Si0.85Ge0.15 oxynitridation in nitric oxide/nitrous oxide ambient

International Nuclear Information System (INIS)

Dasgupta, Anindya; Takoudis, Christos G.; Lei Yuanyuan; Browning, Nigel D.

2003-01-01

Low temperature, nitric oxide (NO)/nitrous oxide (N 2 O) aided, sub-35 Aa Si 0.85 Ge 0.15 oxynitrides have been grown at 550 and 650 deg. C, while the oxynitridation feed gases have been preheated to 900 and 1000 deg. C, respectively, before entering the reaction zone. X-ray photoelectron spectroscopy and secondary ion mass spectroscopy (SIMS) data suggest that NO-assisted oxynitridation incorporates more nitrogen than the N 2 O-assisted one, while there is minimal Ge segregation towards the dielectric/substrate interface in both oxynitridation processes. Moreover, SIMS results suggest that nitrogen is distributed throughout the film in contrast to high temperature Si oxynitridation, where nitrogen incorporation takes place near the dielectric/substrate interface. Z-contrast imaging with scanning transmission electron microscopy shows that the oxynitride grown in NO at 650 degree sign C has a sharp interface with the bulk Si 0.85 Ge 0.15 , while the roughness of the dielectric/Si 0.85 Ge 0.15 substrate interface is less than 2 Aa. These results are discussed in the context of an overall mechanism of SiGe oxynitridation

Annealing effect on thermal conductivity and microhardness of carbon nanotube containing Se80Te16Cu4 glassy composites

Science.gov (United States)

Upadhyay, A. N.; Tiwari, R. S.; Singh, Kedar

2018-02-01

This study deals with the effect of thermal annealing on structural/microstructural, thermal and mechanical behavior of pristine Se80Te16Cu4 and carbon nanotubes (CNTs) containing Se80Te16Cu4 glassy composites. Pristine Se80Te16Cu4, 3 and 5 wt%CNTs-Se80Te16Cu4 glassy composites are annealed in the vicinity of glass transition temperature to onset crystallization temperature (340-380 K). X-ray diffraction (XRD) pattern revealed formation of polycrystalline phases of hexagonal CuSe and trigonal selenium. The indexed d-values in XRD patterns are in well conformity with the d-values obtained after the indexing of the ring pattern of selected area electron diffraction pattern of TEM images. The SEM investigation exhibited that the grain size of the CNTs containing Se80Te16Cu4 glassy composites increased with increasing annealing temperature and decreased at further higher annealing temperature. Thermal conductivity, microhardness exhibited a substantial increase with increasing annealing temperature of 340-360 K and slightly decreases for 380 K. The variation of thermal conductivity and microhardness can be explained by cross-linking formation and voids reduction.

Nitrogen bonding in aluminum oxynitride films

Energy Technology Data Exchange (ETDEWEB)

Wang, Paul W., E-mail: pwang@bradley.edu [Department of Physics, Bradley University, 1501 W. Bradley Ave., Peoria, IL 61625 (United States); Hsu, Jin-Cherng [Department of Physics, Fu Jen Catholic University, Hsinchuang, Taipei Hsien 24205, Taiwan (China); Lin, Yung-Hsin; Chen, Huang-Lu [Graduate Institute of Applied Science and Engineering, Fu Jen Catholic University, Hsinchuang, Taipei Hsien 24205, Taiwan (China)

2010-04-15

Assignment of oxidation states of N{sub 1s} in XPS spectra of aluminum oxynitride by curve fitting is difficult. The XPS curve fitting was previously discussed in the paper published in J. Non-Cryst. Solids, 224 (1998) 31, in which O{sub 1s} photoelectrons from GeO{sub 2} glass were used to illustrate how to fit the XPS spectra. Three different ways were pointed out to eliminate the ambiguity caused by curve fitting such as comparing the data to data from standard samples, investigating the continuous surface modifications caused by slowly sputtering the surface, and monitoring the continuous surface modifications due to gradual increases in surface species under heating, cooling, or irradiation. Our recent work in aluminum oxynitride films provides another example of how to fit the XPS spectra of N{sub 1s} by three different oxidation states of N{sup +}, N{sup 2+}, and N{sup 3+}, by comparison of the measured data to data from previously published results, and by the gradual changes of spectra as functions of the oxygen contents in the films. Three oxidation states in different nitrogen bonding in the aluminum oxynitride, AlO{sub 2}N, Al{sub 2}O{sub 5}N{sub 2}, and AlO{sub 3}N, were clearly deduced.

