study of defects in electron-irradiated single crystal zinc oxide

International Nuclear Information System (INIS)

To, C K; Yang, B; Beling, C D; Fung, S; Ling, C C; Gong, M

2011-01-01

Pressurized melt grown zinc oxide (ZnO) single crystals purchased from Cermet Inc. were irradiated by 2 MeV electrons with fluence of 6x10 17 cm -2 . Isochronal annealing from 100 deg. C - 800 deg. C was performed on the crystals under argon and air ambience. Variable Energy Doppler Broadening Spectroscopy (VEDBS) was carried out on both the as-grown and the irradiated samples at each annealing step. The migration, agglomeration and annealing of grown-in and irradiated-introduced defects were studied. It was observed that the grown-in vacancy-type defects concentration decreased at 300 deg. C and 600 deg. C. For the irradiated sample annealed in argon, the positron trapping vacancy-type defect concentration decreased at 300 deg. C and 600 deg. C. Further annealing the as-grown and irradiated samples in argon increased the S parameter further. For the irradiated sample annealed in air, the vacancy-type defect concentration decreases at 300 deg. C and 700 deg. C.

The electro-oxidation of the mixture of formaldehyde and 2-propanol on gold (100 and (111 single crystal planes in alkaline medium

Directory of Open Access Journals (Sweden)

BRANISLAV Z. NIKOLIC

2000-12-01

Full Text Available The effect of formaldehyde on the oxidation of 2-propanol and vice versa on gold single crystal planes (100 and 111 was studied. An activating effect in the reaction of the simultaneous oxidation of 2-propanol and formaldehyde was obtained on a gold (100 plane. In the case of a gold (111 electrode, the activation effect was not obtained. It was concluded that the adsorption of formaldehyde on the electrode surface prevents the adsorption of poisoning species formed during the electro-oxidation of 2-propanol on the Au(100 plane, while this is not the case on the Au(111 plane. The different behaviour is caused by the difference in the symmetry of the surface atoms of these two Au single-crystal planes.

Dye-Sensitized Solar Cells Based on High Surface Area Nanocrystalline Zinc Oxide Spheres

Directory of Open Access Journals (Sweden)

Pavuluri Srinivasu

2011-01-01

Full Text Available High surface area nanocrystalline zinc oxide material is fabricated using mesoporous nanostructured carbon as a sacrificial template through combustion process. The resulting material is characterized by XRD, N2 adsorption, HR-SEM, and HR-TEM. The nitrogen adsorption measurement indicates that the materials possess BET specific surface area ca. 30 m2/g. Electron microscopy images prove that the zinc oxide spheres possess particle size in the range of 0.12 μm–0.17 μm. The nanocrystalline zinc oxide spheres show 1.0% of energy conversion efficiency for dye-sensitized solar cells.

The Mobility Enhancement of Indium Gallium Zinc Oxide Transistors via Low-temperature Crystallization using a Tantalum Catalytic Layer.

Science.gov (United States)

Shin, Yeonwoo; Kim, Sang Tae; Kim, Kuntae; Kim, Mi Young; Oh, Saeroonter; Jeong, Jae Kyeong

2017-09-07

High-mobility indium gallium zinc oxide (IGZO) thin-film transistors (TFTs) are achieved through low-temperature crystallization enabled via a reaction with a transition metal catalytic layer. For conventional amorphous IGZO TFTs, the active layer crystallizes at thermal annealing temperatures of 600 °C or higher, which is not suitable for displays using a glass substrate. The crystallization temperature is reduced when in contact with a Ta layer, where partial crystallization at the IGZO back-channel occurs with annealing at 300 °C, while complete crystallization of the active layer occurs at 400 °C. The field-effect mobility is significantly boosted to 54.0 cm 2 /V·s for the IGZO device with a metal-induced polycrystalline channel formed at 300 °C compared to 18.1 cm 2 /V·s for an amorphous IGZO TFT without a catalytic layer. This work proposes a facile and effective route to enhance device performance by crystallizing the IGZO layer with standard annealing temperatures, without the introduction of expensive laser irradiation processes.

Re-examination of the crystal structure of the β-pyrochlore oxide superconductor KOs 2O 6 by X-ray and convergent-beam electron diffraction analyses

Science.gov (United States)

Yamaura, Jun-Ichi; Hiroi, Zenji; Tsuda, Kenji; Izawa, Koichi; Ohishi, Yasuo; Tsutsui, Satoshi

2009-01-01

The crystal structure of the β-pyrochlore oxide superconductor KOs 2O 6 is re-examined. A single-crystal X-ray diffraction (XRD) analysis at room temperature first revealed that the compound crystallizes in a cubic structure with the centrosymmetric space group Fd3¯m, as in conventional pyrochlore oxides. Later, however, Schuck et al. claimed a different non-centrosymmetric F4¯3m structure based on their single-crystal XRD analysis. To unambiguously determine the true crystal structure of KOs 2O 6, we carried out high-resolution synchrotron powder X-ray and convergent-beam electron diffraction measurements at room temperature. The space group was determined with high reliability to be centrosymmetric Fd3¯m, not F4¯3m. This confirms the importance of the K atom location in a high-symmetry site, which causes unusually large rattling of the K atom.

TEM study of internal oxidation in an ODS-Eurofer alloy

International Nuclear Information System (INIS)

Klimenkov, M.; Lindau, R.; Moeslang, A.

2009-01-01

Analytical TEM investigations of samples from an oxide dispersion-strengthened Eurofer batch show the formation of new type of precipitates of Fe-Cr-V-O composition and a size of 40-250 nm. Structural HRTEM analysis reveals that the precipitates consist of (Mn,Fe)(Cr,V) 2 O 4 manganese chromium oxide of spinel structure. In some cases, the inclusions order along lines that can reach more than ten micrometers in length. Such lines of large particles might have a negative influence on the mechanical properties of the steel, as was observed. It is assumed that they form by internal oxidation during hot isostatic pressing due to the high oxygen content of the mechanically alloyed powder.

Tunable band structures in digital oxides with layered crystal habits

Science.gov (United States)

Shin, Yongjin; Rondinelli, James M.

2017-11-01

We use density functional calculations to show that heterovalent cation-order sequences enable control over band-gap variations up to several eV and band-gap closure in the bulk band insulator LaSrAlO4. The band-gap control originates from the internal electric fields induced by the digital chemical order, which induces picoscale band bending; the electric-field magnitude is mainly governed by the inequivalent charged monoxide layers afforded by the layered crystal habit. Charge transfer and ionic relaxations across these layers play secondary roles. This understanding is used to construct and validate a descriptor that captures the layer-charge variation and to predict changes in the electronic gap in layered oxides exhibiting antisite defects and in other chemistries.

Low Temperature Synthesis of Metal Oxides by a Supercritical Seed Enhanced Crystallization (SSEC) Process

DEFF Research Database (Denmark)

Jensen, Henrik; Brummerstedt Iversen, Steen; Joensen, Karsten Dan

2006-01-01

A novel method for producing crystalline nanosized metal oxides by a Supercritical Seed Enhanced Crystallization (SSEC) Process has been developed. The process is a modified sol-gel process taking place at temperatures as low as 95 ºC with supercritical CO2 as solvent and polypropylene as seeding...... material. The nanocrystalline product is obtained without having to resort to costly post-reaction processing and the product is obtained directly after the SSEC process. TiO2 powders produced by the SSEC process were shown to have a crystallinity of 60 % and a crystal size of 7.3 ± 2.6 nm....... The crystallinity can be controlled by changing the heating rate of the initial formation of the nanoparticles and the morphology can be altered by changing the process time....

Morphology-dependent electrocatalytic performance of Fe2(MoO43 for electro-oxidation of methanol in alkaline medium

Directory of Open Access Journals (Sweden)

Daoming Zhang

2017-06-01

Full Text Available Electrochemically synthesized nanosphere, nanorod and nanotube Fe2(MoO43 at optimized temperature and current density are characterized with XRD, SEM, TEM, XPS. Crystal lattices of the three types Fe2(MoO43 detected by HRTEM are well matched with the simulation analysis results from Materials Studio 6.0 based on the inorganic crystal structure database (ICSD data and the modified XRD lattice parameters. The ratios of Fe/Mo on the surface resulted from XPS analysis are 1.47, 1.63 and 2.22 respectively for nanosphere, nanorod and nanotube. The mixture of Fe2(MoO43 with polytetrafluoroethylene dispersion are coated on glass carbon substrate as electrode for electrocatalytic performance test by cyclic voltammetries in 0.1 mol/L KOH and 1 mol/L methanol electrolyte. Methanol oxidation peak current density of the Nanotube- Fe2(MoO43/GCEs electrode is 3.27 mA/cm2 higher than 2.8 mA/cm2 of platinum foil electrode, which shows enhanced catalytic activity of Nanotube-Fe2(MoO43/GCEs. The cyclic stability in terms of peak current retention are 91%, 92% and 88% respectively for Nanosphere-Fe2(MoO43/GCE, Nanorod-Fe2(MoO43/GCE and Nanotube-Fe2(MoO43/GCE electrode after 220 cycles. It is concluded that nanosized Fe2(MoO43 could be promising alternative non-noble electro-catalysts for electro-oxidation of methanol in alkaline medium.

TEM and HRTEM of Soot-in-oil particles and agglomerates from internal combustion engines

International Nuclear Information System (INIS)

Fay, M W; Rocca, A La; Shayler, P J

2014-01-01

Over time, the performance of lubricating oil in a diesel engine is affected by the build-up of carbon soot produced by the combustion process. TEM and HRTEM are commonly used to investigate the characteristics of individual and agglomerated particles from diesel exhaust, to understand the structure and distribution of the carbon sheets in the primary particles and the nanostructure morphology. However, high resolution imaging of soot-in-oil is more challenging, as mineral oil is a contaminant for the electron microscope and leads to instability under the electron beam. In this work we compare solvent extraction and centrifugation techniques for removing the mineral oil contaminant, and the effect on particle size distribution

Pressure-induced melting of micellar crystal

DEFF Research Database (Denmark)

Mortensen, K.; Schwahn, D.; Janssen, S.

1993-01-01

that pressure improves the solvent quality of water, thus resulting in decomposition of the micelles and consequent melting of the micellar crystal. The combined pressure and temperature dependence reveals that in spite of the apparent increase of order on the 100 angstrom length scale upon increasing......Aqueous solutions of triblock copolymers of poly(ethylene oxide) and poly(propylene oxide) aggregate at elevated temperatures into micelles which for polymer concentrations greater-than-or-equal-to 20% make a hard sphere crystallization to a cubic micellar crystal. Structural studies show...... temperature (decreasing pressure) the overall entropy increases through the inverted micellar crystallization characteristic....

Czochralski growth and characterization of {beta}-Ga{sub 2}O{sub 3} single crystals

Energy Technology Data Exchange (ETDEWEB)

Galazka, Z.; Uecker, R.; Irmscher, K.; Albrecht, M.; Klimm, D.; Pietsch, M.; Bruetzam, M.; Bertram, R.; Ganschow, S.; Fornari, R. [Leibniz Institute for Crystal Growth, Max-Born-Str. 2, 12489 Berlin (Germany)

2010-12-15

Transparent semiconducting {beta}-Ga{sub 2}O{sub 3} single crystals were grown by the Czochralski method from an iridium crucible under a dynamic protective atmosphere to control partial pressures of volatile species of Ga{sub 2}O{sub 3}. Thermodynamic calculations on different atmospheres containing CO{sub 2}, Ar and O{sub 2} reveal that CO{sub 2} growth atmosphere combined with overpressure significantly decreases evaporation of volatile Ga{sub 2}O{sub 3} species without any harm to iridium crucible. It has been found that CO{sub 2}, besides providing high oxygen concentration at high temperatures, is also acting as a minor reducing agent for Ga{sub 2}O{sub 3}. Different coloration of obtained crystals as well as optical and electrical properties are directly correlated with growth conditions (atmosphere, pressure and temperature gradients), but not with residual impurities. Typical electrical properties of the n-type {beta}-Ga{sub 2}O{sub 3} crystals at room temperature are: {rho} = 0.1 - 0.3 {omega}cm, {mu}{sub n,Hall} = 110 - 150 cm{sup 2}V{sup -1}s{sup -1}, n{sub Hall} = 2 - 6 x 10{sup 17} cm{sup -3} and E{sub Ionisation} = 30 - 40 meV. A decrease of transmission in the IR-region is directly correlated with the free carrier concentration and can be effectively modulated by the dynamic growth atmosphere. Electron paramagnetic resonance (EPR) spectra exhibit an isotropic shallow donor level and anisotropic defect level. According to differential thermal analysis (DTA) measurements, there is substantially no mass change of {beta}-Ga{sub 2}O{sub 3} crystals below 1200 C (i.e. no decomposition) under oxidizing or neutral atmosphere, while the mass gradually decreases with temperature above 1200 C. High resolution transmission electron microscopy (HRTEM) images at atomic resolution show the presence of vacancies, which can be attributed to Ga or O sites, and interstitials, which can likely be attributed to Ga atoms. (copyright 2010 WILEY-VCH Verlag GmbH and Co. KGa

Crystal Structural Effect of AuCu Alloy Nanoparticles on Catalytic CO Oxidation

International Nuclear Information System (INIS)

Zhan, Wangcheng; Wang, Jinglin; Wang, Haifeng; Zhang, Jinshui; Liu, Xiaofei

2017-01-01

Controlling the physical and chemical properties of alloy nanoparticles (NPs) is an important approach to optimize NP catalysis. Unlike other tuning knobs, such as size, shape, and composition, crystal structure has received limited attention and not been well understood for its role in catalysis. This deficiency is mainly due to the difficulty in synthesis and fine-tuning of the NPs’ crystal structure. Here, Exemplifying by AuCu alloy NPs with face centered cubic (fcc) and face centered tetragonal (fct) structure, we demonstrate a remarkable difference in phase segregation and catalytic performance depending on the crystal structure. During the thermal treatment in air, the Cu component in fcc-AuCu alloy NPs segregates more easily onto the alloy surface as compared to that in fct-AuCu alloy NPs. As a result, after annealing at 250 °C in air for 1 h, the fcc- and fct-AuCu alloy NPs are phase transferred into Au/CuO and AuCu/CuO core/shell structures, respectively. More importantly, this variation in heterostructures introduces a significant difference in CO adsorption on two catalysts, leading to a largely enhanced catalytic activity of AuCu/CuO NP catalyst for CO oxidation. Furthermore, the same concept can be extended to other alloy NPs, making it possible to fine-tune NP catalysis for many different chemical reactions.

Crystal Structural Effect of AuCu Alloy Nanoparticles on Catalytic CO Oxidation

Energy Technology Data Exchange (ETDEWEB)

Zhan, Wangcheng [East China Univ. of Science and Technology, Shanghai (China); Wang, Jinglin [East China Univ. of Science and Technology, Shanghai (China); Wang, Haifeng [East China Univ. of Science and Technology, Shanghai (China); Zhang, Jinshui [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Liu, Xiaofei [East China Univ. of Science and Technology, Shanghai (China); Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Zhang, Pengfei [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Chi, Miaofang [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Guo, Yanglong [East China Univ. of Science and Technology, Shanghai (China); Guo, Yun [East China Univ. of Science and Technology, Shanghai (China); Lu, Guanzhong [East China Univ. of Science and Technology, Shanghai (China); Sun, Shouheng [Brown Univ., Providence, RI (United States); Dai, Sheng [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Univ. of Tennessee, Knoxville, TN (United States); Zhu, Huiyuan [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

2017-06-07

Controlling the physical and chemical properties of alloy nanoparticles (NPs) is an important approach to optimize NP catalysis. Unlike other tuning knobs, such as size, shape, and composition, crystal structure has received limited attention and not been well understood for its role in catalysis. This deficiency is mainly due to the difficulty in synthesis and fine-tuning of the NPs’ crystal structure. Here, Exemplifying by AuCu alloy NPs with face centered cubic (fcc) and face centered tetragonal (fct) structure, we demonstrate a remarkable difference in phase segregation and catalytic performance depending on the crystal structure. During the thermal treatment in air, the Cu component in fcc-AuCu alloy NPs segregates more easily onto the alloy surface as compared to that in fct-AuCu alloy NPs. As a result, after annealing at 250 °C in air for 1 h, the fcc- and fct-AuCu alloy NPs are phase transferred into Au/CuO and AuCu/CuO core/shell structures, respectively. More importantly, this variation in heterostructures introduces a significant difference in CO adsorption on two catalysts, leading to a largely enhanced catalytic activity of AuCu/CuO NP catalyst for CO oxidation. Furthermore, the same concept can be extended to other alloy NPs, making it possible to fine-tune NP catalysis for many different chemical reactions.

Studying Impact of Different Precipitating Agents on Crystal Structure, Morphology and Photocatalytic Activity of Bismuth Oxide

Directory of Open Access Journals (Sweden)

Yayuk Astuti

2017-10-01

How to Cite: Astuti, Y., Arnelli, Pardoyo, Fauziyah, A., Nurhayati, S., Wulansari, A.D., Andianingrum, R., Widiyandari, H., Bhaduri, G.A. (2017. Studying Impact of Different Precipitating Agents on Crystal Structure, Morphology and Photocatalytic Activity of Bismuth Oxide. Bulletin of Chemical Reaction Engineering & Catalysis, 12 (3: 478-484 (doi:10.9767/bcrec.12.3.1144.478-484

Investigation of the Fission Products Silver, Palladium and Cadmium in Neutron Irradiated SiC using a Cs-Corrected HRTEM

International Nuclear Information System (INIS)

Rooyen, I.J. van; Olivier, E.J.; Neethling, J.H

2014-01-01

Electron microscopy investigations of selected coated particles from the first advanced gas reactor experiment (AGR-1) at Idaho National Laboratory (INL) provided important information on fission product distribution and chemical composition in the SiC layer. Furthermore, recent STEM analyses led to the discovery of Ag at SiC grain boundaries and triple junctions. As these Ag precipitates were nano-sized, high resolution transmission electron microscopy (HRTEM) was used to provide more information at the atomic level. This paper describes some of the first HRTEM results obtained from the examination of a particle from Compact 4-1-1, which was irradiated to an average burnup of 19.38% fissions per initial metal atom (FIMA), a time-average, volume-averaged temperature of 1072°C; a time-average, peak temperature of 1182°C and an average fast fluence of 4.13x10 21 n/cm 2 . Based on gamma-ray analysis, it is estimated that this particle may have released as much as 10% of its available Ag-110m inventory during irradiation. The HRTEM investigation focused on Ag, Pd, and Cd due to the interest in Ag transport mechanisms and possible correlation with Pd and Ag previously found. Additionally, Compact 4-1-1 contains fuel particles fabricated with a different fuel carrier gas composition and lower deposition temperatures for the SiC layer relative to the Baseline fabrication conditions, which are expected to reduce the concentration of SiC defects resulting from uranium dispersion. Small Ag precipitates were observed at a distance of about 6.5 micron from the inner PyC-SiC interface. Pd, Ag, and Cd were found to co-exist in some of the SiC grain boundaries and triple junctions. This study confirmed the presence of Pd both at inter- and intragranular sites; in the latter case specifically at stacking faults. Small Ag precipitates were observed at a distance of about 6.5 microns from the inner PyC/SiC interface. (author)

Comparison of the redox activities of sol-gel and conventionally prepared Bi-Mo-Ti mixed oxides

Energy Technology Data Exchange (ETDEWEB)

Wildberger, M.; Grundwaldt, J.D.; Mallat, T.; Baiker, A. [Lab. of Technical Chemistry, Swiss Federal Inst. of Technology, ETH-Zentrum, Zuerich (Switzerland)

1998-12-31

Novel sol-gel Bi-Mo-Ti oxides have been prepared and characterized by XRD, XPS, FT-Raman and HRTEM. The surface Bi{sup 3+} and Mo{sup 6+} species of some xerogels and an aerogel could be reduced and oxidized at room temperature, whereas the conventionally prepared reference materials were not reduced by H{sub 2} below 300 C. The unusual redox properties, under very mild conditions, are likely due to the unique morphology of Bi-Mo-oxides stabilized by titania. During butadiene oxidation to furan at above 400 C to sol-gel mixed oxides restructured considerably and their performance was barely better than that of titania-supported Bi-Mo oxides. (orig.)

Synthesis of indium oxide cubic crystals by modified hydrothermal route for application in room temperature flexible ethanol sensors

International Nuclear Information System (INIS)

Seetha, M.; Meena, P.; Mangalaraj, D.; Masuda, Yoshitake; Senthil, K.

2012-01-01

Highlights: ► For the first time HMT is used in the preparation of indium oxide. ► HMT itself acts as base for the precursor and results in cubic indium hydroxide. ► Modified hydrothermal route used for the preparation of cubic indium oxide crystals. ► As a new approach a composite film synthesized with prepared indium oxide. ► Film showed good response to ethanol vapours with quick response and recovery times. - Abstract: Indium oxide cubic crystals were prepared by using hexamethylenetetramine and indium chloride without the addition of any structure directing agents. The chemical route followed in the present work was a modified hydrothermal synthesis. The average crystallite size of the prepared cubes was found to be 40 nm. A blue emission at 418 nm was observed at room temperature when the sample was excited with a 380 nm Xenon lamp. This emission due to oxygen vacancies made the material suitable for gas sensing applications. The synthesized material was made as a composite film with polyvinyl alcohol which was more flexible than the films prepared on glass substrates. This flexible film was used as a sensing element and tested with ethanol vapours at room temperature. The film showed fast response as well as recovery to ethanol vapours with a sensor response of about 1.4 for 100 ppm of the gas.

Crystallization kinetics of a soda lime silica glass with TiO2 addition

International Nuclear Information System (INIS)

De la Parra A, S. M.; Alvarez M, A.; Torres G, L. C.; Sanchez, E. M.

2009-01-01

Studies conducted into Na 2 O-CaO-3SiO 2 glass composition suggest that its phase transformation occurs from the surface towards the interior of the sample. In a study carried out in 1982, it was reported that no addition of nucleating agents modified the mechanism. Taking advantage of the disposition materials synthesized by nanotechnology, in this study TiO 2 in nanometer size was used with the idea that, because of its qualities, it could modify the crystallization mechanism. The glasses obtained as well as the thermally treated samples, were evaluated by the X-ray diffraction (XRD) powder method, differential thermal analysis (DTA), and by optical microscopy and high resolution transmission electron microscopy (HRTEM). Within the range of TiO 2 concentration studied (0 - 10 wt %), 10 wt % of TiO 2 considerably reduced the Na 2 O-2CaO-3SiO 2 phase crystallization process. The crystallization mechanism was not modified and TiO 2 did not form compounds with the matrix components. (Author)

Design of photonic crystal surface emitting lasers with indium-tin-oxide top claddings

Science.gov (United States)

Huang, Shen-Che; Hong, Kuo-Bin; Chiu, Han-Lun; Lan, Shao-Wun; Chang, Tsu-Chi; Li, Heng; Lu, Tien-Chang

2018-02-01

Electrically pumped GaAs-based photonic crystal surface emitting lasers were fabricated using a simple fabrication process by directly capping the indium-tin-oxide transparent conducting thin film as the top cladding layer upon a photonic crystal layer. Optimization of the separate-confinement heterostructures of a laser structure is crucial to improving characteristics by providing advantageous optical confinements. The turn-on voltage, series resistance, threshold current, and slope efficiency of the laser with a 100 × 100 μm2 photonic crystal area operated at room temperature were 1.3 V, 1.5 Ω, 121 mA, and 0.2 W/A, respectively. Furthermore, we demonstrated a single-lobed lasing wavelength of 928.6 nm at 200 mA and a wavelength redshift rate of 0.05 nm/K in temperature-dependent measurements. The device exhibited the maximum output power of approximately 400 mW at an injection current of 2 A; moreover, divergence angles of less than 1° for the unpolarized circular-shaped laser beam were measured at various injection currents. Overall, the low threshold current, excellent beam quality, small divergence, high output power, and high-operating-temperature (up to 343 K) of our devices indicate that they can potentially fill the requirements for next-generation light sources and optoelectronic devices.

Structural, optical investigations of graphene from graphene oxide using green method

International Nuclear Information System (INIS)

Kumar, Dinesh; Shukla, Shobha; Saxena, Sumit

2015-01-01

Graphene nano sheets (GNS) are synthesized from Graphene Oxide (GO) using commercial sugar as a reducing agent. A green and facile approach is followed to synthesize chemically converted GNS using exfoliated GO as precursor. The merit of this method is that both the reducing agents themselves and the oxidized products are environmentally friendly. The prepared materials are characterized with X-ray diffraction (XRD), UV-Visible absorption spectroscopy, High resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED). The results of XRD, UV-vis analysis provide a clear indication of removal of oxygen-containing groups from GO and the formation of GNS

Crystallization of copper metaphosphate glass

Science.gov (United States)

Bae, Byeong-Soo; Weinberg, Michael C.

1993-01-01

The effect of the valence state of copper in copper metaphosphate glass on the crystallization behavior and glass transition temperature has been investigated. The crystallization of copper metaphosphate is initiated from the surface and its main crystalline phase is copper metaphosphate (Cu(PO)3),independent of the (Cu sup 2+)/(Cu(total)). However, the crystal morphology, the relative crystallization rates, and their temperature dependences are affected by the (Cu sup 2+)/(Cu (total)) ratio in the glass. On the other hand, the totally oxidized glass crystallizes from all over the surface. The relative crystallization rate of the reduced glass to the totally oxidized glass is large at low temperature, but small at high temperature. The glass transition temperature of the glass increases as the (Cu sup 2+)/(Cu(total)) ratio is raised. It is also found that the atmosphere used during heat treatment does not influence the crystallization of the reduced glass, except for the formation of a very thin CuO surface layer when heated in air.

Preparation and supercapacitor application of the single crystal nickel hydroxide and oxide nanosheets

Energy Technology Data Exchange (ETDEWEB)

Li, Qing [Department of Materials Science and Engineering, Yunnan University, 650091 Kunming (China); Ni, Haifang [Institute of Materials Science and Engineering, University of Science and Technology Beijing, 100083 Beijing (China); Cai, Yun; Cai, Xiaoyan [Department of Materials Science and Engineering, Yunnan University, 650091 Kunming (China); Liu, Yongjun [Advanced Analysis and Measurement Center, Yunnan University, 650091 Kunming (China); Chen, Gang [Department of Materials Science and Engineering, Yunnan University, 650091 Kunming (China); Fan, Li-Zhen, E-mail: fanlizhen@ustb.edu.cn [Institute of Materials Science and Engineering, University of Science and Technology Beijing, 100083 Beijing (China); Wang, Yude, E-mail: ydwang@ynu.edu.cn [Department of Materials Science and Engineering, Yunnan University, 650091 Kunming (China)

2013-09-01

Graphical abstract: The nickel hydroxide and nickel oxide nanosheets prepared using CTAB at room temperature exhibit a high specific capacitance, prompt charge/discharge rate. - Highlights: • The nickel hydroxide nanosheets were prepared using CTAB at room temperature. • Ni(OH){sub 2} nanosheet can be successfully converted to NiO nanosheet via calcination. • The NiO nanosheet has a specific capacitance of 388 F g{sup −1} at 5 A g{sup −1} in KOH solution. • Anneal temperature impacts capacitive properties as electrode. - Abstract: The single crystalline Ni(OH){sub 2} nanosheets were synthesized by a simple chemical precipitation method using nickel chloride as precursors and ammonia as precipitating agent. The Ni(OH){sub 2} nanosheets were successfully converted to NiO nanosheets via calcination under appropriate conditions. Analytical methods such as X-ray diffraction (XRD) spectra, scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), and Fourier transformed infrared (FTIR) spectra were employed to characterize the morphology and microstructure of the final products. The experimental results revealed that Ni(OH){sub 2} nanosheets were shape-preserved transformed to NiO nanosheets at 250 °C for 24 h. Ni(OH){sub 2} and NiO nanosheets were directly functionalized as supercapacitor electrodes for potential energy storage applications, whose charge–discharge properties, electrochemical impedance spectra, cyclic voltammetry, and cycle performance were examined. The experimental results show that the single-crystalline NiO nanosheets are a promising candidate for the supercapacitor electrode. They exhibit a high specific capacitance, prompt charge/discharge rate.

Composition dependence of spontaneous crystallization of phosphosilicate glass melts during cooling

DEFF Research Database (Denmark)

Liu, S.J.; Zhu, C.F.; Zhang, Y.F.

2012-01-01

Crystallization behavior of alumino-phospho-silicate melts during cooling is studied by means of the differential scanning calorimetry, X-ray diffractometry and viscometry. The results show a pronounced impact of alkaline earth oxide, alkali oxide and fluoride on the crystal type and crystallizat......Crystallization behavior of alumino-phospho-silicate melts during cooling is studied by means of the differential scanning calorimetry, X-ray diffractometry and viscometry. The results show a pronounced impact of alkaline earth oxide, alkali oxide and fluoride on the crystal type...... and crystallization degree. It is found that adding NaF into the studied compositions slightly decreases melt fragility and improves both the glass-forming ability and melt workability. This effect is associated with the unique structural role of NaF compared to the other modifier oxides. It is also found...

Thin dielectric film thickness determination by advanced transmission electron microscopy

Energy Technology Data Exchange (ETDEWEB)

Diebold, A.C.; Foran, B.; Kisielowski, C.; Muller, D.; Pennycook, S.; Principe, E.; Stemmer, S.

2003-09-01

High Resolution Transmission Electron Microscopy (HR-TEM) has been used as the ultimate method of thickness measurement for thin films. The appearance of phase contrast interference patterns in HR-TEM images has long been confused as the appearance of a crystal lattice by non-specialists. Relatively easy to interpret crystal lattice images are now directly observed with the introduction of annular dark field detectors for scanning TEM (STEM). With the recent development of reliable lattice image processing software that creates crystal structure images from phase contrast data, HR-TEM can also provide crystal lattice images. The resolution of both methods was steadily improved reaching now into the sub Angstrom region. Improvements in electron lens and image analysis software are increasing the spatial resolution of both methods. Optimum resolution for STEM requires that the probe beam be highly localized. In STEM, beam localization is enhanced by selection of the correct aperture. When STEM measurement is done using a highly localized probe beam, HR-TEM and STEM measurement of the thickness of silicon oxynitride films agree within experimental error. In this paper, the optimum conditions for HR-TEM and STEM measurement are discussed along with a method for repeatable film thickness determination. The impact of sample thickness is also discussed. The key result in this paper is the proposal of a reproducible method for film thickness determination.

Room-temperature synthesis and enhanced catalytic performance of silver-reduced graphene oxide nanohybrids

International Nuclear Information System (INIS)

Thu, Tran Viet; Ko, Pil Ju; Phuc, Nguyen Huu Huy; Sandhu, Adarsh

2013-01-01

The synthesis of supported, ultrasmall metallic nanoparticles (NPs) is of great importance for catalytic applications. In this study, silver-reduced graphene oxide nanohybrids (Ag–rGO NHs) were prepared by reducing Ag ions and graphene oxide (GO) at room temperature using sodium borohydride (NaBH 4 ) and trisodium citrate. The resulting products were characterized using UV–Vis spectroscopy, X-ray diffraction, Raman spectroscopy, scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), and X-ray photoelectron spectroscopy. The rich chemistry of GO surface provided many sites for the nucleation of Ag ions and efficiently limited their growth. Ag NPs were uniformly grown on basal planes of rGO with a high density (∼1,700 NPs μm −2 ) and well-defined size (3.6 ± 0.6 nm) as evidenced in SEM and HRTEM studies. The resulting Ag–rGO NHs were readily dispersed in water and exhibited enhanced catalytic activity toward the reduction of 4-nitrophenol by NaBH 4 in comparison to unsupported Ag NPs. The role of rGO as an excellent support for Ag catalyst is discussed

Room-temperature synthesis and enhanced catalytic performance of silver-reduced graphene oxide nanohybrids

Energy Technology Data Exchange (ETDEWEB)

Thu, Tran Viet, E-mail: thu@eiiris.tut.ac.jp; Ko, Pil Ju, E-mail: ko@eiiris.tut.ac.jp [Toyohashi University of Technology, Electronics-Inspired Interdisciplinary Research Institute (Japan); Phuc, Nguyen Huu Huy [Toyohashi University of Technology, Department of Electrical and Electronic Information Engineering (Japan); Sandhu, Adarsh [Toyohashi University of Technology, Electronics-Inspired Interdisciplinary Research Institute (Japan)

2013-10-15

The synthesis of supported, ultrasmall metallic nanoparticles (NPs) is of great importance for catalytic applications. In this study, silver-reduced graphene oxide nanohybrids (Ag-rGO NHs) were prepared by reducing Ag ions and graphene oxide (GO) at room temperature using sodium borohydride (NaBH{sub 4}) and trisodium citrate. The resulting products were characterized using UV-Vis spectroscopy, X-ray diffraction, Raman spectroscopy, scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), and X-ray photoelectron spectroscopy. The rich chemistry of GO surface provided many sites for the nucleation of Ag ions and efficiently limited their growth. Ag NPs were uniformly grown on basal planes of rGO with a high density ({approx}1,700 NPs {mu}m{sup -2}) and well-defined size (3.6 {+-} 0.6 nm) as evidenced in SEM and HRTEM studies. The resulting Ag-rGO NHs were readily dispersed in water and exhibited enhanced catalytic activity toward the reduction of 4-nitrophenol by NaBH{sub 4} in comparison to unsupported Ag NPs. The role of rGO as an excellent support for Ag catalyst is discussed.

Crystallization and electrical resistivity of Cu{sub 2}O and CuO obtained by thermal oxidation of Cu thin films on SiO{sub 2}/Si substrates

Energy Technology Data Exchange (ETDEWEB)

De Los Santos Valladares, L., E-mail: ld301@cam.ac.uk [Cavendish Laboratory, University of Cambridge, J.J Thomson Av., Cambridge CB3 0HE (United Kingdom); Materials and Structures Laboratory, Tokyo Institute of Technology, 4259 Nagatsuta-cho, Midori-ku, Yokohama 226-8503 (Japan); Departamento de Fisica, Universidade Federal de Pernambuco, 50670-901, Recife-Pe (Brazil); Salinas, D. Hurtado [Materials and Structures Laboratory, Tokyo Institute of Technology, 4259 Nagatsuta-cho, Midori-ku, Yokohama 226-8503 (Japan); Laboratorio de Ceramicos y Nanomateriales, Facultad de Ciencias Fisicas, Universidad Nacional Mayor de San Marcos, Ap. Postal 14-0149, Lima (Peru); Dominguez, A. Bustamante [Laboratorio de Ceramicos y Nanomateriales, Facultad de Ciencias Fisicas, Universidad Nacional Mayor de San Marcos, Ap. Postal 14-0149, Lima (Peru); Najarro, D. Acosta [Instituto de Fisica, Departamento de Materia Condensada, Universidad Nacional Autonoma de Mexico, Ap. Postal 20-364, CP 01000 (Mexico); Khondaker, S.I. [NanoScience Technology Centre and Department of Physics, University of Central Florida, Orlando, FL 32826 (United States); Mitrelias, T.; Barnes, C.H.W. [Cavendish Laboratory, University of Cambridge, J.J Thomson Av., Cambridge CB3 0HE (United Kingdom); Aguiar, J. Albino [Departamento de Fisica, Universidade Federal de Pernambuco, 50670-901, Recife-Pe (Brazil); Majima, Y. [Materials and Structures Laboratory, Tokyo Institute of Technology, 4259 Nagatsuta-cho, Midori-ku, Yokohama 226-8503 (Japan); CREST, Japan Science and Technology Agency (JST), 4259 Nagatsuta-cho, Midori-ku, Yokohama 226-8503 (Japan)

2012-08-01

In this work, we study the crystallization and electrical resistivity of the formed oxides in a Cu/SiO{sub 2}/Si thin film after thermal oxidation by ex-situ annealing at different temperatures up to 1000 Degree-Sign C. Upon increasing the annealing temperature, from the X ray diffractogram the phase evolution Cu {yields} Cu + Cu{sub 2}O {yields} Cu{sub 2}O {yields} Cu{sub 2}O + CuO {yields} CuO was detected. Pure Cu{sub 2}O films are obtained at 200 Degree-Sign C, whereas uniform CuO films without structural surface defects such as terraces, kinks, porosity or cracks are obtained in the temperature range 300-550 Degree-Sign C. In both oxides, crystallization improves with annealing temperature. A resistivity phase diagram, which is obtained from the current-voltage response, is presented here. The resistivity was expected to increase linearly as a function of the annealing temperature due to evolution of oxides. However, anomalous decreases are observed at different temperatures ranges, this may be related to the improvement of the crystallization and crystallite size when the temperature increases. - Highlights: Black-Right-Pointing-Pointer The crystallization and electrical resistivity of oxides in a Cu films are studied. Black-Right-Pointing-Pointer In annealing Cu films, the phase evolution Cu + Cu{sub 2}O {yields} Cu{sub 2}O {yields} Cu{sub 2}O + CuO {yields} CuO occurs. Black-Right-Pointing-Pointer A resistivity phase diagram, obtained from the current-voltage response, is presented. Black-Right-Pointing-Pointer Some decreases in the resistivity may be related to the crystallization.

Improving the oxidation resistance and stability of Ag nanoparticles by coating with multilayered reduced graphene oxide

Science.gov (United States)

Li, Yahui; Zhang, Huayu; Wu, Bowen; Guo, Zhuo

2017-12-01

A kind of coating nanostructure, Ag nanoparticles coated with multilayered reduced graphene oxide (RGO), is fabricated by employing a three-step reduction method in an orderly manner, which is significantly different from the conventional structures that are simply depositing or doping with Ag nanoparticles on RGO via chemical reduction. The as-prepared nanostructure is investigated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected-area electronic diffraction (SEAD), scanning electron microscopy (SEM), and Fourier transform infrared spectroscopy (FTIR). The results show that the obtained Ag/RGO nanostructure is observed to be a perfect coating structure with well dispersed Ag particles, which is responsible for the remarkable oxidation resistance. The results of XPS spectra indicate the content of metallic Ag is far greater than that of Ag oxides despite of prolonged exposure to the air, which fully demonstrate the excellent stability of thus coating nanostructure.

Atomic Scale Chemical and Structural Characterization of Ceramic Oxide Heterostructure Interfaces

Energy Technology Data Exchange (ETDEWEB)

Singh, R. K.

2003-04-16

The research plan was divided into three tasks: (a) growth of oxide heterostructures for interface engineering using standard thin film deposition techniques, (b) atomic level characterization of oxide heterostructure using such techniques as STEM-2 combined with AFM/STM and conventional high-resolution microscopy (HRTEM), and (c) property measurements of aspects important to oxide heterostructures using standard characterization methods, including dielectric properties and dynamic cathodoluminescence measurements. Each of these topics were further classified on the basis of type of oxide heterostructure. Type I oxide heterostructures consisted of active dielectric layers, including the materials Ba{sub x}Sr{sub 1-x}TiO{sub 3} (BST), Y{sub 2}O{sub 3} and ZrO{sub 2}. Type II heterostructures consisted of ferroelectric active layers such as lanthanum manganate and Type III heterostructures consist of phosphor oxide active layers such as Eu-doped Y{sub 2}O{sub 3}.

Crystal interface and high-resolution electron microscopy—the best partner

Directory of Open Access Journals (Sweden)

H Ichinose

2000-01-01

Full Text Available Several contributions of HRTEM on the interface science are reviewed in chronological order. The first contribution of HRTEM is the observation of gold (113Σ°11 boundary, giving experimental proof of the CSL model. An observation of the asymmetric (112Σ°3 boundary follows. A SiC grain boundary is effectively assessed not by the density of CSL point but the number of dangling bonds in the boundary. A ZnO/Pd interface provides an example that a misfit dislocation does not necessarily accommodate the lattice mismatch. Segregated interface shows characteristic HRTEM image contrast, suggesting change in atomic bonding. An atomic height step in the semiconductor hetero interface is observed by the Chemical Lattice Image technique. In the diamond grain boundary a dangling bond may not elevate the boundary energy, being contradictory of the least dangling bond rule. Super-high resolution of the HVHRTEM enable us to determine atomic species in the grain boundary. Combined use of HRTEM and EELSE allows us to discuss the correlation between atomic structure and nature of the corresponding interface. It is not exaggeration to say that modern interface science does not exist witout HRTEM. On the other hand, many complicated interfaces found by HRTEM remained as unaswered questions. An innovative structural model is requested to appear on the scene.

HR-TEM and FT-Raman dataset of the caffeine interacted Phe–Phe peptide nanotube for possible sensing applications

OpenAIRE

Narayanan, A. Lakshmi; Dhamodaran, M.; Solomon, J. Samu; Karthikeyan, B.; Govindhan, R.

2017-01-01

Sensing ability of caffeine interaction with Phe-Phe annotates (PNTs), is presented (Govindhan et al., 2017; Karthikeyan et al., 2014; Tavagnacco et al., 2013; Kennedy et al., 2011; Wang et al., 2017) [1–5] in this data set. Investigation of synthesized caffeine carrying peptide nanotubes are carried out by FT-Raman spectral analysis and high resolution transmission electron microscopy (HR-TEM). Particle size of the caffeine loaded PNTs is < 40 nm. The FT-Raman spectrum signals are enhanced i...

Microwave Synthesis of Zinc Oxide/Reduced Graphene Oxide Hybrid for Adsorption-Photocatalysis Application

Directory of Open Access Journals (Sweden)

Fatin Saiha Omar

2014-01-01

Full Text Available This work reports on synthesis of zinc oxide/reduced graphene oxide (ZnO/rGO nanocomposites in the presence of diethylenetriamine (DETA via a facile microwave method. The X-ray diffraction (XRD patterns of the nanocomposites correspond to the ZnO hexagonal phase wurtzite structure. The high-resolution transmission electron microscopy (HRTEM images revealed that the ZnO nanorods, with an average length : diameter ratio of 10, were successfully deposited on the rGO sheets. Under the irradiation of sunlight, the nanocomposites showed enhanced adsorption-photocatalysis by more than twofold and photocurrent response by sixfold compared to the ZnO. The excellent photoactivity performance of the nanocomposites is contributed by smaller ZnO nanorod and the presence of rGO that acts as a photosensitizer by transferring electrons to the conduction band of ZnO within the nanocomposite during sunlight illumination.

Desorption of Furfural from Bimetallic Pt-Fe Oxides/Alumina Catalysts

Directory of Open Access Journals (Sweden)

Gloria Lourdes Dimas-Rivera

2014-01-01

Full Text Available In this work, the desorption of furfural, which is a competitive intermediate during the production of biofuel and valuable aromatic compounds, was studied using pure alumina, as well as alumina impregnated with iron and platinum oxides both individually and in combination, using thermogravimetric analysis (TGA. The bimetallic sample exhibited the lowest desorption percentage for furfural. High-resolution transmission electron microscopy (HRTEM imaging revealed the intimate connection between the iron and platinum oxide species on the alumina support. The mechanism of furfural desorption from the Pt-Fe/Al2O3 0.5%-0.5% sample was determined using physisorbed furfural instead of chemisorbed furfural; this mechanism involved the oxidation of the C=O group on furfural by the catalyst. The oxide nanoparticles on γ-Al2O3 support helped to stabilize the furfural molecule on the surface.

Investigation of the Distribution of Fission Products Silver, Palladium and Cadmium in Neutron Irradiated SIC using a Cs Corrected HRTEM

Energy Technology Data Exchange (ETDEWEB)

I. J. van Rooyen; E. Olivier; J. H Neethlin

2014-10-01

Electron microscopy examinations of selected coated particles from the first advanced gas reactor experiment (AGR-1) at Idaho National Laboratory (INL) provided important information on fission product distribution and chemical composition. Furthermore, recent research using STEM analysis led to the discovery of Ag at SiC grain boundaries and triple junctions. As these Ag precipitates were nano-sized, high resolution transmission electron microscopy (HRTEM) examination was used to provide more information at the atomic level. This paper describes some of the first HRTEM results obtained by examining a particle from Compact 4-1-1, which was irradiated to an average burnup of 19.26% fissions per initial metal atom (FIMA), a time average, volume-averaged temperature of 1072°C; a time average, peak temperature of 1182°C and an average fast fluence of 4.13 x 1021 n/cm2. Based on gamma analysis, it is estimated that this particle may have released as much as 10% of its available Ag-110m inventory during irradiation. The HRTEM investigation focused on Ag, Pd, Cd and U due to the interest in Ag transport mechanisms and possible correlation with Pd, Ag and U previously found. Additionally, Compact 4-1-1 contains fuel particles fabricated with a different fuel carrier gas composition and lower deposition temperatures for the SiC layer relative to the Baseline fabrication conditions, which are expected to reduce the concentration of SiC defects resulting from uranium dispersion. Pd, Ag, and Cd were found to co-exist in some of the SiC grain boundaries and triple junctions whilst U was found to be present in the micron-sized precipitates as well as separately in selected areas at grain boundaries. This study confirmed the presence of Pd both at inter- and intragranular positions; in the latter case specifically at stacking faults. Small Pd nodules were observed at a distance of about 6.5 micron from the inner PyC/SiC interface.