Study of the R-(Zr,W)-(O,N) (R = Y, Nd, Sm, Gd, Yb) oxynitride system

Energy Technology Data Exchange (ETDEWEB)

Tessier, Franck, E-mail: Franck.Tessier@univ-rennes1.fr [UMR CNRS 6226 ' Sciences Chimiques de Rennes' , equipe ' Verres et Ceramiques' , Universite de Rennes 1, 35042 Rennes cedex (France); Maillard, Pascal [UMR CNRS 6226 ' Sciences Chimiques de Rennes' , equipe ' Verres et Ceramiques' , Universite de Rennes 1, 35042 Rennes cedex (France); Orhan, Emmanuelle [Laboratoire Science des Procedes Ceramiques et Traitements de Surface, UMR CNRS 6638, Universite de Limoges, 123 Avenue Albert Thomas, 87060 Limoges cedex (France); Chevire, Francois [UMR CNRS 6226 ' Sciences Chimiques de Rennes' , equipe ' Verres et Ceramiques' , Universite de Rennes 1, 35042 Rennes cedex (France)

2010-02-15

The replacement of tantalum by the couple Zr/W within the RTa-O-N systems (R = Y, Nd, Sm, Gd, Yb), enables the preparation of novel oxide and oxynitride phases in the R-Zr-W-O-N system. R{sub 2}Zr{sub 2-x}W{sub x}O{sub 7+x} oxides exhibit the fluorite-type (x < 0.9) and scheelite (x {approx} 1) structures. Corresponding oxynitride compositions are of the fluorite-type and show different colors, for example in the case of ytterbium: pale yellow (x = 0.2 or 0.25), green (x = 0.5-0.8) and brown for the tungsten-rich samples (x = 0.9, 1). Photocatalytic activity measurements have been performed to investigate the overall water splitting behavior of these colored phases.

A novel LaFeO3−XNX oxynitride. Synthesis and characterization

International Nuclear Information System (INIS)

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

2013-01-01

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

Slag corrosion of gamma aluminium oxynitride

Energy Technology Data Exchange (ETDEWEB)

Wang Xidong; Li Wen Chao [Beijing Univ. of Science and Technology, BJ (China). Dept. of Physical Chemistry of Metals; Sichen Du; Seetharaman, S. [Royal Inst. of Tech., Stockholm (Sweden). Dept. of Materials Science and Technology

2002-03-01

Corrosion of {gamma}-aluminium oxynitride (AlON) by CaO-MgO-''FeO''-Al{sub 2}O{sub 3}-SiO{sub 2} melts corresponding to blast furnace slag was examined from 1693 to 1753 K under static and forced convection conditions. An intermediate layer was observed between the unreacted oxynitride and slag. After a certain time interval, the rate of the growth of this layer was found to be equal to the rate of the dissolution of the layer. Slag corrosion of AlON is a strongly thermally activated process, the overall activation energy being 1002 kJ/mol. The rate of corrosion was found to be significantly enhanced by the addition of ''FeO''. (orig.)

Sputtered titanium oxynitride coatings for endosseous applications: Physical and chemical evaluation and first bioactivity assays

Energy Technology Data Exchange (ETDEWEB)

Banakh, Oksana, E-mail: oksana.banakh@he-arc.ch [Institute of Applied Microtechnologies, Haute Ecole Arc Ingénierie (HES-SO), Eplatures-Grise 17, CH-2300 La Chaux-de-Fonds (Switzerland); Moussa, Mira, E-mail: mira.moussa@unige.ch [Laboratory of Biomaterials, University of Geneva, 19, rue Barthelemy Menn, CH-1205 Geneva (Switzerland); Matthey, Joel, E-mail: joel.matthey@he-arc.ch [Institute of Applied Microtechnologies, Haute Ecole Arc Ingénierie (HES-SO), Eplatures-Grise 17, CH-2300 La Chaux-de-Fonds (Switzerland); Pontearso, Alessandro, E-mail: alessandro.pontearso@he-arc.ch [Institute of Applied Microtechnologies, Haute Ecole Arc Ingénierie (HES-SO), Eplatures-Grise 17, CH-2300 La Chaux-de-Fonds (Switzerland); Cattani-Lorente, Maria, E-mail: maria.cattani-lorente@unige.ch [Laboratory of Biomaterials, University of Geneva, 19, rue Barthelemy Menn, CH-1205 Geneva (Switzerland); Sanjines, Rosendo, E-mail: rosendo.sanjines@epfl.ch [Ecole Polytechnique Fédérale de Lausanne (EPFL), Institute of Condensed Matter Physics, Station 3, CH-1015 Lausanne (Switzerland); Fontana, Pierre, E-mail: Pierre.Fontana@hcuge.ch [Haemostasis laboratory, Geneva University Hospital, Rue Gabrielle-Perret-Gentil 4, CH-1205 Geneva (Switzerland); Wiskott, Anselm, E-mail: anselm.wiskott@unige.ch [Laboratory of Biomaterials, University of Geneva, 19, rue Barthelemy Menn, CH-1205 Geneva (Switzerland); Durual, Stephane, E-mail: stephane.durual@unige.ch [Laboratory of Biomaterials, University of Geneva, 19, rue Barthelemy Menn, CH-1205 Geneva (Switzerland)

2014-10-30

Highlights: • Titanium oxynitride coatings (TiN{sub x}O{sub y}) with chemical composition ranging from TiN to TiO{sub 2} were deposited by magnetron sputtering from a metallic Ti target using a mixture of O{sub 2} + N{sub 2}. • The coatings structure as well as physical, chemical and mechanical properties progressively changes as a function of oxygen content in the TiN{sub x}O{sub y.} • All TiN{sub x}O{sub y} coatings show a significantly higher level of bioactivity as compared to bare Ti substrates (1.2 to 1.4 fold increase in cell proliferation). Despite variations in surface chemistry, topography and surface tension observed on films as a function of chemical composition, no significant differences in the films’ biological activity were observed after 3 days of testing. - Abstract: Titanium oxynitride coatings (TiN{sub x}O{sub y}) are considered a promising material for applications in dental implantology due to their high corrosion resistance, their biocompatibility and their superior hardness. Using the sputtering technique, TiN{sub x}O{sub y} films with variable chemical compositions can be deposited. These films may then be set to a desired value by varying the process parameters, that is, the oxygen and nitrogen gas flows. To improve the control of the sputtering process with two reactive gases and to achieve a variable and controllable coating composition, the plasma characteristics were monitored in-situ by optical emission spectroscopy. TiN{sub x}O{sub y} films were deposited onto commercially pure (ASTM 67) microroughened titanium plates by reactive magnetron sputtering. The nitrogen gas flow was kept constant while the oxygen gas flow was adjusted for each deposition run to obtain films with different oxygen and nitrogen contents. The physical and chemical properties of the deposited films were analyzed as a function of oxygen content in the titanium oxynitride. The potential application of the coatings in dental implantology was assessed by

Synthesis of nano-crystalline zirconium aluminium oxynitride (ZrAlON) composite films by dense plasma Focus device

Energy Technology Data Exchange (ETDEWEB)

Khan, I.A.; Hassan, M.; Hussain, T. [Department of Physics, GC University, 54000 Lahore (Pakistan); Ahmad, R., E-mail: ahriaz@gmail.com [Department of Physics, GC University, 54000 Lahore (Pakistan); Zakaullah, M. [Department of Physics, Quaid-i-Azam University, 45320 Islamabad (Pakistan); Rawat, R.S. [National Institute of Education, Nanyang Technological University, Singapore 637616 (Singapore)