Synthesis of indium oxide cubic crystals by modified hydrothermal route for application in room temperature flexible ethanol sensors

Energy Technology Data Exchange (ETDEWEB)

Seetha, M., E-mail: seetha.phy@gmail.com [Department of Physics, SRM University, Kattankulathur, Kancheepuram Dt 603 203 (India); Meena, P. [Department of Physics, PSGR Krishnammal College for Women, Coimbatore 641 046 (India); Mangalaraj, D., E-mail: dmraj800@yahoo.com [DRDO-BU Centre for Life Sciences, Bharathiar University Campus, Coimbatore (India); Department of Nanoscience and Technology, Bharathiar University, Coimbatore 641 014 (India); Masuda, Yoshitake [National Institute of Advanced Industrial Science and Technology (AIST), Nagoya 463-8560 (Japan); Senthil, K. [School of Advanced Materials Science and Engineering, Sungkyunkwan University (Suwon Campus), Cheoncheon-dong 300, Jangan-gu, Suwon 440-746 (Korea, Republic of)

2012-03-15

Highlights: Black-Right-Pointing-Pointer For the first time HMT is used in the preparation of indium oxide. Black-Right-Pointing-Pointer HMT itself acts as base for the precursor and results in cubic indium hydroxide. Black-Right-Pointing-Pointer Modified hydrothermal route used for the preparation of cubic indium oxide crystals. Black-Right-Pointing-Pointer As a new approach a composite film synthesized with prepared indium oxide. Black-Right-Pointing-Pointer Film showed good response to ethanol vapours with quick response and recovery times. - Abstract: Indium oxide cubic crystals were prepared by using hexamethylenetetramine and indium chloride without the addition of any structure directing agents. The chemical route followed in the present work was a modified hydrothermal synthesis. The average crystallite size of the prepared cubes was found to be 40 nm. A blue emission at 418 nm was observed at room temperature when the sample was excited with a 380 nm Xenon lamp. This emission due to oxygen vacancies made the material suitable for gas sensing applications. The synthesized material was made as a composite film with polyvinyl alcohol which was more flexible than the films prepared on glass substrates. This flexible film was used as a sensing element and tested with ethanol vapours at room temperature. The film showed fast response as well as recovery to ethanol vapours with a sensor response of about 1.4 for 100 ppm of the gas.

Low-energy electron observation of graphite and molybdenite crystals. Application to the study of graphite oxidation

International Nuclear Information System (INIS)

David, G.

1969-01-01

The LEED study of cleaved (0001) faces of crystals having a layered structure allowed to investigate flakes free of steps on graphite and molybdenite, to show twinning on natural graphite. By intensity measurements and computation in the case of a kinematical approximation it has been possible to determine an inner potential of 19 eV for graphite and to identify the direction of the Mo-S bond of the surface layer of molybdenite. The oxidation of graphite has been studied by observing changes, in symmetry of the diffraction patterns and by mass spectrometry of the gases evolved during the oxidation. No surface compounds have been detected and the carbon layers appeared to be peeled off one after the other. The oxidation took place at temperatures higher than 520 C under an oxygen pressure of 10 -5 torr. (author) [fr

A versatile Czochralski crystal growth system with automatic diameter control

Science.gov (United States)

Aggarwal, M. D.; Metzl, R.; Wang, W. S.; Choi, J.

1995-07-01

A versatile Czochralski crystal pulling system with automatic diameter control for the growth of nonlinear optical oxide crystals is discussed. Pure and doped bulk single crystals of bismuth silicon oxide (Bi12SiO20) have been successfully grown using this system. The system consists of a regular Czochralski type pulling system with provision for continuous weighing of the growing crystal to provide feedback for power control.

Compositional Tuning, Crystal Growth, and Magnetic Properties of Iron Phosphate Oxide

Science.gov (United States)

Tarne, Michael

Iron phosphate oxide, Fe3PO4O 3, is a crystalline solid featuring magnetic Fe3+ ions on a complex lattice composed of closely-spaced triangles. Previous work from our research group on this compound has proposed a helical magnetic structure below T = 163 K attributed to J1 - J2 competing interactions between nearest-neighbor and next-nearest-neighbor iron atoms. This was based on neutron powder diffraction featuring unique broad, flat-topped magnetic reflections due to needle-like magnetic domains. In order to confirm the magnetic structure and origins of frustration, this thesis will expand upon the research focused on this compound. The first chapter focuses on single crystal growth of Fe3PO 4O3. While neutron powder diffraction provides insight to the magnetic structure, powder and domain averaging obfuscate a conclusive structure for Fe3PO4O3 and single crystal neutron scattering is necessary. Due to the incongruency of melting, single crystal growth has proven challenging. A number of techniques including flux growth, slow cooling, and optical floating zone growth were attempted and success has been achieved via heterogenous chemical vapor transport from FePO 4 using ZrCl4 as a transport agent. These crystals are of sufficient size for single crystal measurements on modern neutron diffractometers. Dilution of the magnetic sublattice in frustrated magnets can also provide insight into the nature of competing spin interactions. Dilution of the Fe 3+ lattice in Fe3PO4O3 is accomplished by substituting non-magnetic Ga3+ to form the solid solution series Fe3-xGaxPO4O3 with x = 0, 0.012, 0.06, 0.25, 0.5, 1.0, 1.5. The magnetic susceptibility and neutron powder diffraction data of these compounds are presented. A dramatic decrease of the both the helical pitch length and the domain size is observed with increasing x; for x > 0.5, the compounds lack long range magnetic order. The phases that do exhibit magnetic order show a decrease in helical pitch with increasing x

Self-Assembly of Single-Crystal Silver Microflakes on Reduced Graphene Oxide and their Use in Ultrasensitive Sensors

KAUST Repository

Chen, Ye

2016-01-19

Compared to 1D structures, 2D structures have higher specific and active surface, which drastically improves electron transfer and extensibility along 2D plane. Herein, 2D-single crystal silver microflakes (AgMFs) are prepared for the first time in situ on reduced graphene oxide (RGO) by solvothermal synthesis with thickness around 100 nm and length around 10 μm. The oriented attachment mechanism is hypothesized to control the silver crystal growth and self-assembly of reduced silver units to form single-crystal AgMF structure on RGO sheets. Employing it as an electrode to fabricate reliable and extremely sensitive pressure sensors verifies the applicability of this novel 2D structure. Contrary to nanowires, 2D microflakes can intercalate better within the polymer matrix to provide an enhanced network for electron movement. The designed sensor can retain more than 4.7 MPa-1 after 10 000 cycles. The design proves functional for monitoring various actions such as wrist movement, squatting, walking, and delicate finger touch with high durability. A highly sensitive and flexible pressure sensor is fabricated based on the self-assembly of silver microflakes on reduced graphene oxide. This sensor exhibits an excellent pressure sensitivity as it can retain more than 4.7 MPa-1 after 10 000 cycles. This system is successfully used to monitor wrist movement, walking, and squatting and can be applied in touch screen panels, robotic systems, and prosthetics. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis of a carbon-coated NiO/MgO core/shell nanocomposite as a Pd electro-catalyst support for ethanol oxidation

International Nuclear Information System (INIS)

Mahendiran, C.; Maiyalagan, T.; Scott, K.; Gedanken, A.

2011-01-01

Highlights: → Carbon coated on NiO/MgO in a core/shell nanostructure is synthesized by RAPET. → The carbon-coated NiO/MgO is supported by Pd. → The electrocatalytic properties of the Pd/(NiO/MgO-C) catalyst for ethanol oxidation studied. - Abstract: Carbon coated on NiO/MgO in a core/shell nanostructure was synthesized by the single-step RAPET (reaction under autogenic pressure at elevated temperatures) technique, and the obtained formation mechanism of the core/shell nanocomposite was presented. The carbon-coated NiO/MgO and its supported Pd catalyst, Pd/(NiO/MgO-C), were characterized by SEM, HR-TEM, XRD and cyclic voltammetry. The X-ray diffraction patterns confirmed the face-centered cubic crystal structure of NiO/MgO. Raman spectroscopy measurements provided structural evidence for the formation of a NiO/MgO composite and the nature of the coated carbon shell. The high-resolution transmission electron microscopy images showed the core and shell morphologies individually. The electrocatalytic properties of the Pd/(NiO/MgO-C) catalyst for ethanol oxidation were investigated in an alkaline solution. The results indicated that the prepared Pd-NiO/MgO-C catalyst has excellent electrocatalytic activity and stability.

Oxide-assisted crack growth in hold-time low-cycle-fatigue of single-crystal superalloys

Directory of Open Access Journals (Sweden)

Suzuki Akane

2014-01-01

Full Text Available Compressive hold-time low-cycle fatigue is one of the important damage modes in Ni-based superalloy hot-gas path components. In strain controlled LCF, the compressive hold typically degrades fatigue life significantly due to creep relaxation and the resultant generation of tensile stress upon returning to zero strain. Crack initiation typically occurs on the surface, and therefore, the cracks are covered with layers of oxides. Recent finite element modeling based on experimental observations has indicated that the in-plane compressive stress in the alumina layer formed on the surface of the bond coat assists rumpling and, eventually, leads to initiation of cracks. The stress in the oxide layer continues to assist crack extension by pushing the alumina layer along the crack front during the compressive hold. In-situ measurements of the growth strains of alumina were performed using high energy synchrotron X-rays at Argonne National Lab. Specimens of single-crystal superalloys with and without aluminide coatings were statically pre-oxidized to form a layer of alumina at 1093 and 982 ∘C. For the in-situ synchrotron measurements, the specimens were heated up to the pre-oxidation temperatures with a heater. The alumina layers on both bare and coated specimens show compressive in-plane strains at both temperatures. The oxide strains on the superalloys showed dependency on temperature; on the other hand, the oxide strains in the aluminide coatings were insensitive to temperature. The magnitude of the compressive strains was larger on the superalloys than the ones on the aluminide coatings.

Synthesis and crystal structure analysis of titanium bismuthide oxide, Ti{sub 8}BiO{sub 7}

Energy Technology Data Exchange (ETDEWEB)

Amano, Shinsaku; Yamane, Hisanori, E-mail: yamane@tagen.tohoku.ac.jp

2016-08-05

Silver metallic luster columnar single crystals of a novel compound, Ti{sub 8}BiO{sub 7}, were synthesized using a bismuth flux. Ti{sub 8}BiO{sub 7} having a new structure type crystallizes in an orthorhombic cell, a = 7.8473(4) Å, b = 16.8295(10) Å, c = 3.0256(2) Å, space group: Cmmm. The Ti atoms enter the sites of isosceles-triangle 3-fold and rectangular 4-fold coordination of O atoms and the site of octahedral 6-fold coordination of O and Bi atoms. O atoms are in the rectangles, tetrahedra, and orthogonal pyramids of Ti atoms. The electrical resistivity measured for a Ti{sub 8}BiO{sub 7} single crystal in the c-axis direction was 6.2 × 10{sup −7} Ωm at 300 K and 1.3 × 10{sup −7} Ωm at 10 K. - Highlights: • A novel bismuthide oxide containing titanium, Ti{sub 8}BiO{sub 7}, was synthesized. • Single crystals of Ti{sub 8}BiO{sub 7} were grown by heating a mixture of Ti and Bi{sub 2}O{sub 3}. • Single crystal X-ray diffraction revealed that Ti{sub 8}BiO{sub 7} has a new structure type. • O atoms and Bi atoms are surrounded by Ti atoms in the structure. • Metallic conduction of Ti{sub 8}BiO{sub 7} was exhibited.

Photonic Crystals with Large Complete Bandgap Composed of an Approximately Ordered Array of Laurel-Crown-Like Structures Fabricated by Employing Anodic Aluminum Oxide Template

Science.gov (United States)

Chan, Der-Sheng; Chau, Yuan-Fong

2013-01-01

An innovative fabrication processes of a photonic crystal composed of an approximately ordered array of laurel-crown-like structures by employing an anodic aluminum oxide (AAO) template is presented. We found that the intensity of the electric field is affected by the microstructure and surface morphology of aluminum foil after etching the scalloped barrier oxide layer (BOL). In addition, the electric current is strongly dependent on the electric field distribution in the scalloped BOL at the pore bottoms. By using a different step potential (DSP) of 30-60 V in series, the proposed photonic crystal is fabricated and possesses a large complete photonic bandgap.

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.

(0 0 1) Facet-exposed anatase-phase TiO{sub 2} nanotube hybrid reduced graphene oxide composite: Synthesis, characterization and application in photocatalytic degradation

Energy Technology Data Exchange (ETDEWEB)

Zhou, Xun [School of Chemical Engineering of Hefei University of Technology, Hefei 230009 (China); Shi, Tiejun, E-mail: stjhfut@163.com [School of Chemical Engineering of Hefei University of Technology, Hefei 230009 (China); Wu, Jing [School of Chemical Engineering of Hefei University of Technology, Hefei 230009 (China); Zhou, Haiou [School of Chemical Engineering of Hefei University of Technology, Hefei 230009 (China); School of Materials and Chemical Engineering of Anhui University of Architecture, Hefei 230901 (China)

2013-12-15

Reduced graphene oxide (RGO) and TiO{sub 2} nanotube (TNT) with (0 0 1) facet-exposed anatase phase are covalently bonded together to synthesize TNT hybrid RGO (RGO-TNT) through consecutive process such as hydrothermal reaction, HCl washing, lyophilization and heat treatment with graphene oxide (GO), TiO{sub 2} powder and high concentration NaOH solution as the starting materials. The TNT with the diameter between 10 and 20 nm characterized by high resolution transmission electron microscopy (HRTEM) is in anatase phase proven by X-ray diffraction (XRD) and HRTEM. Additionally, the more active (0 0 1) facet is exposed identified by HRTEM. More significantly, TNT is bridged to RGO by C-Ti bond by the measurement of X-ray photoelectron spectroscopy (XPS). The photoluminescence (PL) spectra has testified that RGO in RGO-TNT can transfer and accept photoelectrons from TNT. The photocatalytic activity of RGO-TNT for degrading methylene blue (MB) is enhanced by contrast with pure TNT, and changeable by adjusting the mass ratios of GO to TiO{sub 2} powder. Simultaneously, lyophilization is benefit for maintaining the high active surface area of RGO-TNT, which is deeply in relationship with a higher photocatalytic activity. After four running cycles of photocatalytic degradation, RGO-TNT has shown a high stability and perfect reproducibility.

Single Crystal Growth of Pure Co3+ Oxidation State Material LaSrCoO4

Directory of Open Access Journals (Sweden)

Hanjie Guo

2016-08-01

Full Text Available We report on the single crystal growth of the single-layer perovskite cobaltate LaSrCoO4 that was grown by the optical floating zone method using high oxygen pressures. Phase purity and single crystallinity were confirmed by X-ray diffraction techniques. The pure Co3+ oxidation state was confirmed by X-ray absorbtion spectroscopy measurements. A transition to a spin glass state is observed at ∼7 K in magnetic susceptibility and specific heat measurements.

Nanoparticular metal oxide/anatase catalysts

DEFF Research Database (Denmark)

2010-01-01

The present invention concerns a method of preparation of nanoparticular metal oxide catalysts having a narrow particle size distribution. In particular, the invention concerns preparation of nanoparticular metal oxide catalyst precursors comprising combustible crystallization seeds upon which...... the catalyst metai oxide is co-precipitated with the carrier metal oxide, which crystallization seeds are removed by combustion in a final calcining step. The present invention also concerns processes wherein the nanoparticular metal oxide catalysts of the invention are used, such as SCR (deNOx) reactions...

Characterization of single crystal uranium-oxide thin films grown via reactive-gas magnetron sputtering on yttria-stabilized zirconia and sapphire

Energy Technology Data Exchange (ETDEWEB)

Strehle, Melissa M.; Heuser, Brent J., E-mail: bheuser@illinois.edu; Elbakhshwan, Mohamed S.; Han Xiaochun; Gennardo, David J.; Pappas, Harrison K.; Ju, Hyunsu

2012-06-30

The microstructure and valence states of three single crystal thin film systems, UO{sub 2} on (11{sup Macron }02) r-plane sapphire, UO{sub 2} on (001) yttria-stabilized zirconia, and U{sub 3}O{sub 8} on (11{sup Macron }02) r-plane sapphire, grown via reactive-gas magnetron sputtering are analyzed primarily with X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and ultraviolet photoelectron spectroscopy (UPS). XRD analysis indicates the growth of single crystal domains with varying degrees of mosaicity. XPS and UPS analyses yield U-4f, U-5f, O-1s, and O-2p electron binding energies consistent with reported bulk values. A change from p-type to n-type semiconductor behavior induced by preferential sputtering of oxygen during depth profile analysis was observed with both XPS and UPS. Trivalent cation impurities (Nd and Al) in UO{sub 2} lower the Fermi level, shifting the XPS spectral weight. This observation is consistent with hole-doping of a Mott-Hubbard insulator. The uranium oxide-(11{sup Macron }02) sapphire system is unstable with respect to Al interdiffusion across the film-substrate interface at elevated temperature. - Highlights: Black-Right-Pointing-Pointer Single crystal uranium-oxides grown on sapphire and yttria-stabilized zirconia. Black-Right-Pointing-Pointer Anion and cation valence states studied by photoelectron emission spectroscopy. Black-Right-Pointing-Pointer Trivalent Nd and Al impurities lower the Fermi level. Black-Right-Pointing-Pointer Uranium-oxide films on sapphire found to be unstable with respect to Al interdiffusion.

Crystallization kinetics of the Cu50Zr50 metallic glass under isothermal conditions

International Nuclear Information System (INIS)

Gao, Qian; Jian, Zengyun; Xu, Junfeng; Zhu, Man; Chang, Fange; Han, Amin

2016-01-01

Amorphous structure of the melt-spun Cu 50 Zr 50 amorphous alloy ribbons were confirmed by X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HR-TEM). Isothermal crystallization kinetics of these alloy ribbons were investigated using differential scanning calorimetry (DSC). Besides, Arrhenius and Johnson-Mehl-Avrami (JMA) equations were utilized to obtain the isothermal crystallization kinetic parameters. As shown in the results, the local activation energy E α decreases by a large margin at the crystallized volume fraction α<0.1, which proves that crystallization process is increasingly easy. In addition, the local activation energy E α is basically constant at 0.1<α<0.9. Therefore, it turns out that the unchanged barrier is overcome in the crystallization process. Finally, E α rapidly decreases at 0.9<α<1, implying that crystallization becomes easier and easier to proceed. Nucleation activation energy E nucleation is greater than growth activation energy E growth , so nucleation is harder than growth in isothermal process. In terms of the local Avrami exponent n(α), it ranges 1.1–7.4, revealing that isothermal crystallization mechanism is interface-controlled one- two- or three-dimensional growth with different nucleation rates. - Graphical abstract: The local Avrami exponent n(α), it ranges 1.1–7.4, revealing that isothermal crystallization mechanism is interface-controlled one- two- or three-dimensional growth with different nucleation rates. - Highlights: • Isothermal crystallization kinetics of Cu 50 Zr 50 metallic glass was investigated. • The relationship between the local activation energy E α and the crystallized volume fraction α were determined. • The nucleation activation energy E nucleation and grain growth activation energy E growth were obtained. • The local Avrami exponent n(α) was calculated in isothermal model.

On the solid phase crystallization of In{sub 2}O{sub 3}:H transparent conductive oxide films prepared by atomic layer deposition

Energy Technology Data Exchange (ETDEWEB)

Macco, Bart; Verheijen, Marcel A.; Black, Lachlan E.; Melskens, J. [Department of Applied Physics, Eindhoven University of Technology, P.O. Box 513, 5600 MB Eindhoven (Netherlands); Barcones, Beatriz [NanoLab@TU/e, Eindhoven University of Technology, P.O. Box 513, 5600 MB Eindhoven (Netherlands); Kessels, Wilhelmus M. M., E-mail: w.m.m.kessels@tue.nl [Department of Applied Physics, Eindhoven University of Technology, P.O. Box 513, 5600 MB Eindhoven (Netherlands); Solliance Solar Research, High Tech Campus 5, 5656 AE Eindhoven (Netherlands)

2016-08-28

Hydrogen-doped indium oxide (In{sub 2}O{sub 3}:H) has emerged as a highly transparent and conductive oxide, finding its application in a multitude of optoelectronic devices. Recently, we have reported on an atomic layer deposition (ALD) process to prepare high quality In{sub 2}O{sub 3}:H. This process consists of ALD of In{sub 2}O{sub 3}:H films at 100 °C, followed by a solid phase crystallization step at 150–200 °C. In this work, we report on a detailed electron microscopy study of this crystallization process which reveals new insights into the crucial aspects for achieving the large grain size and associated excellent properties of the material. The key finding is that the best optoelectronic properties are obtained by preparing the films at the lowest possible temperature prior to post-deposition annealing. Electron microscopy imaging shows that such films are mostly amorphous, but feature a very low density of embedded crystallites. Upon post-deposition annealing, crystallization proceeds merely from isotropic crystal grain growth of these embedded crystallites rather than by the formation of additional crystallites. The relatively high hydrogen content of 4.2 at. % in these films is thought to cause the absence of additional nucleation, thereby rendering the final grain size and optoelectronic properties solely dependent on the density of embedded crystallites. The temperature-dependent grain growth rate has been determined, from which an activation energy of (1.39 ± 0.04) eV has been extracted. Finally, on the basis of the observed crystallization mechanism, a simple model to fully describe the crystallization process has been developed. This model has been validated with a numerical implementation thereof, which accurately predicts the observed temperature-dependent crystallization behaviour.

Matrix metalloproteinase-20 mediates dental enamel biomineralization by preventing protein occlusion inside apatite crystals.

Science.gov (United States)

Prajapati, Saumya; Tao, Jinhui; Ruan, Qichao; De Yoreo, James J; Moradian-Oldak, Janet

2016-01-01

Reconstruction of enamel-like materials is a central topic of research in dentistry and material sciences. The importance of precise proteolytic mechanisms in amelogenesis to form a hard tissue with more than 95% mineral content has already been reported. A mutation in the Matrix Metalloproteinase-20 (MMP-20) gene results in hypomineralized enamel that is thin, disorganized and breaks from the underlying dentin. We hypothesized that the absence of MMP-20 during amelogenesis results in the occlusion of amelogenin in the enamel hydroxyapatite crystals. We used spectroscopy and electron microscopy techniques to qualitatively and quantitatively analyze occluded proteins within the isolated enamel crystals from MMP-20 null and Wild type (WT) mice. Our results showed that the isolated enamel crystals of MMP-20 null mice had more organic macromolecules occluded inside them than enamel crystals from the WT. The crystal lattice arrangements of MMP-20 null enamel crystals analyzed by High Resolution Transmission Electron Microscopy (HRTEM) were found to be significantly different from those of the WT. Raman studies indicated that the crystallinity of the MMP-20 null enamel crystals was lower than that of the WT. In conclusion, we present a novel functional mechanism of MMP-20, specifically prevention of unwanted organic material entrapped in the forming enamel crystals, which occurs as the result of precise amelogenin cleavage. MMP-20 action guides the growth morphology of the forming hydroxyapatite crystals and enhances their crystallinity. Elucidating such molecular mechanisms can be applied in the design of novel biomaterials for future clinical applications in dental restoration or repair. Copyright © 2015 Elsevier Ltd. All rights reserved.

HRTEM investigation of phase stability in alumina–zirconia ...

Indian Academy of Sciences (India)

tries, at high temperatures, the small diffusion lengths involved can influence the phase stability. The present work ... a function of nanocrystalline size has been shown by Shukla ... and zirconia on a Si(100) single crystal substrate with differ-.

Radium behaviour during ferric oxi-hydroxides crystallization

International Nuclear Information System (INIS)

Bassot, S.; Stammose, D.; Benitah, S.

2004-01-01

In uranium mill tailings, oxides and oxi-hydroxides are responsible of about 70% of the radium immobilization, half being associated to amorphous forms (mainly hydrous ferric oxides and hydrous manganese oxides). With time, crystallization of these amorphous forms can occur, inducing a redistribution of radium between solid and solution. If the amount of mobile radium increases, the impact of these tailings on the environment may become significant. The aim of this study is to determine the amount of radium released in solution during the crystallization process of hydrous ferric oxide (HFO). The transformation of Ra-HFO co-precipitate in crystallized forms (goethite, hematite, is studied by ageing at 40 deg C for different solution compositions. Both solids and solutions are sampled for different times and analysed. The solid evolution is followed by specific area measurements (about 250 m2/g for HFO and about 10-20 m 2 /g for crystallized form) and by determination of the amorphous fraction according to a selective extraction procedure. The solutions were analysed for 226 radium activity, iron concentration and pH. In order to discriminate the part of radium included in the solid and the part of radium fixed on the solid surface, radium sorption onto HFO and crystallized forms is studied as a function of pH. The modelling of the sorption curves with JCHESS 2.0 code allow to point out the mechanisms responsible of the 226-radium distribution between solid and solution during the crystallization process of HFO. (author)

Electro-optical switching of liquid crystals of graphene oxide

Science.gov (United States)

Song, Jang-Kun

Electric field effects on aqueous graphene-oxide (GO) dispersions are reviewed in this chapter. In isotropic and biphasic regimes of GO dispersions, in which the inter-particle friction is low, GO particles sensitively respond to the application of electric field, producing field-induced optical birefringence. The electro-optical sensitivity dramatically decreases as the phase transits to the nematic phase; the increasing inter-particle friction hinders the rotational switching of GO particles. The corresponding Kerr coefficient reaches the maximum near the isotropic to biphasic transition concentration, at which the Kerr coefficient is found be c.a. 1:8 · 10-5 mV-2, the highest value ever reported in all Kerr materials. The exceptionally large Kerr effect arises from the Maxwell- Wagner polarization of GO particles with an extremely large aspect ratio and a thick electrical double layer (EDL). The polarization sensitively depends on the ratio of surface and bulk conductivities in dispersions. As a result, low ion concentration in bulk solvent is highly required to achieve a quality electro-optical switching in GO dispersions. Spontaneous vinylogous carboxylic reaction in GO particles produces H+ ions, resulting in spontaneous degradation of electro-optical response with time, hence the removal of residual ions by using a centrifuge cleaning process significantly improves the electro-optical sensitivity. GO particle size is another important parameter for the Kerr coefficient and the response time. The best performance is observed in a GO dispersion with c.a. 0.5 μm mean size. Dielectrophoretic migration of GO particles can be also used to manipulate GO particles in solution. Using these unique features of GO dispersions, one can fabricate GO liquid crystal devices similar to conventional liquid crystal displays; the large Kerr effect allows fabricating a low power device working at extremely low electric fields.

High resolution transmission electron microscopy studies of {sigma} phase in Ni-based single crystal superalloys

Energy Technology Data Exchange (ETDEWEB)

Sun Fei [Key Laboratory of Liquid Structure and Heredity of Materials, Ministry of Education, Shandong University, Jinan 250061 (China); Zhang Jianxin, E-mail: jianxin@sdu.edu.cn [Key Laboratory of Liquid Structure and Heredity of Materials, Ministry of Education, Shandong University, Jinan 250061 (China); Liu Pan [Institute of Microstructure and Property of Advanced Materials, Beijing University of Technology, Beijing 100124 (China); Feng Qiang [National Center for Materials Service Safety, University of Science and Technology Beijing, Beijing 100083 (China); State Key Laboratory for Advanced Metals and Materials, University of Science and Technology Beijing, Beijing 100083 (China); Han Xiaodong; Mao Shengcheng [Institute of Microstructure and Property of Advanced Materials, Beijing University of Technology, Beijing 100124 (China)

2012-09-25

Graphical abstract: (a) TEM micrograph of {sigma} phase; (b) HRTEM image of {sigma}/{gamma} interface corresponding to the area of the white frame in (a); (c) an enlarged image of area from the white frame in (b). The combination of {sigma}/{gamma} interface appears very well, and a two-atomic-layer step is shown on the {sigma}/{gamma} interface. In addition, {sigma} phase has the orientation relationship of [0 0 1]{sub {gamma}}//[1 1 2{sup Macron }]{sub {sigma}}, (2{sup Macron} 2 0){sub {gamma}}//(1{sup Macron} 1 0){sub {sigma}}, (2{sup Macron }2{sup Macron} 0){sub {gamma}}//(1 1 1){sub {sigma}}; [0 1 1]{sub {gamma}}//[1 1 0]{sub {sigma}}, (1 1{sup Macron} 1){sub {gamma}}//(0 0 1{sup Macron }){sub {sigma}} with the {gamma} phase. Highlights: Black-Right-Pointing-Pointer Elemental characteristic of {sigma} phase is studied by HAADF techniques and EDS analysis. Black-Right-Pointing-Pointer Interfacial characteristics of {sigma}/{gamma} interface are revealed by HRTEM. Black-Right-Pointing-Pointer An atomic structural {sigma}/{gamma} interface with a two-atomic-layer step has been proposed. - Abstract: By means of high resolution transmission electron microscopy (HRTEM) and high-angle annular dark-field image technique (HAADF), morphological of plate-shaped {sigma} phase and interfacial characteristics between plate-shaped {sigma} phase and {gamma} phase in Ni-based single crystal superalloys have been studied. On the basis of HRTEM observations, an atomic structural interface between {sigma} phase and {gamma} phase with a step has been proposed. {sigma} Phase has the relationship of [0 0 1]{sub {gamma}}//[1 1 2{sup Macron }]{sub {sigma}}, (2{sup Macron} 2 0){sub {gamma}}//(1{sup Macron} 1 0){sub {sigma},} (2{sup Macron }2{sup Macron} 0){sub {gamma}}//(1 1 1){sub {sigma}}; [0 1 1]{sub {gamma}}//[1 1 0]{sub {sigma}}, (1 1{sup Macron} 1){sub {gamma}}//(0 0 1{sup Macron }){sub {sigma}} with the {gamma} phase. The compositional characteristics of the {sigma} phase which

Experimental investigation and thermodynamic simulation of the uranium oxide-zirconium oxide-iron oxide system in air

Czech Academy of Sciences Publication Activity Database

Petrov, Y. B.; Udalov, Y. P.; Šubrt, Jan; Bakardjieva, Snejana; Sázavský, P.; Kiselová, M.; Selucký, P.; Bezdička, Petr; Joumeau, C.; Piluso, P.

2011-01-01

Roč. 37, č. 2 (2011), s. 212-229 ISSN 1087-6596 Institutional research plan: CEZ:AV0Z40320502 Keywords : uranium oxide * zirconium oxide * iron oxide * fusibility curve * oxygen partial pressure * crystallization * phase composition Subject RIV: CA - Inorganic Chemistry Impact factor: 0.492, year: 2011

Registration of interstitial anions in irradiated MgO crystals

International Nuclear Information System (INIS)

Surzhikov, A.P.; Pogrebnyak, A.D.

1985-01-01

Possibility of application of positron annihilation for detection in oxides of rare earth metals with interstitial component of Frenkel anion defects is revealed. Magnesium oxide monocrystals with Ca, Si, Fe, Al impurity contents of 0.1 wt.% were investigated. These crystals were irradiated by X-rays (45 kV, 20 μA) and protons (10 MeV). It is shown that heating of magnesium oxide crystals irradiated by protons up to 700 K completely anneals F + -centers. In this case the component disappears inth the pulse distributon at xi=5.0; the subsequent crystal irradiation with X-ray does not lead to its reduction

Crystal growth, structural, optical, thermal, mechanical, laser damage threshold and electrical properties of triphenylphosphine oxide 4-nitrophenol (TP4N) single crystals for nonlinear optical applications

Science.gov (United States)

Karuppasamy, P.; Senthil Pandian, Muthu; Ramasamy, P.; Verma, Sunil

2018-05-01

The optically good quality single crystals of triphenylphosphine oxide 4-nitrophenol (TP4N) with maximum dimension of 15 × 10 × 5 mm3 were grown by slow evaporation solution technique (SEST) at room temperature. The cell dimensions of the grown TP4N crystal were confirmed by single crystal X-ray diffraction (SXRD) and the crystalline purity was confirmed and planes were indexed by powder X-ray diffraction (PXRD) analysis. Functional groups of TP4N crystal were confirmed by Fourier transform infrared (FTIR) spectral analysis. The optical transmittance of the grown crystal was determined by the UV-Vis NIR spectral analysis and it has good optical transparency in the entire visible region. The band tail (Urbach) energy of the grown crystal was analyzed and it appears to be minimum, which indicates that the TP4N has good crystallinity. The position of valence band (Ev) and conduction band (Ec) of the TP4N have been determined from the electron affinity energy (EA) and the ionization energy (EI) of its elements and using the optical band gap. The thermal behaviour of the grown crystal was investigated by thermogravimetric and differential thermal analysis (TG-DTA). Vickers microhardness analysis was carried out to identify the mechanical stability of the grown crystal and their indentation size effect (ISE) was explained by the Meyer's law (ML), Hays-Kendall's (HK) approach, proportional specimen resistance (PSR) model, modified PSR model (MPSR), elastic/plastic deformation (EPD) model and indentation induced cracking (IIC) model. Chemical etching study was carried out to find the etch pit density (EPD) of the grown crystal. Laser damage threshold (LDT) value was measured by using Nd:YAG laser (1064 nm). The dielectric permittivity (ε՛) and dielectric loss (tan δ) as a function of frequency was measured. The electronic polarizability (α) of the TP4N crystal was calculated. It is well matched to the value which was calculated from Clausius-Mossotti relation

HR-TEM and FT-Raman dataset of the caffeine interacted Phe-Phe peptide nanotube for possible sensing applications.

Science.gov (United States)

Narayanan, A Lakshmi; Dhamodaran, M; Solomon, J Samu; Karthikeyan, B; Govindhan, R

2018-02-01

Sensing ability of caffeine interaction with Phe-Phe annotates (PNTs), is presented (Govindhan et al., 2017; Karthikeyan et al., 2014; Tavagnacco et al., 2013; Kennedy et al., 2011; Wang et al., 2017) [1-5] in this data set. Investigation of synthesized caffeine carrying peptide nanotubes are carried out by FT-Raman spectral analysis and high resolution transmission electron microscopy (HR-TEM). Particle size of the caffeine loaded PNTs is < 40 nm. The FT-Raman spectrum signals are enhanced in the region of 400-1700 cm -1 . These data are ideal tool for the applications like biosensing and drug delivery research (DDS).

High mobility In2O3:H transparent conductive oxides prepared by atomic layer deposition and solid phase crystallization

NARCIS (Netherlands)

Macco, B.; Wu, Y.; Vanhemel, D.; Kessels, W.M.M.

2014-01-01

The preparation of high-quality In2O3:H, as transparent conductive oxide (TCO), is demonstrated at low temperatures. Amorphous In2O3:H films were deposited by atomic layer deposition at 100 °C, after which they underwent solid phase crystallization by a short anneal at 200 °C. TEM analysis has shown

Temperature induced complementary switching in titanium oxide resistive random access memory

Energy Technology Data Exchange (ETDEWEB)

Panda, D., E-mail: dpanda@nist.edu [Department of Electronics Engineering, National Institute of Science and Technology, Berhampur, Odisha 761008 (India); Department of Electronics Engineering and Institute of Electronics, National Chiao Tung University, Hsinchu 30010, Taiwan (China); Simanjuntak, F. M.; Tseng, T.-Y. [Department of Electronics Engineering and Institute of Electronics, National Chiao Tung University, Hsinchu 30010, Taiwan (China)

2016-07-15

On the way towards high memory density and computer performance, a considerable development in energy efficiency represents the foremost aspiration in future information technology. Complementary resistive switch consists of two antiserial resistive switching memory (RRAM) elements and allows for the construction of large passive crossbar arrays by solving the sneak path problem in combination with a drastic reduction of the power consumption. Here we present a titanium oxide based complementary RRAM (CRRAM) device with Pt top and TiN bottom electrode. A subsequent post metal annealing at 400°C induces CRRAM. Forming voltage of 4.3 V is required for this device to initiate switching process. The same device also exhibiting bipolar switching at lower compliance current, Ic <50 μA. The CRRAM device have high reliabilities. Formation of intermediate titanium oxi-nitride layer is confirmed from the cross-sectional HRTEM analysis. The origin of complementary switching mechanism have been discussed with AES, HRTEM analysis and schematic diagram. This paper provides valuable data along with analysis on the origin of CRRAM for the application in nanoscale devices.

Fabrication of Poly(styrene-co-maleic anhydride)@Ag Spheres with High Surface Charge Intensity and their Self-Assembly into Photonic Crystal Films.

Science.gov (United States)

Bi, Jiajie; Fan, Genrui; Wu, Suli; Su, Xin; Xia, Hongbo; Zhang, Shu-Fen

2017-10-01

Herein, we developed a method to prepare monodisperse poly(styrene-co-maleic anhydride)@Ag (PSMA@Ag) core-shell microspheres with high surface charge intensity by using an in situ reduction method. In this method, ethylenediamine tetraacetic acid tetrasodium salt (Na 4 EDTA) was used as a reducing agent to promote the growth of Ag, and at the same time endowed the PSMA@Ag spheres with a surface charge. The monodispersity of PSMA and PSMA@Ag and the ordered array of the photonic crystal films were characterized by using SEM. The formation of Ag nanoparticles was confirmed by using TEM, HR-TEM, and XRD characterizations. Due to the existence of surface charges, the obtained PSMA@Ag microspheres easily self-assembled to form photonic crystal structures. In addition, the surface-enhanced Raman scattering (SERS) activity of the PSMA@Ag photonic crystal films was evaluated by detecting the signal from Raman probe molecules, 4-aminothiophenol (4-ATP). The PSMA@Ag photonic crystal films exhibited a high SERS effect, a low detection limit of up to 10 -8 for 4-ATP, good uniformity, and reproducibility.

Structure and chemical composition of supported Pt-Sn electrocatalysts for ethanol oxidation

International Nuclear Information System (INIS)

Jiang Luhua; Sun Gongquan; Sun Shiguo; Liu Jianguo; Tang Shuihua; Li Huanqiao; Zhou Bing; Xin Qin

2005-01-01

Carbon supported PtSn alloy and PtSnO x particles with nominal Pt:Sn ratios of 3:1 were prepared by a modified polyol method. High resolution transmission electron microscopy (HRTEM) and X-ray microchemical analysis were used to characterize the composition, size, distribution, and morphology of PtSn particles. The particles are predominantly single nanocrystals with diameters in the order of 2.0-3.0 nm. According to the XRD results, the lattice constant of Pt in the PtSn alloy is dilated due to Sn atoms penetrating into the Pt crystalline lattice. While for PtSnO x nanoparticles, the lattice constant of Pt only changed a little. HRTEM micrograph of PtSnO x clearly shows that the change of the spacing of Pt (1 1 1) plane is neglectable, meanwhile, SnO 2 nanoparticles, characterized with the nominal 0.264 nm spacing of SnO 2 (1 0 1) plane, were found in the vicinity of Pt particles. In contrast, the HRTEM micrograph of PtSn alloy shows that the spacing of Pt (1 1 1) plane extends to 0.234 nm from the original 0.226 nm. High resolution energy dispersive X-ray spectroscopy (HR-EDS) analyses show that all investigated particles in the two PtSn catalysts represent uniform Pt/Sn compositions very close to the nominal one. Cyclic voltammograms (CV) in sulfuric acid show that the hydrogen ad/desorption was inhibited on the surface of PtSn alloy compared to that on the surface of the PtSnO x catalyst. PtSnO x catalyst showed higher catalytic activity for ethanol electro-oxidation than PtSn alloy from the results of chronoamperometry (CA) analysis and the performance of direct ethanol fuel cells (DEFCs). It is deduced that the unchanged lattice parameter of Pt in the PtSnO x catalyst is favorable to ethanol adsorption and meanwhile, tin oxide in the vicinity of Pt nanoparticles could offer oxygen species conveniently to remove the CO-like species of ethanolic residues to free Pt active sites

High activity of novel Pd/TiO2 nanotube catalysts for methanol electro-oxidation

International Nuclear Information System (INIS)

Wang Mei; Guo Daojun; Li Hulin

2005-01-01

Electro-oxidation of methanol in sulfuric acid solution was studied using palladium well-dispersed on titanium nanotubes, in relation to methanol oxidation processes in the direct oxidation methanol fuel cell. Pd dispersed on titania nanotubes, which leads to high surface area substrates, showed excellent catalytic activities compared to those of pure Pd and Pd-TiO 2 nanoparticles. TEM results show a narrow distribution of TiO 2 nanoparticles whose particle size is about 10nm, and uniform nano-sized TiO 2 nanotubes with 10nm in diameters are seen from HRTEM . A homogeneous structure in the composite nanomaterials is indicated by XRD analysis. The composite electrode activities were measured by cyclic voltammetry (CV) and at 25 deg. C it was found that 3wt% Pd in titania nanotubes had the best activity for methanol oxidation

Effect of nano-oxide particle size on radiation resistance of iron–chromium alloys

Energy Technology Data Exchange (ETDEWEB)

Xu, Weizong; Li, Lulu [Department of Materials Science and Engineering, North Carolina State University, Raleigh, NC 27695 (United States); Valdez, James A. [Materials Science and Technology Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Saber, Mostafa [Department of Mechanical and Materials Engineering, Portland State University, Portland, OR 97201 (United States); Zhu, Yuntian, E-mail: ytzhu@ncsu.edu [Department of Materials Science and Engineering, North Carolina State University, Raleigh, NC 27695 (United States); Koch, Carl C.; Scattergood, Ronald O. [Department of Materials Science and Engineering, North Carolina State University, Raleigh, NC 27695 (United States)

2016-02-15

Radiation resistance of Fe–14Cr alloys under 200 keV He irradiation at 500 °C was systematically investigated with varying sizes of nano oxide Zr, Hf and Cr particles. It is found that these nano oxide particles acted as effective sites for He bubble formation. By statistically analyzing 700–1500 He bubbles at the depth of about 150–700 nm from a series of HRTEM images for each sample, we established the variation of average He bubble size, He bubble density, and swelling percentage along the depth, and found them to be consistent with the He concentration profile calculated from the SIRM program. Oxide particles with sizes less than 3.5–4 nm are found most effective for enhancing radiation resistance in the studied alloy systems.

Economic analysis of crystal growth in space

Science.gov (United States)

Ulrich, D. R.; Chung, A. M.; Yan, C. S.; Mccreight, L. R.

1972-01-01

Many advanced electronic technologies and devices for the 1980's are based on sophisticated compound single crystals, i.e. ceramic oxides and compound semiconductors. Space processing of these electronic crystals with maximum perfection, purity, and size is suggested. No ecomonic or technical justification was found for the growth of silicon single crystals for solid state electronic devices in space.

Enhanced photocatalytic performance of CeO2-TiO2 nanocomposite for degradation of crystal violet dye and industrial waste effluent

Science.gov (United States)

Zahoor, Mehvish; Arshad, Amara; Khan, Yaqoob; Iqbal, Mazhar; Bajwa, Sadia Zafar; Soomro, Razium Ali; Ahmad, Ishaq; Butt, Faheem K.; Iqbal, M. Zubair; Wu, Aiguo; Khan, Waheed S.

2018-03-01

This study presents the synthesis of CeO2-TiO2 nanocomposite and its potential application for the visible light-driven photocatalytic degradation of model crystal violet dye as well as real industrial waste water. The ceria-titania (CeO2-TiO2) nanocomposite material was synthesised using facile hydrothermal route without the assistance of any template molecule. As-prepared composite was characterised by SEM, TEM, HRTEM, XRD, XPS for surface features, morphological and crystalline characters. The formed nanostructures were determined to possess crystal-like geometrical shape and average size less than 100 nm. The as-synthesised nanocomposite was further investigated for their heterogeneous photocatalytic potential against the oxidative degradation of CV dye taken as model pollutant. The photo-catalytic performance of the as-synthesised material was evaluated both under ultra-violet as well as visible light. Best photocatalytic performance was achieved under visible light with complete degradation (100%) exhibited within 60 min of irradiation time. The kinetics of the photocatalytic process were also considered and the reaction rate constant for CeO2-TiO2 nanocomposite was determined to be 0.0125 and 0.0662 min-1 for ultra-violet and visible region, respectively. In addition, the as-synthesised nanocomposite demonstrated promising results when considered for the photo-catalytic degradation of coloured industrial waste water collected from local textile industry situated in Faisalabad region of Pakistan. Enhanced photo-catalytic performance of CeO2-TiO2 nanocomposite was proposed owing to heterostructure formation leading to reduced electron-hole recombination.