2009-04-01

Zirconium aluminium oxynitride multiphase composite film is deposited on zirconium substrate using energetic nitrogen ions delivered from dense plasma Focus device. X-ray diffractometer (XRD) results show that five Focus shots are sufficient to initiate the nucleation of ZrN and Al{sub 2}O{sub 3} whereas 10 Focus shots are sufficient to initiate the nucleation of AlN. XRD results reveal that crystal growth of nitrides/oxides increases by increasing Focus shots (up to 30 Focus shots) and resputtering of the previously deposited film is taken place by further increase in Focus shots (40 Focus shots). Scanning electron microscopic (SEM) results indicate the uniform distribution of spherical grains ({approx}35 nm). A smoother surface is observed for 20 Focus shots at 0 deg. angular position. SEM results also show a net-type microstructure (thread like features) of the sample treated for 30 Focus shots whereas rough surface morphology is observed for 40 Focus shots. Energy dispersive spectroscopic profiles show the distribution of different elements present in the deposited composite films. A typical microhardness value of the deposited composite films is 5255 {+-} 10 MPa for 10 grams imposed load which is 3.3 times than the microhardness values of unexposed sample. The microhardness values of the exposed samples increases with increasing Focus shots (up to 30 Focus shots) and decreases for 40 Focus shots treatment due to resputtering of the previously deposited composite film. The microhardness values of the composite films decreases by increasing the sample's angular position.

Germanium nitride and oxynitride films for surface passivation of Ge radiation detectors

Energy Technology Data Exchange (ETDEWEB)

Maggioni, G., E-mail: maggioni@lnl.infn.it [Dipartimento di Fisica e Astronomia G. Galilei, Università di Padova, Via Marzolo 8, I-35131 Padova (Italy); Laboratori Nazionali di Legnaro, Istituto Nazionale di Fisica Nucleare, Viale dell’Universita’2, I-35020 Legnaro, Padova (Italy); Carturan, S. [Dipartimento di Fisica e Astronomia G. Galilei, Università di Padova, Via Marzolo 8, I-35131 Padova (Italy); Laboratori Nazionali di Legnaro, Istituto Nazionale di Fisica Nucleare, Viale dell’Universita’2, I-35020 Legnaro, Padova (Italy); Fiorese, L. [Laboratori Nazionali di Legnaro, Istituto Nazionale di Fisica Nucleare, Viale dell’Universita’2, I-35020 Legnaro, Padova (Italy); Dipartimento di Ingegneria dei Materiali e delle Tecnologie Industriali, Università di Trento, Via Mesiano 77, I-38050 Povo, Trento (Italy); Pinto, N.; Caproli, F. [Scuola di Scienze e Tecnologie, Sezione di Fisica, Università di Camerino, Via Madonna delle Carceri 9, Camerino (Italy); INFN, Sezione di Perugia, Perugia (Italy); Napoli, D.R. [Laboratori Nazionali di Legnaro, Istituto Nazionale di Fisica Nucleare, Viale dell’Universita’2, I-35020 Legnaro, Padova (Italy); Giarola, M.; Mariotto, G. [Dipartimento di Informatica—Università di Verona, Strada le Grazie 15, I-37134 Verona (Italy)

2017-01-30

Highlights: • A surface passivation method for HPGe radiation detectors is proposed. • Highly insulating GeNx- and GeOxNy-based layers are deposited at room temperature. • Deposition parameters affect composition and electrical properties of the layers. • The improved performance of a GeNx-coated HPGe diode is assessed. - Abstract: This work reports a detailed investigation of the properties of germanium nitride and oxynitride films to be applied as passivation layers to Ge radiation detectors. All the samples were deposited at room temperature by reactive RF magnetron sputtering. A strong correlation was found between the deposition parameters, such as deposition rate, substrate bias and atmosphere composition, and the oxygen and nitrogen content in the film matrix. We found that all the films were very poorly crystallized, consisting of very small Ge nitride and oxynitride nanocrystallites, and electrically insulating, with the resistivity changing from three to six orders of magnitude as a function of temperature. A preliminary test of these films as passivation layers was successfully performed by depositing a germanium nitride film on the intrinsic surface of a high-purity germanium (HPGe) diode and measuring the improved performance, in terms of leakage current, with respect to a reference passivated diode. All these interesting results allow us to envisage the application of this coating technology to the surface passivation of germanium-based radiation detectors.

NEXAFS characterization and reactivity studies of bimetallic vanadium molybdenum oxynitride hydrotreating catalysts

Energy Technology Data Exchange (ETDEWEB)

Kapoor, R.; Oyama, S.T. [Virginia Polytechnic Inst., Blacksburg, VA (United States); Fruehberger, B.; Chen, J.G. [Exxon Research and Engineering Company, Annandale, NJ (United States)

1997-02-27

The surface and bulk compositions of vanadium molybdenum oxynitride (V{sub 2}MoO{sub 1.7}N{sub 2.4}), prepared by temperature-programmed reaction (TPR) of vanadium molybdenum oxide (V{sub 2}MoO{sub 8}) with ammonia, have been characterized using near-edge X-ray absorption fine structure (NEXAFS) spectroscopy. The NEXAFS data were recorded at the K-edges of nitrogen and oxygen, the L-edge of vanadium, and the M-edge of molybdenum. The nitrogen K-edge region of V-Mo oxynitride shows the characteristic NEXAFS features of early-transition-metal nitrides, although these features are different from those of either VN or Mo{sub 2}N. Furthermore, comparison of the electron yield and fluorescence yield measurements also reveals that the oxidation state is different for vanadium near the surface region and for vanadium in the bulk, which is estimated to be 2.8 {+-} 0.3 and 3.8 {+-} 0.3, respectively. The oxidation state of bulk molybdenum is also estimated to be 4.4 {+-} 0.3. The X-ray diffraction pattern shows that the bulk phase of the bimetallic oxide is different from the pure monometallic oxide phases but the oxynitride has a cubic structure that resembles the pure vanadium and molybdenum nitride phases. The V-Mo oxide as prepared shows a preferential orientation of [001] crystallographic planes which is lost during the nitridation process. This shows that the solid state transformation V{sub 2}MoO{sub 8} {yields} V{sub 2}MoO{sub 1.7}N{sub 2.4} is not topotactic. 27 refs., 8 figs., 1 tab.

Structures and photocatalytic behavior of tantalum-oxynitride thin films

International Nuclear Information System (INIS)

Hsieh, J.H.; Li, Chuan; Liang, H.C.

2011-01-01

Tantalum oxynitride films were created by direct nitridation/oxidation during rapid thermal annealing at temperatures 450-700 deg. C. Instead of during deposition, this post process may be proved to be an alternative way to make transition metallic oxynitride films. With sufficient supply of oxygen flow (≥ 30 sccm), TaO x N y was formed as examined from X-ray diffraction (XRD) analysis. This oxynitride film has a broad optical absorption over the range of visible light and sufficient photocatalytic function. For optical absorption, the films' transmittance and reflectance were measured by a UV-VIS-NIR spectrophotometer with wavelengths ranging from 300 to 900 nm. The broad visible light absorption is associated with the formation of band gap in TaO x N y film, which was examined by the theoretical calculations combining the Beer-Lambert law and Tauc formula. Lastly, the photocatalysis of TaO x N y was gauged by the photodegradation test which measured the reduction of light absorbance affected by the decomposition of methylene blue (C 16 H 18 N 3 SCl.3H 2 O) on TaO x N y under visible light irradiation.

AC-Conductivity measurements on γ-aluminium oxynitride

NARCIS (Netherlands)

Willems, H.X.; Hal, van P.F.; Metselaar, R.; With, de G.