Radiation-damage recovery in undoped and oxidized Li doped Mg O crystals implanted with lithium ions

Energy Technology Data Exchange (ETDEWEB)

Alves, E. E-mail: ealves@itn.pt; Silva, R.C. da; Pinto, J.V.; Monteiro, T.; Savoini, B.; Caceres, D.; Gonzalez, R.; Chen, Y

2003-05-01

Undoped MgO and oxidized Li-doped MgO single crystals were implanted with 1 x 10{sup 17} Li{sup +}/cm{sup 2} at 175 keV. The Rutherford backscattering spectrometry (RBS)/channeling data obtained after implantation shows that damage was produced throughout the entire range of the implanted ions. Optical absorption measurements indicate that after implantation the most intense band occurs at {approx}5.0 eV, which has been associated with anion vacancies. After annealing at 450 K the intensity of the oxygen-vacancy band decreases monotonically with temperature and completely disappears at 950 K. A broad extinction band centered at {approx}2.14 eV associated with lithium precipitates emerges gradually and anneals out at 1250 K. RBS/channeling shows that recovery of the implantation damage is completed after annealing the oxidized samples at 1250 K.

Fission products silver, palladium, and cadmium identification in neutron-irradiated SiC TRISO particles using a Cs-Corrected HRTEM

Energy Technology Data Exchange (ETDEWEB)

Rooyen, I.J. van, E-mail: isabella.vanrooyen@inl.gov [Fuel Design and Development Department, Idaho National Laboratory, P.O. Box 1625, Idaho Falls, ID, 83415-6188 (United States); Olivier, E.J.; Neethling, J.H. [Centre for High Resolution Electron Microscopy, Department of Physics, Nelson Mandela Metropolitan University, Port Elizabeth (South Africa)

2016-08-01

Electron microscopy investigations of selected coated particles from the first advanced gas reactor experiment at Idaho National Laboratory provided important information on fission product distribution and chemical composition in the silicon-carbide (SiC) layer. Silver precipitates were nano-sized, and therefore high-resolution transmission electron microscopy (HRTEM) was used to provide more information at the atomic level. Based on gamma-ray analysis, this particle which was irradiated to an average burnup of 19.38% fissions per initial metal atom, may have released as much as 10% of its available Ag-110 m inventory during irradiation. The HRTEM investigation focused on silver, palladium, and cadmium due to interest in silver transport mechanisms and possible correlation with palladium and silver previously found. Palladium, silver, and cadmium were found to co-exist in some of the SiC grain boundaries and triple junctions. This study confirmed palladium both at inter and intragranular sites. Phosphor was identified in SiC grain boundaries and triple points. - Highlights: • First high resolution electron microscopy fission product nano-structural locations of irradiated TRISO coated particles. • Pd observed inside SiC grains in proximity to planar defects e.g. stacking faults. • Ag co-exists with Pd and Cd only may suggest a Pd-assisted transport mechanism. • First finding of neutron transmutation product P, in SiC layer of TRISO coated particles. No direct link to Ag transport. • No significant Pd corrosion of SiC observed even at this high resolution images.

Crystal Structure of Mammalian Cysteine dioxygenase: A Novel Mononuclear Iron Center for Cysteine Thiol Oxidation

Energy Technology Data Exchange (ETDEWEB)

Simmons,C.; Liu, Q.; Huang, Q.; Hao, Q.; Begley, T.; Karplus, P.; Stipanuk, M.

2006-01-01

Cysteine dioxygenase is a mononuclear iron-dependent enzyme responsible for the oxidation of cysteine with molecular oxygen to form cysteinesulfinate. This reaction commits cysteine to either catabolism to sulfate and pyruvate or to the taurine biosynthetic pathway. Cysteine dioxygenase is a member of the cupin superfamily of proteins. The crystal structure of recombinant rat cysteine dioxygenase has been determined to 1.5 Angstroms resolution, and these results confirm the canonical cupin {beta}-sandwich fold and the rare cysteinyl-tyrosine intramolecular crosslink (between Cys93 and Tyr157) seen in the recently reported murine cysteine dioxygenase structure. In contrast to the catalytically inactive mononuclear Ni(II) metallocenter present in the murine structure, crystallization of a catalytically competent preparation of rat cysteine dioxygenase revealed a novel tetrahedrally coordinated mononuclear iron center involving three histidines (His86, His88, and His140) and a water molecule. Attempts to acquire a structure with bound ligand using either co-crystallization or soaks with cysteine revealed the formation of a mixed disulfide involving Cys164 near the active site, which may explain previously observed substrate inhibition. This work provides a framework for understanding the molecular mechanisms involved in thiol dioxygenation and sets the stage for exploring the chemistry of both the novel mononuclear iron center and the catalytic role of the cysteinyl-tyrosine linkage.

Improving the chemical compatibility of sealing glass for solid oxide fuel cells: Blocking the reactive species by controlled crystallization

Science.gov (United States)

Zhang, Teng; Zou, Qi; Zeng, Fanrong; Wang, Shaorong; Tang, Dian; Yang, Hiswen

2012-10-01

The chemical compatibility of sealing glass is of great importance for Solid oxide fuel cell (SOFC). In this work, the interfacial reaction between sealing glass and Cr-containing interconnect alloy is characterized by reacting Cr2O3 powders with a representative SrO-containing glass crystallized by different heat-treatment schedules. The crystalline structure and crystalline content of sealing glass are determined by X-ray diffraction. The results show that the fraction of Cr6+ decreases from 39.8 ± 1.9% for quenched glass to 8.2 ± 0.4% for glass crystallized at 900 °C for 2 h. In addition, the interfacial reaction can be further reduced with increasing crystallization temperature and time as well as the addition of nucleation agent (TiO2). The formation of some Sr-containing crystalline phases, Sr2SiO4 and Sr(TiO3), contributes to the improvement of chemical compatibility of sealing glass, in agreement with the results of thermodynamic calculations.

Oxidative stress by monosodium urate crystals promotes renal cell apoptosis through mitochondrial caspase-dependent pathway in human embryonic kidney 293 cells: mechanism for urate-induced nephropathy.

Science.gov (United States)

Choe, Jung-Yoon; Park, Ki-Yeun; Kim, Seong-Kyu

2015-01-01

The aim of this study is to clarify the effect of oxidative stress on monosodium urate (MSU)-mediated apoptosis of renal cells. Quantitative real-time polymerase chain reaction and immunoblotting for Bcl-2, caspase-9, caspase-3, iNOS, cyclooxygenase-2 (COX-2), interleukin-1β (IL-1β), IL-18, TNF receptor-associated factor-6 (TRAF-6), and mitogen-activated protein kinases were performed on human embryonic kidney 293 (HEK293) cells, which were stimulated by MSU crystals. Fluorescence-activated cell sorting was performed using annexin V for assessment of apoptosis. Reactive oxygen species (ROS) were measured. IL-1β siRNA was used for blocking IL-1β expression. MSU crystals promoted ROS, iNOS, and COX-2 expression and also increased TRAF-6 and IL-1β expression in HEK293 cells, which was inhibited by an antioxidant ascorbic acid. Caspase-dependent renal cell apoptosis was induced through attenuation of Bcl-2 and enhanced caspase-3 and caspase-9 expression by MSU crystals, which was significantly reversed by ascorbic acid and transfection of IL-1β siRNA to HEK293 cells. Ascorbic acid inhibited phosphorylation of extracellular signal-regulated kinase and Jun N-terminal protein kinase stimulated by MSU crystals. ROS accumulation and iNOS and COX-2 mRNA expression by MSU crystals was also suppressed by transfection with IL-1β siRNA. Oxidative stress generated by MSU crystals promotes renal apoptosis through the mitochondrial caspase-dependent apoptosis pathway.

Crystallization and melting behavior of poly(ethylene oxide) and its blend with styrene-based ionomer using time-resolved SAXS/WAXS experiments

Energy Technology Data Exchange (ETDEWEB)

Slusarczyk, CzesLaw, E-mail: cslusarczyk@ath.bielsko.pl [Institute of Textile Engineering and Polymer Materials, University of Bielsko-BiaLa, ul. Willowa 2, 43-309 Bielsko-BiaLa (Poland)

2011-10-15

Time-resolved synchrotron wide- and small-angle X-ray scattering experiments were used to investigate the crystallization behavior and microstructure development of neat poly(ethylene oxide) (PEO) and its 50/50 blend with ionomer containing 6.4 mol% of sodium acrylate. The apparent lateral crystal sizes D{sub (120)} and D{sub (112)/(004)} were derived from the WAXS profiles. It was found that D{sub (120)} and D{sub (112)/(004)} of PEO in the blend are almost independent of temperature and are smaller when compared to those of neat PEO sample. The evolution of morphological parameters extracted from time-resolved SAXS profiles such as the long period L, the lamellar crystal thickness l{sub C} and the amorphous layer thickness l{sub A}, shows that the crystallization process of neat PEO follows the nucleation theory. The lamellar crystal thickness l{sub C} shows a single linear dependence on inverse supercooling, over the whole temperature range investigated. In contrast, the crystallization process of PEO in the blend (i.e. in the presence of interactions with the ionomer) follows the nucleation theory only in the narrow supercooling range. It was found also that the morphology of the blend consists of a broad population of lamellar crystal thicknesses. During heating lamellae melt in the reversed sequence of their formation.

High-pressure synthesis and single-crystal structure elucidation of the indium oxide-borate In{sub 4}O{sub 2}B{sub 2}O{sub 7}

Energy Technology Data Exchange (ETDEWEB)

Ortner, Teresa S.; Vitzthum, Daniela; Heymann, Gunter; Huppertz, Hubert [Department of General, Inorganic and Theoretical Chemistry, Centre of Chemistry and Biomedicine (CCB), Leopold-Franzens-University Innsbruck (Austria)

2017-12-29

The indium oxide-borate In{sub 4}O{sub 2}B{sub 2}O{sub 7} was synthesized under high-pressure/high-temperature conditions at 12.5 GPa/1420 K using a Walker-type multianvil apparatus. Single-crystal X-ray structure elucidation showed edge-sharing OIn{sub 4} tetrahedra and B{sub 2}O{sub 7} units building up the oxide-borate. It crystallizes with Z = 8 in the monoclinic space group P2{sub 1}/n (no. 14) with a = 1016.54(3), b = 964.55(3), c = 1382.66(4) pm, and β = 109.7(1) . The compound was also characterized by powder X-ray diffraction and vibrational spectroscopy. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Redox process catalysed by growing crystal-strengite, FePO4,2H2O, crystallizing from solution with iron(II) and hydroxylamine

Science.gov (United States)

Lundager Madsen, Hans Erik

2014-09-01

In an attempt to grow pure crystals of the iron(II) phosphate vivianite, Fe3(PO4)2,8H2O, from a solution of Mohr's salt, Fe(NH4)2(SO4)2,6H2O, added to a solution of ammonium phosphate, hydroxylammonium chloride, NH3OHCl, was added to the iron(II) stock solution to eliminate oxidation of iron(II) by oxygen from the air. However, the effect turned out to be the opposite of the expected: whereas hydroxylamine reduces iron(III) in bulk solution, it acted as a strong oxidant in the presence of growing iron phosphate crystals, causing the crystallization of the iron(III) phosphate strengite, FePO4,2H2O, as the only solid phase. Evidently the crystal surface catalyses oxidation of iron(II) by hydroxylamine. The usual composite kinetics of spiral growth and surface nucleation was found. The surface-nucleation part yielded edge free energy λ in the range 12-45 pJ/m, virtually independent of temperature and in the range typical for phosphates of divalent metals. The scatter of values for λ presumably arises from contributions from different crystal forms to the overall growth rate. The low mean value points to strong adsorption of iron(II), which is subsequently oxidized at the crystal surface, forming strengite. The state of the system did not tend to thermodynamic equilibrium, but to a metastable state, presumably controlled by the iron(II) rich surface layer of the crystal. In addition to crystal growth, it was possible to measure nucleation kinetics by light scattering (turbidimetry). A point of transition from heterogeneous to homogeneous nucleation was found, and from the results for the homogeneous domain a rather precise value of crystal surface free energy γ=55 mJ/m2 was found. This is a relatively low value as well, indicating that the redox process plays a role already at the nucleation stage.

Tuning crystal phase of NiS_x through electro-oxidized nickel foam: A novel route for preparing efficient electrocatalysts for oxygen evolution reaction

International Nuclear Information System (INIS)

Li, Xiao; Shang, Xiao; Rao, Yi; Dong, Bin; Han, Guan-Qun; Hu, Wen-Hui; Liu, Yan-Ru; Yan, Kai-Li; Chi, Jing-Qi; Chai, Yong-Ming; Liu, Chen-Guang

2017-01-01

Highlights: • Electro-oxidized nickel foam as a support has been used to prepare NiS_x phases. • Ni(OH)_2 layer on electro-oxidized NF is responsible for the growth of β-NiS. • NiS_x/NF(Ox) composed of β-NiS and Ni_3S_2 has enhanced electrocatalytic activity. • The growth mechanisms of mixed NiS_x phases of NiS_x/NF(Ox) have been discussed. - Abstract: A facile solvothermal sulfurization using electro-oxidized nickel foam (NF(Ox)) as support has been applied to prepare NiS_x/NF(Ox) electrocatalyst with highly efficient activity for oxygen evolution reaction (OER). XRD patterns confirm the composition of NiS_x/NF(Ox): two kinds of crystal phase including β-NiS and Ni_3S_2. While using bare NF as support under identical conditions, only Ni_3S_2 phase can be detected. SEM images reveal two kinds of morphologies of NiS_x/NF(Ox) including pyramids structure of β-NiS and nanorod-like structure of Ni_3S_2, which implies the tuning effect of electro-pretreatment of NF on the selective preparation of NiS_x crystal phase. It can be speculated that Ni(OH)_2 layer derived from electro-oxidized NF is responsible for the growth of β-NiS while metallic Ni is transformed into Ni_2S_3 during sulfurization. Electrochemical measurements for OER indicate the enhanced electrocatalytic activity of NiS_x/NF(Ox) with a small overpotential of 72 mV to reach 10 mA cm"−"2 compared with Ni_3S_2/NF, which may be ascribed to the improved electron-transfer kinetics relating to the unique atomic configurations and crystalline structures of β-NiS. The electro-oxidation pretreatment of nickel foam provides a simple and convenient method by tuning different NiS_x crystal phases for preparing excellent OER eletrocatalysts.

Solvothermal crystallization of nanocrystals of metal oxides

International Nuclear Information System (INIS)

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

2008-01-01

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

Solvothermal crystallization of nanocrystals of metal oxides

Science.gov (United States)

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

2008-07-01

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

Radiation Damage in Scintillating Crystals

CERN Document Server

Zhu Ren Yuan

1998-01-01

Crystal Calorimetry in future high energy physics experiments faces a new challenge to maintain its precision in a hostile radiation environment. This paper discusses the effects of radiation damage in scintillating crystals, and concludes that the predominant radiation damage effect in crystal scintillators is the radiation induced absorption, or color center formation, not the loss of the scintillation light yield. The importance of maintaining crystal's light response uniformity and the feasibility to build a precision crystal calorimeter under radiation are elaborated. The mechanism of the radiation damage in scintillating crystals is also discussed. While the damage in alkali halides is found to be caused by the oxygen or hydroxyl contamination, it is the structure defects, such as oxygen vacancies, cause damage in oxides. Material analysis methods used to reach these conclusions are presented in details.

Heterogeneous Reaction of SO2 on Manganese Oxides: the Effect of Crystal Structure and Relative Humidity.

Science.gov (United States)

Yang, Weiwei; Zhang, Jianghao; Ma, Qingxin; Zhao, Yan; Liu, Yongchun; He, Hong

2017-07-03

Manganese oxides from anthropogenic sources can promote the formation of sulfate through catalytic oxidation of SO 2 . In this study, the kinetics of SO 2 reactions on MnO 2 with different morphologies (α, β, γ and δ) was investigated using flow tube reactor and in situ Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS). Under dry conditions, the reactivity towards SO 2 uptake was highest on δ-MnO 2 but lowest on β-MnO 2 , with a geometric uptake coefficient (γ obs ) of (2.42 ± 0.13) ×10 -2 and a corrected uptake coefficient (γ c ) of (1.48 ± 0.21) ×10 -6 for the former while γ obs of (3.35 ± 0.43) ×10 -3 and γ c of (7.46 ± 2.97) ×10 -7 for the latter. Under wet conditions, the presence of water altered the chemical form of sulfate and was in favor for the heterogeneous oxidation of SO 2 . The maximum sulfate formation rate was reached at 25% RH and 45% for δ-MnO 2 and γ-MnO 2 , respectively, possibly due to their different crystal structures. The results suggest that morphologies and RH are important factors influencing the heterogeneous reaction of SO 2 on mineral aerosols, and that aqueous oxidation process involving transition metals of Mn might be a potential important pathway for SO 2 oxidation in the atmosphere.

Crystal structure and luminescence properties of the first hydride oxide chloride with divalent europium. LiEu{sub 2}HOCl{sub 2}

Energy Technology Data Exchange (ETDEWEB)

Rudolph, Daniel; Schleid, Thomas [Institute for Inorganic Chemistry, University of Stuttgart (Germany); Enseling, David; Juestel, Thomas [Department of Chemical Engineering, Muenster University of Applied Sciences, Steinfurt (Germany)

2017-11-17

The mixed-anionic hydride oxide chloride LiEu{sub 2}HOCl{sub 2} with divalent europium was synthesized by the reduction of Eu{sub 2}O{sub 3} with LiH in a LiCl flux at 750 C for 4 d in silica-jacketed niobium capsules. According to structure determination by single-crystal X-ray diffraction the yellow compound crystallizes in the orthorhombic space group Cmcm (a = 1492.30(11) pm, b = 570.12(4) pm, c = 1143.71(8) pm, Z = 8) with a crystal structure closely related to that one of the quaternary hydride oxide LiLa{sub 2}HO{sub 3} and the hydride nitride LiSr{sub 2}H{sub 2}N. On the other hand it can also be derived from the PbFCl-type structure of EuHCl showing astonishingly short Eu{sup 2+}..Eu{sup 2+} contacts of 326 and 329 pm. Both crystallographically different Eu{sup 2+} cations have nine anionic neighbors, while all other ions (Li{sup +}, H{sup -}, O{sup 2-} and Cl{sup -}) reside in six-membered coordination spheres. LiEu{sub 2}OCl{sub 2}H exhibits a bright yellow luminescence with an emission maximum at 581 nm upon excitation at 440 nm. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Oxidation of {phi}'-aluminium oxynitride

Energy Technology Data Exchange (ETDEWEB)

Xolin, E. [Universite de Lyon, INSA-Lyon, MATEIS, UMR CNRS 5510, 20, av Albert Einstein, F-69621 Villeurbanne cedex (France); Jorand, Y., E-mail: Yves.Jorand@insa-lyon.f [Universite de Lyon, INSA-Lyon, MATEIS, UMR CNRS 5510, 20, av Albert Einstein, F-69621 Villeurbanne cedex (France); Olagnon, C.; Gremillard, L. [Universite de Lyon, INSA-Lyon, MATEIS, UMR CNRS 5510, 20, av Albert Einstein, F-69621 Villeurbanne cedex (France)

2011-03-15

Research highlights: Oxidation of {phi}'-AlON has been studied for the first time. First corrosion products are {gamma}-alumina. Low density {alpha}-alumina is formed at high temperature. Grains are extensively cracked after oxidation. The low density of the {alpha}-alumina is due to a network of nanometric porosities. - Abstract: The oxidation in air of single crystal {phi}'-aluminium oxynitride (AlON) grains has been characterized by thermogravimetry and X-ray diffraction in the 1273-1673 K range. Two oxidation stages have been observed, suggesting the formation of a transitional phase. Below 1473 K, oxidation results in the apparition of platelets and noodle-like crystals on the surface of the initially faceted single crystals. Above 1473 K, low density {alpha}-alumina polycrystals start forming on the grain surface and grow towards the grain core with increasing temperature or time. Their low density is mainly due to the presence of a network of nano-porosities.

Effect of polar surfaces on organic molecular crystals

Science.gov (United States)

Sharia, Onise; Tsyshevskiy, Roman; Kuklja, Maija; University of Maryland College Park Team

Polar oxide materials reveal intriguing opportunities in the field of electronics, superconductivity and nanotechnology. While behavior of polar surfaces has been widely studied on oxide materials and oxide-oxide interfaces, manifestations and properties of polar surfaces in molecular crystals are still poorly understood. Here we discover that the polar catastrophe phenomenon, known on oxides, also takes place in molecular materials as illustrated with an example of cyclotetramethylene tetranitramine (HMX) crystals. We show that the surface charge separation is a feasible compensation mechanism to counterbalance the macroscopic dipole moment and remove the electrostatic instability. We discuss the role of surface charge on degradation of polar surfaces, electrical conductivity, optical band-gap closure and surface metallization. Research is supported by the US ONR (Grants N00014-16-1-2069 and N00014-16-1-2346) and NSF. We used NERSC, XSEDE and MARCC computational resources.

Human nitric oxide biomarker as potential NO donor in conjunction with superparamagnetic iron oxide @ gold core shell nanoparticles for cancer therapeutics.

Science.gov (United States)

Singh, Nimisha; Patel, Khushbu; Sahoo, Suban K; Kumar, Rajender

2018-03-01

Nitric oxide releasing superparamagnetic (Fe 3 O 4 -Au@NTHP) nanoparticles were synthesized by conjugation of human biomarker of nitric oxide, N-nitrosothioproline with iron oxide-gold (Fe 3 O 4 -Au) core shell nanoparticles. The structure and morphology of the prepared nanoparticles were confirmed by ATR-FTIR, HR-TEM, EDAX, XPS, DLS and VSM measurements. N-nitrosothioproline is a natural molecule and nontoxic to humans. Thus, the core shell nanoparticles prepared were highly biocompatible. The prepared Fe 3 O 4 -Au@NTHP nanoparticles also provided an excellent release of nitric oxide in dark and upon light irradiation for cancer treatment. The amount of NO release was controllable with the wavelength of light and time of irradiation. The developed nanoparticles provided efficient cellular uptake and good cytotoxicity in picomolar range when tested on HeLa cancerous cells. These nanoparticles on account of their controllable NO release can also be used to release small amount of NO for killing cancerous cells without any toxic effect. Furthermore, the magnetic and photochemical properties of these nanoparticles provides dual platform for magneto therapy and phototherapy for cancer treatment. Copyright © 2017 Elsevier B.V. All rights reserved.

Tribological improvements of carbon-carbon composites by infiltration of atomic layer deposited lubricious nanostructured ceramic oxides

Science.gov (United States)

Mohseni, Hamidreza

A number of investigators have reported enhancement in oxidation and wear resistant of carbon-carbon composites (CCC) in the presence of protective coating layers. However, application of a surface and subsurface coating system that can preserve its oxidation and wear resistance along with maintaining lubricity at high temperature remains unsolved. To this end, thermodynamically stable protective oxides (ZnO/Al2O3/ZrO2) have been deposited by atomic layer deposition (ALD) to infiltrate porous CCC and graphite foams in order to improve the thermal stability and wear resistance in low and high speed sliding contacts. Characterization of microstructural evolution was achieved by using energy dispersive x-ray spectroscopy (EDS) mapping in scanning electron microscope (SEM) coupled with focused ion beam (FIB), x-ray tomography, high resolution transmission electron microscopy (HRTEM), scanning transmission electron microscopy (STEM) and X-ray diffraction (XRD). Evaluation of the tribological properties of CCC coated with abovementioned ALD thin films were performed by employing low speed pure sliding tribometer and a high speed/frequency reciprocating rig to simulate the fretting wear behavior at ambient temperature and elevated temperatures of 400°C. It was determined with x-ray tomography imaging and EDS mapping that ALD ZnO/Al2O3/ZrO2 nanolaminates and baseline ZrO2 coatings exhibited excellent conformality and pore-filling capabilities down to ˜100 microm and 1.5 mm in the porous CCC and graphite foam, respectively, which were dependent on the exposure time of the ALD precursors. XRD and HRTEM determined the crystalline phases of {0002} textured ZnO (wurtzite), amorphous Al2O3, and {101}-tetragonal ZrO2. Significant improvements up to ˜65% in the sliding and fretting wear factors were determined for the nanolaminates in comparison to the uncoated CCC. A tribochemical sliding-induced mechanically mixed layer (MML) was found to be responsible for these improvements

Spectroscopic and crystallographic studies of YAG:Pr4+ single crystals

International Nuclear Information System (INIS)

Pawlak, D.; Frukacz, Z.; Mierczyk, Z.; Suchocki, A.; Zachara, J.

1998-01-01

Y 3 Al 5 O 12 single crystals doped with praseodymium and magnesium ions have been prepared. The reversible color change of this crystal is observed when annealing in oxidizing or reducing atmospheres. The change is ascribed to the formation of Pr 4+ in the as-grown crystal, caused by the second dopant, Mg 2+ . The absorption spectra of YAG:Pr,Mg in the range 200-1100 nm, as grown and annealed in air and H 2 /N 2 atmosphere, are presented and discussed. Additional broad absorption bands are observed for the as-grown crystals and those annealed in oxidizing atmosphere. Crystallographic investigations of the original crystal and after annealing in a reducing atmosphere as described above, show no distinct structural differences. A redox mechanism is proposed to explain the color change during annealing. (orig.)

Surface texture of single-crystal silicon oxidized under a thin V{sub 2}O{sub 5} layer

Energy Technology Data Exchange (ETDEWEB)

Nikitin, S. E., E-mail: nikitin@mail.ioffe.ru; Verbitskiy, V. N.; Nashchekin, A. V.; Trapeznikova, I. N.; Bobyl, A. V.; Terukova, E. E. [Russian Academy of Sciences, Ioffe Physical–Technical Institute (Russian Federation)

2017-01-15

The process of surface texturing of single-crystal silicon oxidized under a V{sub 2}O{sub 5} layer is studied. Intense silicon oxidation at the Si–V{sub 2}O{sub 5} interface begins at a temperature of 903 K which is 200 K below than upon silicon thermal oxidation in an oxygen atmosphere. A silicon dioxide layer 30–50 nm thick with SiO{sub 2} inclusions in silicon depth up to 400 nm is formed at the V{sub 2}O{sub 5}–Si interface. The diffusion coefficient of atomic oxygen through the silicon-dioxide layer at 903 K is determined (D ≥ 2 × 10{sup –15} cm{sup 2} s{sup –1}). A model of low-temperature silicon oxidation, based on atomic oxygen diffusion from V{sub 2}O{sub 5} through the SiO{sub 2} layer to silicon, and SiO{sub x} precipitate formation in silicon is proposed. After removing the V{sub 2}O{sub 5} and silicon-dioxide layers, texture is formed on the silicon surface, which intensely scatters light in the wavelength range of 300–550 nm and is important in the texturing of the front and rear surfaces of solar cells.

A study on new types of metallic photonic crystals

International Nuclear Information System (INIS)

Ahmed, M.I.

2013-01-01

In this thesis, I tried to synthesize a one dimension dielectric photonic crystal. I have succeeded in depositing single layers of zinc oxide and magnesium oxide on glass substrates. Each single layer was characterized by a scanning electron microscope, X-ray diffraction, A Mirue interferometer, and a spectrophotometer. The refractive indices, extinction coefficients, and absorption coefficients of each single layer were calculated from the measured transmittance, reflectance, and thickness data. Using the calculated parameters (refractive indices) and measured parameters (thicknesses) the transmission spectrum of the one dimension photonic crystal composed of zinc oxide and magnesium oxide was modelled. Using the transfer matrix method, a comparative study of the one dimension-dielectric and metallic photonic crystals was done. Effect of the refractive index difference, filling factor, number of periods, Plasmon frequency, damping coefficient, and incidence angle on the transmittance of the dielectric and metallic photonic crystal was carried out. A multilayered structure composed of Silver and Gallium Nitride was designed to transmit in the visible region, block UV frequencies, and reflect the IR and microwave frequencies. Using a combination of MaxwellGarnett Approximation and the transfer matrix method; the properties of a nanocomposite photonic crystal consisting of Cryolite and spherical nanoparticles of silver distributed in a dielectric matrix of titanium dioxide was studied. Effect of the nanoparticle concentration, lattice constant and incidence angle on the polaritonic and structure photonic band gap were studied.

Synthesis of single-crystal PbS nanorods via a simple hydrothermal process using PEO-PPO-PEO triblock copolymer as a structure-directing agent

International Nuclear Information System (INIS)

Bu Junfu; Nie Chageng; Liang Jinxia; Sun Lan; Xie Zhaoxiong; Wu Qi; Lin Changjian

2011-01-01

Single-crystal PbS nanorods were successfully synthesized through a simple hydrothermal route using PEO-PPO-PEO triblock copolymer (P123) as a structure-directing agent. The XRD pattern indicates that the crystal structure of the nanorods is face-centre-cubic rocksalt. A SEM image shows that the nanorods have a diameter of 40-70 nm and a length of 200-600 nm, and both tips exhibit taper-like structures. HRTEM and SAED images reveal the single-crystalline nature of the nanorods with the growth along the (111) direction. The experimental results indicated that the P123 concentration and reaction temperature played important roles in controlling the morphology of the PbS nanostructures. The optical property of PbS nanorods was investigated by UV-Vis absorption spectroscopy and the band structure was calculated by the B3LYP hybrid density functional theory.

Design and characterization of Ga-doped indium tin oxide films for pixel electrode in liquid crystal display

International Nuclear Information System (INIS)

Choi, J.H.; Kang, S.H.; Oh, H.S.; Yu, T.H.; Sohn, I.S.

2013-01-01

Indium tin oxide (ITO) thin films doped with various metal atoms were investigated in terms of phase transition behavior and electro-optical properties for the purpose of upgrading ITO and indium zinc oxide (IZO) films, commonly used for pixel electrodes in flat panel displays. We explored Ce, Mg, Zn, and Ga atoms as dopants to ITO by the co-sputtering technique, and Ga-doped ITO films (In:Sn:Ga = 87.4:6.7:5.9 at.%) showed the phase transition behavior at 210 °C within 20 min with high visible transmittance of 91% and low resistivity of 0.22 mΩ cm. The film also showed etching rate similar to amorphous ITO, and no etching residue on glass surfaces. These results were confirmed with the film formed from a single Ga-doped ITO target with slightly different compositions (In:Sn:Ga = 87:9:4 at.%). Compared to the ITO target, Ga-doped ITO target left 1/4 less nodules on the target surface after sputtering. These results suggest that Ga-doped ITO films could be an excellent alternative to ITO and IZO for pixel electrodes in thin film transistor liquid crystal display (TFT-LCD). - Highlights: ► We report Ga-doped In–Sn–O films for a pixel electrode in liquid crystal display. ► Ga-doped In–Sn–O films show phase transition behavior at 210 °C. ► Ga-doped In–Sn–O films show high wet etchability and low resistivity

The core structure of a Frank dislocation in Ni3(Al,Nb)

International Nuclear Information System (INIS)

Bonnet, R.; Loubradou, M.; Derder, C.; Catana, A.

1991-01-01

This paper reports on the core structures of dislocations in L1 2 crystals, in view of understanding the anomalous yield behavior of strength with increasing temperature. Theoretical approaches have been proposed for explaining the dissociations of these dislocations, and experimental evidences have been reported for such dissociations using either the weak beam technique or more recently the HRTEM (High Resolution Transmission Electron Microscopy) technique. Recent HRTEM results show that for Ni 3 A1 the partial dislocations 1/2 left-angle 110 right-angle which limit an APB (Antiphase Boundary) lying on (001) are only split over 0.1 - 0.3 nm along (111) planes, producing very high energy CSF's (Complex Stacking Faults) which limit an SISF (superlattice Intrinsic Stacking Fault) extended on a (111) plane. Concerning the 1/2 left-angle 111 right-angle Frank dislocation, which limits an SESF (Superlattice Extrinsic Stacking Fault), there are no reported results yet. Let us note, however, that for aluminum HRTEM images of Frank dislocation loops have been studied. This lack of information in the L1 2 crystals motivated the present HRTEM study

Interfacial Interaction in Anodic Aluminum Oxide Templates Modifies Morphology, Surface Area, and Crystallization of Polyamide-6 Nanofibers.

Science.gov (United States)

Xue, Junhui; Xu, Yizhuang; Jin, Zhaoxia

2016-03-08

Here, we demonstrated that, when the precipitation process of polyamide-6 (PA6) solution happens in cylindrical channels of an anodized aluminum oxide membrane (AAO), interface interactions between a solid surface, solvent, non-solvent, and PA6 will influence the obtained polymer nanostructures, resulting in complex morphologies, increased surface area, and crystallization changes. With the enhancing interaction of PA6 and the AAO surface, the morphology of PA6 nanostructures changes from solid nanofibers, mesoporous, to bamboo-like, while at the same time, metastable γ-phase domains increase in these PA6 nanostructures. Brunauer-Emmett-Teller (BET) surface areas of solid, bamboo-like, and mesoporous PA6 nanofibers rise from 16, 20.9, to 25 m(2)/g. This study shows that interfacial interaction in AAO template fabrication can be used in manipulating the morphology and crystallization of one-dimensional polymer nanostructures. It also provides us a simple and novel method to create porous PA6 nanofibers with a large surface area.

Continuous bioscorodite crystallization in CSTRs for arsenic removal and disposal

NARCIS (Netherlands)

Gonzalez-Contreras, P.A.; Weijma, J.; Buisman, C.J.N.

2012-01-01

In CSTRs, ferrous iron was biologically oxidized followed by crystallization of scorodite (FeAsO4·2H2O) at pH 1.2 and 72 °C. The CSTRs were fed with 2.8 g L-1 arsenate and 2.4 g L-1 ferrous and operated at an HRT of 40 h, without seed addition or crystal recirculation. Both oxidation and

Zeolite Encapsulated Nanocrystalline CuO: A Redox Catalyst for the Oxidation of Secondary Alcohols

Directory of Open Access Journals (Sweden)

Sakthivel Vijaikumar

2008-01-01

Full Text Available Zeolite encapsulated nanocrystalline CuO is synthesized and characterized by powder XRD and HRTEM analyses which clearly show that the particles are less than 15 nm and the nanoparticles are highly dispersed. This nano CuO encapsulated CuY zeolite is used as catalyst in the oxidation of aromatic secondary alcohols. CuY zeolite acts as an efficient support for nano CuO, by stabilizing it and preventing its aggregation. Plausible mechanisms for the formation of the various products are also given.

Enhanced activity and stability of copper oxide/γ-alumina catalyst in catalytic wet-air oxidation: Critical roles of cerium incorporation

Science.gov (United States)

Zhang, Yongli; Zhou, Yanbo; Peng, Chao; Shi, Junjun; Wang, Qingyu; He, Lingfeng; Shi, Liang

2018-04-01

By successive impregnation method, the Ce-modified Cu-O/γ-Al2O3 catalyst was prepared and characterized using nitrogen adsorption-desorption, scanning electron microscopy energy dispersive X-ray analysis (SEM-EDS), high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman, and H2-Temperature programming reduction (H2-TPR). In catalytic wet-air oxidation (CWAO) process for the printing and dyeing wastewater (PDW), the effects of Ce addition on performance, mechanism and kinetics of the catalyst were investigated. The Ce addition increases the Brunauer-Emmett-Teller (BET) surface area and pore volume of the catalyst and makes the active components uniformly distributed on the catalyst surface. Formation of a stable CuAl2O4 solid solution by anchoring Cu onto the γ-Al2O3 crystal lattice leads to a significant decrease in metal leaching of the Ce-modified catalyst. The proportion of lattice oxygen in the catalyst substantially increases and the apparent activation energy of Cu-O/γ-Al2O3 catalyst decreases owing to Ce addition. Therefore, the catalytic activity and stability of the Ce-modified catalyst are considerably improved. The scavengers experiments identify the active species existed in the CWAO reaction system, with the order of reactivity: h+ > O2•- > H2O2 > HO•. This novel Cu-Ce-O/γ-Al2O3 catalyst has great potential in applications for treatment of concentrated organic wastewater due to its superior catalytic activity and improved stability.

Caracterización mediante HRTEM de un acero AISI4140 nitrurado por postdescarga micro-ondas

Directory of Open Access Journals (Sweden)

Béjar-Gómez, L.

2005-12-01

Full Text Available An analysis of the nitrides formed in an AISI 4140 steel nitrided by postdischarge microwave nitriding treatment was carried out by high resolution transmission electron microscopy (HRTEM, fast Fourier transform (FFT and nanoanalysis. The steel samples were nitrided below of the eutectoid transformation point (590 °C, after nitriding the samples were cooling slowly inside in the reactor whit an argon atmosphere. The analysis were carried out in a FEG-TEM PHILIPS TECNAI F20 at 200 Kv. The results showed the morphology and size of the nitrides ε-Fe_2-3N and γ’-Fe₄N, which had coherency whit the matrix. By other hand the following crystallographic relations were determined: (110 Fe-α ║ (1001 ε-Fe_2-3N ║ (110 γ’-Fe₄N and [1-1 0]Fe-α ║ [1 0-1 0] ε-Fe_2-3N ║ [0 1 1] Fe₄N.

Un análisis de las fases de nitruros formados en un acero AISI 4140, nitrurado mediante condiciones de postdescarga micro-ondas, se llevó a cabo por microscopía electrónica de transmisión de alta resolución (HRTEM, rápida transformada de Fourier (FFT y nanoanálisis. Las muestras de acero fueron nitruradas por debajo del punto de transformación eutectoide (590 °C; después del tratamiento de nitruración las piezas fueron enfriadas lentamente dentro del reactor con una atmósfera de argón. Los análisis se realizaron en un microscopio Philips con cañón de emisión de campo Tecnai F20 a 200 Kv (PHILIPS FEG-TEM TECNAI F20. Los resultados mostraron la morfología y tamaño de los nitruros de hierro ε-Fe_2-3N y γ’-Fe₄N, los cuáles mostraron coherencia con la matriz. Además, se obtuvo la siguiente relación de coherencia entre precipitados y matriz: (110 Fe-α ║ (1001 ε-Fe_2-3N ║ (110 γ’-Fe₄N y [1-1 0]Fe-α ║ [1 0-1 0] ε-Fe_2-3N ║ [0 1 1] Fe₄N.

In situ observation of the impact of surface oxidation on the crystallization mechanism of GeTe phase-change thin films by scanning transmission electron microscopy

Science.gov (United States)

Berthier, R.; Bernier, N.; Cooper, D.; Sabbione, C.; Hippert, F.; Noé, P.

2017-09-01

The crystallization mechanisms of prototypical GeTe phase-change material thin films have been investigated by in situ scanning transmission electron microscopy annealing experiments. A novel sample preparation method has been developed to improve sample quality and stability during in situ annealing, enabling quantitative analysis and live recording of phase change events. Results show that for an uncapped 100 nm thick GeTe layer, exposure to air after fabrication leads to composition changes which promote heterogeneous nucleation at the oxidized surface. We also demonstrate that protecting the GeTe layer with a 10 nm SiN capping layer prevents nucleation at the surface and allows volume nucleation at a temperature 50 °C higher than the onset of crystallization in the oxidized sample. Our results have important implications regarding the integration of these materials in confined memory cells.

Change of the work function and potential barrier transparency of W(100) and GaAs(110) single crystals during removing the inherent surface oxide layer

International Nuclear Information System (INIS)

Asalkhanov, Yu.I.; Saneev, Eh.L.

2002-01-01

Changes of current voltage characteristics of slow monoenergetic electron beam through the surfaces of W(100) and GaAs(100) single crystals have been measured in the process of surface oxide layers elimination. It is shown that work function is decreased and transparency coefficient of surface potential barrier is increased under increasing the temperature of vacuum annealing. Peculiarities of surface potential change under oxide layer elimination in metals and semiconductors are discussed [ru

Damage and recovery of skin barrier function after glycolic acid chemical peeling and crystal microdermabrasion.

Science.gov (United States)

Song, Ji Youn; Kang, Hyun A; Kim, Mi-Yeon; Park, Young Min; Kim, Hyung Ok

2004-03-01

Superficial chemical peeling and microdermabrasion have become increasingly popular methods for producing facial rejuvenation. However, there are few studies reporting the skin barrier function changes after these procedures. To evaluate objectively the degree of damage visually and the time needed for the skin barrier function to recover after glycolic acid peeling and aluminum oxide crystal microdermabrasion using noninvasive bioengineering methods. Superficial chemical peeling using 30%, 50%, and 70% glycolic acid and aluminum oxide crystal microdermabrasion were used on the volar forearm of 13 healthy women. The skin response was measured by a visual observation and using an evaporimeter, corneometer, and colorimeter before and after peeling at set time intervals. Both glycolic acid peeling and aluminum oxide crystal microdermabrasion induced significant damage to the skin barrier function immediately after the procedure, and the degree of damage was less severe after the aluminum oxide crystal microdermabrasion compared with glycolic acid peeling. The damaged skin barrier function had recovered within 24 hours after both procedures. The degree of erythema induction was less severe after the aluminum oxide crystal microdermabrasion compared with the glycolic acid peeling procedure. The degree of erythema induced after the glycolic acid peeling procedure was not proportional to the peeling solution concentration used. The erythema subsided within 1 day after the aluminum oxide crystal microdermabrasion procedure and within 4 days after the glycolic acid peeling procedure. These results suggest that the skin barrier function is damaged after the glycolic acid peeling and aluminum oxide crystal microdermabrasion procedure but recovers within 1 to 4 days. Therefore, repeating the superficial peeling procedure at 2-week intervals will allow sufficient time for the damaged skin to recover its barrier function.

Reduction reactions applied for synthesizing different nano-structured materials

Energy Technology Data Exchange (ETDEWEB)

Albuquerque Brocchi, Eduardo de; Correia de Siqueira, Rogério Navarro [Department of Materials Engineering, PUC-Rio, Rua Marquês de São Vicente, 225, Gávea, 22453-900 Rio de Janeiro, RJ (Brazil); Motta, Marcelo Senna [Basck Ltd. (United Kingdom); Moura, Francisco José, E-mail: moura@puc-rio.br [Department of Materials Engineering, PUC-Rio, Rua Marquês de São Vicente, 225, Gávea, 22453-900 Rio de Janeiro, RJ (Brazil); Solórzano-Naranjo, Ivan Guillermo [Department of Materials Engineering, PUC-Rio, Rua Marquês de São Vicente, 225, Gávea, 22453-900 Rio de Janeiro, RJ (Brazil)

2013-06-15

Different materials have been synthesized by alternative routes: nitrates thermal decomposition to prepare oxide or co-formed oxides and reduction by hydrogen or graphite to obtain mixed oxides, composites or alloys. These chemical-based synthesis routes are described and thermodynamics studies and kinetics data are presented to support its feasibility. In addition, selective reduction reactions have been applied to successfully produce metal/ceramic composites, and alloys. Structural characterization has been carried out by X-ray Diffraction and, more extensively, Transmission Electron Microscopy operating in conventional diffraction contrast (CTEM) and high-resolution mode (HRTEM), indicated the possibility of obtaining oxide and alloy crystals of sizes ranging between 20 and 40 nm. - Highlights: • The viability in obtaining Ni–Co, Cu–Al, Mn–Al co-formed nano oxides was evaluated. • Partial and complete H{sub 2} reduction were used to produce alloy, composite and Spinel. • XRD, TEM and HREM techniques were used to characterize the obtained nanostructures.

Oxidation behavior of a single-crystal Ni-base superalloy between 900 and 1000 {sup o}C in air

Energy Technology Data Exchange (ETDEWEB)

Liu, C.T., E-mail: liuchunting76@yahoo.com.c [College of Electromechanical Engineering, Qingdao University of Science and Technology, Qingdao 266061 (China); Ma, J. [College of Materials Science and Engineering, Qingdao University of Science and Technology, Qingdao 266061 (China); Sun, X.F. [State Key Laboratory for Corrosion and Protection, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016 (China)

2010-02-18

The oxidation behavior of a single-crystal Ni-base superalloy DD32 was studied in air at 900 and 1000 {sup o}C and analyzed by X-ray diffraction (XRD), scanning electron microscopy, combined with energy-dispersive X-ray spectroscopy (SEM/EDS). At 900 and 1000 {sup o}C, two oxidation steps appear in the oxidation kinetics. The first one is controlled by NiO growth and the second by Al{sub 2}O{sub 3} growth until a continuous Al{sub 2}O{sub 3} layer formed under the previously grown NiO layer after a critical time. The variations in the chemical composition due to segregations, which resulted from the solidification process, led to the formation of different kinds of oxide scale on the dendritic and interdendritic area during oxidation between 900 and 1000 {sup o}C. The scales formed between 900 and 1000 {sup o}C were complicated, and consisted of three layers: an outer columnar NiO layer with a small amount of CoO, an intermediate layer mainly composed of W{sub 20}O{sub 58}, CrTaO{sub 4}, a small amount of spinels NiCr{sub 2}O{sub 4}, NiAl{sub 2}O{sub 4} and CoAl{sub 2}O{sub 4}, an inner continuous layer of {alpha}-Al{sub 2}O{sub 3}.

Spent-fuel special-studies progress report: probable mechanisms for oxidation and dissolution of single-crystal UO2 surfaces

International Nuclear Information System (INIS)

Wang, R.

1981-03-01

Due to the complexity of the structural, microstructural and compositional characteristics of spent fuel, basic leaching and dissolution mechanisms were studied with UO 2 matrix material, specifically with single-crystal UO 2 , to isolate individual contributory factors. The effects of oxidation and oxidation-dissolution were investigated in different oxidation conditions, such as in air, oxygenated solutions and deionized water containing H 2 O 2 . In addition, the effects of temperature on dissolution of UO 2 were studied in autoclaves at 75 and 150 0 C. Also, oxidation and dissolution measurements were investigated via electrochemical methods to determine if those techniques could be applied to the characterization of leaching and dissolution of spent fuel in a hot cell. Finally, the effects of radiation were explored since the radiolysis of water may create a localized oxidizing condition at or near the spent fuel-solution interface, even in neutral or reducing conditions as commonly found in deep geological environments. The oxidation and oxidation-dissolution mechanisms for UO 2 are proposed as follows: The UO 2 surface is first oxidized in solution to form a UO/sub 2+x/ surface layer several angstroms thick. This oxidized surface has a high dissolution rate since the UO/sub 2+x/ reacts with the dissolved O 2 , or H 2 O 2 , to form uranyl complex ions in a U(VI) state. As the uranyl ions exceed the solubility limits in solution, they become hydrolyzed to form solid deposits and suspended particles of UO 3 hydrates. The thickness and porosity of the deposited UO 3 hydrate surface-film is dependent on temperature, pH and deposition time. A long-term dissolution rate is then determined by the nature of the surface film, such as porosity, solubility and mechanical properties

An improved method of preparation of nanoparticular metal oxide catalysts

DEFF Research Database (Denmark)

2014-01-01

The present invention concerns an improved method of preparation of nanoparticular vanadium oxide/anatase titania catalysts having a narrow particle size distribution. In particular, the invention concerns preparation of nanoparticular vanadium oxide/anatase titania catalyst precursors comprising...... combustible crystallization seeds upon which the catalyst metal oxide is coprecipitated with the carrier metal oxide, which crystallization seeds are removed by combustion in a final calcining step....

Oxidation of mullite-zirconia-alumina-silicon carbide composites

International Nuclear Information System (INIS)

Baudin, C.; Moya, J.S.

1990-01-01

This paper reports the isothermal oxidation of mullite-alumina-zirconia-silicon carbide composites obtained by reaction sintering studied in the temperature interval 800 degrees to 1400 degrees C. The kinetics of the oxidation process was related to the viscosity of the surface glassy layer as well as to the crystallization of the surface film. The oxidation kinetics was halted to T ≤ 1300 degrees C, presumably because of crystallization

Single crystal growth of yttrium calcium oxy borate (YCOB) crystals by flux technique and their characterization. CP-3.5

International Nuclear Information System (INIS)

Arun Kumar, R.; Senthilkumar, M.; Dhanasekaran, R.

2007-01-01

Yttrium calcium oxy borate single crystals were grown by the flux technique for the first time. Polycrystalline YCOB material was prepared by solid state reaction method. Single crystals of YCOB were grown using boron-tri-oxide flux. Several transparent single crystals of dimensions 10 x 5 x 5 mm 3 were obtained. The grown crystals were characterized by powder XRD and UV- VIS-NIR studies. The results of powder XRD confirm the crystalline structure of YCOB. The UV- VIS-NIR transmission spectrum reveals that the crystal is highly transparent (above 75%) from ultraviolet (220 nm) to near IR regions enabling it as a suitable candidate for high power UV applications

Morphology and Chemical Composition of soot particles emitted by Wood-burning Cook-Stoves: a HRTEM, XPS and Elastic backscattering Studies.

Science.gov (United States)

Carabali-Sandoval, G. A., Sr.; Castro, T.; Peralta, O.; De la Cruz, W.; Días, J.; Amelines, O.; Rivera-Hernández, M.; Varela, A.; Muñoz-Muñoz, F.; Policroniades, R.; Murillo, G.; Moreno, E.

2014-12-01

The morphology, microstructure and the chemical composition on surface of soot particles were studied by using high resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS) and elastic backscattering spectrometry. In order to obtain freshly soot particles emitted by home-made wood-burning cook stoves, copper grids for Transmission Electron Microscope (TEM) were placed on the last two of an 8-stages MOUDI cascade impactor. The analysis of HRTEM micrographs revealed the nanostructure and the particle size of soot particles. The XPS survey spectra show a large carbon peak around 285 eV and the oxygen signal at 533 eV. Some differences observed in the carbon/oxygen (C/O) ratio of the particles probably depend on the combustion process efficiency of each cook-stove analyzed. The C-1s XPS spectra show an asymmetric broad peak and other with low intensity that corresponds to sp2 and sp3hybridization, which were fitted with a convolution using Gaussian functions. Elastic backscattering technique allows a chemical elemental analysis of samples and confirms the presence of C, O and Si observed by XPS. Additionally, the morphological properties of soot aggregates were analyzed calculating the border-based fractal dimension (Df). Particles exhibit complex shapes with high values of Df. Also, real-time absorption (σabs) and scattering (σsct) coefficients of fine (with aerodynamic diameter < 2.5 µm) soot particles were measured. The trend in σabs and σsct indicate that the cooking process has two important combustion stages which varied in its flaming strength, being vigorous in the first stage and soft in the second one.

In situ observation of shear-driven amorphization in silicon crystals

Energy Technology Data Exchange (ETDEWEB)

He, Yang; Zhong, Li; Fan, Feifei; Wang, Chongmin; Zhu, Ting; Mao, Scott X.

2016-09-19

Amorphous materials have attracted great interest in the scientific and technological fields. An amorphous solid usually forms under the externally driven conditions of melt-quenching, irradiation and severe mechanical deformation. However, its dynamic formation process remains elusive. Here we report the in situ atomic-scale observation of dynamic amorphization processes during mechanical straining of nanoscale silicon crystals by high resolution transmission electron microscopy (HRTEM). We observe the shear-driven amorphization (SDA) occurring in a dominant shear band. The SDA involves a sequence of processes starting with the shear-induced diamond-cubic to diamond-hexagonal phase transition that is followed by dislocation nucleation and accumulation in the newly formed phase, leading to the formation of amorphous silicon. The SDA formation through diamond-hexagonal phase is rationalized by its structural conformity with the order in the paracrystalline amorphous silicon, which maybe widely applied to diamond-cubic materials. Besides, the activation of SDA is orientation-dependent through the competition between full dislocation nucleation and partial gliding.

Crystal growth under external electric fields

International Nuclear Information System (INIS)

Uda, Satoshi; Koizumi, Haruhiko; Nozawa, Jun; Fujiwara, Kozo

2014-01-01

This is a review article concerning the crystal growth under external electric fields that has been studied in our lab for the past 10 years. An external field is applied electrostatically either through an electrically insulating phase or a direct injection of an electric current to the solid-interface-liquid. The former changes the chemical potential of both solid and liquid and controls the phase relationship while the latter modifies the transport and partitioning of ionic solutes in the oxide melt during crystallization and changes the solute distribution in the crystal

Crystal growth under external electric fields

Energy Technology Data Exchange (ETDEWEB)

Uda, Satoshi; Koizumi, Haruhiko; Nozawa, Jun; Fujiwara, Kozo [Institute for Materials Research, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai, Miyagi 980-8577 (Japan)

2014-10-06

This is a review article concerning the crystal growth under external electric fields that has been studied in our lab for the past 10 years. An external field is applied electrostatically either through an electrically insulating phase or a direct injection of an electric current to the solid-interface-liquid. The former changes the chemical potential of both solid and liquid and controls the phase relationship while the latter modifies the transport and partitioning of ionic solutes in the oxide melt during crystallization and changes the solute distribution in the crystal.

Electrochemistry of hydrous oxide films

International Nuclear Information System (INIS)

Burke, L.D.; Lyons, M.E.G.

1986-01-01

The formation, acid-base properties, structural aspects, and transport processes of hydrous oxide films are discussed. Classical and nonclassical theoretical models of the oxide-solution interface are compared. Monolayer oxidation, behavior, and crystal growth of oxides on platinum, palladium, gold, iridium, rhodium, ruthenium, and some non-noble metals, including tungsten, are reviewed and compared

Final Report - Effects of High Spinel and Chromium Oxide Crystal Contents on Simulated HLW Vitrification in DM100 Melter Tests, VSL-09R1520-1, Rev. 0, dated 6/22/09

Energy Technology Data Exchange (ETDEWEB)

Kruger, Albert A.; Matlack, K. S.; Kot, W.; Pegg, I. L.; Chaudhuri, M.; Lutze, W.

2013-11-13

The principal objective of the work was to evaluate the effects of spinel and chromium oxide particles on WTP HLW melter operations and potential impacts on melter life. This was accomplished through a combination of crucible-scale tests, settling and rheological tests, and tests on the DM100 melter system. Crucible testing was designed to develop and identify HLW glass compositions with high waste loadings that exhibit formation of crystalline spinel and/or chromium oxide phases up to relatively high crystal contents (i.e., > 1 vol%). Characterization of crystal settling and the effects on melt rheology was performed on the HLW glass formulations. Appropriate candidate HLW glass formulations were selected, based on characterization results, to support subsequent melter tests. In the present work, crucible melts were formulated that exhibit up to about 4.4 vol% crystallization.

Low-temperature positron lifetime and Doppler-broadening measurements for single-crystal nickel oxide containing cation vacancies

International Nuclear Information System (INIS)

Waber, J.T.; Snead, C.L. Jr.; Lynn, K.G.

1985-01-01

Lifetime and Doppler-broadening measurements for positron annihilation in substoichiometric nickelous oxide have been made concomitantly from liquid-helium to room temperature. The concentration of cation vacancies is readily controlled by altering the ambient oxygen pressure while annealing the crystals at 1673 0 K. It was found that neither of the three lifetimes observed or their relative intensities varied significantly with the oxygen pressure, and the bulk rate only increased slightly when the specimen was cooled from room to liquid-helium temperatures. These results are interpreted as indicating that some of the positrons are trapped by the existing cation vacancies and a smaller fraction by vacancy clusters

Freeform Fabrication of Magnetophotonic Crystals with Diamond Lattices of Oxide and Metallic Glasses for Terahertz Wave Control by Micro Patterning Stereolithography and Low Temperature Sintering

Directory of Open Access Journals (Sweden)

Maasa Nakano

2013-04-01

Full Text Available Micrometer order magnetophotonic crystals with periodic arranged metallic glass and oxide glass composite materials were fabricated by stereolithographic method to reflect electromagnetic waves in terahertz frequency ranges through Bragg diffraction. In the fabrication process, the photo sensitive acrylic resin paste mixed with micrometer sized metallic glass of Fe72B14.4Si9.6Nb4 and oxide glass of B2O3·Bi2O3 particles was spread on a metal substrate, and cross sectional images of ultra violet ray were exposed. Through the layer by layer stacking, micro lattice structures with a diamond type periodic arrangement were successfully formed. The composite structures could be obtained through the dewaxing and sintering process with the lower temperature under the transition point of metallic glass. Transmission spectra of the terahertz waves through the magnetophotonic crystals were measured by using a terahertz time domain spectroscopy.

Atomic Layer-Deposited Molybdenum Oxide/Carbon Nanotube Hybrid Electrodes: The Influence of Crystal Structure on Lithium-Ion Capacitor Performance.

Science.gov (United States)

Fleischmann, Simon; Zeiger, Marco; Quade, Antje; Kruth, Angela; Presser, Volker

2018-05-25

Merging of supercapacitors and batteries promises the creation of electrochemical energy storage devices that combine high specific energy, power, and cycling stability. For that purpose, lithium-ion capacitors (LICs) that store energy by lithiation reactions at the negative electrode and double-layer formation at the positive electrode are currently investigated. In this study, we explore the suitability of molybdenum oxide as a negative electrode material in LICs for the first time. Molybdenum oxide-carbon nanotube hybrid materials were synthesized via atomic layer deposition, and different crystal structures and morphologies were obtained by post-deposition annealing. These model materials are first structurally characterized and electrochemically evaluated in half-cells. Benchmarking in LIC full-cells revealed the influences of crystal structure, half-cell capacity, and rate handling on the actual device level performance metrics. The energy efficiency, specific energy, and power are mainly influenced by the overpotential and kinetics of the lithiation reaction during charging. Optimized LIC cells show a maximum specific energy of about 70 W·h·kg -1 and a high specific power of 4 kW·kg -1 at 34 W·h·kg -1 . The longevity of the LIC cells is drastically increased without significantly reducing the energy by preventing a deep cell discharge, hindering the negative electrode from crossing its anodic potential limit.

Direct observations of the MOF (UiO-66) structure by transmission electron microscopy

KAUST Repository

Zhu, Liangkui

2013-01-01

As a demonstration of ab initio structure characterizations of nano metal organic framework (MOF) crystals by high resolution transmission electron microscopy (HRTEM) and electron diffraction tomography methods, a Zr-MOF (UiO-66) structure was determined and further confirmed by Rietveld refinements of powder X-ray diffraction. HRTEM gave direct imaging of the channels. © 2013 The Royal Society of Chemistry.

Tuning crystal phase of NiS{sub x} through electro-oxidized nickel foam: A novel route for preparing efficient electrocatalysts for oxygen evolution reaction

Energy Technology Data Exchange (ETDEWEB)

Li, Xiao; Shang, Xiao [State Key Laboratory of Heavy Oil Processing, China University of Petroleum (East China), Qingdao 266580 (China); Rao, Yi [State Key Laboratory of Heavy Oil Processing, China University of Petroleum (East China), Qingdao 266580 (China); College of Science, China University of Petroleum (East China), Qingdao 266580, PR China (China); Dong, Bin, E-mail: dongbin@upc.edu.cn [State Key Laboratory of Heavy Oil Processing, China University of Petroleum (East China), Qingdao 266580 (China); College of Science, China University of Petroleum (East China), Qingdao 266580, PR China (China); Han, Guan-Qun [State Key Laboratory of Heavy Oil Processing, China University of Petroleum (East China), Qingdao 266580 (China); College of Science, China University of Petroleum (East China), Qingdao 266580, PR China (China); Hu, Wen-Hui; Liu, Yan-Ru; Yan, Kai-Li; Chi, Jing-Qi; Chai, Yong-Ming [State Key Laboratory of Heavy Oil Processing, China University of Petroleum (East China), Qingdao 266580 (China); Liu, Chen-Guang, E-mail: cgliu@upc.edu.cn [State Key Laboratory of Heavy Oil Processing, China University of Petroleum (East China), Qingdao 266580 (China)

2017-02-28

Highlights: • Electro-oxidized nickel foam as a support has been used to prepare NiS{sub x} phases. • Ni(OH){sub 2} layer on electro-oxidized NF is responsible for the growth of β-NiS. • NiS{sub x}/NF(Ox) composed of β-NiS and Ni{sub 3}S{sub 2} has enhanced electrocatalytic activity. • The growth mechanisms of mixed NiS{sub x} phases of NiS{sub x}/NF(Ox) have been discussed. - Abstract: A facile solvothermal sulfurization using electro-oxidized nickel foam (NF(Ox)) as support has been applied to prepare NiS{sub x}/NF(Ox) electrocatalyst with highly efficient activity for oxygen evolution reaction (OER). XRD patterns confirm the composition of NiS{sub x}/NF(Ox): two kinds of crystal phase including β-NiS and Ni{sub 3}S{sub 2}. While using bare NF as support under identical conditions, only Ni{sub 3}S{sub 2} phase can be detected. SEM images reveal two kinds of morphologies of NiS{sub x}/NF(Ox) including pyramids structure of β-NiS and nanorod-like structure of Ni{sub 3}S{sub 2}, which implies the tuning effect of electro-pretreatment of NF on the selective preparation of NiS{sub x} crystal phase. It can be speculated that Ni(OH){sub 2} layer derived from electro-oxidized NF is responsible for the growth of β-NiS while metallic Ni is transformed into Ni{sub 2}S{sub 3} during sulfurization. Electrochemical measurements for OER indicate the enhanced electrocatalytic activity of NiS{sub x}/NF(Ox) with a small overpotential of 72 mV to reach 10 mA cm{sup −2} compared with Ni{sub 3}S{sub 2}/NF, which may be ascribed to the improved electron-transfer kinetics relating to the unique atomic configurations and crystalline structures of β-NiS. The electro-oxidation pretreatment of nickel foam provides a simple and convenient method by tuning different NiS{sub x} crystal phases for preparing excellent OER eletrocatalysts.

Growth of high-temperature superconductor crystals from flux

International Nuclear Information System (INIS)

Demianets, L.N.; Bykov, A.B.; Melnikov, O.K.; Stishov, S.M.

1991-01-01

Crystallization of high-temperature superconductors was studied in La-Sr-Cu-O, Y-Ba-Cu-O and Bi-Sr-Ca-Cu-O systems. Platelet crystals YBa 2 Cu 3 Osub(6.5+x) were obtained by spontaneous crystallization from homogeneous nonstoichiometric melts enriched in barium and copper oxides. Lasub(2-x)Sr x CuO 4 was prepared by slow cooling of melts enriched in copper oxide. Bi 2 (Sr, Ca)sub(n+1)Cu n O y , (n=1;2) was obtained by melting zone travelling. The crystals show transition to superconducting state at T=93K, ΔT 0.2-0.5 K (Y, Ba cuprate), T=87K, ΔT 2K (Bi, Sr, Ca-cuprate). La, Sr-cuprate single crystals obtained by Czochralski method did not show transition to superconducting state. For flux-grown crystals T c was 5-26 K depending on the composition, growth and heat treatment. The short characterization of some accessory phases (Ba 3 Y 2 Cu 3 PtO 10 , Casub(1.75)Srsub(1.5)Cusub(0.75)PtO 6 , BaCuO 2 , Ba 41 Cu 44 O 84 Cl 2 ) is reported. (author). 15 ref s., 8 figs

Improved photovoltaic performance from inorganic perovskite oxide thin films with mixed crystal phases

Science.gov (United States)

Chakrabartty, Joyprokash; Harnagea, Catalin; Celikin, Mert; Rosei, Federico; Nechache, Riad

2018-05-01

Inorganic ferroelectric perovskites are attracting attention for the realization of highly stable photovoltaic cells with large open-circuit voltages. However, the power conversion efficiencies of devices have been limited so far. Here, we report a power conversion efficiency of 4.20% under 1 sun illumination from Bi-Mn-O composite thin films with mixed BiMnO3 and BiMn2O5 crystal phases. We show that the photocurrent density and photovoltage mainly develop across grain boundaries and interfaces rather than within the grains. We also experimentally demonstrate that the open-circuit voltage and short-circuit photocurrent measured in the films are tunable by varying the electrical resistance of the device, which in turn is controlled by externally applying voltage pulses. The exploitation of multifunctional properties of composite oxides provides an alternative route towards achieving highly stable, high-efficiency photovoltaic solar energy conversion.

A framework for analysing relationships between chemical composition and crystal structure in metal oxides

International Nuclear Information System (INIS)

Thomas, N.W.

1991-01-01

A computer program has been written to characterize the coordination polyhedra of metal cations in terms of their volumes and polyhedral elements, i.e. corners, edges and faces. The sharing of these corners, edges and faces between polyhedra is also quantitatively monitored. In order to develop the methodology, attention is focused on ternary oxides containing the Al 3+ ion, whose structures were retrieved from the Inorganic Crystal Structure Database (ICSD). This also permits an objective assessment of the applicability of Pauling's rules. The influence of ionic valence on the structures of these compounds is examined, by calculating electrostatic bond strengths. Although Pauling's second rule is not supported in detail, the calculation of oxygen-ion valence reveals a basic structural requirement, that the average calculated oxygen-ion valence in any ionic oxide structure is equal to 2. The analysis is further developed to define a general method for the prediction of novel chemical compositions likely to adopt a given desired structure. The polyhedral volumes of this structure are calculated, and use is made of standard ionic radii for cations in sixfold coordination. The electroneutrality principle is invoked to take valence considerations into account. This method can be used to guide the development of new compositions of ceramic materials with certain desirable physical properties. (orig.)

Magnetostriction of Tb-Dy-Fe crystals

International Nuclear Information System (INIS)

Mei Wu; Okane, T.; Umeda, T.

1998-01-01

left angle 111 right angle -oriented twin free Tb-Dy-Fe single crystals, left angle 112 right angle - and left angle 110 right angle -oriented twinned ''single'' Tb-Dy-Fe crystals were prepared using floating zone melting crystal growth methods. Magnetostrictive performances of the crystals were investigated. Better low-field properties were observed in the left angle 110 right angle twinned crystals than in the left angle 112 right angle crystals. The highest properties were achieved in the left angle 111 right angle twin free single crystals. Even though there were still oxidized particles in the present left angle 111 right angle single crystals, a large magnetostrictive jump of 1700 ppm and a very low saturation magnetic field of 500 Oe were obtained. To understand magnetization and magnetostriction of different Tb-Dy-Fe crystals, theoretical modeling was carried out based on a simplified domain rotation model. Magnetization moment rotation paths of different domains were simulated and hence the resultant magnetostriction was obtained, which could adequately account for the experimental results of different crystals. The limitation of the domain rotation model was also discussed. (orig.)

Experimental evidence and structural modeling of nonstoichiometric (010) surfaces coexisting in hydroxyapatite nano-crystals.

Science.gov (United States)

Ospina, C A; Terra, J; Ramirez, A J; Farina, M; Ellis, D E; Rossi, A M

2012-01-01

High-resolution transmission electron microscopy (HRTEM) and ab initio quantum-mechanical calculations of electronic structure were combined to investigate the structure of the hydroxyapatite (HA) (010) surface, which plays an important role in HA interactions with biological media. HA was synthesized by in vitro precipitation at 37°C. HRTEM images revealed thin elongated rod nanoparticles with preferential growth along the [001] direction and terminations parallel to the (010) plane. The focal series reconstruction (FSR) technique was applied to develop an atomic-scale structural model of the high-resolution images. The HRTEM simulations identified the coexistence of two structurally distinct terminations for (010) surfaces: a rather flat Ca(II)-terminated surface and a zig-zag structure with open OH channels. Density functional theory (DFT) was applied in a periodic slab plane-wave pseudopotential approach to refine details of atomic coordination and bond lengths of Ca(I) and Ca(II) sites in hydrated HA (010) surfaces, starting from the HRTEM model. Copyright © 2011 Elsevier B.V. All rights reserved.

Green synthesis of Ni-Nb oxide catalysts for low-temperature oxidative dehydrogenation of ethane

KAUST Repository

Zhu, Haibo; Rosenfeld, Devon C.; Anjum, Dalaver H.; Caps, Valerie; Basset, Jean-Marie

2015-01-01

The straightforward solid-state grinding of a mixture of Ni nitrate and Nb oxalate crystals led to, after mild calcination (T<400°C), nanostructured Ni-Nb oxide composites. These new materials efficiently catalyzed the oxidative dehydrogenation (ODH

Crystal structure and defects of Zr4Co4Si7( V-phase) investigated by high resolution transmission electron microscope

International Nuclear Information System (INIS)

Mao, J.F.; Ye, H.Q.; Ning, X.G.; He, L.L.; Yang, D.Z.

1997-01-01

The results of high resolution transmission electron microscope (HRTEM) observation and image simulation show that Zr 4 Co 4 Si 7 possesses the same structure type of Zr 4 Co 4 Ge 7 . Adding of Fe or Ni into the Zr 4 Co 4 Si 7 compound, except that the dimensions changed slightly, does not change the lattice type and coordination in the crystal structure, maintaining the V-phase structure. Also, twins with coherent boundaries and with partially coherent at interfaces are observed. The image conditions of Zr 4 Co 4 Si 7 and the structure differences between Zr 4 Co 4 Si 7 and tetrahedral close-packed phases are also discussed. copyright 1997 Materials Research Society

Clad modified optical fiber gas sensors based on nanocrystalline nickel oxide embedded coatings

Science.gov (United States)

Yamini, K.; Renganathan, B.; Ganesan, A. R.; Prakash, T.

2017-07-01

A clad modified optical fiber gas sensor for sensing volatile organic compound vapours (VOCs) such as formaldehyde (HCHO), ammonia (NH3), ethanol (C2H5OH) and methanol (CH3OH) up to 500 ppm was studied using nanocrystalline nickel oxide embedded coatings. Prior to the measurements, nickel oxide in two different crystallite sizes such as 24 nm and 76 nm was synthesized by calcination of reverse precipitated nickel hydroxide subsequently at 450 °C and 900 °C for 30 min. Then, samples physical properties were characterized using X-ray diffraction (XRD), thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FESEM) and high resolution transmission electron microscopy (HRTEM). Our gas sensing measurement concludes that the lower crystallite size (24 nm) nickel oxide nanocrystals exhibits superior performance to formaldehyde and ethanol vapours as compared with other two VOCs, the observed experimental results were discussed in detail.

Deposition of thin layer (monoatomic layer) of barium on gold single crystal surfaces and studies of its oxidation employing X-ray photoelectron spectroscopy

International Nuclear Information System (INIS)

Ahmad, H.; Ahmad, R.; Khalid, M.; Alvi, R.A.

2007-01-01

Due to the high reactivity of barium with oxygen, some oxygen diffuse into the bulk to form bulk oxide and it is very difficult to differentiate the oxide over layer and the bulk oxide. To study the oxidation of barium surface layer, a thin layer (monolayer) of barium is developed over gold single crystal surface. Gold is selected as support because it is one of the least reactive metal in transition metal group and have very low probability of reaction with oxygen at room temperature (300K). Nitrous oxide (N/sub 2/O) was used as oxidant. Thin layer of barium was deposited on Au(100) surface. The barium coverage on gold surface was calculated that varied from 0.4 to 1.4 monolayer (ML). Photoelectron spectra for O(ls), N(ls), Ba (3d), and Au (4f) have been recorded on X-ray photoelectron spectrometer at different binding energy region specific for each element. The decomposition of nitrous oxide has been observed in all cases. It has found that nitrogen is evolved in the gaseous state and oxygen is adsorbed/chemisorbed on barium over layer. (author)

A nanogravimmetric investigation of the charging processes on ruthenium oxide thin films and their effect on methanol oxidation

International Nuclear Information System (INIS)

Santos, M.C.; Cogo, L.; Tanimoto, S.T.; Calegaro, M.L.; Bulhoes, L.O.S

2006-01-01

The charging processes and methanol oxidation that occur during the oxidation-reduction cycles in a ruthenium oxide thin film electrode (deposited by the sol-gel method on Pt covered quartz crystals) were investigated by using cyclic voltammetry, chronoamperometry and electrochemical quartz crystal nanobalance techniques. The ruthenium oxide rutile phase structure was determined by X-ray diffraction analysis. The results obtained during the charging of rutile ruthenium oxide films indicate that in the anodic sweep the transition from Ru(II) to Ru(VI) occurs followed by proton de-intercalation. In the cathodic sweep, electron injection occurs followed by proton intercalation, leading to Ru(II). The proton intercalation/de-intercalation processes can be inferred from the mass/charge relationship which gives a slope close to 1 g mol -1 (multiplied by the Faraday constant) corresponding to the molar mass of hydrogen. From the chronoamperometric measurements, charge and mass saturation of the RuO 2 thin films was observed (440 ng cm -2 ) during the charging processes, which is related to the total number of active sites in these films. Using the electrochemical quartz crystal nanobalance technique to study the methanol oxidation reaction at these films was possible to demonstrate that bulk oxidation occurs without the formation of strongly adsorbed intermediates such as CO ads , demonstrating that Pt electrodes modified by ruthenium oxide particles can be promising catalysts for the methanol oxidation as already shown in the literature

At last! The single-crystal X-ray structure of a naturally occurring sample of the ilmenite-type oxide FeCrO3.

Science.gov (United States)

Pérez-Cruz, María Ana; Elizalde-González, María de la Paz; Escudero, Roberto; Bernès, Sylvain; Silva-González, Rutilo; Reyes-Ortega, Yasmi

2015-10-01

A natural single crystal of the ferrimagnetic oxide FeCrO3, which was found in an opencast mine situated in the San Luis Potosí State in Mexico, has been characterized in order to elucidate some outstanding issues about the actual structure of this material. The single-crystal X-ray analysis unambiguously shows that transition metal cations are segregated in alternating layers normal to the threefold crystallographic axis, affording a structure isomorphous to that of ilmenite (FeTiO3), in the space group R3̅. The possible occurrence of cation antisite and vacancy defects is below the limit of detection available from X-ray data. Structural and magnetic results are in agreement with the coherent slow intergrowth of magnetic phases provided by the two antiferromagnetic corundum-type parent oxides Fe2O3 (hematite) and Cr2O3 (eskolaite). Our results are consistent with the most recent density functional theory (DFT) studies carried out on digital FeCrO3 [Sadat Nabi & Pentcheva (2011). Phys. Rev. B, 83, 214424], and suggest that synthetic samples of FeCrO3 might present a cation distribution different to that of the ilmenite structural type.

Growth of emerald single crystals

International Nuclear Information System (INIS)

Bukin, G.V.; Godovikov, A.A.; Klyakin, V.A.; Sobolev, V.S.

1986-01-01

In addition to its use for jewelry, emerald can also be used in low-noise microwave amplifiers. The authors discuss flux crystallization of emerald and note that when emerald is grown by this method, it is desirable to use solvents which dissolve emerald with minimum deviations from congruence but at the same time with sufficient high efficiency. Emerald synthesis and crystal growth from slowly cooled solutions is discussed as another possibility. The techniques are examined. Vapor synthesis and growht of beryl crystals re reviewed and the authors experimentally study the seeded CVD crystallization of beryl from BeO, Al 2 O 3 and SiO 2 oxides, by using complex compounds as carrier agents. The color of crystals of emerald and other varieties of beryl is detemined by slelective light absorption in teh visible part of the spectrum and depends on the density and structural positions of chromphore ions: chromium, iron, vanadium, nickel, manganese and cobalt

Novel Pt-Ru nanoparticles formed by vapour deposition as efficient electrocatalyst for methanol oxidation

International Nuclear Information System (INIS)

Sivakumar, Pasupathi; Ishak, Randa; Tricoli, Vincenzo

2005-01-01

Bimetallic Pt-Ru nanoparticles supported on carbon substrates have been prepared reproducibly by a simple method that utilizes commercially available metal-organic precursors at low temperature in vacuum. Particles morphology, composition and structure have been investigated using HRTEM, EDX, selected area electron diffraction (SAED) and powder XRD analysis. TEM shows that the obtained nanoparticles are homogeneously dispersed on the substrate surface and exhibit narrow size distribution, the average diameter being ca. 2 nm. Point resolved EDX analysis demonstrates co-presence of both Pt and Ru in each particle, thereby indicating that truly bimetallic nanoparticles have been obtained. Moreover, EDX performed on several areas of the sample evidences uniform particles composition. The latter can be controlled very easily and effectively by regulating the operation temperature during particles preparation. HRTEM imaging shows that the particles possess crystalline structure. Both SAED and XRD analyses indicate presence of nanoparticles exhibiting structure consistent with that of an f.c.c. Pt-Ru alloy. Besides the f.c.c. alloy, an additional crystalline phase might also be present as noticed by SAED. These nanoparticles display electrocatalytic activity with regard to methanol oxidation as evidenced by cyclic voltammetry (CV)

Incorporation and release of drug into/from superparamagnetic iron oxide nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Maver, Uros; Bele, Marjan [National Institute of Chemistry Slovenia, Hajdrihova 19, 1000 Ljubljana (Slovenia); Makovec, Darko; Campelj, Stanislav [Jozef Stefan Institute, Jamova 39, 1000 Ljubljana (Slovenia); Jamnik, Janko [National Institute of Chemistry Slovenia, Hajdrihova 19, 1000 Ljubljana (Slovenia); Gaberscek, Miran [National Institute of Chemistry Slovenia, Hajdrihova 19, 1000 Ljubljana (Slovenia)], E-mail: miran.gaberscek@ki.si

2009-10-15

The aim of this study was to attach a model drug (naproxen) onto superparamagnetic iron oxide nanoparticles (SPION). First, SPION were coated with thin layer of silica that contained micropores. We demonstrated that such surface functionalization could be optimized by the use of citric acid which prevented SPION agglomeration during the procedure. HRTEM investigation showed a uniform 1-2-nm-thick silica coating around SPION. This coating did not affect significantly the magnetic properties of the SPION. Into the coated SPION we successfully incorporated about 30 wt% of naproxen. The latter was readily released after immersion into a testing solution. The composites could be interesting for potential use in diagnostics.

Incorporation and release of drug into/from superparamagnetic iron oxide nanoparticles

International Nuclear Information System (INIS)

Maver, Uros; Bele, Marjan; Makovec, Darko; Campelj, Stanislav; Jamnik, Janko; Gaberscek, Miran

2009-01-01

The aim of this study was to attach a model drug (naproxen) onto superparamagnetic iron oxide nanoparticles (SPION). First, SPION were coated with thin layer of silica that contained micropores. We demonstrated that such surface functionalization could be optimized by the use of citric acid which prevented SPION agglomeration during the procedure. HRTEM investigation showed a uniform 1-2-nm-thick silica coating around SPION. This coating did not affect significantly the magnetic properties of the SPION. Into the coated SPION we successfully incorporated about 30 wt% of naproxen. The latter was readily released after immersion into a testing solution. The composites could be interesting for potential use in diagnostics.

21 CFR 186.1374 - Iron oxides.

Science.gov (United States)

2010-04-01

... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Iron oxides. 186.1374 Section 186.1374 Food and... Substances Affirmed as GRAS § 186.1374 Iron oxides. (a) Iron oxides (oxides of iron, CAS Reg. No. 1332-37-2) are undefined mixtures of iron (II) oxide (CAS Reg. No. 1345-25-1, black cubic crystals) and iron (III...

Fiber Strength of Hi Nicalon(TM) S After Oxidation and Scale Crystallization in Si(OH)4 Saturated Steam (Postprint)

Science.gov (United States)

2017-02-06

transmission electron microscopy. At 700°C and higher, if SiO2 glass scales got too thick they often dewetted the SiC fibers and would spheroidize... SiO2 glass wicked to the spheroids as fast as it formed on the dewetted SiC surface, causing faster oxidation. SiO2 crystallization to cristobalite... glass scales got too thick they often dewetted the SiC fibers and would spheroidize. SiO2 glass wicked to the spheroids as fast as it formed on the

Microstructures and mechanical properties of 9Cr oxide dispersion strengthened steel produced by spark plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Xie, Rui [Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), School of Materials Science and Engineering, Northeastern University, Shenyang 110819 (China); School of Metallurgy, Northeastern University, Shenyang 110819 (China); Lu, Zheng, E-mail: luz@atm.neu.edu.cn [Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), School of Materials Science and Engineering, Northeastern University, Shenyang 110819 (China); Lu, Chenyang; Li, Zhengyuan [Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), School of Materials Science and Engineering, Northeastern University, Shenyang 110819 (China); Ding, Xueyong [School of Metallurgy, Northeastern University, Shenyang 110819 (China); Liu, Chunming [Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), School of Materials Science and Engineering, Northeastern University, Shenyang 110819 (China)

2017-02-15

Highlights: • A 9Cr-ODS steel was produced by mechanical alloying and spark plasma sintering. • Bimodal grain size distribution was observed. • Formation mechanism of bimodal grain size distribution was discussed. • The size and number density of nanoscale particles were obtained by SAXS and HRTEM. • The contribution of nano-sized particles to yield strength is dominating. - Abstract: 9Cr oxide dispersion strengthened (ODS) steel was fabricated by mechanical alloying (MA) and spark plasma sintering (SPS). The nano-sized particles, grain size distribution and mechanical properties of 9Cr-ODS steel sintered at 950 °C were studied by synchrotron radiation small angle X-ray scattering (SAXS), high-resolution transmission electron microscopy (HRTEM), electron backscatter diffraction (EBSD) and tensile experiment. The results showed that bimodal grain size distribution in the matrix is observed, which is attributed to the heterogeneous recrystallization process during the SPS. High-density nano-sized Y{sub 2}Ti{sub 2}O{sub 7} and some large oxides of Cr{sub 2}Mn(Ti)O{sub 4} are formed in 9Cr-ODS steel. The number density and average size of Y{sub 2}Ti{sub 2}O{sub 7} obtained from SAXS are 4.72 × 10{sup 22}/m{sup 3} and 4.4 nm, respectively. The yield strengths of 9Cr-ODS steel fabricated by SPS are compared with the typical 9Cr-ODS steel produced by HIP.

Comprehensive characterization of ball-milled powders simulating a tribofilm system

Energy Technology Data Exchange (ETDEWEB)

Häusler, I., E-mail: ines.haeusler@bam.de; Dörfel, I., E-mail: Ilona.doerfel@bam.de; Peplinski, B., E-mail: Burkhard.peplinski@bam.de; Dietrich, P.M., E-mail: Paul.dietrich@yahoo.de; Unger, W.E.S., E-mail: Wolfgang.Unger@bam.de; Österle, W., E-mail: Werner.Oesterle@bam.de

2016-01-15

A model system was used to simulate the properties of tribofilms which form during automotive braking. The model system was prepared by ball milling of a blend of 70 vol.% iron oxides, 15 vol.% molybdenum disulfide and 15 vol.% graphite. The resulting mixture was characterized by X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and various transmission electron microscopic (TEM) methods, including energy dispersive X-ray spectroscopy (EDXS), high resolution investigations (HRTEM) with corresponding simulation of the HRTEM images, diffraction methods such as scanning nano-beam electron diffraction (SNBED) and selected area electron diffraction (SAED). It could be shown that the ball milling caused a reduction of the grain size of the initial components to the nanometer range. Sometimes even amorphization or partial break-down of the crystal structure was observed for MoS{sub 2} and graphite. Moreover, chemical reactions lead to a formation of surface coverings of the nanoparticles by amorphous material, molybdenum oxides, and iron sulfates as derived from XPS. - Highlights: • Ball milling of iron oxides, MoS{sub 2}, and graphite to simulate a tribofilm • Increasing coefficient of friction after ball milling of the model blend • Drastically change of the diffraction pattern of the powder mixture • TEM & XPS showed the components of the milled mixture and the process during milling. • MoS{sub 2} and graphite suffered a loss in translation symmetry or became amorphous.

Direct synthesis of Sb{sub 2}O{sub 3} nanoparticles via hydrolysis-precipitation method

Energy Technology Data Exchange (ETDEWEB)

Hu, Yuehua [Department of Inorganic Materials, School of Resources Processing and Bioengineering, Central South University, Changsha 410083 (China); Zhang, Huihui [Department of Inorganic Materials, School of Resources Processing and Bioengineering, Central South University, Changsha 410083 (China); Yang, Huaming [Department of Inorganic Materials, School of Resources Processing and Bioengineering, Central South University, Changsha 410083 (China)]. E-mail: hmyang@mail.csu.edu.cn

2007-01-31

Antimony oxide (Sb{sub 2}O{sub 3}) has wide applications as conductive materials, effective catalyst, functional filler and optical materials. Nanocrystalline Sb{sub 2}O{sub 3} has been successfully synthesized by hydrolysis-precipitation method. The samples were characterized by means of transmission electron microscopy (TEM), high-resolution TEM (HRTEM) images, X-ray diffraction (XRD) and differential thermal analysis (DTA). The average crystal size of the Sb{sub 2}O{sub 3} nanoparticles increases with increasing the reaction temperature. TEM image of the as-synthesized nanocrystalline Sb{sub 2}O{sub 3} shows rod-like structure. HRTEM images indicate a preferred directional growth of the Sb{sub 2}O{sub 3} nanoparticles. The electrochemical behaviors of Sb{sub 2}O{sub 3} electrodes have been primarily investigated by cyclic voltammetry (CV) in lithium hexafluorophosphate (LiPF{sub 6}) solution. Sb{sub 2}O{sub 3} nanocrystallite phase has prominent effect on the electrochemical properties. The results indicate that nanocrystalline Sb{sub 2}O{sub 3} synthesized by hydrolysis-precipitation method shows potential application in the field of the electrode materials.

Radiation defects in oxide crystals doped with rare earth ions

NARCIS (Netherlands)

Matkovskii, A; Durygin, A; Suchocki, A; Sugak, D; Wallrafen, F; Vakiv, M

1999-01-01

The nature of stable and transient color centers in Y3Al5O12, Gd3Ca5O12, YAlO3 and LiNbO3 crystals is studied. The color centers are created by various types of irradiation. The effect of irradiation on crystal optical properties in visible and ultraviolet range is presented.

Positron Spectroscopy of Hydrothermally Grown Actinide Oxides

Science.gov (United States)

2014-03-27

actinide oxides . The work described here is an attempt to characterize the quality of crystals using positron annihilation spectroscopy (PALS). The...Upadhyaya, R. V. Muraleedharan, B. D. Sharma and K. G. Prasad, " Positron lifetime studies on thorium oxide powders," Philosohical Magazine A, vol. 45... crystals . A strong foundation for actinide PALS studies was laid, but further work is required to build a more effective system. Positron Spectroscopy

Crystallization of a stringent response factor from Aquifex aeolicus

DEFF Research Database (Denmark)

Kristensen, Ole; Laurberg, Martin; Gajhede, Michael

2002-01-01

a = 50.8, b = 70.3, c = 90.9 A. Methionine residues were introduced by mutation and deliberate oxidation of the protein allowed us to produce additional crystal forms with reproducible diffraction ability and increased phasing potential. This is the first report on the crystallization of a member...

Crystal Structure of Tetragonal Form of La2NiO4+x

Science.gov (United States)

Kajitani, Tsuyoshi; Hosoya, Syoichi; Hirabayashi, Makoto; Fukuda, Tsuguo; Onozuka, Takashi

1989-10-01

The crystal structure of the title oxide was studied by means of the X-ray and neutron single crystal diffraction measurements. At room temperature, the tetragonal crystal structure is P42/ncm-type (No. 138), which is one of the subgroup of the space group I4/mmm. The lattice parameters of a sample annealed and slowly cooled in oxygen atmosphere from 673 K are a{=}b{=}5.4640(1) Å and c{=}12.6719(2) Å, while the oxygen content, x{=}0.10(4), was determined from obtained neutron data. The title oxide undergoes a tetragonal (P42/ncm)/tetragonal (I4/mmm) phase transition at about 560 K. The transition temperature is almost identical both in the annealed and as-grown crystals.

PHOTOCATALYTIC ACTIVITIES of Ag+ DOPED ZIF-8 and ZIF-L CRYSTALS

Directory of Open Access Journals (Sweden)

Berna Topuz

2016-09-01

Full Text Available Photocatalysis is expected to contribute to the solution of environmental problems such as water and air pollution in the near future. The design of photocatalysts with high electron-hole generation rates, high surface areas and high light absorption capacities is crucial in producing sustainable and cost-effective photocatalytic processes. Titania, zirconia, copper oxide, zinc oxide, iron oxide are widely used photocatalysts which have good light absorption capacities with moderate surface areas depending on the synthesis conditions. In the last decade metal organic frameworks (MOFs have been used in photocatalytic applications due to their very high surface areas up to 1000s of m2/g and adequate light absorption capacities. In this study zeolitic imidazolate framework (ZIF based MOF photocatalytsts were prepared and the effect of silver (Ag doping on the photocatalytic activity of ZIF-8 and ZIF-L crystals was investigated. Ag doped ZIF-8 and ZIF-L crystals were prepared and their activities in the photocatalytic removal of methylene blue (MB dye under UV irradiation were determined for the first time in the literature. Doped ZIF-8 and ZIF-L crystals showed better photocatalytic activities compared to the undoped crystals. 100% of MB was removed with 5 mole% Ag+ doped ZIF-8 in 40 min. The photocatalytic activity decreased beyond 5% doping level since Ag+ ions may have segregated due to a possible solid state solubility limit of Ag+ ions in the crystal lattice of ZIF-8. ZIF-L crystals possessed lower photocatalytic activities compared to ZIF-8 crystals.