1995-01-01

AC-conductivity measurements were performed on aluminium oxynitrides (Alons) because of their interesting defect structure. Although it became apparent that these Alons are not stable in the temperature range used, the electrical properties of the materials could be measured with impedance

Young's modulus and fracture toughness of silicon nitride ceramics at elevated temperature

Energy Technology Data Exchange (ETDEWEB)

Rouxel, T. [Rennes Univ. (France). Lab. de Recherche en Mecanique Applicee

2002-07-01

The temperature dependencies of Young's modulus (E) and fracture toughness (K{sub 1c}) of several silicon nitride-based monolithic and composite materials, are reviewed. A transition range is observed between 1130 and 1180 C on the E(T) curves, which is systematically 150 to 200 C above the T{sub g} of oxynitride glasses of composition close to that of the intergranular glassy pockets. It is thus supposed that this transition reflects the behaviour of the interfacial glassy films. The higher the glassy phase content, the higher is the temperature sensitivity. The presence of SiC particles greatly attenuates the sensitivity. Thus, Young's modulus decreases more slowly with temperature and fracture toughness changes little up to 1300 C. The K{sub 1c} (T) curves exhibit four different stages which are discussed and interpreted on the basis of a theoretical model. (orig.)

Composition-induced structural, electrical, and magnetic phase transitions in AX-type mixed-valence cobalt oxynitride epitaxial thin films

Energy Technology Data Exchange (ETDEWEB)

Takahashi, Jumpei; Oka, Daichi [Department of Chemistry, School of Science, The University of Tokyo, 7-3-1 Hongo, Bunkyo, Tokyo 113-0033 (Japan); Kanagawa Academy of Science and Technology (KAST), 3-2-1 Sakado, Takatsu, Kawasaki 213-0012 (Japan); Hirose, Yasushi, E-mail: hirose@chem.s.u-tokyo.ac.jp; Yang, Chang; Fukumura, Tomoteru; Hasegawa, Tetsuya [Department of Chemistry, School of Science, The University of Tokyo, 7-3-1 Hongo, Bunkyo, Tokyo 113-0033 (Japan); Kanagawa Academy of Science and Technology (KAST), 3-2-1 Sakado, Takatsu, Kawasaki 213-0012 (Japan); CREST, Japan Science and Technology Agency, 7-3-1 Hongo, Bunkyo, Tokyo 113-0033 (Japan); Nakao, Shoichiro [Kanagawa Academy of Science and Technology (KAST), 3-2-1 Sakado, Takatsu, Kawasaki 213-0012 (Japan); CREST, Japan Science and Technology Agency, 7-3-1 Hongo, Bunkyo, Tokyo 113-0033 (Japan); Harayama, Isao; Sekiba, Daiichiro [University of Tsukuba Tandem Accelerator Complex (UTTAC), 1-1-1 Tennoudai, Tsukuba, Ibaraki 305-8577 (Japan)

2015-12-07

Synthesis of mid- to late-transition metal oxynitrides is generally difficult by conventional thermal ammonolysis because of thermal instability. In this letter, we synthesized epitaxial thin films of AX-type phase-pure cobalt oxynitrides (CoO{sub x}N{sub y}) by using nitrogen-plasma-assisted pulsed laser deposition and investigated their structural, electrical, and magnetic properties. The CoO{sub x}N{sub y} thin films with 0 ≤ y/(x + y) ≤ 0.63 grown on MgO (100) substrates showed a structural phase transition from rock salt (RS) to zinc blend at the nitrogen content y/(x + y) ∼ 0.5. As the nitrogen content increased, the room-temperature electrical resistivity of the CoO{sub x}N{sub y} thin films monotonically decreased from the order of 10{sup 5} Ω cm to 10{sup −4} Ω cm. Furthermore, we observed an insulator-to-metal transition at y/(x + y) ∼ 0.34 in the RS-CoO{sub x}N{sub y} phase, which has not yet been reported in Co{sup 2+}/Co{sup 3+} mixed-valence cobalt oxides with octahedral coordination. The low resistivity in the RS-CoO{sub x}N{sub y} phase, on the 10{sup −3} Ω cm order, may have originated from the intermediate spin state of Co{sup 3+} stabilized by the lowered crystal field symmetry of the CoO{sub 6−n}N{sub n} octahedra (n = 1, 2,…5). Magnetization measurements suggested that a magnetic phase transition occurred in the RS-CoO{sub x}N{sub y} films during the insulator-to-metal transition. These results demonstrate that low-temperature epitaxial growth is a promising approach for exploring novel electronic functionalities in oxynitrides.