Studies on Optical and Electrical Properties of Hafnium Oxide Nanoparticles

Science.gov (United States)

Jayaraman, Venkatachalam; Sagadevan, Suresh; Sudhakar, Rajesh

2017-07-01

In this paper, the synthesis and physico-chemical properties of hafnium oxide nanoparticles (HfO2 NPs) are analyzed and reported. The synthesis was carried out by the precipitation route by using hafnium tetrachloride (HfCl4) as precursor material with potassium hydroxide (KOH) dissolved in Millipore water. In the precipitation technique, the chemical reaction is comparatively simple, low-cost and non-toxic compared to other synthetic methods. The synthesized HfO2 NPs were characterized by using powder x-ray diffraction (PXRD), ultraviolet-visible (UV-Vis) spectroscopy, Raman analysis, and high-resolution transmission electron microscopy (HRTEM). The monoclinic structure of the HfO2 NPs was resolved utilizing x-ray diffraction (XRD). The optical properties were studied from the UV-Vis absorption spectrum. The optical band gap of the HfO2NPs was observed to be 5.1 eV. The Raman spectrum shows the presence of HfO2 NPs. The HRTEM image showed that the HfO2 NPs were of spherical shape with an average particle size of around 28 nm. The energy-dispersive x-ray spectroscopy (EDS) spectrum obviously demonstrated the presence of HfO2 NPs. Analysis and studies on the dielectric properties of the HfO2 NPs such as the dielectric constant, the dielectric loss, and alternating current (AC) conductivity were carried out at varying frequencies and temperatures.

Promotion of the oxidation of carbon monoxide at stepped platinum single-crystal electrodes in alkaline media by lithium and beryllium cations.

Science.gov (United States)

Stoffelsma, Chantal; Rodriguez, Paramaconi; Garcia, Gonzalo; Garcia-Araez, Nuria; Strmcnik, Dusan; Marković, Nenad M; Koper, Marc T M

2010-11-17

The role of alkali cations (Li(+), Na(+), K(+), Cs(+), and Be(2+)) on the blank voltammetric response and the oxidative stripping of carbon monoxide from stepped Pt single-crystal electrodes in alkaline media has been investigated by cyclic voltammetry. A strong influence of the nature of the cation on both the blank voltammetric profile and the CO oxidation is observed and related to the influence of the cation on the specific adsorption of OH on the platinum surface. Especially Li(+) and Be(2+) cations markedly affect the adsorption of OH and thereby have a significant promoting effect on CO(ads) oxidation. The voltammetric experiments suggest that, on Pt(111), the influence of Li(+) (and Be(2+)) is primarily through a weakening of the repulsive interactions between the OH in the OH adlayer, whereas in the presence of steps also, the onset of OH adsorption is at a lower potential, both on steps and on terraces.

Beginner’s guide to flux crystal growth

CERN Document Server

Tachibana, Makoto

2017-01-01

This book introduces the principles and techniques of crystal growth by the flux method, which is arguably the most useful way to obtain millimeter- to centimeter-sized single crystals for physical research. As it is possible to find an appropriate solvent (“flux”) for nearly all inorganic materials, the flux method can be applied to the growth of many crystals ranging from transition metal oxides to intermetallic compounds. Both important principles and experimental procedures are described in a clear and accessible manner. Practical advice on various aspects of the experiment, which is not readily available in the literature, will assist the beginning graduate students in setting up the lab and conducting successful crystal growth. The mechanisms of crystal growth at an elementary level are also provided to better understand the techniques and to help in assessing the quality of the crystals. The book also contains many photographs of beautiful crystals with important physical properties of current inte...

Quantitative atom column position analysis at the incommensurate interfaces of a (PbS)1.14NbS2 misfit layered compound with aberration-corrected HRTEM

International Nuclear Information System (INIS)

Garbrecht, M.; Spiecker, E.; Tillmann, K.; Jaeger, W.

2011-01-01

Aberration-corrected HRTEM is applied to explore the potential of NCSI contrast imaging to quantitatively analyse the complex atomic structure of misfit layered compounds and their incommensurate interfaces. Using the (PbS) 1.14 NbS 2 misfit layered compound as a model system it is shown that atom column position analyses at the incommensurate interfaces can be performed with precisions reaching a statistical accuracy of ±6 pm. The procedure adopted for these studies compares experimental images taken from compound regions free of defects and interface modulations with a structure model derived from XRD experiments and with multi-slice image simulations for the corresponding NCSI contrast conditions used. The high precision achievable in such experiments is confirmed by a detailed quantitative analysis of the atom column positions at the incommensurate interfaces, proving a tetragonal distortion of the monochalcogenide sublattice. -- Research Highlights: → Quantitative aberration-corrected HRTEM analysis of atomic column positions in (PbS) 1.14 NbS 2 misfit layered compound reveals tetragonal distortion of the PbS subsystem. → Detailed comparison of multi-slice simulations with the experimental NCSI contrast condition imaging results lead to a high precision (better than 10 pm) for determining the positions of atoms. → Precision in gaining information of local structure at atomic scale is demonstrated, which may not be accessible by means of X-ray and neutron diffraction analysis.

Consecutive dynamic resolutions of phosphine oxides

NARCIS (Netherlands)

Kortmann, Felix A.; Chang, Mu-Chieh; Otten, Edwin; Couzijn, Erik P. A.; Lutz, Martin; Minnaard, Adriaan J.

2013-01-01

A crystallization-induced asymmetric transformation (CIAT) involving a radical-mediated racemization provides access to enantiopure secondary phosphine oxides. A consecutive CIAT is used to prepare enantio-and diastereo-pure tert-butyl(hydroxyalkyl)phenylphosphine oxides.

Naturally occurring clay nanoparticles in Latosols of Brazil central region: detection and characterization

Science.gov (United States)

Dominika Dybowska, Agnieszka; Luciene Maltoni, Katia; Piella, Jordi; Najorka, Jens; Puntes, Victor; Valsami-Jones, Eugenia

2015-04-01

Stability and reactivity of minerals change as a particle size function, which makes mineral nanoparticles (defined here as sieved (53 µm) to remove the sand fraction. The clay fraction was collected by siphoning the supernatant, conditioned in 1000 ml cylinder, according to the Stock's law. This fraction was further processed by re-suspension in water, sonication and repeated centrifugation, to separate the fraction smaller than 100nm. This material, called here the soil "nanofraction", was analyzed using a range of techniques: 1) nanoparticle size/morphology and crystallinity with Transmission Electron Microscopy (TEM operateing in scanning (HAADF-STEM) and High Resolution (HRTEM) mode), 2) size distribution in water with Dynamic Light Scattering (DLS) and surface charge estimated from electrophoretic mobility measurements 3) crystal phase and crystallite size with X-ray Diffraction (XRD) 4) Chemical composition by quantitative analysis of elements (e.g., Si, Fe, Al, Ti) and their spatial distribution with HRTEM/EDS elemental mappings. The nanofraction had an average hydrodynamic particle diameter ranging from 83 to 92nm with a low polydispersity index of 0.13-0.17 and was found highly stable in aqueous suspension (no change in average particle size up to several months of storage). Particle surface charge (in water) ranged from -31mV to -34.5mV (pH = 5.7 - 6.2), this reflects the predominantly negative surface charge of kaolinites in soil environment effectively screening the positive charge of Fe oxides. Kaolinites appeared as single crystals (pseudo hexagonal platelets) while Fe oxides occurred mostly as micro-aggregates, with individual particles often not morphologically distinct with particle size <10nm. In addition, several anatase (TiO2) nanoparticles were also found. Both kaolinites and Fe oxides nanoparticles were crystalline, as evidenced from XRD measurements and HRTEM imaging. Distinction between different crystalline forms of Fe oxides (mainly

The photorefractive characteristics of bismuth-oxide doped lithium niobate crystals

International Nuclear Information System (INIS)

Zheng, Dahuai; Yao, Jiaying; Kong, Yongfa; Liu, Shiguo; Zhang, Ling; Chen, Shaolin; Xu, Jingjun

2015-01-01

Bismuth-doped lithium niobate (LN:Bi) crystals were grown by Czochralski method and their optical damage resistance, photorefraction, absorption spectra, and defect energy levels were investigated. The experimental results indicate that the photorefractive properties of LN:Bi were enhanced as compared with congruent one, the photorefractive response time was greatly shortened, the photorefractive sensitivity was increased, and the diffraction efficiency of near-stoichiometric LN:Bi (SLN:Bi) reached 31.72% and 49.08% at 532 nm and 488 nm laser, respectively (light intensity of 400 mW/cm 2 ). An absorption peak at about 350 nm was observed in the absorption spectrum of LN:Bi. And the defect energy levels simulation indicates new defect levels appear in the forbidden gap of LN:Bi crystals. Therefore bismuth can act as photorefractive centers in LN crystals

The photorefractive characteristics of bismuth-oxide doped lithium niobate crystals

Energy Technology Data Exchange (ETDEWEB)

Zheng, Dahuai; Yao, Jiaying [School of Physics, Nankai University, Tianjin 300071 (China); Collaborative Innovation Center of Chemical Science and Engineering (Tianjin), Tianjin 300072 (China); Kong, Yongfa, E-mail: kongyf@nankai.edu.cn [School of Physics, Nankai University, Tianjin 300071 (China); MOE Key Laboratory of Weak-Light Nonlinear Photonics and TEDA Applied Physics School, Nankai University, Tianjin 300457 (China); R and D Center, Taishan Sports Industry Group, Leling 253600 (China); Collaborative Innovation Center of Chemical Science and Engineering (Tianjin), Tianjin 300072 (China); Liu, Shiguo [School of Physics, Nankai University, Tianjin 300071 (China); Zhang, Ling; Chen, Shaolin [MOE Key Laboratory of Weak-Light Nonlinear Photonics and TEDA Applied Physics School, Nankai University, Tianjin 300457 (China); Xu, Jingjun [School of Physics, Nankai University, Tianjin 300071 (China); MOE Key Laboratory of Weak-Light Nonlinear Photonics and TEDA Applied Physics School, Nankai University, Tianjin 300457 (China); Collaborative Innovation Center of Chemical Science and Engineering (Tianjin), Tianjin 300072 (China)

2015-01-15

Bismuth-doped lithium niobate (LN:Bi) crystals were grown by Czochralski method and their optical damage resistance, photorefraction, absorption spectra, and defect energy levels were investigated. The experimental results indicate that the photorefractive properties of LN:Bi were enhanced as compared with congruent one, the photorefractive response time was greatly shortened, the photorefractive sensitivity was increased, and the diffraction efficiency of near-stoichiometric LN:Bi (SLN:Bi) reached 31.72% and 49.08% at 532 nm and 488 nm laser, respectively (light intensity of 400 mW/cm{sup 2}). An absorption peak at about 350 nm was observed in the absorption spectrum of LN:Bi. And the defect energy levels simulation indicates new defect levels appear in the forbidden gap of LN:Bi crystals. Therefore bismuth can act as photorefractive centers in LN crystals.

Development of Kinetics for Soot Oxidation at High Pressures Under Fuel-Lean Conditions

Energy Technology Data Exchange (ETDEWEB)

Lighty, JoAnn [Univ. of Utah, Salt Lake City, UT (United States); Vander Wal, Randy [Pennsylvania State Univ., University Park, PA (United States)

2014-04-21

The focus of the proposed research was to develop kinetic models for soot oxidation with the hope of developing a validated, predictive, multi-­scale, combustion model to optimize the design and operation of evolving fuels in advanced engines for transportation applications. The work focused on the relatively unstudied area of the fundamental mechanism for soot oxidation. The objectives include understanding of the kinetics of soot oxidation by O2 under high pressure which require: 1) development of intrinsic kinetics for the surface oxidation, which takes into account the dependence of reactivity upon nanostructure and 2) evolution of nanostructure and its impact upon oxidation rate and 3) inclusion of internal surface area development and possible fragmentation resulting from pore development and /or surface oxidation. These objectives were explored for a variety of pure fuel components and surrogate fuels. This project was a joint effort between the University of Utah (UU) and Pennsylvania State University (Penn State). The work at the UU focuses on experimental studies using a two-­stage burner and a high- pressure thermogravimetric analyzer (TGA). Penn State provided HRTEM images and guidance in the fringe analysis algorithms and parameter quantification for the images. This report focuses on completion done under supplemental funding.

Final Report: The Impact of Carbonate on Surface Protonation, Electron Transfer and Crystallization Reactions in Iron Oxide Nanoparticles and Colloids

Energy Technology Data Exchange (ETDEWEB)

Dixon, David Adams [The University of Alabama

2013-07-02

This project addresses key issues of importance in the geochemical behavior of iron oxides and in the geochemical cycling of carbon and iron. For Fe, we are specifically studying the influence of carbonate on electron transfer reactions, solid phase transformations, and the binding of carbonate to reactive sites on the edges of particles. The emphasis on carbonate arises because it is widely present in the natural environment, is known to bind strongly to oxide surfaces, is reactive on the time scales of interest, and has a speciation driven by acid-base reactions. The geochemical behavior of carbonate strongly influences global climate change and CO{sub 2} sequestration technologies. Our goal is to answer key questions with regards to specific site binding, electron transfer reactions, and crystallization reactions of iron oxides that impact both the geochemical cycling of iron and CO{sub 2} species. Our work is focused on the molecular level description of carbonate chemistry in solution including the prediction of isotope fractionation factors. We have also done work on critical atmospheric species.

Origin for the shape of Au small crystals formed inside sapphire by ion implantation

International Nuclear Information System (INIS)

Ohkubo, M.; Hioki, T.

1989-01-01

In ion-implanted oxides, precipitation is usually formed except the case of forming solid solution. The precipitation comprises the metallic particles of implanted atoms, the oxide of implanted atoms, the metal of matrix elements, the compound of implanted atoms and matrix and so on. In particular, the metallic particles of implanted atoms are frequently faceted. From the facets, the equilibrium shape of crystals can be imagined. The equilibrium shape is determined so that the surface free energy is to be minimized. However, the shape of the metallic particles precipitated inside oxides should not be such equilibrium shape because they come in contact with foreign crystals. As the result, in the precipitation phenomena induced by ion implantation, the crystal structures of precipitated particles and substrates, the crystallographic relation between two crystals, interfacial energy and so on must be taken in consideration. In this paper, the report is made on the shape of the metallic gold particles formed inside sapphires by ion implantation that it was caused by only the crystal habit of sapphires regardless of the above-mentioned complexity. (K.I.)

Growth of single-crystal W whiskers during humid H2/N2 reduction of Ni, Fe-Ni, and Co-Ni doped tungsten oxide

International Nuclear Information System (INIS)

Wang Shiliang; He Yuehui; Zou Jou; Wang Yong; Huang Han

2009-01-01

Numbers of W whiskers were obtained by reducing Ni, Ni-Fe, and Ni-Co doped tungsten oxide in a mixed atmosphere of humid H 2 and N 2 . The phases and morphologies of the reduction products were characterized by XRD and SEM. Intensive TEM and EDS analyses showed that the obtained whiskers were W single crystals which typical have alloyed particles (Ni-W, Fe-Ni, or Co-Ni-W) at the growth tips. The formed W whiskers were presumed to be induced by the alloyed particles. Our experimental results revealed that, during the reduction process of tungsten oxide, the pre-reduced Ni, Fe-Ni, or Co-Ni particles not only served as nucleation aids for the initial growth of W phase from W oxide but also played the roles of catalysts during the reductive decomposition of gaseous WO 2 (OH) 2 .

Single crystal growth of pure and Nd-doped Y2O3 by flotating zone method with Xe arc lamp imaging furnace

International Nuclear Information System (INIS)

Tsuiki, H.; Kitazawa, K.; Fueki, K.; Masumoto, T.; Shiroki, K.

1980-01-01

Single crystals of undoped and Nd-doped yttrium oxide were grown by the floating zone method with a Xe arc lamp imaging furnace. The crystals were grown in the and directions. Transparent and subgrain-free single crystals were obtained at a growth rate of 30-60 mm/h for the undoped yttrium oxide. Facets of the cubic [100] and [211] were observed though the high temperature phase of the crystal is hexagonal. Dislocation densities of undoped yttrium oxide are given. (orig./WE)

Crystal-contact engineering to obtain a crystal form of the Kelch domain of human Keap1 suitable for ligand-soaking experiments

International Nuclear Information System (INIS)

Hörer, Stefan; Reinert, Dirk; Ostmann, Katja; Hoevels, Yvette; Nar, Herbert

2013-01-01

A mutant of the Kelch domain of the human Keap1 protein has been designed in order to enable the soaking of small-molecule ligands. The apo structure of this mutant is reported at 1.98 Å resolution and the suitability of the crystal system has been demonstrated by the structure of the mutated Keap1 Kelch domain in complex with a cyclic peptide derived from Nrf2. Keap1 is a substrate adaptor protein for a Cul3-dependent ubiquitin ligase complex and plays an important role in the cellular response to oxidative stress. It binds Nrf2 with its Kelch domain and thus triggers the ubiquitinylation and degradation of Nrf2. Oxidative stress prevents the degradation of Nrf2 and leads to the activation of cytoprotective genes. Therefore, Keap1 is an attractive drug target in inflammatory diseases. The support of a medicinal chemistry effort by structural research requires a robust crystallization system in which the crystals are preferably suited for performing soaking experiments. This facilitates the generation of protein–ligand complexes in a routine and high-throughput manner. The structure of human Keap1 has been described previously. In this crystal form, however, the binding site for Nrf2 was blocked by a crystal contact. This interaction was analysed and mutations were introduced to disrupt this crystal contact. One double mutation (E540A/E542A) crystallized in a new crystal form in which the binding site for Nrf2 was not blocked and was accessible to small-molecule ligands. The crystal structures of the apo form of the mutated Keap1 Kelch domain (1.98 Å resolution) and of the complex with an Nrf2-derived peptide obtained by soaking (2.20 Å resolution) are reported

Synthesis of graphene oxide and reduced graphene oxide by needle platy natural vein graphite

Energy Technology Data Exchange (ETDEWEB)

Rathnayake, R.M.N.M. [National Institute of Fundamental Studies, Kandy (Sri Lanka); Graduate School of Engineering, Toyota Technological Institute, 2-12-1 Hisakata, Tempaku, Nagoya 468-8511 (Japan); Wijayasinghe, H.W.M.A.C., E-mail: athulawijaya@gmail.com [National Institute of Fundamental Studies, Kandy (Sri Lanka); Pitawala, H.M.T.G.A. [Department of Geology, University of Peradeniya, Peradeniya (Sri Lanka); Yoshimura, Masamichi; Huang, Hsin-Hui [Graduate School of Engineering, Toyota Technological Institute, 2-12-1 Hisakata, Tempaku, Nagoya 468-8511 (Japan)

2017-01-30

Highlights: • The high purity of this form of needle platy natural vein graphite is expected to synthesize GO and rGO readily and efficiently, as compared to the synthetic and less pure graphite raw materials. • Production of large-scale GO and rGO for industrial applications can be achieved by using this highly crystalline NPG vein graphite, and it adds value to the natural resources. • High quality, few-layer, and cost effective GO and rGO can achieve great results using this low cost, natural graphite. - Abstract: Among natural graphite varieties, needle platy vein graphite (NPG) has very high purity. Therefore, it is readily used to prepare graphene oxide (GO) and reduced graphene oxide (rGO). In this study, GO and rGO were prepared using chemical oxidation and reduction process, respectively. The synthesized materials were characterized by X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), and Fourier transform infrared (FTIR) spectroscopy. XRD studies confirmed the increase of the interlayer spacing of GO and rGO in between 3.35 to 8.66 A°. AFM studies showed the layer height of rGO to be 1.05 nm after the reduction process. TEM micrographs clearly illustrated that the prepared GO has more than 25 layers, while the rGO has only less than 15 layers. Furthermore, the effect of chemical oxidation and reduction processes on surface morphology of graphite were clearly observed in FESEM micrographs. The calculated R{sub O/C} of GO and rGO using XPS analysis are 5.37% and 1.77%, respectively. The present study revealed the successful and cost effective nature of the chemical oxidation, and the reduction processes for the production of GO and rGO out of natural vein graphite.

Synthesis of graphene oxide and reduced graphene oxide by needle platy natural vein graphite

International Nuclear Information System (INIS)

Rathnayake, R.M.N.M.; Wijayasinghe, H.W.M.A.C.; Pitawala, H.M.T.G.A.; Yoshimura, Masamichi; Huang, Hsin-Hui

2017-01-01

Highlights: • The high purity of this form of needle platy natural vein graphite is expected to synthesize GO and rGO readily and efficiently, as compared to the synthetic and less pure graphite raw materials. • Production of large-scale GO and rGO for industrial applications can be achieved by using this highly crystalline NPG vein graphite, and it adds value to the natural resources. • High quality, few-layer, and cost effective GO and rGO can achieve great results using this low cost, natural graphite. - Abstract: Among natural graphite varieties, needle platy vein graphite (NPG) has very high purity. Therefore, it is readily used to prepare graphene oxide (GO) and reduced graphene oxide (rGO). In this study, GO and rGO were prepared using chemical oxidation and reduction process, respectively. The synthesized materials were characterized by X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), and Fourier transform infrared (FTIR) spectroscopy. XRD studies confirmed the increase of the interlayer spacing of GO and rGO in between 3.35 to 8.66 A°. AFM studies showed the layer height of rGO to be 1.05 nm after the reduction process. TEM micrographs clearly illustrated that the prepared GO has more than 25 layers, while the rGO has only less than 15 layers. Furthermore, the effect of chemical oxidation and reduction processes on surface morphology of graphite were clearly observed in FESEM micrographs. The calculated R_O_/_C of GO and rGO using XPS analysis are 5.37% and 1.77%, respectively. The present study revealed the successful and cost effective nature of the chemical oxidation, and the reduction processes for the production of GO and rGO out of natural vein graphite.

Morphology and phase transformations of tin oxide nanostructures synthesized by the hydrothermal method in the presence of dicarboxylic acids

International Nuclear Information System (INIS)

Zima, Tatyana; Bataev, Ivan

2016-01-01

A new approach to the synthesis of non-stoichiometric tin oxide structures with different morphologies and the phase compositions has been evaluated. The nanostructures were synthesized by hydrothermal treatment of the mixtures of dicarboxylic acids ― aminoterephthalic or oxalic ― with nanocrystalline SnO 2 powder, which was obtained via the sol-gel technology. The products were characterized by Raman and IR spectroscopy, SEM, HRTEM, and XRD analysis. It was shown that the controlled addition of a dicarboxylic acid leads not only to a change in the morphology of the nanostructures, but also to SnO 2 –SnO 2 /Sn 3 O 4 –Sn 3 O 4 –SnO phase transformations. A single-phase Sn 3 O 4 in the form of the well-separated hexagonal nanoplates and mixed SnO 2 /Sn 3 O 4 phases in the form of hierarchical flower-like structures were obtained in the presence of organic additives. The effects of concentration, redox activity of the acids and heat treatment on the basic characteristics of the synthesized tin oxide nanostructures and phase transformations in the synthesized materials are discussed. - Graphical abstract: The controlled addition of aminoterephthalic or oxalic acid leads not only to a change in the morphology of the nanostructures, but also to SnO 2 –SnO 2 /Sn 3 O 4 –Sn 3 O 4 –SnO phase transformations. - Highlights: • A new approach to the synthesis of non-stoichiometric tin oxide structures is studied. • Tin oxide structures are synthesized via hydrothermal method with dicarboxylic acids. • Morphology and phase composition are changed with redox activity and dosage of acid. • The redox activity of acid has an effect on ratio of SnO and SnO 2 in crystal structure. • A pure phase Sn 3 O 4 nanoplates and SnO 2 /Sn 3 O 4 hierarchical structures are formed.

Fergusonite-type CeNbO{sub 4+δ}: Single crystal growth, symmetry revision and conductivity

Energy Technology Data Exchange (ETDEWEB)

Bayliss, Ryan D. [Department of Materials, Imperial College London, Prince Consort Road, London, SW7 2BP (United Kingdom); Pramana, Stevin S.; An, Tao; Wei, Fengxia; Kloc, Christian L. [School of Materials Science and Engineering, 50 Nanyang Avenue, Nanyang Technological University, 639798 (Singapore); White, Andrew J.P. [Chemical Crystallography Laboratory, Department of Chemistry, Imperial College London, Exhibition Road, London, SW7 2AZ (United Kingdom); Skinner, Stephen J. [Department of Materials, Imperial College London, Prince Consort Road, London, SW7 2BP (United Kingdom); White, Timothy J. [School of Materials Science and Engineering, 50 Nanyang Avenue, Nanyang Technological University, 639798 (Singapore); Baikie, Tom, E-mail: tbaikie@ntu.edu.sg [School of Materials Science and Engineering, 50 Nanyang Avenue, Nanyang Technological University, 639798 (Singapore)

2013-08-15

Large fergusonite-type (ABO{sub 4}, A=Ce, B=Nb) oxide crystals, a prototype electrolyte composition for solid oxide fuel cells (SOFC), were prepared for the first time in a floating zone mirror furnace under air or argon atmospheres. While CeNbO{sub 4} grown in air contained CeNbO{sub 4.08} as a minor impurity that compromised structural analysis, the argon atmosphere yielded a single phase crystal of monoclinic CeNbO{sub 4}, as confirmed by selected area electron diffraction, powder and single crystal X-ray diffraction. The structure was determined in the standard space group setting C12/c1 (No. 15), rather than the commonly adopted I12/a1. AC impedance spectroscopy conducted under argon found that stoichiometric CeNbO{sub 4} single crystals showed lower conductivity compared to CeNbO{sub 4+δ} confirming interstitial oxygen can penetrate through fergusonite and is responsible for the higher conductivity associated with these oxides. - Graphical abstract: Large fergusonite-type CeNbO{sub 4} crystals were prepared for the first time in a floating zone mirror furnace. Crystal growth in an argon atmosphere yielded a single phase monoclinic CeNbO4, as confirmed by selected area electron diffraction, powder and single crystal X-ray diffraction. The structure was determined in the standard space group setting C12/c1 (No. 15), rather than the commonly adopted I12/a1. AC impedance spectroscopy found CeNbO{sub 4} single crystals showed lower conductivity compared to CeNbO{sub 4+δ} confirming interstitial oxygen can penetrate through fergusonite and is responsible for the higher conductivity associated with these oxides. Highlights: • Preparation of single crystals of CeNbO{sub 4} using a floating zone mirror furnace. • Correction to the crystal symmetry of the monoclinic form of CeNbO{sub 4}. • Report the conductivity of a single crystal of CeNbO{sub 4}.

Zirconium oxide deposits (ZrO2) and titanium oxide (TiO2) on 304l stainless steel

International Nuclear Information System (INIS)

Davila N, M. L.

2015-01-01

This research project aims to carry out the surface and electrochemical characterization to obtain the optimum conditions of the hydrothermal deposits of zirconium oxide ZrO 2 (baddeleyite) and titanium oxide TiO 2 (anatase and rutile phases) on 304l stainless steel, simulating an inhibiting protective layer. 304l steel specimens were cut, pre-oxidized in water at a temperature of 288 degrees Celsius and 8 MPa, similar to those of a typical BWR conditions. From the titanium oxide anatase crystalline phase, the rutile phase was obtained by a heat treatment at 1000 degrees Celsius. The Sigma-Aldrich pre-oxidized powders and steel 304l were characterized using techniques of X-ray diffraction, scanning electron microscopy, X-ray dispersive energy, chemical mapping and Raman spectrometry. The pre-oxidized steel has two oxide layers, an inner layer with nano metric crystals and another outer of larger crystals to 1μm, with the formation of hematite and magnetite, this predominating. The surface that contacted the sample holder has larger crystals. Hydrothermal deposits were carry out from suspensions of 10, 100 and 1000 ppm, of the crystal phases of anatase, rutile and baddeleyite, on the pre-oxidized steel at a temperature of 150 degrees Celsius for 2 and 7 days, samples were analyzed by X-ray diffraction, scanning electron microscopy, X-ray dispersive energy, Raman spectrometry and Tafel polarization. The suspension to 1000 ppm for 7 days coated surface most; the baddeleyite deposit is noticed more homogeneous than anatase and rutile. The deposit is favored when hematite and magnetite crystals are larger. The chemical mapping on deposits show that even after being immersed in water to 288 degrees Celsius during 30 days, the deposits are still present although a loss is observed. A reference electrode was assembled to conduct electrochemical tests of Tafel able to withstand a temperature of 288 degrees Celsius and pressure of 8 MPa. The baddeleyite deposit presented

Consecutive dynamic resolutions of phosphine oxides

NARCIS (Netherlands)

Kortmann, Felix A.; Chang, Mu Chieh; Otten, Edwin; Couzijn, Erik P A; Lutz, Martin|info:eu-repo/dai/nl/304828971; Minnaard, Adriaan J.

2014-01-01

A crystallization-induced asymmetric transformation (CIAT) involving a radical-mediated racemization provides access to enantiopure secondary phosphine oxides. A consecutive CIAT is used to prepare enantio- and diastereo-pure tert-butyl(hydroxyalkyl)phenylphosphine oxides. © 2014 The Royal Society

Praseodymium Cuprate Thin Film Cathodes for Intermediate Temperature Solid Oxide Fuel Cells: Roles of Doping, Orientation, and Crystal Structure.

Science.gov (United States)

Mukherjee, Kunal; Hayamizu, Yoshiaki; Kim, Chang Sub; Kolchina, Liudmila M; Mazo, Galina N; Istomin, Sergey Ya; Bishop, Sean R; Tuller, Harry L

2016-12-21

Highly textured thin films of undoped, Ce-doped, and Sr-doped Pr 2 CuO 4 were synthesized on single crystal YSZ substrates using pulsed laser deposition to investigate their area-specific resistance (ASR) as cathodes in solid-oxide fuel cells (SOFCs). The effects of T' and T* crystal structures, donor and acceptor doping, and a-axis and c-axis orientation on ASR were systematically studied using electrochemical impedance spectroscopy on half cells. The addition of both Ce and Sr dopants resulted in improvements in ASR in c-axis oriented films, as did the T* crystal structure with the a-axis orientation. Pr 1.6 Sr 0.4 CuO 4 is identified as a potential cathode material with nearly an order of magnitude faster oxygen reduction reaction kinetics at 600 °C compared to thin films of the commonly studied cathode material La 0.6 Sr 0.4 Co 0.8 Fe 0.2 O 3-δ . Orientation control of the cuprate films on YSZ was achieved using seed layers, and the anisotropy in the ASR was found to be less than an order of magnitude. The rare-earth doped cuprate was found to be a versatile system for study of relationships between bulk properties and the oxygen reduction reaction, critical for improving SOFC performance.

Sol-gel synthesis of Bi3.25La0.75Ti3O12 nanotubes

International Nuclear Information System (INIS)

Wang Wen; Ke Hua; Rao Jiancun; Feng Jinbiao; Feng Ming; Jia Dechang; Zhou Yu

2011-01-01

Research highlights: → One-dimensional (1D) ferroelectrics have been successfully synthesized. The sol-gel template synthesis is a versatile and inexpensive technique for producing nanostructures, and particularly facilitates the fabrication of complex oxide nanotubes or nanowires. Compared with the synthesis of the general nanotubes such as carbon nanotubes with simple crystal structure, the synthesis of ferroelectric compound is difficult due to the multielement and the complex crystal structures of these ferroelectrics. Herein, we report the synthesis of one-dimensional BLT nanotubes on anodic alumina (AAO) templates by immersing a template membrane in sol without polymeric additive. - Abstract: Ferroelectric Bi 3.25 La 0.75 Ti 3 O 12 (BLT) nanotubes were synthesized by sol-gel technique using nanochannel porous anodic aluminum oxide (AAO) templates, and were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM). BLT nanotubes with diameter of around 240 nm and the wall thickness of about 25 nm exhibited a single orthorhombic perovskite structure and highly preferential crystal growth along the [1 1 7] orientation, which have smooth wall morphologies and well-defined diameters corresponding to the diameter of the applied template. The formation mechanism of BLT nanotubes was discussed.

Sol-gel synthesis of Bi{sub 3.25}La{sub 0.75}Ti{sub 3}O{sub 12} nanotubes

Energy Technology Data Exchange (ETDEWEB)

Wang Wen, E-mail: wangwen@hit.edu.cn [Institute for Advanced Ceramics, School of Materials Science and Engineering, Harbin Institute of Technology, No. 92 West Da-Zhi Street, Harbin 150001, Heilongjiang (China); Hua, Ke; Jiancun, Rao; Jinbiao, Feng; Ming, Feng; Dechang, Jia; Yu, Zhou [Institute for Advanced Ceramics, School of Materials Science and Engineering, Harbin Institute of Technology, No. 92 West Da-Zhi Street, Harbin 150001, Heilongjiang (China)

2011-04-07

Research highlights: > One-dimensional (1D) ferroelectrics have been successfully synthesized. The sol-gel template synthesis is a versatile and inexpensive technique for producing nanostructures, and particularly facilitates the fabrication of complex oxide nanotubes or nanowires. Compared with the synthesis of the general nanotubes such as carbon nanotubes with simple crystal structure, the synthesis of ferroelectric compound is difficult due to the multielement and the complex crystal structures of these ferroelectrics. Herein, we report the synthesis of one-dimensional BLT nanotubes on anodic alumina (AAO) templates by immersing a template membrane in sol without polymeric additive. - Abstract: Ferroelectric Bi{sub 3.25}La{sub 0.75}Ti{sub 3}O{sub 12} (BLT) nanotubes were synthesized by sol-gel technique using nanochannel porous anodic aluminum oxide (AAO) templates, and were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM). BLT nanotubes with diameter of around 240 nm and the wall thickness of about 25 nm exhibited a single orthorhombic perovskite structure and highly preferential crystal growth along the [1 1 7] orientation, which have smooth wall morphologies and well-defined diameters corresponding to the diameter of the applied template. The formation mechanism of BLT nanotubes was discussed.

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

Science.gov (United States)

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

2016-09-01

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

Preparation and structural characterization of SnO2 and GeO2 methanol steam reforming thin film model catalysts by (HR)TEM

International Nuclear Information System (INIS)

Lorenz, Harald; Zhao Qian; Turner, Stuart; Lebedev, Oleg I.; Van Tendeloo, Gustaaf; Kloetzer, Bernhard; Rameshan, Christoph; Penner, Simon

2010-01-01

Structure, morphology and composition of different tin oxide and germanium oxide thin film catalysts for the methanol steam reforming (MSR) reaction have been studied by a combination of (high-resolution) transmission electron microscopy, selected area electron diffraction, dark-field imaging and electron energy-loss spectroscopy. Deposition of the thin films on NaCl(0 0 1) cleavage faces has been carried out by thermal evaporation of the respective SnO 2 and GeO 2 powders in varying oxygen partial pressures and at different substrate temperatures. Preparation of tin oxide films in high oxygen pressures (10 -1 Pa) exclusively resulted in SnO phases, at and above 473 K substrate temperature epitaxial growth of SnO on NaCl(0 0 1) leads to well-ordered films. For lower oxygen partial pressures (10 -3 to 10 -2 Pa), mixtures of SnO and β-Sn are obtained. Well-ordered SnO 2 films, as verified by electron diffraction patterns and energy-loss spectra, are only obtained after post-oxidation of SnO films at temperatures T ≥ 673 K in 10 5 Pa O 2 . Preparation of GeO x films inevitably results in amorphous films with a composition close to GeO 2 , which cannot be crystallized by annealing treatments in oxygen or hydrogen at temperatures comparable to SnO/SnO 2 . Similarities and differences to neighbouring oxides relevant for selective MSR in the third group of the periodic system (In 2 O 3 and Ga 2 O 3 ) are also discussed with the aim of cross-correlation in formation of nanomaterials, and ultimately, also catalytic properties.

Preliminary neutron diffraction analysis of challenging human manganese superoxide dismutase crystals.

Science.gov (United States)

Azadmanesh, Jahaun; Trickel, Scott R; Weiss, Kevin L; Coates, Leighton; Borgstahl, Gloria E O

2017-04-01

Superoxide dismutases (SODs) are enzymes that protect against oxidative stress by dismutation of superoxide into oxygen and hydrogen peroxide through cyclic reduction and oxidation of the active-site metal. The complete enzymatic mechanisms of SODs are unknown since data on the positions of hydrogen are limited. Here, methods are presented for large crystal growth and neutron data collection of human manganese SOD (MnSOD) using perdeuteration and the MaNDi beamline at Oak Ridge National Laboratory. The crystal from which the human MnSOD data set was obtained is the crystal with the largest unit-cell edge (240 Å) from which data have been collected via neutron diffraction to sufficient resolution (2.30 Å) where hydrogen positions can be observed.

Effects of Borax on the Reduction of Pre-oxidized Panzhihua Ilmenite

Science.gov (United States)

Guo, Yufeng; Zheng, Fuqiang; Jiang, Tao; Chen, Feng; Wang, Shuai; Qiu, Guanzhou

2018-01-01

The effects of borax (sodium borate) on the enhancement reduction of pre-oxidized Panzhihua ilmenite were investigated. The effects of borax on the mineral phase transformation, microstructures, crystal cell parameter, melting point and Mg distribution were studied to reveal the mechanism of enhancement reduction. Under the constant reduction conditions, the borax could reduce the reduction activation energy of pre-oxidized ilmenite. The reduction kinetics analysis indicated that the reduction rate was controlled by interfacial chemical reaction. The reduction activation energy of the pre-oxidized ilmenite with 4% borax was 80.263 kJ/mol, which was 28.585 kJ/mol less than that of the pre-oxidized ilmenite without borax. Borax could eliminate the migration of Mg into the reduced particle center. The crystal cell parameter of the reduced product was increased by adding borax. Borax could improve the growth of dendritic crystals in the pre-oxidized ilmenite.

Influence of radiational oxidation on the kinetics of electrization of polypropylene by electron irradiation

International Nuclear Information System (INIS)

Rozno, A.G.; Romanov, A.V.; Sukhov, N.L.; Gromov, V.V.; Ershov, B.G.

1992-01-01

Kinetics of volumetric electric charge and accumulation of paramagnetic centres (PMC) in polypropylene (PP) of two crystal modifications, subjected to radiational oxidation were studied. A correlation between volumetric charge and PMC in radiationally oxidation PP was detected. Considerable influence of crystal phase on the processes of charging and radiational oxidation was revealed

Atomic Scale Structure-Chemistry Relationships at Oxide Catalyst Surfaces and Interfaces

Science.gov (United States)

McBriarty, Martin E.

Oxide catalysts are integral to chemical production, fuel refining, and the removal of environmental pollutants. However, the atomic-scale phenomena which lead to the useful reactive properties of catalyst materials are not sufficiently understood. In this work, the tools of surface and interface science and electronic structure theory are applied to investigate the structure and chemical properties of catalytically active particles and ultrathin films supported on oxide single crystals. These studies focus on structure-property relationships in vanadium oxide, tungsten oxide, and mixed V-W oxides on the surfaces of alpha-Al2O3 and alpha-Fe2O 3 (0001)-oriented single crystal substrates, two materials with nearly identical crystal structures but drastically different chemical properties. In situ synchrotron X-ray standing wave (XSW) measurements are sensitive to changes in the atomic-scale geometry of single crystal model catalyst surfaces through chemical reaction cycles, while X-ray photoelectron spectroscopy (XPS) reveals corresponding chemical changes. Experimental results agree with theoretical calculations of surface structures, allowing for detailed electronic structure investigations and predictions of surface chemical phenomena. The surface configurations and oxidation states of V and W are found to depend on the coverage of each, and reversible structural shifts accompany chemical state changes through reduction-oxidation cycles. Substrate-dependent effects suggest how the choice of oxide support material may affect catalytic behavior. Additionally, the structure and chemistry of W deposited on alpha-Fe 2O3 nanopowders is studied using X-ray absorption fine structure (XAFS) measurements in an attempt to bridge single crystal surface studies with real catalysts. These investigations of catalytically active material surfaces can inform the rational design of new catalysts for more efficient and sustainable chemistry.

Gold Nanoparticles Supported on Fibrous Silica Nanospheres (KCC-1) as Efficient Heterogeneous Catalysts for CO Oxidation

KAUST Repository

Qureshi, Ziyauddin S.; Sarawade, Pradip B.; Hussain, Irshad; Zhu, Haibo; Al-Johani, Hind; Anjum, Dalaver H.; Hedhili, Mohamed N.; Maity, Niladri; D'Elia, Valerio; Basset, Jean-Marie

2016-01-01

Gold nanoparticles (Au NPs) of different sizes were supported on fibrous silica nanospheres (KCC-1) by various methods. The size and the location of the Au NPs on the support were found to depend on the preparation method. The KCC-1-supported Au NPs were thoroughly characterized by using HR-TEM, XRD, X-ray photoelectron spectroscopy, UV, and Brunauer-Emmett-Teller surface area measurements and were applied in catalysis for the oxidation of CO. The catalytic performance is discussed in relation to the morphological properties of KCC-1. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Gold Nanoparticles Supported on Fibrous Silica Nanospheres (KCC-1) as Efficient Heterogeneous Catalysts for CO Oxidation

KAUST Repository

Qureshi, Ziyauddin S.

2016-04-13

Gold nanoparticles (Au NPs) of different sizes were supported on fibrous silica nanospheres (KCC-1) by various methods. The size and the location of the Au NPs on the support were found to depend on the preparation method. The KCC-1-supported Au NPs were thoroughly characterized by using HR-TEM, XRD, X-ray photoelectron spectroscopy, UV, and Brunauer-Emmett-Teller surface area measurements and were applied in catalysis for the oxidation of CO. The catalytic performance is discussed in relation to the morphological properties of KCC-1. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The special features of the crystal structure and properties of oxides with mixed conductivity based on lanthanum gallate

Science.gov (United States)

Politova, E. D.; Ivanov, S. A.; Kaleva, G. M.; Mosunov, A. V.; Rusakov, V. S.

2008-10-01

The paper presents a review of works on the synthesis, structural composition effects, phase transitions, and electrical conductivity properties of multicomponent solid solutions based on heterosubstituted lanthanum gallate (La,A)(Ga,M)O3 - y . High-temperature phase transitions and structural and charge ordering effects were studied. The presence of iron cations in different valence states was proved; the relative contents of these cations depended on the x parameter and nonstoichiometry parameter y of the base composition. For M = Fe, antiferromagnetic ordering was observed; its temperature interval was determined by the concentration of iron cations in the high-spin state. The total conductivity was found to increase as the concentration of transition metal cations grew because of an increase in the electronic conductivity component. The data on structural parameters and dc and ac conductivity substantiated the conclusion that the highest ionic conductivity and permeability to oxygen were characteristic of iron-containing oxides. The results obtained are evidence that crystal chemical factors play a determining role in the formation of the ion-conducting properties of anion-deficient perovskite-like oxides.

On chemical activity of heavy metal oxides

International Nuclear Information System (INIS)

Mechev, V.V.

1994-01-01

Interaction of solid oxides of heavy nonferrous metals with sulfur and carbon is investigated. The results are discussed. Direct dependence of chemical activity of oxides on disordering of their crystal lattice at heating is established. Beginning of interaction in the systems studied is accompanied by change of oxide conductivity type

Comparing electron tomography and HRTEM slicing methods as tools to measure the thickness of nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Alloyeau, D., E-mail: alloyeau.damien@gmail.com [Laboratoire Materiaux et Phenomenes Quantiques, Universite Paris 7/CNRS, UMR 7162, 2 Place Jussieu, 75251 Paris (France); Laboratoire d' Etude des Microstructures - ONERA/CNRS, UMR 104, B.P. 72, 92322 Chatillon (France); Ricolleau, C. [Laboratoire Materiaux et Phenomenes Quantiques, Universite Paris 7/CNRS, UMR 7162, 2 Place Jussieu, 75251 Paris (France); Oikawa, T. [Laboratoire Materiaux et Phenomenes Quantiques, Universite Paris 7/CNRS, UMR 7162, 2 Place Jussieu, 75251 Paris (France); JEOL (Europe) SAS, Espace Claude Monet, 1 Allee de Giverny, 78290 Croissy-sur-Seine (France); Langlois, C. [Laboratoire Materiaux et Phenomenes Quantiques, Universite Paris 7/CNRS, UMR 7162, 2 Place Jussieu, 75251 Paris (France); Le Bouar, Y.; Loiseau, A. [Laboratoire d' Etude des Microstructures - ONERA/CNRS, UMR 104, B.P. 72, 92322 Chatillon (France)

2009-06-15

Nanoparticles' morphology is a key parameter in the understanding of their thermodynamical, optical, magnetic and catalytic properties. In general, nanoparticles, observed in transmission electron microscopy (TEM), are viewed in projection so that the determination of their thickness (along the projection direction) with respect to their projected lateral size is highly questionable. To date, the widely used methods to measure nanoparticles thickness in a transmission electron microscope are to use cross-section images or focal series in high-resolution transmission electron microscopy imaging (HRTEM 'slicing'). In this paper, we compare the focal series method with the electron tomography method to show that both techniques yield similar particle thickness in a range of size from 1 to 5 nm, but the electron tomography method provides better statistics since more particles can be analyzed at one time. For this purpose, we have compared, on the same samples, the nanoparticles thickness measurements obtained from focal series with the ones determined from cross-section profiles of tomograms (tomogram slicing) perpendicular to the plane of the substrate supporting the nanoparticles. The methodology is finally applied to the comparison of CoPt nanoparticles annealed ex situ at two different temperatures to illustrate the accuracy of the techniques in detecting small particle thickness changes.

Structural and interfacial characteristics of thin (2 films grown by electron cyclotron resonance plasma oxidation on [100] Si substrates

International Nuclear Information System (INIS)

Nguyen, T.D.; Carl, D.A.; Hess, D.W.; Lieberman, M.A.; Gronsky, R.

1991-04-01

The feasibility of fabricating ultra-thin SiO 2 films on the order of a few nanometer thickness has been demonstrated. SiO 2 thin films of approximately 7 nm thickness have been produced by ion flux-controlled Electron Cyclotron Resonance plasma oxidation at low temperature on [100] Si substrates, in reproducible fashion. Electrical measurements of these films indicate that they have characteristics comparable to those of thermally grown oxides. The thickness of the films was determined by ellipsometry, and further confirmed by cross-sectional High-Resolution Transmission Electron Microscopy. Comparison between the ECR and the thermal oxide films shows that the ECR films are uniform and continuous over at least a few microns in lateral direction, similar to the thermal oxide films grown at comparable thickness. In addition, HRTEM images reveal a thin (1--1.5 nm) crystalline interfacial layer between the ECR film and the [100] substrate. Thinner oxide films of approximately 5 nm thickness have also been attempted, but so far have resulted in nonuniform coverage. Reproducibility at this thickness is difficult to achieve

Coupling between crystal structure and magnetism in transition-metal oxides

Science.gov (United States)

Barton, Phillip Thomas

Transition-metal oxides exhibit a fascinating array of phenomena ranging from superconductivity to negative thermal expansion to catalysis. This dissertation focuses on magnetism, which is integral to engineering applications such as data storage, electric motors/generators, and transformers. The investigative approach follows structure-property relationships from materials science and draws on intuition from solid-state chemistry. The interplay between crystal structure and magnetic properties is studied experimentally in order to enhance the understanding of magnetostructural coupling mechanisms and provide insight into avenues for tuning behavior. A combination of diffraction and physical property measurements were used to study structural and magnetic phase transitions as a function of chemical composition, temperature, and magnetic field. The systems examined are of importance in Li-ion battery electrochemistry, condensed-matter physics, solid-state chemistry, and p-type transparent conducting oxides. The materials were prepared by solid-state reaction of powder reagents at high temperatures for periods lasting tens of hours. The first project discussed is of a solid solution between NiO, a correlated insulator, and LiNiO2, a layered battery cathode. Despite the deceptive structural and compositional simplicity of this system, a complete understanding of its complex magnetic properties has remained elusive. This study shows that nanoscale domains of chemical order form at intermediate compositions, creating interfaces between antiferromagnetism and ferrimagnetism that give rise to magnetic exchange bias. A simple model of the magnetism is presented along with a comprehensive phase diagram. The second set of investigations focus on the Ge-Co-O system where the spin-orbit coupling of Co(II) plays a significant role. GeCo2O 4 is reported to exhibit unusual magnetic behavior that arises from Ising spin in its spinel crystal structure. Studies by variable

Mechanical properties of melt-derived erbium oxide

International Nuclear Information System (INIS)

Neuman, A.D.; Blacic, M.J.; Platero, M.; Romero, R.S.; McClellan, K.J.; Petrovic, J.J.

1998-01-01

Erbium oxide (Er 2 O 3 ) is a rare earth oxide that is chemically and thermally stable and has a melting point of 2,430 C. There is relatively little information available regarding single crystal growth of erbia or the properties of erbia. In this study, erbia single crystals have been grown in a Xenon Optical Floating Zone Unit (XeOFZ) capable of melting materials at temperatures up to 3,000 C. Erbia was melt synthesized in the XeOFZ unit in a container less fashion, proving for little chance of contamination. Crystals were grown in compressed air and in reducing atmospheres. A recurring problem with melt synthesis of erbia is the appearance of flakes at the edges of the melt zone during growth; these flakes disrupt the growth process. The processing details and an initial survey of the physical properties of erbia single crystals is discussed

Synthesis and luminescence of CePO4 and CePO4:Tb hollow and core-shell microspheres composed of single-crystal nanorods

International Nuclear Information System (INIS)

Guan Mingyun; Sun Jianhua; Han Min; Xu Zheng; Tao Feifei; Yin Gui; Wei Xianwen; Zhu Jianmin; Jiang Xiqun

2007-01-01

Lanthanide phosphate microspheres composed of single-crystal CePO 4 and CePO 4 :Tb nanorods were successfully synthesized, respectively, using the functionalized composite aggregate as a template, which is composed of P123, H 6 P 4 O 13 and Ce 3+ , and also as a resource of reaction species with high chemical potential. The shape and the phase structure of the CePO 4 nanocrystal can be easily controlled via adjusting reaction temperature, monomer concentration and annealing temperature. SEM images show the spherical superstructure composed of nanorods. HRTEM and SAED images reveal the single-crystalline nature of nanorod and TEM images show the hollow interiors of the superstructure. XRD patterns indicate that the crystal structure of the nanorods is hexagonal before and monoclinic after annealing. The formation mechanism was proposed. Strong UV and green luminescence were observed for the CePO 4 and CePO 4 :Tb microspheres, respectively. The synthesis method can be extended to the fabrication of NRHS and core-shell microspheres of other rare-earth or doped LnPO 4 materials for wide applications

A highly efficient microfluidic nano biochip based on nanostructured nickel oxide.

Science.gov (United States)

Ali, Md Azahar; Solanki, Pratima R; Patel, Manoj K; Dhayani, Hemant; Agrawal, Ved Varun; John, Renu; Malhotra, Bansi D

2013-04-07

We present results of the studies relating to fabrication of a microfluidic biosensor chip based on nickel oxide nanorods (NRs-NiO) that is capable of directly measuring the concentration of total cholesterol in human blood through electrochemical detection. Using this chip we demonstrate, with high reliability and in a time efficient manner, the detection of cholesterol present in buffer solutions at clinically relevant concentrations. The microfluidic channel has been fabricated onto a nickel oxide nanorod-based electrode co-immobilized with cholesterol esterase (ChEt) and cholesterol oxidase (ChOx) that serves as the working electrode. Bare indium tin oxide served as the counter electrode. A Ag/AgCl wire introduced to the outlet of the microchannel acts as a reference electrode. The fabricated NiO nanorod-based electrode has been characterized using X-ray diffraction, Raman spectroscopy, HR-TEM, FT-IR, UV-visible spectroscopy and electrochemical techniques. The presented NRs-NiO based microfluidic sensor exhibits linearity in the range of 1.5-10.3 mM, a high sensitivity of 0.12 mA mM(-1) cm(-2) and a low value of 0.16 mM of the Michaelis-Menten constant (Km).

Room temperature ferromagnetism of tin oxide nanocrystal based on synthesis methods

Energy Technology Data Exchange (ETDEWEB)

Sakthiraj, K.; Hema, M. [Department of Physics, Kamaraj College of Engineering and Technology, Virudhunagar 626001, Tamil Nadu (India); Balachandrakumar, K. [Department of Physics, Raja Doraisingam Government Arts College, Sivagangai 630561, Tamil Nadu (India)

2016-04-15

The experimental conditions used in the preparation of nanocrystalline oxide materials play an important role in the room temperature ferromagnetism of the product. In the present work, a comparison was made between sol–gel, microwave assisted sol–gel and hydrothermal methods for preparing tin oxide nanocrystal. X-ray diffraction analysis indicates the formation of tetragonal rutile phase structure for all the samples. The crystallite size was estimated from the HRTEM images and it is around 6–12 nm. Using optical absorbance measurement, the band gap energy value of the samples has been calculated. It reveals the existence of quantum confinement effect in all the prepared samples. Photoluminescence (PL) spectra confirms that the luminescence process originates from the structural defects such as oxygen vacancies present in the samples. Room temperature hysteresis loop was clearly observed in M–H curve of all the samples. But the sol–gel derived sample shows the higher values of saturation magnetization (M{sub s}) and remanence (M{sub r}) than other two samples. This study reveals that the sol–gel method is superior to the other two methods for producing room temperature ferromagnetism in tin oxide nanocrystal.

Microstructure and Mechanical Property of 12Cr Oxide Dispersion Strengthened Steel

Science.gov (United States)

Xu, Haijian; Lu, Zheng; Jia, Chunyan; Gao, Hao; Liu, Chunming

2016-03-01

Nanostructured oxide dispersion strengthened (ODS) steels with nominal compositions (wt%): Fe-12Cr-2W-0.3Ti-0.3Y2O3 were produced by mechanical alloying and hot isostatic pressing. The microstructure was characterized by means of electron microscopy (EBSD, TEM and HRTEM) and the hardness and the tensile properties at different temperatures were measured. The results showed that the ultimate tensile strength of the fabricated 12Cr-ODS steel reached nearly 1,100 MPa at room temperature and maintained around 340 MPa at 700°C. Nano-oxide particles with size ranging from several nm to 30 nm and the number density was 3.6 × 1020/m3 were observed by TEM. Following heat treatment, including normalizing at 1,100°C for 1 h and tempering at 750°C for 2 h, the average grain size was a little decreased. The number of nano-oxide particles increased and the number density was 8.9 × 1020/m3. Specimens showed much higher ductility and there was a slight increase of ultimate tensile strength and Vickers hardness at the same time.

As-Deposited (La1-xSrx)(Ga1-y-zMgyCoz)O3-(x+y+z)/2 Crystallized Thin Films Prepared by Pulsed Laser Deposition for Application to Solid Oxide Fuel Cell Electrolyte

Science.gov (United States)

Mitsugi, Fumiaki; Kanazawa, Seiji; Ohkubo, Toshikazu; Nomoto, Yukiharu; Ishihara, Tatsumi; Takita, Yusaku

2004-01-01

Doped lanthanum gallate (La1-xSrx)(Ga1-y-zMgyCoz)O3-(x+y+z)/2 (LSGMCO) perovskite oxide films were deposited on a quartz glass, LaAlO3 single-crystal substrate and porous anode electrode of a solid oxide fuel cell (SOFC) by pulsed laser deposition. It was necessary to increase the substrate temperature up to 800°C for a crystallization of the LSGMCO films. The film deposited on the LaAlO3 single-crystal substrate grew along the c-axis. The as-deposited LSGMCO thick film fabricated on the porous substrate at 800°C and at an oxygen pressure of 20Pa was formed from polycrystal columns and showed a high conductivity of 0.7S/cm at a measurement temperature of 800°C. The activation energies were 0.72 eV at 600-800°C and 1.05 eV at 400-600°C.

Molecular-level chemistry of model single-crystal oxide surfaces with model halogenated compounds

Science.gov (United States)

Adib, Kaveh

Synchrotron-based X-ray photoelectron spectroscopy (XPS), temperature-programmed desorption (TPD) and low energy electron diffraction (LEED) have been used to investigate, at a molecular level, the chemistry of different terminations of single crystal iron-oxide surfaces with probe molecules (CCl4 and D2O). Comparisons of the reactivity of these surfaces towards CCl4, indicate that the presence of an uncapped surface Fe cation (strong Lewis acid site) and an adjacent oxygen site capped by that cation can effect the C-Cl bond cleavage in CCl4, resulting in dissociatively adsorbed Cl-adatoms and carbon-containing fragments. If in addition to these sites, an uncapped surface oxygen (Lewis base) site is also available, the carbon-containing moiety can then move that site, coordinate itself with that uncapped oxygen, and stabilize itself. At a later step, the carbon-containing fragment may form a strong covalent bond with the uncapped oxygen and may even abstract that surface oxygen. On the other hand, if an uncapped oxygen is not available to stabilize the carbon-containing fragment, the surface coordination will not occur and upon the subsequent thermal annealing of the surface the Cl-adatoms and the carbon-containing fragments will recombine and desorb as CCl4. Finally, the presence of surface deuteroxyls blocking the strong Lewis acid and base sites of the reactive surface, passivates this surface. Such a deuteroxylated surface will be unreactive towards CCl 4. Such a molecular level understanding of the surface chemistry of metal-oxides will have applications in the areas of selective catalysis, including environmental catalysis, and chemical sensor technology.

Subset geometric phase analysis method for deformation evaluation of HRTEM images

Energy Technology Data Exchange (ETDEWEB)

Zhang, Hongye [School of Aerospace Engineering, Beijing Institute of Technology, Beijing 100081 (China); Liu, Zhanwei, E-mail: liuzw@bit.edu.cn [School of Aerospace Engineering, Beijing Institute of Technology, Beijing 100081 (China); Wen, Huihui [School of Aerospace Engineering, Beijing Institute of Technology, Beijing 100081 (China); Xie, Huimin, E-mail: xiehm@mail.tsinghua.edu.cn [AML, Department of Engineering Mechanics, Tsinghua University, Beijing 100084 (China); Liu, Chao [Institute of Semiconductors, Chinese Academy of Sciences, Beijing 100083 (China)

2016-12-15

Geometrical phase analysis (GPA) is typically a powerful tool to investigate the deformation in high resolution transmission electron microscopy images and has been used in various fields. The traditional GPA method using the fast Fourier transform, referred to as global-GPA (G-GPA) here, is based on the relationship between the displacement and the phase difference. In this paper, a subset-GPA (S-GPA) is introduced for further improvement. The S-GPA performs the windowed Fourier transform block by block in the image. The maximum strain measurement scale of the GPA method is theoretically analyzed on the basic of the phase spectrum extraction process. The upper limit is one third of the atomic spacing. The results of various numerical simulations verified that the S-GPA method performs better than the traditional G-GPA method in both the homogeneous and inhomogeneous deformation conditions, with the evaluation parameter of calculation reliability of S-GPA 10% higher than G-GPA. Specifically, the measurement accuracy of S-GPA is about three times higher than the G-GPA when calculating small strain (less than 2000με). For the large strain (greater than 150000με), the measurement accuracy of S-GPA is about 50% higher than that of the G-GPA. Besides, the S-GPA method can significantly eliminate the phase filling effect, while the G-GPA cannot. The S-GPA method has been successfully applied to analyze the strain field distribution in an lnGaAs/InAlAs supperlattice heterostructure. - Highlights: • A subset-GPA method, performing the windowed Fourier transform block by block in HRTEM image, is systematically introduced. • According to the theoretical analysis, the upper limit of absolute maximum strain of GPA method is 1/3. • The measurement accuracy of S-GPA is about three times higher than that of the G-GPA when calculating small strain. • The measurement capability of S-GPA is about 50 percent higher than that of the G-GPA when calculating large strain. �

Ge-Au eutectic bonding of Ge (100) single crystals

International Nuclear Information System (INIS)

Knowlton, W.B.; Beeman, J.W.; Emes, J.H.; Loretto, D.; Itoh, K.M.; Haller, E.E.

1993-01-01

The author present preliminary results on the eutectic bonding between two (100) Ge single crystal surfaces using thin films of Au ranging from 900 angstrom/surface to 300 angstrom/surface and Pd (10% the thickness of Au). Following bonding, plan view optical microscopy (OM) of the cleaved interface of samples with Au thicknesses ≤ 500 angstrom/surface show a eutectic morphology more conducive to phonon transmission through the bond interface. High resolution transmission electron microscopy (HRTEM) cross sectional interface studies of a 300 angstrom/surface Au sample show epitaxial growth of Ge. In sections of the bond, lattice continuity of the Ge is apparent through the interface. TEM studies also reveal heteroepitaxial growth of Au with a Au-Ge lattice mismatch of less than 2%. Eutectic bonds with 200 angstrom/surface Au have been attained with characterization pending. An optical polishing technique for Ge has been optimized to insure intimate contact between the Ge surfaces prior to bonding. Interferometry analysis of the optically polished Ge surface shows that surface height fluctuations lie within ±150 angstrom across an interval of lmm. Characterization of phonon transmission through the interface is discussed with respect to low temperature detection of ballistic phonons

Bismuth oxide nanotubes-graphene fiber-based flexible supercapacitors

Science.gov (United States)

Gopalsamy, Karthikeyan; Xu, Zhen; Zheng, Bingna; Huang, Tieqi; Kou, Liang; Zhao, Xiaoli; Gao, Chao

2014-07-01

Graphene-bismuth oxide nanotube fiber as electrode material for constituting flexible supercapacitors using a PVA/H3PO4 gel electrolyte is reported with a high specific capacitance (Ca) of 69.3 mF cm-2 (for a single electrode) and 17.3 mF cm-2 (for the whole device) at 0.1 mA cm-2, respectively. Our approach opens the door to metal oxide-graphene hybrid fibers and high-performance flexible electronics.Graphene-bismuth oxide nanotube fiber as electrode material for constituting flexible supercapacitors using a PVA/H3PO4 gel electrolyte is reported with a high specific capacitance (Ca) of 69.3 mF cm-2 (for a single electrode) and 17.3 mF cm-2 (for the whole device) at 0.1 mA cm-2, respectively. Our approach opens the door to metal oxide-graphene hybrid fibers and high-performance flexible electronics. Electronic supplementary information (ESI) available: Equations and characterization. SEM images of GGO, XRD and XPS of Bi2O3 NTs, HRTEM images and EDX Spectra of Bi2O3 NT5-GF, CV curves of Bi2O3NT5-GF, Bi2O3 NTs and bismuth nitrate in three-electrode system (vs. Ag/AgCl). CV and GCD curves of Bi2O3 NT1-GF and Bi2O3 NT3-GF. See DOI: 10.1039/c4nr02615b

Lyotropic Liquid Crystal Phases from Anisotropic Nanomaterials

Directory of Open Access Journals (Sweden)

Ingo Dierking

2017-10-01

Full Text Available Liquid crystals are an integral part of a mature display technology, also establishing themselves in other applications, such as spatial light modulators, telecommunication technology, photonics, or sensors, just to name a few of the non-display applications. In recent years, there has been an increasing trend to add various nanomaterials to liquid crystals, which is motivated by several aspects of materials development. (i addition of nanomaterials can change and thus tune the properties of the liquid crystal; (ii novel functionalities can be added to the liquid crystal; and (iii the self-organization of the liquid crystalline state can be exploited to template ordered structures or to transfer order onto dispersed nanomaterials. Much of the research effort has been concentrated on thermotropic systems, which change order as a function of temperature. Here we review the other side of the medal, the formation and properties of ordered, anisotropic fluid phases, liquid crystals, by addition of shape-anisotropic nanomaterials to isotropic liquids. Several classes of materials will be discussed, inorganic and mineral liquid crystals, viruses, nanotubes and nanorods, as well as graphene oxide.

Monitoring of morphology and physical properties of cultured cells using a micro camera and a quartz crystal with transparent indium tin oxide electrodes after injections of glutaraldehyde and trypsin

International Nuclear Information System (INIS)

Kang, Hyen-Wook; Ida, Kazumi; Yamamoto, Yuji; Muramatsu, Hiroshi

2008-01-01

For investigating the effects of chemical stimulation to cultured cells, we have developed a quartz crystal sensor system with a micro charge-coupled device (CCD) camera that enables microphotograph imaging simultaneously with quartz crystal measurement. Human hepatoma cell line (HepG2) cells were cultured on the quartz crystal through a collagen film. The electrode of the quartz crystal was made of indium tin oxide (ITO) transparent electrodes that enable to obtain a transparent mode photograph. Glutaraldehyde and trypsin were injected to the chamber of the cells, respectively. The response of the quartz crystal was monitored and microphotographs were recorded, and the resonance frequency and resonance resistance were analyzed with an F-R diagram that plotted the resonance frequency and resonance resistance. In the case of the glutaraldehyde injection, the cells responded in two steps that included the fast response of the cross-linking reaction and the successive internal change in the cells. In the case of the trypsin injection, the responses included two processes. In the first step, cell adhesion factors were cleaved and the cell structure became round, and in the next step, the cells were deposited on the quartz crystal surface and the surface of the cells was directly in contact with the quartz crystal surface

Transformation of Goethite to Hematite Nanocrystallines by High Energy Ball Milling

Directory of Open Access Journals (Sweden)

O. M. Lemine

2014-01-01

Full Text Available α-Fe2O3 nanocrystallines were prepared by direct transformation via high energy ball milling treatment for α-FeOOH powder. X-ray diffraction, Rietveld analysis, TEM, and vibrating sample magnetometer (VSM are used to characterize the samples obtained after several milling times. Phase identification using Rietveld analysis showed that the goethite is transformed to hematite nanocrystalline after 40 hours of milling. HRTEM confirm that the obtained phase is mostly a single-crystal structure. This result suggested that the mechanochemical reaction is an efficient way to prepare some iron oxides nanocrystallines from raw materials which are abundant in the nature. The mechanism of the formation of hematite is discussed in text.

Bismuth iron oxide thin films using atomic layer deposition of alternating bismuth oxide and iron oxide layers

Energy Technology Data Exchange (ETDEWEB)

Puttaswamy, Manjunath; Vehkamäki, Marko [University of Helsinki, Department of Chemistry, P.O. Box 55, FI-00014 Helsinki (Finland); Kukli, Kaupo, E-mail: kaupo.kukli@helsinki.fi [University of Helsinki, Department of Chemistry, P.O. Box 55, FI-00014 Helsinki (Finland); University of Tartu, Institute of Physics, W. Ostwald 1, EE-50411 Tartu (Estonia); Dimri, Mukesh Chandra [National Institute of Chemical Physics and Biophysics, Akadeemia tee 23, EE-12618 Tallinn (Estonia); Kemell, Marianna; Hatanpää, Timo; Heikkilä, Mikko J. [University of Helsinki, Department of Chemistry, P.O. Box 55, FI-00014 Helsinki (Finland); Mizohata, Kenichiro [University of Helsinki, Department of Physics, P.O. Box 64, FI-00014 Helsinki (Finland); Stern, Raivo [National Institute of Chemical Physics and Biophysics, Akadeemia tee 23, EE-12618 Tallinn (Estonia); Ritala, Mikko; Leskelä, Markku [University of Helsinki, Department of Chemistry, P.O. Box 55, FI-00014 Helsinki (Finland)

2016-07-29

Bismuth iron oxide films with varying contributions from Fe{sub 2}O{sub 3} or Bi{sub 2}O{sub 3} were prepared using atomic layer deposition. Bismuth (III) 2,3-dimethyl-2-butoxide, was used as the bismuth source, iron(III) tert-butoxide as the iron source and water vapor as the oxygen source. The films were deposited as stacks of alternate Bi{sub 2}O{sub 3} and Fe{sub 2}O{sub 3} layers. Films grown at 140 °C to the thickness of 200–220 nm were amorphous, but crystallized upon post-deposition annealing at 500 °C in nitrogen. Annealing of films with intermittent bismuth and iron oxide layers grown to different thicknesses influenced their surface morphology, crystal structure, composition, electrical and magnetic properties. Implications of multiferroic performance were recognized in the films with the remanent charge polarization varying from 1 to 5 μC/cm{sup 2} and magnetic coercivity varying from a few up to 8000 A/m. - Highlights: • Bismuth iron oxide thin films were grown by atomic layer deposition at 140 °C. • The major phase formed in the films upon annealing at 500 °C was BiFeO{sub 3}. • BiFeO{sub 3} films and films containing excess Bi favored electrical charge polarization. • Slight excess of iron oxide enhanced saturative magnetization behavior.

Efficient production of ultrapure manganese oxides via electrodeposition.

Science.gov (United States)

Cheney, Marcos A; Joo, Sang Woo; Banerjee, Arghya; Min, Bong-Ki

2012-08-01

A new process for the production of electrolytic amorphous nanomanganese oxides (EAMD) with uniform size and morphology is described. EAMD are produced for the first time by cathodic deposition from a basic aqueous solution of potassium permanganate at a constant temperature of 16°C. The synthesized materials are characterized by XRD, SEM, TEM, and HRTEM. The materials produced at 5.0 V at constant temperature are amorphous with homogeneous size and morphology with an average particle size around 20 nm, which appears to be much lesser than the previously reported anodic EAMD. A potentiostatic electrodeposition with much lesser deposition rate (with respect to previously reported anodic depositions) is considered to be the reason behind the very low and homogenous particle size distribution due to the lesser agglomeration of our as-synthesized nanoparticles. Copyright © 2012 Elsevier Inc. All rights reserved.

Protons in neutron-irradiated and thermochemically reduced MgO crystals doped with lithium impurities

International Nuclear Information System (INIS)

Gonzalez, R.; Pareja, R.; Chen, Y.

1992-01-01

H - (hydride) ions have been observed in lithium-doped MgO crystals which have been neutron irradiated or thermochemically reduced (TCR). Infrared-absorption measurements have been used to identify the local modes of the H - ions in these crystals. The concentration of the H - ions in the neutron-irradiated crystals is found to be far less than that found in the TCR crystals. The thermal stability of H - and oxygen vacancies in both oxidizing and reducing atmospheres are investigated. The emergence of sharp structures due to OH - ions is attributed to the displacements of substitutional Li + ions, leaving behind unperturbed OH - ions, via a mechanism of rapid radiation-induced diffusion during irradiation in a reactor. Results of neutron-irradiated MgO:Li, which had previously been oxidized at high temperature, are also presented

Hydrothermal-reduction synthesis of manganese oxide nanomaterials for electrochemical supercapacitors.

Science.gov (United States)

Zhang, Xiong; Chen, Yao; Yu, Peng; Ma, Yanwei

2010-11-01

In the present work, amorphous manganese oxide nanomaterials have been synthesized by a common hydrothermal method based on the redox reaction between MnO4(-) and Fe(2+) under an acidic condition. The synthesized MnO2 samples were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and electrochemical studies. XRD results showed that amorphous manganese oxide phase was obtained. XPS quantitative analysis revealed that the atomic ratio of Mn to Fe was 3.5 in the MnO2 samples. TEM images showed the porous structure of the samples. Electrochemical properties of the MnO2 electrodes were studied using cyclic voltammetry and galvanostatic charge-discharge cycling in 1 M Na2SO4 aqueous electrolyte, which showed excellent pseudocapacitance properties. A specific capacitance of 192 Fg(-1) at a current density of 0.5 Ag(-1) was obtained at the potential window from -0.1 to 0.9 V (vs. SCE).

Structure and catalytic reactivity of Rh oxides

DEFF Research Database (Denmark)

Gustafson, J.; Westerström, R.; Resta, A.

2009-01-01

Using a combination of experimental and theoretical techniques, we show that a thin RhO2 surface oxide film forms prior to the bulk Rh2O3 corundum oxide on all close-packed single crystal Rh surfaces. Based on previous reports, we argue that the RhO2 surface oxide also forms on vicinal Rh surface...

The resolution of acyclic P-stereogenic phosphine oxides via the formation of diastereomeric complexes: A case study on ethyl-(2-methylphenyl)-phenylphosphine oxide.

Science.gov (United States)

Bagi, Péter; Varga, Bence; Szilágyi, András; Karaghiosoff, Konstantin; Czugler, Mátyás; Fogassy, Elemér; Keglevich, György

2018-04-01

As an example of acyclic P-chiral phosphine oxides, the resolution of ethyl-(2-methylphenyl)-phenylphosphine oxide was elaborated with TADDOL derivatives, or with calcium salts of the tartaric acid derivatives. Besides the study on the resolving agents, several purification methods were developed in order to prepare enantiopure ethyl-(2-methylphenyl)-phenylphosphine oxide. It was found that the title phosphine oxide is a racemic crystal-forming compound, and the recrystallization of the enantiomeric mixtures could be used for the preparation of pure enantiomers. According to our best method, the (R)-ethyl-(2-methylphenyl)-phenylphosphine oxide could be obtained with an enantiomeric excess of 99% and in a yield of 47%. Complete racemization of the enantiomerically enriched phosphine oxide could be accomplished via the formation of a chlorophosphonium salt. Characterization of the crystal structures of the enantiopure phosphine oxide was complemented with that of the diastereomeric intermediate. X-ray analysis revealed the main nonbonding interactions responsible for enantiomeric recognition. © 2018 Wiley Periodicals, Inc.

The catalytic activity of several tungsten oxides for the oxidation of propene

International Nuclear Information System (INIS)

De Rossi, S.; Schiavello, M.; Rome Univ.; Iguchi, E.; Tilley, R.J.D.

1976-01-01

A study has been made of the catalytic oxidation of propene over the oxides WO 3 , WOsub(2,95), WOsub(2,90), WOsub(2,72) and Wo 2 , which were selected because they possess specific features of chemical and structural interest rather than for their catalytic ability. It was found that the oxides WOsub(2,95), WOsub(2,90) and WOsub(2,72) all selectively produce acrolein in small amounts. The oxides WO 3 and WO 2 were non-selective and rather inactive. The results are discussed in terms of a mechanism involving both variable valence in the crystal and the specific structural geometry of these compounds. (orig.) [de

The genesis of the newly discovered giant Wuben magmatic Fe-Ti oxide deposit in the Emeishan Large Igneous Province: a product of the late-stage redistribution and sorting of crystal slurries

Science.gov (United States)

Bai, Zhong-Jie; Zhong, Hong; Zhu, Wei-Guang; Hu, Wen-Jun; Chen, Cai-Jie

2018-04-01

A giant Fe-Ti oxide deposit hosted by the Wuben mafic intrusion has recently been discovered in the Pan-Xi area of the Emeishan Large Igneous Province (ELIP). The evolved compositions of the gangue minerals within the Fe-Ti oxide ores indicate that they formed during later stages of magma differentiation than those within the neighboring Panzhihua intrusion or other ore-bearing intrusions in this area. The rocks from the Wuben intrusion and MZb of the Panzhihua intrusion contain compositionally similar silicate minerals and have similar titanomagnetite/ilmenite ratios, suggesting that the former is related to and probably connected to the latter by subsurface magmatic conduits. This indicates that unconsolidated minerals that formed in the MZb flowed as crystal slurries into the Wuben magma chamber during the later stages of evolution of the parental magma. The later secondary enrichment of Fe-Ti oxides by mechanical redistribution and the sorting of crystals as a result of density and size differences generated the Wuben massive Fe-Ti oxide bodies. The ilmenite was commonly saturated in the magma at late stage of differentiation in the ELIP, thereby the associated deposit contains much higher contents of ilmenite. This indicates that future exploration for Fe-Ti oxide mineralization in the ELIP should not merely focus on the lower parts of large layered intrusions but should also include nearby relatively small intrusions or even the upper parts of large intrusions, especially as ilmenite-enriched Fe-Ti oxide deposits may have greater economic value than ilmenite-poor deposits.

Silica functionalized Cu(II) acetylacetonate Schiff base complex: An efficient catalyst for the oxidative condensation reaction of benzyl alcohol with amines

Science.gov (United States)

Anbarasu, G.; Malathy, M.; Karthikeyan, P.; Rajavel, R.

2017-09-01

Silica functionalized Cu(II) acetylacetonate Schiff base complex via the one pot reaction of silica functionalized 3-aminopropyltriethoxysilane with acetyl acetone and copper acetate has been reported. The synthesized material was well characterized by analytical techniques such as FT-IR, UV-DRS, XRD, SEM-EDX, HR-TEM, EPR, ICP-AES and BET analysis. The characterization results confirmed the grafting of Cu(II) Schiff base complex on the silica surface. The catalytic activity of synthesized silica functionalized Cu(II) acetylacetonate Schiff base complex was evaluated through the oxidative condensation reaction of benzyl alcohol to imine.

Au and Pd nanoparticles supported on CeO{sub 2}, TiO{sub 2}, and Mn{sub 2}O{sub 3} oxides

Energy Technology Data Exchange (ETDEWEB)

Nascente, P.A.P., E-mail: nascente@ufscar.br [Federal University of Sao Carlos, Department of Materials Engineering, Sao Carlos, SP (Brazil); Maluf, S.S.; Afonso, C.R.M. [Federal University of Sao Carlos, Department of Materials Engineering, Sao Carlos, SP (Brazil); Landers, R. [State University of Campinas, Institute of Physics, Department of Applied Physics, Campinas, SP (Brazil); Pinheiro, A.N.; Leite, E.R. [Federal University of Sao Carlos, Department of Chemistry, Sao Carlos, SP (Brazil)

2014-10-01

Highlights: • CeO{sub 2}, TiO{sub 2}, and Mn{sub 2}O{sub 3} supported Au and Pd nanoparticles. • Additions of 0.5 wt% of Au and Pd onto CeO{sub 2}, TiO{sub 2}, and Mn{sub 2}O{sub 3} supports. • Characterization by XRD, XPS, EDS, TEM, HRTEM, STEM, and EFTEM. - Abstract: Gold and palladium nanoparticles were incorporated on CeO{sub 2}, TiO{sub 2}, and Mn{sub 2}O{sub 3} supports prepared by a sol–gel method. The samples were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM), high resolution TEM (HRTEM), scanning TEM (STEM) in high angle annular dark field mode (HAADF), and energy filtered TEM (EFTEM) using electron energy loss spectroscopy (EELS). The XRD diffractograms presented sharp and intense peaks indicating that the samples are highly crystalline, but it did not detected any peak corresponding to Au or Pd phases. This indicates that the Au and Pd NPs were incorporated into the structures of the oxides. It was not possible to obtain an Au 4f spectrum for Au/Mn{sub 2}O{sub 3} due to an overlap with the Mn 3p spectrum. The XPS Au 4f spectra for Au/CeO{sub 2} and Au/TiO{sub 2} present negative chemical shifts that could be attributed to particle-size-related properties. The XPS Pd 3d spectra indicate that for both CeO{sub 2} and TiO{sub 2} substrates, the Pd NPs were in the metallic state, while for the Mn{sub 2}O{sub 3} substrate, the Pd NPs were oxidized. The HRTEM results show the formation of nanocrystalline oxides having particles sizes between 50 and 200 nm. TEM micrographs show that the addition of Au caused the formation of Au clusters in between the CeO{sub 2} NPS, formation of Au NPs for the TiO{sub 2} support, and homogeneous distribution of Au clusters for the Mn{sub 2}O{sub 3} support. The addition of Pd yielded a homogeneous dispersion throughout the CeO{sub 2} and TiO{sub 2}, but caused the formation of Pd clusters for the Mn{sub 2}O

Hydrogen Annealing Of Single-Crystal Superalloys

Science.gov (United States)

Smialek, James L.; Schaeffer, John C.; Murphy, Wendy

1995-01-01

Annealing at temperature equal to or greater than 2,200 degrees F in atmosphere of hydrogen found to increase ability of single-crystal superalloys to resist oxidation when subsequently exposed to oxidizing atmospheres at temperatures almost as high. Supperalloys in question are principal constituents of hot-stage airfoils (blades) in aircraft and ground-based turbine engines; also used in other high-temperature applications like chemical-processing plants, coal-gasification plants, petrochemical refineries, and boilers. Hydrogen anneal provides resistance to oxidation without decreasing fatigue strength and without need for coating or reactive sulfur-gettering constituents. In comparison with coating, hydrogen annealing costs less. Benefits extend to stainless steels, nickel/chromium, and nickel-base alloys, subject to same scale-adhesion and oxidation-resistance considerations, except that scale is chromia instead of alumina.

Stable narrow spacing dual-wavelength Q-switched graphene oxide embedded in a photonic crystal fiber

International Nuclear Information System (INIS)

Ahmad, H; Soltanian, M R K; Alimadad, M; Harun, S W

2014-01-01

An ultra-stable dual-wavelength saturable absorber based on a cladding-embedded commercial graphene oxide (GO) solution by capillary action in a solid core photonic crystal fiber (PCF) is demonstrated for the first time. The saturation absorption property is achieved through evanescent coupling between the guided light and the cladding-filled graphene layers. Stable spacing dual-wavelength fiber lasing is attained by controlling the polarization state of a simple 0.9 m long ring of highly doped Leikki Er80-8/125 erbium-doped fiber as the primary gain medium with PCF, polarization controller and tunable bandpass filter. Embedded GO is used to generate the desired pulsed output, and the laser is capable of generating pulses having a repetition rate of 24 kHz with an average output power and pulse energy of 0.167 mW and 8.98 nJ, respectively, at the maximum pump power of 220 mW. (paper)

Antimicrobial and antioxidant potentials of biosynthesized colloidal zinc oxide nanoparticles for a fortified cold cream formulation: A potent nanocosmeceutical application.

Science.gov (United States)

S, Sonia; H, Linda Jeeva Kumari; K, Ruckmani; M, Sivakumar

2017-10-01

Nanocosmeceuticals are promising applications of nanotechnology in personal care industries. Zinc oxide is an inorganic material that is non-toxic and skin compatible with self-cleansing and microbicidal properties. Herein, exploitation of colloidal zinc oxide nanoparticles (ZnONps) as potent biomaterial for a topical formulation of cosmetic and dermatological significance is employed. ZnONps were green synthesized using environmentally benign Adhatoda vasica leaf extract and characterized by UV-Vis absorption spectroscopy, Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), dynamic light scattering (DLS), high-resolution transmission electron microscopy (HR-TEM) and energy-dispersive X-ray spectroscopy (EDX). The results reveal that the biosynthesized ZnONps exhibit an absorption peak at 352nm. XRD and HR-TEM analyses confirm the hexagonal wurtzite structure of ZnONps with particle size of about 10nm to 12nm. Elemental analysis by EDX confirms the presence of zinc and oxygen. Zeta potential of -24.6mV affirms the stability of nanoparticles. The antibacterial and antifungal activities of biosynthesized ZnONps exhibit mean zone of inhibition from 08.667±0.282 to 21.666±0.447 (mm) and 09.000±0.177 to 19.000±0.307 (mm) respectively, in a dose-dependent manner. The IC 50 value exerted from the antioxidant activity of ZnONps is found to be 139.27μgmL -1 . ZnONps infused cold cream formulation of microbicidal and antioxidant properties was further tested against clinical skin pathogens. The nano-based cold cream exhibited significant inhibitory action against Candida sp., which showed resistance against a commercial antifungal cream (2%). Therefore, this study demonstrates the exploitation of ZnONps as promising colloidal drug carriers in cosmeceuticals that can significantly alleviate human skin infections and oxidative stress induced cellular damage. Copyright © 2017 Elsevier B.V. All rights reserved.

Ore-forming adakitic porphyry produced by fractional crystallization of oxidized basaltic magmas in a subcrustal chamber (Jiamate, East Junggar, NW China)

Science.gov (United States)

Hong, Tao; Xu, Xing-Wang; Gao, Jun; Peters, Stephen; Zhang, Di; Jielili, Reyaniguli; Xiang, Peng; Li, Hao; Wu, Chu; You, Jun; Liu, Jie; Ke, Qiang

2018-01-01

Adakitic intrusions are supposed to have a close genetic and spatial relationship to porphyry Cu deposits. However, the genesis of adakitic intrusions is still under dispute. Here, we describe newly discovered intrusive complex rocks, which are composed of ore-bearing, layered magnetite-bearing gabbroic and adakitic rocks in Jiamate, East Junggar, NW China. These Jiamate Complex intrusions have diagnostic petrologic, geochronologic and geochemical signatures that indicate they were all generated from the same oxidized precursor magma source. Additionally, these layered rocks underwent the same fractional crystallization process as the ore-bearing adakitic rocks in the adjacent Kalaxiangar Porphyry Cu Belt (KPCB) in an oceanic island arc (OIA) setting. The rocks studied for this paper include layered magnetite-bearing gabbroic intrusive rocks that contain: (1) gradual contact changes between lithological units of mafic and intermediate rocks, (2) geochemical signatures that are the same as those found in oceanic island arc (OIA) rocks, (3) typical adakitic geochemistry, and (4) similar characteristics and apparent fractional crystallization relationships of ultra-basic to basic rocks to those in the nearby Beitashan Formation and to ore-bearing adakitic rocks in the KPCB. They also display similar zircon U-Pb and zircon Hf model ages.The Jiamate Complex intrusions contain intergrowths of magnetite and layered gabbro, and the intermediate-acidic intrusions of the Complex display typical adakitic affinities. Moreover, in conjunction with previously published geochronological and geochemistry data of the mafic rocks in the Beitashan Formation and in the KPCB area, additional data generated for the Jiamate Complex intrusions rocks indicate that they were formed from fractional crystallization processes. The Jiamate Complex intrusions most likely were derived from a metasomatized mantle wedge that was underplated at the root of the Saur oceanic island arc (Saur OIA). The

Ore-forming adakitic porphyry produced by fractional crystallization of oxidized basaltic magmas in a subcrustal chamber (Jiamate, East Junggar, NW China)

Science.gov (United States)

Hong, Tao; Xu, Xing-Wang; Gao, Jun; Peters, Stephen G.; Zhang, Di; Jielili, Reyaniguli; Xiang, Peng; Li, Hao; Wu, Chu; You, Jun; Liu, Jie; Ke, Qiang

2018-01-01

Adakitic intrusions are supposed to have a close genetic and spatial relationship to porphyry Cu deposits. However, the genesis of adakitic intrusions is still under dispute. Here, we describe newly discovered intrusive complex rocks, which are composed of ore-bearing, layered magnetite-bearing gabbroic and adakitic rocks in Jiamate, East Junggar, NW China. These Jiamate Complex intrusions have diagnostic petrologic, geochronologic and geochemical signatures that indicate they were all generated from the same oxidized precursor magma source. Additionally, these layered rocks underwent the same fractional crystallization process as the ore-bearing adakitic rocks in the adjacent Kalaxiangar Porphyry Cu Belt (KPCB) in an oceanic island arc (OIA) setting. The rocks studied for this paper include layered magnetite-bearing gabbroic intrusive rocks that contain: (1) gradual contact changes between lithological units of mafic and intermediate rocks, (2) geochemical signatures that are the same as those found in oceanic island arc (OIA) rocks, (3) typical adakitic geochemistry, and (4) similar characteristics and apparent fractional crystallization relationships of ultra-basic to basic rocks to those in the nearby Beitashan Formation and to ore-bearing adakitic rocks in the KPCB. They also display similar zircon U-Pb and zircon Hf model ages. The Jiamate Complex intrusions contain intergrowths of magnetite and layered gabbro, and the intermediate-acidic intrusions of the Complex display typical adakitic affinities. Moreover, in conjunction with previously published geochronological and geochemistry data of the mafic rocks in the Beitashan Formation and in the KPCB area, additional data generated for the Jiamate Complex intrusions rocks indicate that they were formed from fractional crystallization processes. The Jiamate Complex intrusions most likely were derived from a metasomatized mantle wedge that was underplated at the root of the Saur oceanic island arc (Saur OIA

Non-isothermal cold crystallization kinetics of poly(3-hydoxybutyrate) filled with zinc oxide

Energy Technology Data Exchange (ETDEWEB)

Ries, Andreas, E-mail: ries750@yahoo.com.br [Electrical Engineering Department, Federal University of Paraíba, João Pessoa, PB 58051-900 (Brazil); Canedo, Eduardo L. [Materials Engineering Department, Federal University of Campina Grande, Campina Grande, PB 58429-900 (Brazil); Souto, Cícero R. [Electrical Engineering Department, Federal University of Paraíba, João Pessoa, PB 58051-900 (Brazil); Wellen, Renate M.R. [Materials Engineering Department, Federal University of Paraíba, João Pessoa, PB 58051-900 (Brazil)

2016-08-10

Highlights: • Non-isothermal cold crystallization kinetics of PHB filled with ZnO is presented. • Pseudo-Avrami model is best for describing an individual crystallization condition. • Mo model is allows to judge the kinetics of a condition untested in this work. • ZnO affects the kinetics irregularly. - Abstract: The non-isothermal cold crystallization kinetics of poly(3-hydroxybutyrate) (PHB) and PHB-ZnO composites, with ZnO content of 1%, 5% and 10% per weight, was investigated at different heating rates (5, 7.5, 10, 15, 20 and 30 °C/min) using differential scanning calorimetry. Both, Kissinger and Friedman activation energies predict correctly the slowest and fastest crystallizing composition. It was further found, that ZnO can neither be classified as a crystallization accelerator, nor as a crystallization inhibitor; its action is strongly concentration dependent. The empirical Pseudo-Avrami model has the best overall capability for fitting the experimental kinetic data. However, since the Pseudo-Avrami exponent was found to vary irregularly with heating rate and filler content, this model should not be applied for kinetic predictions of an arbitrary composition or an untested heating rate. In such cases, Mo's model should be used.

Iron-sulfide crystals in probe deposits

DEFF Research Database (Denmark)

Laursen, Karin; Frandsen, Flemming

1998-01-01

Iron-sulfides were observed in deposits collected on a probe inserted at the top of the furnace of a coal-fired power station in Denmark. The chemical composition of the iron-sulfides is equivalent to pyrrhotite (FeS). The pyrrhotites are present as crystals and, based on the shape of the crystals......: (1) impact of low viscous droplets of iron sulfide; and (2) sulfur diffusion. Previous research on the influence of pyrite on slagging focused on the decomposition of pyrite into pyrrhotite and especially on the oxidation stage of this product during impact on the heat transfer surfaces...

Surface chemistry on interstellar oxide grains

International Nuclear Information System (INIS)

Denison, P.; Williams, D.A.

1981-01-01

Detailed calculations are made to test the predictions of Duley, Millar and Williams (1978) concerning the chemical reactivity of interstellar oxide grains. A method is established for calculating interaction energies between atoms and the perfect crystal with or without surface vacancy sites. The possibility of reactions between incident atoms and absorbed atoms is investigated. It is concluded that H 2 formation can occur on the perfect crystal surfaces, and that for other diatomic molecules the important formation sites are the Fsub(s)- and V 2- sub(s)-centres. The outline by Duley, Millar and Williams (1979) of interstellar oxide grain growth and destruction is justified by these calculations. (author)

Ultrasmall-angle X-ray scattering analysis of photonic crystal structure

International Nuclear Information System (INIS)

Abramova, V. V.; Sinitskii, A. S.; Grigor'eva, N. A.; Grigor'ev, S. V.; Belov, D. V.; Petukhov, A. V.; Mistonov, A. A.; Vasil'eva, A. V.; Tret'yakov, Yu. D.

2009-01-01

The results of an ultrasmall-angle X-ray scattering study of iron(III) oxide inverse opal thin films are presented. The photonic crystals examined are shown to have fcc structure with amount of stacking faults varying among the samples. The method used in this study makes it possible to easily distinguish between samples with predominantly twinned fcc structure and nearly perfect fcc stacking. The difference observed between samples fabricated under identical conditions is attributed to random layer stacking in the self-assembled colloidal crystals used as templates for fabricating the inverse opals. The present method provides a versatile tool for analyzing photonic crystal structure in studies of inverse opals made of various materials, colloidal crystals, and three-dimensional photonic crystals of other types.

Single-crystal growth of ceria-based materials

International Nuclear Information System (INIS)

Ulbrich, Gregor

2015-01-01

In this work it could be shown that Skull-Melting is a suitable method for growing ceria single crystals. Twenty different ceria-based single crystals could be manufactured. It was possible to dope ceria single crystals with Gd, Sm, Y, Zr, Ti, Ta, and Pr in different concentrations. Also co-doping with the named metals was realized. However, there remain some problems for growing ceria-based single crystals by Skull-Melting. As ignition metal zirconium was used because no ceria-based material works well. For that reason all single crystals show small zirconium contamination. Another problem is the formation of oxygen by the heat-induced reduction of ceria during the melting process. Because of that the skull of sintered material is often destroyed by gas pressure. This problem had to be solved individually for every single crystal. The obtained single crystals were characterized using different methods. To ensure the single crystal character the y were examined by Laue diffraction. All manufactured crystals are single crystals. Also powder diffraction patterns of the milled and oxidized samples were measured. For the determination of symmetry and metric the structural parameters were analyzed by the Rietveld method. All synthesized materials crystallize in space group Fm-3m known from calcium fluoride. The cubic lattice parameter a was determined for all crystals. In the case of series with different cerium and zirconium concentrations a linear correlation between cerium content and cubic lattice parameter was detected. The elemental composition was determined by WDX. All crystals show a homogeneous elemental distribution. The oxygen content was calculated because the WDX method isn't useful for determination.

Mechanism of spark generation from Japanese toy firework (senko-hanabi). ; Structural-Oxidizing reaction of micro graphite crystals in molten K sub 2 Sn. Senko hanabi no jikkenteki kosatsu. ; Yoyu K sub 2 Sn chu no sekiboku bikessho no kozo teki sanka hanno

Energy Technology Data Exchange (ETDEWEB)

Ito, H. (The University, of Tokyo, Tokyo (Japan))

1991-12-20

Considerations were given on the spark generating mechanism of graphite particles in molten salt polysulfide through experiments on Japanese sparklers. The firework composition mixed consisted of two kinds: KNO{sub 3}, S, amorphous carbons, charcoal and lamp black, and K{sub 2}CO{sub 3}, S, charcoal and lamp black. The main constituent in fire balls is molten salt polysulfide. The O{sub 2} generated from combustion oxidizes C and S, whereas the generated K{sub 2}CO{sub 3} reacts with S to produce K{sub 2}Sn. In the KNO{sub 3} system, the calorific power reaches the maximum with lamp black contained at 10-15%. This is thought because the K{sup +} expands the space between the graphite crystal layers making the oxidation to take place more easily into their inner sides. On the one hand, the calorific power reduced with the lamp black at more than 16% would be because the lamp black clogging the crystalline spaces restricting the oxidation. It is thought that condensation and decomposition of micro graphite crystals occur simultaneously in the fire balls. It is also believed that the micro graphite crystals jumped out as a result of gas pressure from inside the crystals generated with the progress of oxidation break off at once because of the resistance of air together with the effect of the K{sup +} in the salt polysulfide (mutual separation of each layer). 9 refs., 6 figs., 1 tab.

Crystallization and preliminary X-ray crystallographic analysis of a new crystal form of hydroxylamine oxidoreductase from Nitrosomonas europaea

International Nuclear Information System (INIS)

Cedervall, Peder E.; Hooper, Alan B.; Wilmot, Carrie M.

2009-01-01

A new crystal form of N. europaea hydroxylamine oxidoreductase (space group P2 1 2 1 2) diffracted to 2.25 Å resolution at a third-generation synchrotron X-ray source. Hydroxylamine oxidoreductase (HAO) from Nitrosomonas europaea is a homotrimeric protein that catalyzes the oxidation of hydroxylamine to nitrite. Each monomer, with a molecular weight of 67.1 kDa, contains seven c-type hemes and one heme P460, the porphyrin ring of which is covalently linked to a tyrosine residue from an adjacent subunit. HAO was first crystallized and structurally characterized at a resolution of 2.8 Å in 1997. The structure was solved in space group P6 3 and suffered from merohedral twinning. Here, a crystallization procedure is presented that yielded untwinned crystals belonging to space group P2 1 2 1 2, which diffracted to 2.25 Å resolution and contained one trimer in the asymmetric unit. The unit-cell parameters were a = 140.7, b = 142.6, c = 107.4 Å

Mucin 4 Gene Silencing Reduces Oxidative Stress and Calcium Oxalate Crystal Formation in Renal Tubular Epithelial Cells Through the Extracellular Signal-Regulated Kinase Signaling Pathway in Nephrolithiasis Rat Model

Directory of Open Access Journals (Sweden)

Ling Sun

2018-05-01

Full Text Available Background/Aims: Nephrolithiasis plagues a great number of patients all over the world. Increasing evidence shows that the extracellular signal-regulated kinase (ERK signaling pathway and renal tubular epithelial cell (RTEC dysfunction and attrition are central to the pathogenesis of kidney diseases. Mucin 4 (MUC4 is reported as an activator of ERK signaling pathway in epithelial cells. In this study, using rat models of calcium oxalate (CaOx nephrolithiasis, the present study aims to define the roles of MUC4 and ERK signaling pathway as contributors to oxidative stress and CaOx crystal formation in RTEC. Methods: Data sets of nephrolithiasis were searched using GEO database and a heat flow map was drawn. Then MUC4 function was predicted. Wistar rats were prepared for the purpose of model establishment of ethylene glycol and ammonium chloride induced CaOx nephrolithiasis. In order to assess the detailed regulatory mechanism of MUC4 silencing on the ERK signaling pathway and RTEC, we used recombinant plasmid to downregulate MUC4 expression in Wistar rat-based models. Samples from rat urine, serum and kidney tissues were reviewed to identify oxalic acid and calcium contents, BUN, Cr, Ca2+ and P3+ levels, calcium crystal formation in renal tubules and MUC4 positive expression rate. Finally, RT-qPCR, Western blot analysis, and ELISA were employed to access oxidative stress state and CaOx crystal formation in RTEC. Results: Initially, MUC4 was found to have an influence on the process of nephrolithiasis. MUC4 was upregulated in the CaOx nephrolithiasis model rats. We proved that the silencing of MUC4 triggered the inactivation of ERK signaling pathway. Following the silencing of MUC4 or the inhibition of ERK signaling pathway, the oxalic acid and calcium contents in rat urine, BUN, Cr, Ca2+ and P3+ levels in rat serum, p-ERK1/2, MCP-1 and OPN expressions in RTEC and H2O2 and MDA levels in the cultured supernatant were downregulated, but the GSH

Ni–Ta–O mixed oxide catalysts for the low temperature oxidative dehydrogenation of ethane to ethylene

KAUST Repository

Zhu, Haibo

2015-09-01

The "wet" sol-gel and "dry" solid-state methods were used to prepare Ni-Ta-O mixed oxide catalysts. The resulting Ni-Ta oxides exhibit high activity and selectivity for the low temperature oxidative dehydrogenation of ethane to ethylene. The Ta/(Ni + Ta) atomic ratios (varying from 0 to 0.11 in "wet" sol-gel method, and from 0 to 0.20 in "dry" solid-state method) as well as the preparation methods used in the synthesis, play important roles in controlling catalyst structure, activity, selectivity and stability in the oxidative dehydrogenation of ethane. Electron microscopy characterizations (TEM, EELS mapping, and HAADF-STEM) clearly demonstrate that the Ta atoms are inserted into NiO crystal lattice, resulting in the formation of a new Ni-Ta oxide solid solution. More Ta atoms are found to be located at the lattice sites of crystal surface in sol-gel catalyst. While, a small amount of thin layer of Ta2O5 clusters are detected in solid-state catalyst. Further characterization by XRD, N2 adsorption, SEM, H2-TPR, XPS, and Raman techniques reveal different properties of these two Ni-Ta oxides. Due to the different properties of the Ni-Ta oxide catalysts prepared by two distinct approaches, they exhibit different catalytic behaviors in the ethane oxidative dehydrogenation reaction at low temperature. Thus, the catalytic performance of Ni-Ta-O mixed oxide catalysts can be systematically modified and tuned by selecting a suitable synthesis method, and then varying the Ta content. ©2015 Elsevier Inc. All rights reserved.

Crystal growth and optical properties of Gd admixed Ce-doped Lu.sub.2./sub.Si.sub.2./sub.O.sub.7./sub. single crystals

Czech Academy of Sciences Publication Activity Database

Horiai, T.; Kurosawa, S.; Murakami, R.; Yamaji, A.; Shoji, Y.; Ohashi, Y.; Pejchal, Jan; Kamada, K.; Yokota, Y.; Yoshikawa, A.

2017-01-01

Roč. 468, Jun (2017), s. 391-394 ISSN 0022-0248 Grant - others:AV ČR(CZ) JSPS-17-18 Program:Bilaterální spolupráce Institutional support: RVO:68378271 Keywords : growth from melt * seed crystals * single crystal growth * oxides * scintillator materials Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 1.751, year: 2016

Interface and oxide traps in high-κ hafnium oxide films

International Nuclear Information System (INIS)

Wong, H.; Zhan, N.; Ng, K.L.; Poon, M.C.; Kok, C.W.

2004-01-01

The origins of the interface trap generation and the effects of thermal annealing on the interface and bulk trap distributions are studied in detail. We found that oxidation of the HfO 2 /Si interface, removal of deep trap centers, and crystallization of the as-deposited film will take place during the post-deposition annealing (PDA). These processes will result in the removal of interface traps and deep oxide traps and introduce a large amount of shallow oxide traps at the grain boundaries of the polycrystalline film. Thus, trade-off has to be made in considering the interface trap density and oxide trap density when conducting PDA. In addition, the high interface trap and oxide trap densities of the HfO 2 films suggest that we may have to use the SiO 2 /HfO 2 stack or hafnium silicate structure for better device performance

Facile Synthesis of Copper Oxide Nanoparticles via Electrospinning

Directory of Open Access Journals (Sweden)

Abdullah Khalil

2014-01-01

Full Text Available A novel approach for synthesizing copper oxide (CuO nanoparticles (NPs through electrospinning is reported. The approach is based on producing rough and discontinuous electrospun nanofibers from a precursor based on copper acetate salt and polyvinyl alcohol (PVA polymer. Selectively removing the polymeric phase from the fibers produced highly rough CuO nanofibers, which were composed of NPs that are weakly held together in a one-dimensional (1D manner. Sonication in a suitable liquid under controlled conditions completely disintegrated the nanofibers into NPs, resulting in the formation of uniform CuO NPs suspension. Aberration corrected high resolution transmission electron microscope (HRTEM showed that the obtained NPs are highly crystalline and nearly sphere-like with a diameter of 30 to 70 nm. Thus, electrospinning, which is a low cost and industrially scalable technique, can also be employed for economic and large scale synthesis of NPs.

High mobility In{sub 2}O{sub 3}:H transparent conductive oxides prepared by atomic layer deposition and solid phase crystallization

Energy Technology Data Exchange (ETDEWEB)

Macco, B.; Wu, Y.; Vanhemel, D. [Department of Applied Physics, Eindhoven University of Technology (Netherlands); Kessels, W.M.M. [Department of Applied Physics, Eindhoven University of Technology (Netherlands); Solliance Solar Research, Eindhoven (Netherlands)

2014-12-01

The preparation of high-quality In{sub 2}O{sub 3}:H, as transparent conductive oxide (TCO), is demonstrated at low temperatures. Amorphous In{sub 2}O{sub 3}:H films were deposited by atomic layer deposition at 100 C, after which they underwent solid phase crystallization by a short anneal at 200 C. TEM analysis has shown that this approach can yield films with a lateral grain size of a few hundred nm, resulting in electron mobility values as high as 138 cm{sup 2}/V s at a device-relevant carrier density of 1.8 x 10{sup 20} cm{sup -3}. Due to the extremely high electron mobility, the crystallized films simultaneously exhibit a very low resistivity (0.27 mΩ cm) and a negligible free carrier absorption. In conjunction with the low temperature processing, this renders these films ideal candidates for front TCO layers in for example silicon heterojunction solar cells and other sensitive optoelectronic applications. (copyright 2014 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

Crystallization and diffraction analysis of thioredoxin reductase from Streptomyces coelicolor

International Nuclear Information System (INIS)

Koháryová, Michaela; Brynda, Jiří; Řezáčová, Pavlína; Kollárová, Marta

2011-01-01

Thioredoxin reductase from S. coelicolor was crystallized and diffraction data were collected to 2.4 Å resolution. Thioredoxin reductases are homodimeric flavoenzymes that catalyze the transfer of electrons from NADPH to oxidized thioredoxin substrate. Bacterial thioredoxin reductases represent a promising target for the development of new antibiotics. Recombinant thioredoxin reductase TrxB from Streptomyces coelicolor was crystallized using the hanging-drop vapour-diffusion method. X-ray diffraction data were collected from cryocooled crystals to 2.4 Å resolution using a synchrotron-radiation source. The crystals belonged to the primitive monoclinic space group P2 1 , with unit-cell parameters a = 82.9, b = 60.6, c = 135.4 Å, α = γ = 90.0, β = 96.5°

Probing and tuning the size, morphology, chemistry and structure of nanoscale cerium oxide

Science.gov (United States)

Kuchibhatla, Satyanarayana Vnt

Cerium oxide (ceria)-based materials in the nanoscale regime are of significant fundamental and technological interest. Nanoceria in pure and doped forms has current and potential use in solid oxide fuel cells, catalysis, UV-screening, chemical mechanical planarization, oxygen sensors, and bio-medical applications. The characteristic feature of Ce to switch between the +3 and +4 oxidation states renders oxygen buffering capability to ceria. The ease of this transformation was expected to be enhanced in the nanoceria. In most the practical scenarios, it is necessary to have a stable suspension of ceria nanoparticles (CNPs) over longer periods of time. However, the existing literature is confined to short term studies pertaining to synthesis and property evaluation. Having understood the need for a comprehensive understanding of the CNP suspensions, this dissertation is primarily aimed at understanding the behavior of CNPs in various chemical and physical environments. We have synthesized CNPs in the absence of any surfactants at room temperature and studied the aging characteristics. After gaining some understanding about the behavior of this functional oxide, the synthesis environment and aging temperature were varied, and their affects were carefully analyzed using various materials analysis techniques such as high resolution transmission electron microscopy (HRTEM), UV-Visible spectroscopy (UV-Vis), and X-ray photoelectron spectroscopy (XPS). When the CNPs were aged at room temperature in as-synthesized condition, they were observed to spontaneously assemble and evolve as fractal superoctahedral structures. The reasons for this unique polycrystalline morphology were attributed to the symmetry driven assembly of the individual truncated octahedral and octahedral seed of the ceria. HRTEM and Fast Fourier Transform (FFT) analyses were used to explain the agglomeration behavior and evolution of the octahedral morphology. Some of the observations were supported by

Switchable Photonic Crystals Using One-Dimensional Confined Liquid Crystals for Photonic Device Application.

Science.gov (United States)

Ryu, Seong Ho; Gim, Min-Jun; Lee, Wonsuk; Choi, Suk-Won; Yoon, Dong Ki

2017-01-25

Photonic crystals (PCs) have recently attracted considerable attention, with much effort devoted to photonic bandgap (PBG) control for varying the reflected color. Here, fabrication of a modulated one-dimensional (1D) anodic aluminum oxide (AAO) PC with a periodic porous structure is reported. The PBG of the fabricated PC can be reversibly changed by switching the ultraviolet (UV) light on/off. The AAO nanopores contain a mixture of photoresponsive liquid crystals (LCs) with irradiation-activated cis/trans photoisomerizable azobenzene. The resultant mixture of LCs in the porous AAO film exhibits a reversible PBG, depending on the cis/trans configuration of azobenzene molecules. The PBG switching is reliable over many cycles, suggesting that the fabricated device can be used in optical and photonic applications such as light modulators, smart windows, and sensors.

Gentamicin coated iron oxide nanoparticles as novel antibacterial agents

Science.gov (United States)

Bhattacharya, Proma; Neogi, Sudarsan

2017-09-01

Applications of different types of magnetic nanoparticles for biomedical purposes started a long time back. The concept of surface functionalization of the iron oxide nanoparticles with antibiotics is a novel technique which paves the path for further application of these nanoparticles by virtue of their property of superparamagnetism. In this paper, we have synthesized novel iron oxide nanoparticles surface functionalized with Gentamicin. The average size of the particles, concluded from the HR-TEM images, came to be around 14 nm and 10 nm for unmodified and modified nanoparticles, respectively. The magnetization curve M(H) obtained for these nanoparticles are typical of superparamagnetic nature and having almost zero values of coercivity and remanance. The release properties of the drug coated nanoparticles were studied; obtaining an S shaped profile, indicating the initial burst effect followed by gradual sustained release. In vitro investigations against various gram positive and gram negative strains viz Staphylococcus aureus, Escherichia coli, Pseudomonas aeruginosa and Bacillus subtilis indicated significant antibacterial efficiency of the drug-nanoparticle conjugate. The MIC values indicated that a small amount like 0.2 mg ml-1 of drug capped particles induce about 98% bacterial death. The novelty of the work lies in the drug capping of the nanoparticles, which retains the superparamagnetic nature of the iron oxide nanoparticles and the medical properties of the drug simultaneously, which is found to extremely blood compatible.

Biological water-oxidizing complex: a nano-sized manganese-calcium oxide in a protein environment.

Science.gov (United States)

Najafpour, Mohammad Mahdi; Moghaddam, Atefeh Nemati; Yang, Young Nam; Aro, Eva-Mari; Carpentier, Robert; Eaton-Rye, Julian J; Lee, Choon-Hwan; Allakhverdiev, Suleyman I

2012-10-01

The resolution of Photosystem II (PS II) crystals has been improved using isolated PS II from the thermophilic cyanobacterium Thermosynechococcus vulcanus. The new 1.9 Å resolution data have provided detailed information on the structure of the water-oxidizing complex (Umena et al. Nature 473: 55-61, 2011). The atomic level structure of the manganese-calcium cluster is important for understanding the mechanism of water oxidation and to design an efficient catalyst for water oxidation in artificial photosynthetic systems. Here, we have briefly reviewed our knowledge of the structure and function of the cluster.

Revisiting the relevance of using a constant voltage step to improve electrochemical performances of Li-rich lamellar oxides

Science.gov (United States)

Pradon, A.; Caldes, M. T.; Petit, P.-E.; La Fontaine, C.; Elkaim, E.; Tessier, C.; Ouvrard, G.; Dumont, E.

2018-03-01

A Li-rich lamellar oxide was cycled at high potential and the relevance of using a constant voltage step (CVS) at the end of the charge, needed for industrial application, was investigated by electrochemical performance, X-ray diffraction (XRD) and high resolution transmission electron microscopy (HRTEM). Electrochemical studies at 4.7 and 4.5 V with and without CVS showed that capacity and voltage fading occurred mostly when cells operated at high potential. After cycling, 3D-type defects involving transition metals trapped in lithium layer were observed by HRTEM into the electrode bulk. These defects are responsible for the voltage fading. XRD microstrain parameter was used to evaluate defects rate in aged materials subjected to a CVS, showing more 3D-type defects when cycled at 4.7 V than at 4.5 V. The time spent at high potential at the end of the charge as well as the value of the upper potential limit, are both relevant parameters to voltage decay. The use of a CVS at the end of the charge needs at the same time, a reduced upper potential window in order to minimize 3D-type defects occurrence. Unfortunately, this approach is still not sufficient to prevent voltage fading.

Direct observations of the MOF (UiO-66) structure by transmission electron microscopy

KAUST Repository

Zhu, Liangkui; Zhang, Daliang; Xue, Ming; Li, Huan; Qiu, Shilun

2013-01-01

As a demonstration of ab initio structure characterizations of nano metal organic framework (MOF) crystals by high resolution transmission electron microscopy (HRTEM) and electron diffraction tomography methods, a Zr-MOF (UiO-66) structure

Crystal structure and ionic conduction path of solid electrolytic materials by high temperature neutron diffraction method

International Nuclear Information System (INIS)

Yashima, Masatomo; Nomura, Katsuhiro

2005-01-01

Research of the distribution of oxide ions and the ionic conduction path of bismuth oxide (Bi 2 O 3 ), cerium oxide (CeO 2 ) and lanthanum gallate ((La 0.8 Sr 0.2 )(Ga 0.8 Mg 0.15 Co 0.05 )O 3-δ ) is stated. The high temperature neutron diffraction method, analytical method such as Rietveld method, crystal structure analysis of ionic conductor and MEM (Maximum- Entropy Method) are explained. The nuclear density distribution of oxide ions in bismuth oxide showed so larger distribution in the direction of and than Bi ions that the oxide ions conducted these direction in the crystal. The nuclear density distribution of oxide ions of cerium oxide indicated larger distribution in the direction of than Ce ions and its tendency was remarkable at high temperature. Accordingly, the oxide ions conducted in the direction of and . The oxide ions distribution in lanthanum gallate compound was larger and complicated than positive ions. The oxide ions conducted to by describing an arc between the two stable positions. The nuclear density on the conduction path increased with increasing temperature. This above result corresponded to increase of oxide ion conductivity in the area. (S.Y.)

Coloration of chromium-doped yttrium aluminum garnet single-crystal fibers using a divalent codopant

International Nuclear Information System (INIS)

Tissue, B.M.; Jia, W.; Lu, L.; Yen, W.M.

1991-01-01

We have grown single-crystal fibers of Cr:YAG and Cr,Ca:YAG under oxidizing and reducing conditions by the laser-heated-pedestal-growth method. The Cr:YAG crystals were light green due to Cr 3+ in octahedral sites, while the Cr,Ca:YAG crystals were brown. The presence of the divalent codopant was the dominant factor determining the coloration in these single-crystal fibers, while the oxidizing power of the growth atmosphere had little effect on the coloration. The Cr,Ca:YAG had a broad absorption band centered at 1.03 μm and fluoresced from 1.1 to 1.7 μm, with a room-temperature lifetime of 3.5 μs. The presence of both chromium and a divalent codopant were necessary to create the optically-active center which produces the near-infrared emission. Doping with only Ca 2+ created a different coloration with absorption in the blue and ultraviolet. The coloration in the Cr,Ca:YAG is attributed to Cr 4+ and is produced in as-grown crystals without irradiation or annealing, as has been necessary in previous work

Design of Higher-k and More Stable Rare Earth Oxides as Gate Dielectrics for Advanced CMOS Devices

Directory of Open Access Journals (Sweden)

Yi Zhao

2012-08-01

Full Text Available High permittivity (k gate dielectric films are widely studied to substitute SiO₂ as gate oxides to suppress the unacceptable gate leakage current when the traditional SiO₂ gate oxide becomes ultrathin. For high-k gate oxides, several material properties are dominantly important. The first one, undoubtedly, is permittivity. It has been well studied by many groups in terms of how to obtain a higher permittivity for popular high-k oxides, like HfO₂ and La₂O₃. The second one is crystallization behavior. Although it’s still under the debate whether an amorphous film is definitely better than ploy-crystallized oxide film as a gate oxide upon considering the crystal boundaries induced leakage current, the crystallization behavior should be well understood for a high-k gate oxide because it could also, to some degree, determine the permittivity of the high-k oxide. Finally, some high-k gate oxides, especially rare earth oxides (like La₂O₃, are not stable in air and very hygroscopic, forming hydroxide. This topic has been well investigated in over the years and significant progresses have been achieved. In this paper, I will intensively review the most recent progresses of the experimental and theoretical studies for preparing higher-k and more stable, in terms of hygroscopic tolerance and crystallization behavior, Hf- and La-based ternary high-k gate oxides.

Size modulation of nanocrystalline silicon embedded in amorphous silicon oxide by Cat-CVD

International Nuclear Information System (INIS)

Matsumoto, Y.; Godavarthi, S.; Ortega, M.; Sanchez, V.; Velumani, S.; Mallick, P.S.

2011-01-01

Different issues related to controlling size of nanocrystalline silicon (nc-Si) embedded in hydrogenated amorphous silicon oxide (a-SiO x :H) deposited by catalytic chemical vapor deposition (Cat-CVD) have been reported. Films were deposited using tantalum (Ta) and tungsten (W) filaments and it is observed that films deposited using tantalum filament resulted in good control on the properties. The parameters which can affect the size of nc-Si domains have been studied which include hydrogen flow rate, catalyst and substrate temperatures. The deposited samples are characterized by X-ray diffraction, HRTEM and micro-Raman spectroscopy, for determining the size of the deposited nc-Si. The crystallite formation starts for Ta-catalyst around the temperature of 1700 o C.

Sequential crystallization and morphology of triple crystalline biodegradable PEO-b-PCL-b-PLLA triblock terpolymers

KAUST Repository

Palacios, Jordana; Mugica, Agurtzane; Zubitur, Manuela; Iturrospe, Amaia; Arbe, A.; Liu, Guoming; Wang, Dujin; Zhao, Junpeng; Hadjichristidis, Nikolaos; Muller, Alejandro

2016-01-01

The sequential crystallization of poly(ethylene oxide)-b-poly(e-caprolactone)-b-poly(L-lactide) (PEO-b-PCL-b-PLLA) triblock terpolymers, in which the three blocks are able to crystallize separately and sequentially from the melt, is presented. Two

Studies on the optoelectronic properties of the thermally evaporated tin-doped indium oxide nanostructures

Energy Technology Data Exchange (ETDEWEB)

Pan, Ko-Ying [Department of Materials Science and Engineering, National Tsing Hua University, Hsinchu 300, Taiwan, ROC (China); Lin, Liang-Da [Institute of Materials Science and Nanotechnology, Chinese Culture University, Taipei 111, Taiwan, ROC (China); Chang, Li-Wei [Department of Materials Science and Engineering, National Tsing Hua University, Hsinchu 300, Taiwan, ROC (China); Shih, Han C., E-mail: hcshih@mx.nthu.edu.tw [Department of Materials Science and Engineering, National Tsing Hua University, Hsinchu 300, Taiwan, ROC (China); Institute of Materials Science and Nanotechnology, Chinese Culture University, Taipei 111, Taiwan, ROC (China)

2013-05-15

Indium oxide (In{sub 2}O{sub 3}) nanorods, nanotowers and tin-doped (Sn:In = 1:100) indium oxide (ITO) nanorods have been fabricated by thermal evaporation. The morphology, microstructure and chemical composition of these three nanoproducts are characterized by FE-SEM, HRTEM and XPS. To further investigate the optoelectronic properties, the I–V curves and cathodoluminescence (CL) spectra are measured. The electrical resistivity of In{sub 2}O{sub 3} nanorods, nanotowers and ITO nanorods are 1.32 kΩ, 0.65 kΩ and 0.063 kΩ, respectively. CL spectra of these three nanoproducts clearly indicate that tin-doped (Sn:In = 1:100) indium oxide (ITO) nanorods cause a blue shift. No doubt ITO nanorods obtain the highest performance among these three nanoproducts, and this also means that Sn-doped In{sub 2}O{sub 3} nanostructures would be the best way to enhance the optoelectronic properties. Additionally, the growing mechanism and the optoelectronic properties of these three nanostructures are discussed. This study is beneficial to the applications of In{sub 2}O{sub 3} nanorods, nanotowers and ITO nanorods in optoelectronic nanodevices.

Development of hierarchically porous cobalt oxide for enhanced photo-oxidation of indoor pollutants

Energy Technology Data Exchange (ETDEWEB)

Cheng, J. P., E-mail: chengjp@zju.edu.cn [Zhejiang University, State Key Laboratory of Silicon Materials, Department of Materials Science and Engineering (China); Shereef, Anas; Gray, Kimberly A., E-mail: k-gray@northwestern.edu [Northwestern University, Center for Catalysis and Surface Science (United States); Wu, Jinsong [Northwestern University, Department of Materials Science and Engineering (United States)

2015-03-15

Porous cobalt oxide was successfully prepared by precipitation of cobalt hydroxide followed by low temperature thermal decomposition. The morphologies of the resultant oxides remained as the corresponding hydroxides, although the morphology of cobalt hydroxides was greatly influenced by the precursor salts. The cobalt oxides with average crystal size less than 20 nm were characterized by X-ray diffraction, scanning electron microscope, BET surface area, and XPS analysis. The photocatalytic activities of the various cobalt oxides morphologies were investigated by comparing the photo-degradation of acetaldehyde under simulated solar illumination. Relative to their low order structures and reference titania samples, the hierarchical nanostructures of cobalt oxide showed excellent abilities to rapidly degrade acetaldehyde, a model air pollutant. This was attributed to the unique nature of these hierarchical cobalt oxide nanoassemblies, which contained many catalytically active reaction sites and open pores.

The formation of crystals in glasses containing rare earth oxides

Energy Technology Data Exchange (ETDEWEB)

Fadzil, Syazwani Mohd [Pohang University of Science and Technology (POSTECH), Pohang (Korea, Republic of); Hrma, Pavel [Pohang University of Science and Technology (POSTECH), Pohang, South Korea and Pacific Northwest National Laboratory, Richland, Washington (United States); Crum, Jarrod [Pacific Northwest National Laboratory, Richland, Washington (United States); Siong, Khoo Kok; Ngatiman, Mohammad Fadzlee; Said, Riduan Mt [National University of Malaysia, Bandar Baru Bangi, Selangor (Malaysia)

2014-02-12

Korean spent nuclear fuel will reach the capacity of the available temporary storage by 2016. Pyroprocessing and direct disposal seems to be an alternative way to manage and reuse spent nuclear fuel while avoiding the wet reprocessing technology. Pyroprocessing produces several wastes streams, including metals, salts, and rare earths, which must be converted into stabilized form. A suitable form for rare earth immobilization is borosilicate glass. The borosilicate glass form exhibits excellent durability, allows a high waste loading, and is easy to process. In this work, we combined the rare earths waste of composition (in wt%) 39.2Nd{sub 2}O{sub 3}–22.7CeO{sub 2}–11.7La{sub 2}O{sub 3}–10.9PrO{sub 2}–1.3Eu{sub 2}O{sub 3}–1.3Gd{sub 2}O{sub 3}–8.1Sm{sub 2}O{sub 3}–4.8Y{sub 2}O{sub 3} with a baseline glass of composition 60.2SiO{sub 2}–16.0B{sub 2}O{sub 3}–12.6Na{sub 2}O–3.8Al{sub 2}O{sub 3}–5.7CaO–1.7ZrO{sub 2}. Crystallization in waste glasses occurs as the waste loading increases. It may produce complicate glass processing and affect the product quality. To study crystal formation, we initially made glasses containing 5%, 10% and 15% of La{sub 2}O{sub 3} and then glasses with 5%, 10% and 15% of the complete rare earth mix. Samples were heat-treated for 24 hours at temperatures 800°C to 1150°C in 50°C increments. Quenched samples were analyzed using an optical microscope, scanning electron microscope with energy dispersive spectroscopy, and x-ray diffraction. Stillwellite (LaBSiO{sub 5}) and oxyapatite (Ca{sub 2}La{sub 8}Si{sub 6}O{sub 26}) were found in glasses containing La{sub 2}O{sub 3}, while oxyapatite (Ca{sub 2}La{sub 8}Si{sub 6}O{sub 26} and NaNd{sub 9}Si{sub 6}O{sub 26}) precipitated in glasses with additions of mixed rare earths. The liquidus temperature (T{sub L}) of the glasses containing 5%, 10% and 15% La{sub 2}O{sub 3} were 800°C, 959°C and 986°C, respectively; while T{sub L} was 825°C, 1059°C and 1267°C for glasses

Spectroscopic studies of surface-gas interactions and catalyst restructuring at ambient pressure: mind the gap!

International Nuclear Information System (INIS)

Rupprechter, Guenther; Weilach, Christian

2008-01-01

Recent progress in the application of surface vibrational spectroscopy at ambient pressure allows us to monitor surface-gas interactions and heterogeneous catalytic reactions under conditions approaching those of technical catalysis. The surface specificity of photon-based methods such as polarization modulation infrared reflection absorption spectroscopy (PM-IRAS) and sum frequency generation (SFG) spectroscopy is utilized to monitor catalytically active surfaces while they function at high pressure and high temperature. Together with complementary information from high-pressure x-ray photoelectron spectroscopy (HP-XPS) and high-resolution transmission electron microscopy (HRTEM), reaction mechanisms can be deduced on a molecular level. Well defined model catalysts, prepared under ultrahigh vacuum (UHV), are typically employed in such studies, including smooth and stepped single crystals, thin oxide films, and oxide-supported nanoparticles. A number of studies on unsupported and supported noble metal (Pd, Rh) catalysts are presented, focusing on the transformation of the catalysts from the 'as-prepared' to the 'active state'. This often involves pronounced alterations in catalyst structure and composition, for example the creation of surface carbon phases, surface oxides or surface alloys, as well as nanoparticle restructuring. The reactivity studies include CH 3 OH, CH 4 and CO oxidation with gas phase analysis by gas chromatography and mass spectrometry. Differing results between studies under ultrahigh vacuum and ambient pressure, and between studies on single crystals and supported nanoparticles, demonstrate the importance of 'minding the gap' between idealized and realistic conditions

Crystallization behavior of ZrO{sub 2}−3Y{sub 2}O{sub 3}−xSrO precursor powders synthesized by a coprecipitation process

Energy Technology Data Exchange (ETDEWEB)

Chu, Hsueh-Liang [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta- Hsueh Road, Tainan 70101, Taiwan (China); Hwang, Weng-Sing [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta- Hsueh Road, Tainan 70101, Taiwan (China); Institute of Nanotechnology and Microsystems Engineering, National Cheng Kung University, 1 Ta- Hsueh Road, Tainan 70101, Taiwan (China); Du, Je-Kang [Department of Dentistry, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80708, Taiwan (China); Department of Dentistry, Kaohsiung Medical University, Chung Ho Memorial Hospital, 100 Tzyou 1st Road, Kaohsiung 80708, Taiwan (China); Chen, Ker-Kong, E-mail: enamel@kmu.edu.tw [Department of Dentistry, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80708, Taiwan (China); Department of Dentistry, Kaohsiung Medical University, Chung Ho Memorial Hospital, 100 Tzyou 1st Road, Kaohsiung 80708, Taiwan (China); Wang, Moo-Chin, E-mail: mcwang@kmu.edu.tw [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80708, Taiwan (China)

2016-09-05

Crystallization behaviors of ZrO{sub 2}−3Y{sub 2}O{sub 3}−xSrO precursor powders were studied with zirconium nitrate (Zr(NO{sub 3}){sub 4}·xH{sub 2}O), yttrium nitrate (Y(NO{sub 3}){sub 3}·6H{sub 2}O) and strontium nitrate (Sr(NO{sub 3}){sub 2}) constituting the initial materials. Differential thermal analysis (DTA), X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), nano beam electron diffraction (NBED) and high-resolution TEM (HRTEM) were utilized to characterize the crystallization behavior of ZrO{sub 2}−3Y{sub 2}O{sub 3}−xSrO precursor powders. The activation energies of tetragonal ZrO{sub 2} (t-ZrO{sub 2}) crystallization were 389.1, 327.6, and 315.1 kJ/mol with SrO content for 1, 2, and 3 mol%, respectively, obtained with a non-isothermal method. The growth morphology parameter and growth mechanism index were close to 2.0 and 1.0, respectively, showing that t-ZrO{sub 2} had a plate-like morphology. - Highlights: • The single phase of tetragonal ZrO{sub 2} formed when calcined at 923 K for 2 h. • ZrO{sub 2}−3Y{sub 2}O{sub 3}−2SrO precursor powders crystallization is at 765.6 K. • The activation energy of t-ZrO{sub 2} crystallization was 389.1 kJ/mol with 1 mol% SrO. • The growth morphology and index of crystallization were close to 2.0 and 1.0.

Synthesis and crystal structure of the first Sc-Nb-O-N phases

Energy Technology Data Exchange (ETDEWEB)

Orthmann, Steven; Lerch, Martin [Institut fuer Chemie, Technische Universitaet Berlin (Germany)

2017-11-17

Synthesis of phase-pure materials in the system Sc-Nb-O-N is challenging. In this contribution we report on the preparation of the first scandium niobium oxide nitrides via reaction of water-saturated gaseous ammonia or an ammonia-oxygen mixture with amorphous scandium niobium oxides. Two new phases were obtained: rutile-type ScNb{sub 4}O{sub 7}N{sub 3}, which crystallizes in space group P4{sub 2}/mnm, and an anion-deficient fluorite-type Sc{sub 2}Nb(O,N,⬜){sub 6} phase crystallizing in space group Fm anti 3m. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Modification of mechanical properties of single crystal aluminum oxide by ion beam induced structural changes

International Nuclear Information System (INIS)

Ensinger, W.; Nowak, R.; Horino, Y.; Baba, K.

1993-01-01

The mechanical behaviour of ceramics is essentially determined by their surface qualities. As a surface modification technique, ion implantation provides the possibility to modify the mechanical properties of ceramics. Highly energetic ions are implanted into the near-surface region of a material and modify its composition and structure. Ions of aluminum, oxygen, nickel and tantalum were implanted into single-crystal α-aluminum oxide. Three-point bending tests showed that an increase in flexural strength of up to 30% could be obtained after implantation of aluminum and oxygen. Nickel and tantalum ion implantation increased the fracture toughness. Indentation tests with Knoop and Vickers diamonds and comparison of the lengths of the developed radial cracks showed that ion implantation leads to a reaction in cracking. The observed effects are assigned to radiation induced structural changes of the ceramic. Ion bombardment leads to radiation damage and formation of compressive stress. In case of tantalum implantation, the implanted near-surface zone becomes amorphous. These effects make the ceramic more resistant to fracture. (orig.)

Slow neutron scattering in molecular crystals. 5-4

International Nuclear Information System (INIS)

Inoue, Kazuhiko

1976-01-01

The utilization of incoherent inelastic neutron scattering (INS) as a probe for molecular crystals is reviewed. In particular, some typical examples of the measurement of incoherent inelastic neutron scattering spectra (INSS) in molecular crystals are presented in the first section of this report. The results of measurement are shown for theta-xylene, benzene, polypropylene oxide, deuteride, and formic acid. The second section presents an equation for the incoherent scattering cross section of a crystal by dividing the molecular motion into the outer and inner modes. Phonon expansion is also used for the easy understanding of the relation between the INSS and the dynamic characteristics of molecular crystals. In the third section, the measured results are analyzed on the basis of the theory presented in the previous section. And the difference between the van der Waals bond and the hydrogen bond is shortly discussed. (Aoki, K.)

Effects of oxygen gas pressure on properties of iron oxide films grown by pulsed laser deposition

International Nuclear Information System (INIS)

Guo, Qixin; Shi, Wangzhou; Liu, Feng; Arita, Makoto; Ikoma, Yoshifumi; Saito, Katsuhiko; Tanaka, Tooru; Nishio, Mitsuhiro

2013-01-01

Highlights: ► Pulsed laser deposition is a promising technique for growing iron oxide films. ► Crystal structure of the iron oxide films strongly depends on oxygen gas pressure. ► Optimum of the oxygen gas pressure leads single phase magnetite films with high crystal quality. -- Abstract: Iron oxide films were grown on sapphire substrates by pulsed laser deposition at oxygen gas pressures between 1 × 10 −5 and 1 × 10 −1 Pa with a substrate temperature of 600 °C. Atomic force microscope, X-ray diffraction, Raman spectroscopy, X-ray absorption fine structure, and vibrational sample magnetometer analysis revealed that surface morphology and crystal structure of the iron oxide films strongly depend on the oxygen gas pressure during the growth and the optimum oxygen gas pressure range is very narrow around 1 × 10 −3 Pa for obtaining single phase magnetite films with high crystal quality

Crystallization kinetics and optical properties of titanium-lithium tetraborate glass containing europium oxide

Energy Technology Data Exchange (ETDEWEB)

Mohamed, E.A. [Al Azhar University, Department of Physics, Faculty of Science (Girl' s Branch), Cairo (Egypt); Ratep, A. [Ain Shams University, Physics Department, Faculty of Girls, Cairo (Egypt); Abdel-Khalek, E.K.; Kashif, I. [Al-Azhar University, Department of Physics, Faculty of Science, Cairo (Egypt)

2017-07-15

The crystallization kinetics and optical properties of [60 Li{sub 2}B{sub 4}O{sub 7}-30 TiO{sub 2}-10 Eu{sub 2}O{sub 3}] (mol%) glass sample have been investigated. The present glass sample exhibits three crystallization exothermic peaks (T{sub p1}, T{sub p2,} and T{sub p3}) corresponding to the formation of LiBO{sub 2}, Li{sub 2}B{sub 4}O{sub 7,} and EuTiO{sub 3} phases, respectively. The presence of phase separation in the glass sample has been confirmed by scanning electron microscopic (SEM). The mean values of Avrami exponent (n = 3.1 and 4) around T{sub p1} and T{sub p2}, indicate that the bulk crystallization with a constant number of nuclei and with an increasing number of nuclei, respectively. The values of the local activation energy as a function of the fraction of crystallization (0.1 ≤ χ ≤ 0.9) decrease for the crystallization of LiBO{sub 2} and EuTiO{sub 3} and increase for the crystallization of Li{sub 2}B{sub 4}O{sub 7}. The values of n(χ) for T{sub p3} and T{sub p2} in the range (0.1 ≤ χ ≤ 0.9) and (0.1 ≤ χ ≤ 0.4), respectively, are larger than 4 indicate that the presence of anomalous in Avrami exponent. The trend of Judd-Ofelt intensity parameters (Ω{sub 2} > Ω{sub 4} > Ω{sub 6}) and the bonding parameter (δ) indicate that the lower symmetry and the highest covalent nature of the bonding around Eu{sup 3+} ions. (orig.)

Rare earth oxide doping in oxide cathodes

International Nuclear Information System (INIS)

Engelsen, Daniel den; Gaertner, Georg

2006-01-01

The effect on life performance and poisoning with O 2 by doping oxide cathodes with rare earth oxides and pseudo rare earth oxides, notably yttria, is qualitatively explained in terms of electrolysis of BaO during emission of electrons. Doped cathodes show less electrolysis and consume therefore less Ba during life: consequently, doped cathodes have a better life performance. However, the lower Ba-production makes doped cathodes more sensitive to oxygen poisoning. The experimentally found relation between conductivity and yttria concentration was the motive to propose a new model for the crystal imperfections in BaO. In this new imperfection model most Y 3+ -ions will combine with barium vacancies, therefore, the increase of the conductivity is modest and also the effect on the position of the Fermi level is modest. By assuming a combination of bulk and surface conductivity, the agreement between experiment and theory can be improved further

Interactions of Graphene Oxide Nanomaterials with Natural Organic Matter and Metal Oxide Surfaces

Science.gov (United States)

Interactions of graphene oxide (GO) with silica surfaces were investigated using a quartz crystal microbalance with dissipation monitoring (QCM-D). Both GO deposition and release were monitored on silica- and poly-l-lysine (PLL) coated surfaces as a function of GO concentration a...

Synthesis and characterization of new oxides and oxynitrides of niobium; Synthese und Charakterisierung neuer Oxide und Oxidnitride des Niobs

Energy Technology Data Exchange (ETDEWEB)

Orthmann, Steven

2017-11-02

By different synthesis routes the first oxide nitrides in the series scandium-niobium-oxygen-nitrogen could be synthesized and characterized. ScNb{sub 4}O{sub 7}N{sub 3}, which crystallizes in the rutile-type structure, exhibit a band gap of 2.62 eV after a short oxidation. Furthermore anion-deficit NbSc{sub 2}(O,N,□){sub 6} with fluorite-type structure could be synthesized. UV-Vis measurements point to a band gap of 3.36 eV after a short oxidation of the product. In the series zirconium-niobium-oxygen-nitrogen new oxides and oxide nitrides could be synthesized. By replacing zirconium with hafnium isotopical compounds with comparable composition could be obtained. The crystal structure of these new compounds is discussed respecting magnetism and the results of electron microscopy and neutron diffraction. By partially substitution of niobium with magnesium or zinc three additional oxide nitrides with the compositions Mg{sub 2}Nb{sub 4}O{sub 2}N{sub 5}, Zn{sub 2}NbO{sub 0,3}N{sub 2,8}, and ZnNb{sub 3}O{sub 0,1}N{sub 4,5}, showing a tetragonal Nb{sub 4}N{sub 5}-type structure, could be synthesized.

Synthesis engineering of iron oxide raspberry-shaped nanostructures.

Science.gov (United States)

Gerber, O; Pichon, B P; Ihiawakrim, D; Florea, I; Moldovan, S; Ersen, O; Begin, D; Grenèche, J-M; Lemonnier, S; Barraud, E; Begin-Colin, S

2017-01-07

Magnetic porous nanostructures consisting of oriented aggregates of iron oxide nanocrystals display very interesting properties such as a lower oxidation state of magnetite, and enhanced saturation magnetization in comparison with individual nanoparticles of similar sizes and porosity. However, the formation mechanism of these promising nanostructures is not well understood, which hampers the fine tuning of their magnetic properties, for instance by doping them with other elements. Therefore the formation mechanism of porous raspberry shaped nanostructures (RSNs) synthesized by a one-pot polyol solvothermal method has been investigated in detail from the early stages by using a wide panel of characterization techniques, and especially by performing original in situ HR-TEM studies in temperature. A time-resolved study showed the intermediate formation of an amorphous iron alkoxide phase with a plate-like lamellar structure (PLS). Then, the fine investigation of PLS transformation upon heating up to 500 °C confirmed that the synthesis of RSNs involves two iron precursors: the starting one (hydrated iron chlorides) and the in situ formed iron alkoxide precursor which decomposes with time and heating and contributes to the growth step of nanostructures. Such an understanding of the formation mechanism of RSNs is necessary to envision efficient and rational enhancement of their magnetic properties.

Practical aspects of the use of the X(2) holder for HRTEM-quality TEM sample preparation by FIB.

Science.gov (United States)

van Mierlo, Willem; Geiger, Dorin; Robins, Alan; Stumpf, Matthias; Ray, Mary Louise; Fischione, Paul; Kaiser, Ute

2014-12-01

The X(2) holder enables the effective production of thin, electron transparent samples for high-resolution transmission electron microscopy (HRTEM). Improvements to the X(2) holder for high-quality transmission electron microscopy (TEM) sample preparation are presented in this paper. We discuss the influence of backscattered electrons (BSE) from the sample holder in determining the lamella thickness in situ and demonstrate that a significant improvement in thickness determination can be achieved by comparatively simple means using the relative BSE intensity. We show (using Monte Carlo simulations) that by taking into account the finite collection angle of the electron backscatter detector, an approximately 20% underestimation of the lamella thickness in a silicon sample can be avoided. However, a correct thickness determination for light-element lamellas still remains a problem with the backscatter method; we introduce a more accurate method using the energy dispersive X-ray spectroscopy (EDX) signal for in situ thickness determination. Finally, we demonstrate how to produce a thin lamella with a nearly damage-free surface using the X(2) holder in combination with sub-kV polishing in the Fischione Instruments׳ NanoMill(®) TEM specimen preparation system. Copyright © 2014 Elsevier B.V. All rights reserved.

The magnetic characterization of Fe doped TiO{sub 2} semiconducting oxide nanoparticles synthesized by sol–gel method

Energy Technology Data Exchange (ETDEWEB)

Yeganeh, M., E-mail: mahboubeh.yeganeh@yahoo.co.uk [Department of Physics, Kosar University of Bojnord, P.O. Box 94104455 (Iran, Islamic Republic of); Shahtahmasebi, N.; Kompany, A. [Department of Physics, Ferdowsi University of Mashhad (Iran, Islamic Republic of); Karimipour, M. [Department of Physics, Vali-e-Asr University of Rafsanjan (Iran, Islamic Republic of); Razavi, F. [Department of Physics, Brock University (Canada); Nasralla, N.H.S. [Electron Microscope and Thin Film Department, Physics Division, 33 El Buhouth st., Dokki, 12622 Giza (Egypt); Šiller, L. [School of Chemical Engineering and Advanced Materials, Newcastle University, NE1 7RU (United Kingdom)

2017-04-15

In this work Fe doped TiO{sub 2} nanoparticles were synthesized at different Fe/Ti molar ratio from 1% to 5% by sol-gel technique. The post annealing of the samples was carried out at T=400, 600, and 800 °C. HRTEM of the samples revealed that the mean size of the nanoparticles increases from about 8 nm to about 100 nm as the annealing temperature increased. SQUID magnetometry of 1% and 5% Fe doped TiO{sub 2} has shown mixed ferromagnetic and paramagnetic phases within the crystal while ferromagnetic order with T{sub c} about 350 K was only observed in 5% Fe:TiO{sub 2} sample annealed at T=800 °C. The oxygen vacancy mediated ferromagnetic (FM) interaction could be responsible for the observed FM.

Graphene Oxide-Gallic Acid Nanodelivery System for Cancer Therapy

Science.gov (United States)

Dorniani, Dena; Saifullah, Bullo; Barahuie, Farahnaz; Arulselvan, Palanisamy; Hussein, Mohd Zobir Bin; Fakurazi, Sharida; Twyman, Lance J.

2016-11-01

Despite the technological advancement in the biomedical science, cancer remains a life-threatening disease. In this study, we designed an anticancer nanodelivery system using graphene oxide (GO) as nanocarrier for an active anticancer agent gallic acid (GA). The successful formation nanocomposite (GOGA) was characterized using XRD, FTIR, HRTEM, Raman, and UV/Vis spectroscopy. The release study shows that the release of GA from the designed anticancer nanocomposite (GOGA) occurs in a sustained manner in phosphate-buffered saline (PBS) solution at pH 7.4. In in vitro biological studies, normal fibroblast (3T3) and liver cancer cells (HepG2) were treated with different concentrations of GO, GOGA, and GA for 72 h. The GOGA nanocomposite showed the inhibitory effect to cancer cell growth without affecting normal cell growth. The results of this research are highly encouraging to go further for in vivo studies.

Generation of laser-induced periodic surface structures in indium-tin-oxide thin films and two-photon lithography of ma-N photoresist by sub-15 femtosecond laser microscopy for liquid crystal cell application

Science.gov (United States)

Klötzer, Madlen; Afshar, Maziar; Feili, Dara; Seidel, Helmut; König, Karsten; Straub, Martin

2015-03-01

Indium-tin-oxide (ITO) is a widely used electrode material for liquid crystal cell applications because of its transparency in the visible spectral range and its high electrical conductivity. Important examples of applications are displays and optical phase modulators. We report on subwavelength periodic structuring and precise laser cutting of 150 nm thick indium-tin-oxide films on glass substrates, which were deposited by magnetron reactive DC-sputtering from an indiumtin target in a low-pressure oxygen atmosphere. In order to obtain nanostructured electrodes laser-induced periodic surface structures with a period of approximately 100 nm were generated using tightly focused high-repetition rate sub-15 femtosecond pulsed Ti:sapphire laser light, which was scanned across the sample by galvanometric mirrors. Three-dimensional spacers were produced by multiphoton photopolymerization in ma-N 2410 negative-tone photoresist spin-coated on top of the ITO layers. The nanostructured electrodes were aligned in parallel to set up an electrically switchable nematic liquid crystal cell.

Sub-2 nm SnO2 nanocrystals: A reduction/oxidation chemical reaction synthesis and optical properties

International Nuclear Information System (INIS)

Zhang Hui; Du Ning; Chen Bindi; Cui Tianfeng; Yang Deren

2008-01-01

A simple reduction/oxidation chemical solution approach at room temperature has been developed to synthesize ultrafine SnO 2 nanocrystals, in which NaBH 4 is used as a reducing agent instead of mineralizers such as sodium hydroxide, ammonia, and alcohol. The morphology, structure, and optical property of the ultrafine SnO 2 nanocrystals have been characterized by high-resolution transmission electron microscopy (HRTEM), X-ray powder diffraction (XRD), differential scanning calorimetry and thermogravimetric analysis (DSC-TGA), X-ray photoelectron spectroscopy (XPS) and UV-vis absorption spectroscopy. It is indicated that the uniform tetragonal ultrafine SnO 2 nanocrystals with the size below 2 nm have been fabricated at room temperature. The band gap of the ultrafine SnO 2 nanocrystals is about 4.1 eV, exhibiting 0.5 eV blue shift from that of the bulk SnO 2 (3.6 eV). Furthermore, the mechanism for the reduction/oxidation chemical reaction synthesis of the ultrafine SnO 2 nanocrystals has been preliminary presented

Preparation of nano-iron oxide red pigment powders by use of cyanided tailings

International Nuclear Information System (INIS)

Li Dengxin; Gao Guolong; Meng Fanling; Ji Chong

2008-01-01

On one hand, cyanided tailings are one kind of pollutants. On the other hand, they contain a lot of valuable elements. So utilization of them can bring social and environmental benefits. In this paper, cyanided tailings were used to prepare nano-iron oxide red pigment powders by an ammonia process with urea as precipitant. At first, cyanided tailings were oxidized by nitric acid. Then, the oxidizing mixture was separated into solid and liquid parts. The liquid mixture was reduced by scrap iron and the impurity of it was removed by use of NH 3 .H 2 O. Then, the seed crystal of γ-FeOOH was obtained, when the pure liquid reacted with ammonia liquid at the selected experimental conditions. At last, nano-iron oxide red pigment powders were prepared. The structure, morphology and size distribution of seed crystal and iron oxide red were characterized systematically by means of X-ray diffraction (XRD), transmission electron microscope (TEM) and laser particle size analyzer (LPSA). The results revealed that typical iron oxide nanoparticles were α-Fe 2 O 3 with particle size of 50-70 nm. Furthermore, the factors that affected the hue and quality of the seed crystal and iron oxide red pigment were also discussed

HRTEM imaging of atoms at sub-Angstroem resolution

International Nuclear Information System (INIS)

O'Keefe, Michael A.; Allard, Lawrence F.; Blom, Douglas A.

2005-01-01

John Cowley and his group at Arizona State University pioneered the use of transmission electron microscopy for high-resolution imaging. Images were achieved three decades ago showing the crystal unit cell content at better than 4 A resolution. This achievement enabled researchers to pinpoint the positions of heavy atom columns within the unit cell. Lighter atoms appear as resolution is improved to sub-Angstroem levels. Currently, advanced microscopes can image the columns of the light atoms (carbon, oxygen, nitrogen) that are present in many complex structures, and even the lithium atoms present in some battery materials. Sub-Angstroem imaging, initially achieved by focal-series reconstruction of the specimen exit surface wave, will become commonplace for next-generation electron microscopes with C s -corrected lenses and monochromated electron beams. Resolution can be quantified in terms of peak separation and inter-peak minimum, but the limits imposed on the attainable resolution by the properties of the microscope specimen need to be considered. At extreme resolution the 'size' of atoms can mean that they will not be resolved even when spaced farther apart than the resolution of the microscope. (author)

HRTEM Imaging of Atoms at Sub-Angstrom Resolution

Energy Technology Data Exchange (ETDEWEB)

O' Keefe, Michael A.; Allard, Lawrence F.; Blom, Douglas A.

2005-04-06

John Cowley and his group at Arizona State University pioneered the use of transmission electron microscopy (TEM) for high-resolution imaging. Images were achieved three decades ago showing the crystal unit cell content at better than 4 Angstrom resolution. This achievement enabled researchers to pinpoint the positions of heavy atom columns within the unit cell. Lighter atoms appear as resolution is improved to sub-Angstrom levels. Currently, advanced microscopes can image the columns of the light atoms (carbon, oxygen, nitrogen) that are present in many complex structures, and even the lithium atoms present in some battery materials. Sub-Angstrom imaging, initially achieved by focal-series reconstruction of the specimen exit surface wave, will become common place for next-generation electron microscopes with CS-corrected lenses and monochromated electron beams. Resolution can be quantified in terms of peak separation and inter-peak minimum, but the limits imposed on the attainable resolution by the properties of the micro-scope specimen need to be considered. At extreme resolution the ''size'' of atoms can mean that they will not be resolved even when spaced farther apart than the resolution of the microscope.

Conversion of Jatropha curcas oil into biodiesel using re-crystallized hydrotalcite

International Nuclear Information System (INIS)

Helwani, Z.; Aziz, N.; Bakar, M.Z.A.; Mukhtar, H.; Kim, J.; Othman, M.R.

2013-01-01

Graphical abstract: XRD pattern of a mixed oxide and re-crystallized hydrotalcite after contacting with carbonate solution. The sample re-crystallized despite being exposed to high temperature. The increased crystallinity at higher calcination temperature was due to aluminum progressively incorporated into the MgO network. At low temperature, aluminum diffused slowly and did not reach the crystallite core. XRD pattern of (a) mixed oxide at 450 °C, (b) hydrotalcite at 450 °C (c) hydrotalcite at 650 °C and (d) hydrotalcite at 850 °C. - Highlights: • Synthetic hydrotalcite (HT) was prepared from combustion method. • The sample was able to re-crystallize despite being exposed to high temperature. • HT catalyst promoted conversion of Jatropha curcas oil into biodiesel. • Conversion of 75.2% was achieved with promising conditions. - Abstract: Biodiesel production from biomass is considered renewable and the use of biomass offers huge opportunity in bio-based economy market. In this work, biodiesel was produced from Jatropha curcas oil using synthetic hydrotalcite (HT) catalyst. The catalyst was obtained through combustion, in which, saccharose was used as fuel. The highest conversion of jatropha oil to biodiesel at 75.2% was achieved using re-crystallized HT from its mixed oxides when reaction was carried out at 65 °C with a methanol:jatropha oil molar ratio of 12:1, a reaction time of 6 h and a catalyst loading of 4 wt.%. The HT calcined at 850 °C contained medium basic strength sites and suitable pore medium that favored the chemical reaction

Electron paramagnetic resonance study of Ce doped partially stabilized ZrO2 crystals

Directory of Open Access Journals (Sweden)

Mikhail А. Borik

2017-09-01

Full Text Available ZrO2 (PSZ solid solutions crystals stabilized with yttrium and cerium oxides have been studied using electron paramagnetic resonance (EPR in the X and Q ranges. Zr3+ have been observed centers in the as-annealed ZrO2 crystals stabilized only by yttrium oxide (2.8 mol% Y2O3. Another type of paramagnetic-O-centers appear as a result of CeO2 addition to ZrO2 crystals along with yttrium oxide. To estimate the concentration of Ce3+ ions in PZS crystals, we recorded the EPR spectra in the presence of a reference at 7 K. Paramagnetic Ce3+ ions have been identified and their relative amount in the PSZ crystals before and after high-temperature heat treatment has been assessed. Annealing in air leads decreases the concentration of Ce3+ ions for all the test compositions and changes the color of the crystals from red to white. After annealing of the sample 2.0Y0.8Ce3Zr, the amount of paramagnetic Ce3+ ions decreased approximately twofold. Paramagnetic centers from Ce3+ have not been detected in the specimen with a low cerium content of 0.1 mol% after annealing which indicates the complete transition of Ce3+ to the Ce4+ state. We show that the forming cerium paramagnetic centers are bound by strong exchange interactions. No angular dependence of the EPR lines of the paramagnetic Ce3+ cations on the applied external magnetic field has been observed. Probable origin of the absence of angular dependence is that the impurity rare-earth ions are located close to one another, forming impurity clusters with an effective spin of Seff=1/2.

Containerless solidification of undercooled oxide and metallic eutectic melts

International Nuclear Information System (INIS)

Li Mingjun; Nagashio, Kosuke; Kuribayashi, Kazuhiko

2004-01-01

A high-speed video was employed to monitor the in situ recalescence of undercooled oxide Al 2 O 3 -36.8 at.% ZrO 2 and metallic Ni-18.7 at.% Sn eutectics that were processed on an aero-acoustic levitator and an electromagnetic levitator, respectively. For the oxide eutectic, the entire sample becomes brighter and brighter without any clear recalescence front during spontaneous crystallization. When the sample was seeded at desired undercoolings, crystallization started from the seeding point and then spread through the entire sample. Microstructures of the oxide solidified via both the spontaneous crystallization and external seeding consist of many independent eutectic colonies at the sample surface, indicating that copious nucleation takes place regardless of melt undercooling and solidification mode. For the metallic eutectics, two kinds of recalescence are visualized. The surface and cross sectional microstructures reveal that copious nucleation is also responsible for the formation of independent eutectic colonies distributing within the entire sample. It is not possible to measure the growth velocity of a single eutectic colony using optical techniques under the usual magnification. The conventional nucleation concept derived from single-phase alloys may not be applicable to the free solidification of the undercooled double-phase oxide and metallic eutectic systems

Study on crystallization behaviour of co-polyamide 66 containing ...

Indian Academy of Sciences (India)

Triaryl phosphine oxide (TPO) compounds, which as a type of flame ... The image of .... ation rate and crystallization properties of FR-PA66 were ..... Polarized optical microscopy images for (a) PA66 and (b) FR-PA66 after constant temperature ...

Growth and luminescent properties of Yb3+--doped oxide single crystals for scintillator application

International Nuclear Information System (INIS)

Yoshikawa, A.; Ogino, H.; Shim, J.B.; Nikl, M.; Solovieva, N.; Fukuda, T.

2004-01-01

Rod-shaped (Lu 1-x Yb x ) 3 Al 5 O 12 with x=0.05, 0.15, 0.30 and (Y 1-x Yb x )AlO 3 with x=0.05, 0.10, 0.30 single crystals were grown by the micro-pulling-down method. Edge-defined film-fed growth method was used to prepare (Y 0.9 Yb 0.1 )VO 4 crystal, while Ca 8 (La 1.98 Yb 0.02 )(PO 4 ) 6 O 2 crystal was grown by the Czochralski method. Luminescence of these crystals was studied with main attention paid to the charge transfer emission of Yb 3+ . Temperature tuned decay times in the time scale of units--tens of nanosecond was measured as a feature possibly interesting for an application in scintillation detectors in positron emission tomography

Synthesis of TiO2 nanoparticles containing Fe, Si, and V using multiple diffusion flames and catalytic oxidation capability of carbon-coated nanoparticles

KAUST Repository

Ismail, Mohamed; Memon, Nasir K.; Hedhili, Mohamed N.; Anjum, Dalaver H.; Chung, Suk-Ho

2016-01-01

Titanium dioxide (TiO2) nanoparticles containing iron, silicon, and vanadium are synthesized using multiple diffusion flames. The growth of carbon-coated (C–TiO2), carbon-coated with iron oxide (Fe/C–TiO2), silica-coated (Si–TiO2), and vanadium-doped (V–TiO2) TiO2 nanoparticles is demonstrated using a single-step process. Hydrogen, oxygen, and argon are utilized to establish the flame, with titanium tetraisopropoxide (TTIP) as the precursor for TiO2. For the growth of Fe/C–TiO2 nanoparticles, TTIP is mixed with xylene and ferrocene. While for the growth of Si–TiO2 and V–TiO2, TTIP is mixed with hexamethyldisiloxane (HMDSO) and vanadium (V) oxytriisopropoxide, respectively. The synthesized nanoparticles are characterized using high-resolution transmission electron microscopy (HRTEM) with energy-filtered TEM for elemental mapping (of Si, C, O, and Ti), X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), nitrogen adsorption BET surface area analysis, and thermogravimetric analysis. Anatase is the dominant phase for the C–TiO2, Fe/C–TiO2, and Si–TiO2 nanoparticles, whereas rutile is the dominant phase for the V–TiO2 nanoparticles. For C–TiO2 and Fe/C–TiO2, the nanoparticles are coated with about 3-5-nm thickness of carbon. The iron-based TiO2 nanoparticles significantly improve the catalytic oxidation of carbon, where complete oxidation of carbon occurs at a temperature of 470 °C (with iron) compared to 610 °C (without iron). Enhanced catalytic oxidation properties are also observed for model soot particles, Printex-U, when mixed with Fe/C-TiO2. With regards to Si–TiO2 nanoparticles, a uniform coating of 3 to 8 nm of silicon dioxide is observed around the TiO2 particles. This coating mainly occurs due to variance in the chemical reaction rates of the precursors. Finally, with regards to V–TiO2, vanadium is doped within the TiO2 nanoparticles as visualized by HRTEM and XPS further confirms the formation of

Synthesis of TiO2 nanoparticles containing Fe, Si, and V using multiple diffusion flames and catalytic oxidation capability of carbon-coated nanoparticles

KAUST Repository

Ismail, Mohamed

2016-01-19

Titanium dioxide (TiO2) nanoparticles containing iron, silicon, and vanadium are synthesized using multiple diffusion flames. The growth of carbon-coated (C–TiO2), carbon-coated with iron oxide (Fe/C–TiO2), silica-coated (Si–TiO2), and vanadium-doped (V–TiO2) TiO2 nanoparticles is demonstrated using a single-step process. Hydrogen, oxygen, and argon are utilized to establish the flame, with titanium tetraisopropoxide (TTIP) as the precursor for TiO2. For the growth of Fe/C–TiO2 nanoparticles, TTIP is mixed with xylene and ferrocene. While for the growth of Si–TiO2 and V–TiO2, TTIP is mixed with hexamethyldisiloxane (HMDSO) and vanadium (V) oxytriisopropoxide, respectively. The synthesized nanoparticles are characterized using high-resolution transmission electron microscopy (HRTEM) with energy-filtered TEM for elemental mapping (of Si, C, O, and Ti), X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), nitrogen adsorption BET surface area analysis, and thermogravimetric analysis. Anatase is the dominant phase for the C–TiO2, Fe/C–TiO2, and Si–TiO2 nanoparticles, whereas rutile is the dominant phase for the V–TiO2 nanoparticles. For C–TiO2 and Fe/C–TiO2, the nanoparticles are coated with about 3-5-nm thickness of carbon. The iron-based TiO2 nanoparticles significantly improve the catalytic oxidation of carbon, where complete oxidation of carbon occurs at a temperature of 470 °C (with iron) compared to 610 °C (without iron). Enhanced catalytic oxidation properties are also observed for model soot particles, Printex-U, when mixed with Fe/C-TiO2. With regards to Si–TiO2 nanoparticles, a uniform coating of 3 to 8 nm of silicon dioxide is observed around the TiO2 particles. This coating mainly occurs due to variance in the chemical reaction rates of the precursors. Finally, with regards to V–TiO2, vanadium is doped within the TiO2 nanoparticles as visualized by HRTEM and XPS further confirms the formation of

Rh promoted La0.75Sr0.25(Fe0.8Co0.2)1−xGaxO3-δ perovskite catalysts: Characterization and catalytic performance for methane partial oxidation to synthesis gas

International Nuclear Information System (INIS)

Palcheva, R.; Olsbye, U.; Palcut, M.; Rauwel, P.; Tyuliev, G.; Velinov, N.; Fjellvåg, H.H.

2015-01-01

Graphical abstract: - Highlights: • Perovskites type-oxide La 0.75 Sr 0.25 (Fe 0.8 Co 0.2 ) 1−x Ga x O 3-δ (x = 0.1, 0.25, 0.4) prepared by the sol–gel citrate method. • Bulk and surface analysis to determine catalysts composition evolution. • Anaerobic catalytic partial oxidation of methane to syngas at 600 °C in a pulse apparatus over Rh promoted perovskites. • The catalysts showed high stability and selectivity. - Abstract: Synthesis gas production via selective oxidation of methane at 600 °C in a pulse reaction over La 0.75 Sr 0.25 (Fe 0.8 Co 0.2 ) 1−x Ga x O 3-δ (x = 0.1, 0.25, 0.4) perovskite-supported rhodium catalysts, was investigated. The perovskite oxides were prepared by sol–gel citrate method and characterized by X-ray Diffraction (XRD), Moessbauer Spectroscopy (MS), Temperature Programmed Reduction (TPR-H 2 ), X-ray Photoelectron Spectroscopy (XPS) and High Resolution Transmission Electron Microscopy (HRTEM). According to XRD analysis, the synthesized samples were a single perovskite phase. The perovskite structure of Ga substituted samples remained stable after TPR-H 2 , as confirmed by XRD. Data of MS identified Fe 3+ ions in two distinctive coordination environments, and Fe 4+ ions. The Rh 2 O 3 thin overlayer was detected by the HRTEM for the Rh impregnated perovskite oxides. During the interaction of methane with oxidized perovskite-supported Rh (0.5 wt.%) catalysts, besides CO, H 2 , and surface carbon, CO 2 and H 2 O were formed. The Rh perovskite catalyst with x = 0.25 gallium exhibits the highest catalytic activity of 83% at 600 °C. The CO selectivity was affected by the reducibility of La 0.75 Sr 0.25 (Fe 0.8 Co 0.2 ) 1−x Ga x O 3-δ perovskite materials.

Molybdenum Oxides - From Fundamentals to Functionality.

Science.gov (United States)

de Castro, Isabela Alves; Datta, Robi Shankar; Ou, Jian Zhen; Castellanos-Gomez, Andres; Sriram, Sharath; Daeneke, Torben; Kalantar-Zadeh, Kourosh

2017-10-01

The properties and applications of molybdenum oxides are reviewed in depth. Molybdenum is found in various oxide stoichiometries, which have been employed for different high-value research and commercial applications. The great chemical and physical characteristics of molybdenum oxides make them versatile and highly tunable for incorporation in optical, electronic, catalytic, bio, and energy systems. Variations in the oxidation states allow manipulation of the crystal structure, morphology, oxygen vacancies, and dopants, to control and engineer electronic states. Despite this overwhelming functionality and potential, a definitive resource on molybdenum oxide is still unavailable. The aim here is to provide such a resource, while presenting an insightful outlook into future prospective applications for molybdenum oxides. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Catalytic CO Oxidation over Au Nanoparticles Loaded Nanoporous Nickel Phosphate Composite

Directory of Open Access Journals (Sweden)

Xiaonan Leng

2015-01-01

Full Text Available Au/nickel phosphate-5 (Au/VSB-5 composite with the noble metal loading amount of 1.43 wt.% is prepared by using microporous VSB-5 nanocrystals as the support. Carbon monoxide (CO oxidation reaction is carried out over the sample with several catalytic cycles. Complete conversion of CO is achieved at 238°C over the catalyst at the first catalytic cycle. The catalytic activity improved greatly at the second cycle with the complete conversion fulfilled at 198°C and preserved for the other cycles. A series of experiments such as X-ray diffraction (XRD, high resolution transmission electron microscopy (HRTEM, ultraviolet-visible (UV-vis spectroscopy, and X-ray photoelectron spectroscopy (XPS are carried out to characterize the catalysts before and after the reaction to study the factors influencing this promotion at the second cycle.

The adsorption of L-phenylalanine on oxidized single-walled carbon nanotubes.

Science.gov (United States)

Piao, Lingyu; Liu, Quanrun; Li, Yongdan; Wang, Chen

2009-02-01

A simple and green approach was proceeded to obtain a stable single-walled carbon nanotubes (SWNTs)/L-phenylalanine (Phe) solution. The oxidized SWNTs (OSWNT) were used in this work. The scanning electron microscopy (SEM), High-resolution transmission electron microscopy (HRTEM), Raman spectrometer, Fourier transform-infrared resonance (FT-IR), Ultraviolet-visible (UV-vis) spectroscopy, Thermogravimetric analysis (TGA) and High performance liquid chromatography (HPLC) were joined together to investigate the interaction between OSWNT and Phe. The OSWNT became soluble in the water and formed a stable solution since the Phe was adsorbed. The absorbed amount of Phe on the OSWNT is around 33 wt%. Adsorption of the Phe was mainly carried out on the OSWNT with smaller diameters. The Phe molecules were absorbed on the OSWNT by conjunct interaction of the pi-pi stacking, hydrogen bond and part of covalent bond.

Advanced Scale Bridging Microstructure Analysis of Single Crystal Ni-Base Superalloys

Czech Academy of Sciences Publication Activity Database

Parsa, A. B.; Wollgramm, P.; Buck, H.; Somsen, C.; Kostka, A.; Povstugar, I.; Choi, P.-P.; Raabe, D.; Dlouhý, Antonín; Müller, J.; Spiecker, E.; Demtroder, K.; Schreuer, J.; Neuking, K.; Eggeler, G.

2015-01-01

Roč. 17, č. 2 (2015), s. 216-230 ISSN 1438-1656 Institutional support: RVO:68081723 Keywords : High temperature materials * Nickel based superalloys * EPMA * HRTEM Subject RIV: JG - Metallurgy Impact factor: 1.817, year: 2015

Atomic layer deposition of calcium oxide and calcium hafnium oxide films using calcium cyclopentadienyl precursor

International Nuclear Information System (INIS)

Kukli, Kaupo; Ritala, Mikko; Sajavaara, Timo; Haenninen, Timo; Leskelae, Markku

2006-01-01

Calcium oxide and calcium hafnium oxide thin films were grown by atomic layer deposition on borosilicate glass and silicon substrates in the temperature range of 205-300 o C. The calcium oxide films were grown from novel calcium cyclopentadienyl precursor and water. Calcium oxide films possessed refractive index 1.75-1.80. Calcium oxide films grown without Al 2 O 3 capping layer occurred hygroscopic and converted to Ca(OH) 2 after exposure to air. As-deposited CaO films were (200)-oriented. CaO covered with Al 2 O 3 capping layers contained relatively low amounts of hydrogen and re-oriented into (111) direction upon annealing at 900 o C. In order to examine the application of CaO in high-permittivity dielectric layers, mixtures of Ca and Hf oxides were grown by alternate CaO and HfO 2 growth cycles at 230 and 300 o C. HfCl 4 was used as a hafnium precursor. When grown at 230 o C, the films were amorphous with equal amounts of Ca and Hf constituents (15 at.%). These films crystallized upon annealing at 750 o C, showing X-ray diffraction peaks characteristic of hafnium-rich phases such as Ca 2 Hf 7 O 16 or Ca 6 Hf 19 O 44 . At 300 o C, the relative Ca content remained below 8 at.%. The crystallized phase well matched with rhombohedral Ca 2 Hf 7 O 16 . The dielectric films grown on Si(100) substrates possessed effective permittivity values in the range of 12.8-14.2

Buried oxide layer in silicon

Science.gov (United States)

Sadana, Devendra Kumar; Holland, Orin Wayne

2001-01-01

A process for forming Silicon-On-Insulator is described incorporating the steps of ion implantation of oxygen into a silicon substrate at elevated temperature, ion implanting oxygen at a temperature below 200.degree. C. at a lower dose to form an amorphous silicon layer, and annealing steps to form a mixture of defective single crystal silicon and polycrystalline silicon or polycrystalline silicon alone and then silicon oxide from the amorphous silicon layer to form a continuous silicon oxide layer below the surface of the silicon substrate to provide an isolated superficial layer of silicon. The invention overcomes the problem of buried isolated islands of silicon oxide forming a discontinuous buried oxide layer.

The Low-Temperature Crystallization and Interface Characteristics of ZnInSnO/In Films Using a Bias-Crystallization Mechanism

International Nuclear Information System (INIS)

Chen, K. J.; Chen, K.J.; Hung, F.Y.; Lui, T.S.; Chang, S.J.; Hu, Z.S.

2012-01-01

This study presents a successful bias crystallization mechanism (BCM) based on an indium/glass substrate and applies it to fabrication of ZnInSnO (ZITO) transparent conductive oxide (TCO) films. The effects of bias-crystallization on electrical and structural properties of ZITO/In structure indicate that the current-induced Joule heating and interface diffusion were critical factors for low-temperature crystallization. With biases of 4 V and 0.1 A, the resistivity of the ZITO film was reduced from 3.08x10 -4 Ω * cm to 6.3x10 -5 Ω * cm. This reduction was attributed to the bias-induced energy, which caused indium atoms to diffuse into the ZITO matrix. This effectuated crystallizing the amorphous ZITO (a-ZITO) matrix at a lower temperature (approximately 170 degree C) for a short period (≤20 min) during a bias test. The low-temperature BCM developed for this study obtained an efficient conventional annealed treatment (higher temperature), possessed energy-saving and speed advantages, and can be considered a candidate for application in photoelectric industries.

Study of the surface crystallization and resistance to dissolution of niobium phosphate glasses for nuclear waste immobilization

International Nuclear Information System (INIS)

Vieira, Heveline

2008-01-01

The surface crystallization and the dissolution rate of three phosphate glass compositions containing different amounts of niobium oxide were studied. The glasses were named Nb30, Nb37, and Nb44 according to the nominal content of niobium oxide in the glass composition. The three compositions were evaluated keeping the P 2 O 5 /K 2 O ratio constant and varying the amount of Nb 2 O 5 . These glasses were produced by melting appropriate chemical compounds at 1500 deg C for 0.5 hour. The crystalline phases which were nucleated on the glass surface after heat treatment were determined by X-ray diffraction. The crystalline structures depend on the amount of niobium oxide in the glass composition. The crystal morphologies were observed by using an optical microscope, and their characteristics are specific for each kind of crystalline phase. The crystal growth rate and the surface nuclei density were determined for each glass composition, and they depend on each crystalline phase nucleated on the surface. From the differential thermal analysis curves it was determined that the Nb44 glass containing 46.5 mol por cent of niobium oxide is the most thermally stable against crystallization when compared to the Nb30 and Nb37 glasses. According to the activation energies determined for crystal growth on the surface of each glass type, the Nb44 glass can also be considered the most resistant one against crystallization. The dissolution rate for the Nb44 glass after 14 days immersed in an aqueous solution with pH equals to 7 at 90 deg C is the lowest (9.0 x 10 -7 g. cm -2 . day -1 ) when compared to the other two glass compositions. The dissolution rates in acidic and neutral solutions of all studied glasses meet the international standards for materials which can be used in the immobilization of nuclear wastes. (author)

Optimization of a Liquid Crystal-based Sensory Platform for Monitoring Enzymatic Glucose Oxidation

Energy Technology Data Exchange (ETDEWEB)

Wei, Yibin; Jang, Chang-Hyun [Gachon University, Seongnam (Korea, Republic of)

2016-05-15

Managing glucose levels in human blood is extremely important for the treatment of diabetes. Here, an innovative sensory strategy has been developed to monitor the enzymatic activities of glucose and glucose oxidase by using confined liquid crystal (LC) birefringent droplet patterns. Acidic products released during the glucose oxidation process lead to a slight decrease in the pH of aqueous systems that can be monitored by pH-sensitive LC materials. Of the existing pH-sensitive LC materials, dodecanoic acid-doped 4-cyano-4'-pentylbiphenyl is inexpensive and easily adjusted to satisfy the 7.4 ± 0.05 pH requirement of human blood. Moreover, the orientational alignment of capillary-confined pH-responsive LCs can be disrupted at the aqueous/LC interface following a slight decrease in the critical pH of aqueous reaction systems, which results in an optical signal that can be observed with the naked eye by using polarizing optical microscopy. Based on the stable LC droplet patterns generated by the cylindrical confinement system, the functionalized LCs can selectively detect glucose at concentrations as low as 0.1 pM. This study further advances the previously reported LC-based glucose monitoring systems by reducing production costs and instituting a smarter LC sensory design. This improved system shows potential for the use in clinical bioassay applications.

Semiconductor monolayer assemblies with oriented crystal faces

KAUST Repository

Ma, Guijun; Takata, Tsuyoshi; Katayama, Masao; Zhang, Fuxiang; Moriya, Yosuke; Takanabe, Kazuhiro; Kubota, Jun; Domen, Kazunari

2012-01-01

Fabrication of two-dimensional monolayers of crystalline oxide and oxynitride particles was attempted on glass plate substrates. X-Ray diffraction patterns of the assemblies show only specific crystal facets, indicative of the uniform orientation of the particles on the substrate. The selectivity afforded by this immobilization technique enables the organization of randomly distributed polycrystalline powders in a controlled manner.

Chemical state analysis of oxide thin films using a high resolution double crystal X-ray fluorescence spectrometer

International Nuclear Information System (INIS)

Masuda, Hirohisa; Morinaga, Kenji; Ohta, Yoshio.

1995-01-01

The chemical state analysis of r.f.-sputtered amorphous oxide thin films was determined by a high resolution X-ray fluorescence spectrometer with double crystals. The polymerization degree of silicate anions in the silicate film was as same as a target (α-Quartz). The oxygen coordination number of Al 3+ ions in the aluminate film was different from a target (α-Al 2 O 3 ), and it was a mixture of 4 and 6 in a spinel-like structure. In CaO-SiO 2 and CaO-Al 2 O 3 films, when the film thickness is thin at the beginning of sputtering, the composition of films are in the shortage of CaO. But when the film thickness become thicker, the composition of films become as same as the target. From the results above, the chemical state of films and their variations with film thickness can be clarified by using the apparatus. (author)

Influence of metal induced crystallization parameters on the performance of polycrystalline silicon thin film transistors

International Nuclear Information System (INIS)

Pereira, L.; Barquinha, P.; Fortunato, E.; Martins, R.

2005-01-01

In this work, metal induced crystallization using nickel was employed to obtain polycrystalline silicon by crystallization of amorphous films for thin film transistor applications. The devices were produced through only one lithographic process with a bottom gate configuration using a new gate dielectric consisting of a multi-layer of aluminum oxide/titanium oxide produced by atomic layer deposition. The best results were obtained for TFTs with the active layer of poly-Si crystallized for 20 h at 500 deg. C using a nickel layer of 0.5 nm where the effective mobility is 45.5 cm 2 V -1 s -1 . The threshold voltage, the on/off current ratio and the sub-threshold voltage are, respectively, 11.9 V, 5.55x10 4 and 2.49 V/dec

Synthesis and growth of single crystals of PrCl3

International Nuclear Information System (INIS)

Pei, Jen Shieh.

1984-01-01

An efficient method for growth of high optical quality single crystals of PrCl 3 . The method consists in careful drying of the hydrated chloride, PrCl 3 . 7H 2 O, with a protective atmosphere of anhydrous HCl and Ar. A subsequent growth was done by the zone melting technique. The hydrated chloride had prepared from dissolution of the oxide Pr 6 O 11 in hydrochloric acid. The grown crystals had characterized fluorescence and x-ray diffraction measurements. (Author) [pt

NONLINEAR OPTICAL MOLECULAR CRYSTAL BASED ON 2,6-DIAMINOPYRIDINE: SYNTHESIS AND CHARACTERIZATION

Directory of Open Access Journals (Sweden)

I. M. Pavlovetc

2014-05-01

Full Text Available The paper deals with investigation of a new nonlinear optical material based on nonlinear optical chromophore (4-Nitrophenol and aminopyridine (2,6-Diaminopyridine. Calculation results are presented for molecular packing in the crystalline compound, based on the given components. According to these results the finite material must have a noncentrosymmetric lattice, which determines the presence of the second order nonlinear optical response. Investigations carried out in this work confirm these calculations. Results of experiments are given describing the co-crystallization of these components and the following re-crystallization of the obtained material. In order to get a monocrystal form, the optimal conditions for the synthesis of molecular crystals based on these components are determined. Sufficiently large homogeneous crystals are obtained, that gave the possibility to record their spectra in the visible and near infrared parts of the spectrum, to determine their nonlinear optical properties and the level of homogeneity. Their optical (optical transmission and optical laser damage threshold and nonlinear optical properties are presented. For observation and measurement of the nonlinear optical properties an installation was built which implements the comparative method for measurements of nonlinear optical properties. A potassium titanyl oxide phosphate crystal was used as a sample for comparison. Results are given for the conversion efficiency of the primary laser radiation in the second optical harmonic relative to the signal obtained on the potassium titanyl oxide phosphate crystal. Obtained results show that the molecular co-crystal based on 2,6-Diaminopyridine is a promising nonlinear optical material for generating the second optical harmonic on the Nd: YAG laser (532 nm.

HfO2 - rare earth oxide systems in the region with high content of rare earth oxide

International Nuclear Information System (INIS)

Shevchenko, A.V.; Lopato, L.M.

1982-01-01

Using the methods of annealing and hardenings (10 2 -10 4 deg/s cooling rate) and differential thermal analysis elements of state diagrams of HfO 2 - rare earth oxide (rare earths-La, Pr, Nd, Sm, Gd, Tb, Dy, Y, Er, Yb, Lu, Sc) systems from 1800 deg C up to melting in the range of 60-100 mol% rare earth oxide concentration were constructed. Regularities of HfQ 2 addition effect on high-temperature polymorphic transformations of rare earth oxides were studied. Results of investigation were discussed from viewpoint of crystal chemistry

HRTEM analysis on nanocrystalline BaTiO3 and PbTiO3: size effects on ferroelectric phase transition temperature

International Nuclear Information System (INIS)

Bursill, L.A.; Jiang, B.; Peng, J.L.; Zhong, W.L.; Zhang, P.L.

1997-01-01

High-Resolution Transmission Electron Microscopic studies of nanocrystaline particles of BaTiO 3 and PbTiO 3 are reported. There are characteristic differences observed for BaTiO 3 prepared using sol gel (SG) and steric acid gel (SAG) methods. The former exhibit a critical size below which there is no paraelectric/ferroelectric phase transition, whereas BaTiO 3 prepared via the SAG route remained cubic for all conditions. The SAG preparations always showed chemical intergrowth defects whereas the SG preparations were single phase. Atomic resolution images of both varieties showed interesting surface steps and surface relaxations/reconstructions of some facets. Nanocrystalline PbTiO 3 prepared by the SG route remains tetragonal, albeit with decreasing c/a ratio, down to 25nm diameter. HRTEM observations of nanocrystalline PbTiO 3 are also presented. X-ray diffraction, dielectric and Raman scattering measurements also demonstrate pronounced size effects. The relationship between the observed nanostructures and size effects on the physical properties is discussed. 6 refs., 1 tab., 6 figs

Non-equilibrium oxidation states of zirconium during early stages of metal oxidation

International Nuclear Information System (INIS)

Ma, Wen; Yildiz, Bilge; Herbert, F. William; Senanayake, Sanjaya D.

2015-01-01

The chemical state of Zr during the initial, self-limiting stage of oxidation on single crystal zirconium (0001), with oxide thickness on the order of 1 nm, was probed by synchrotron x-ray photoelectron spectroscopy. Quantitative analysis of the Zr 3d spectrum by the spectrum reconstruction method demonstrated the formation of Zr 1+ , Zr 2+ , and Zr 3+ as non-equilibrium oxidation states, in addition to Zr 4+ in the stoichiometric ZrO 2 . This finding resolves the long-debated question of whether it is possible to form any valence states between Zr 0 and Zr 4+ at the metal-oxide interface. The presence of local strong electric fields and the minimization of interfacial energy are assessed and demonstrated as mechanisms that can drive the formation of these non-equilibrium valence states of Zr