Composition-induced structural, electrical, and magnetic phase transitions in AX-type mixed-valence cobalt oxynitride epitaxial thin films

International Nuclear Information System (INIS)

Takahashi, Jumpei; Oka, Daichi; Hirose, Yasushi; Yang, Chang; Fukumura, Tomoteru; Hasegawa, Tetsuya; Nakao, Shoichiro; Harayama, Isao; Sekiba, Daiichiro

2015-01-01

Synthesis of mid- to late-transition metal oxynitrides is generally difficult by conventional thermal ammonolysis because of thermal instability. In this letter, we synthesized epitaxial thin films of AX-type phase-pure cobalt oxynitrides (CoO x N y ) by using nitrogen-plasma-assisted pulsed laser deposition and investigated their structural, electrical, and magnetic properties. The CoO x N y thin films with 0 ≤ y/(x + y) ≤ 0.63 grown on MgO (100) substrates showed a structural phase transition from rock salt (RS) to zinc blend at the nitrogen content y/(x + y) ∼ 0.5. As the nitrogen content increased, the room-temperature electrical resistivity of the CoO x N y thin films monotonically decreased from the order of 10 5  Ω cm to 10 −4  Ω cm. Furthermore, we observed an insulator-to-metal transition at y/(x + y) ∼ 0.34 in the RS-CoO x N y phase, which has not yet been reported in Co 2+ /Co 3+ mixed-valence cobalt oxides with octahedral coordination. The low resistivity in the RS-CoO x N y phase, on the 10 −3  Ω cm order, may have originated from the intermediate spin state of Co 3+ stabilized by the lowered crystal field symmetry of the CoO 6−n N n octahedra (n = 1, 2,…5). Magnetization measurements suggested that a magnetic phase transition occurred in the RS-CoO x N y films during the insulator-to-metal transition. These results demonstrate that low-temperature epitaxial growth is a promising approach for exploring novel electronic functionalities in oxynitrides

Optimization of silicon oxynitrides by plasma-enhanced chemical vapor deposition for an interferometric biosensor

Science.gov (United States)

Choo, Sung Joong; Lee, Byung-Chul; Lee, Sang-Myung; Park, Jung Ho; Shin, Hyun-Joon

2009-09-01

In this paper, silicon oxynitride layers deposited with different plasma-enhanced chemical vapor deposition (PECVD) conditions were fabricated and optimized, in order to make an interferometric sensor for detecting biochemical reactions. For the optimization of PECVD silicon oxynitride layers, the influence of the N2O/SiH4 gas flow ratio was investigated. RF power in the PEVCD process was also adjusted under the optimized N2O/SiH4 gas flow ratio. The optimized silicon oxynitride layer was deposited with 15 W in chamber under 25/150 sccm of N2O/SiH4 gas flow rates. The clad layer was deposited with 20 W in chamber under 400/150 sccm of N2O/SiH4 gas flow condition. An integrated Mach-Zehnder interferometric biosensor based on optical waveguide technology was fabricated under the optimized PECVD conditions. The adsorption reaction between bovine serum albumin (BSA) and the silicon oxynitride surface was performed and verified with this device.

Photoswitchable molecular dipole antennas with tailored coherent coupling in glassy composite

DEFF Research Database (Denmark)

Elbahri, Mady; Zillohu, Ahnaf Usman; Gothe, Bastian

2015-01-01

. We also introduce the concept of 'tailored molecular photonic coupling' while highlighting the role of interferences for the design of optically active media by adjusting the photonic response of the medium with the real and imaginary refractive index of photoswitchable molecules in the 'ON' state...... alteration of photochromic molecular dipole antennas. We successfully demonstrate the concept of Brewster wavelength, which is based on the dipolar interaction between radiating dipoles and the surrounding matrix possessing a net dipole moment, as a key tool for highly localized sensing of matrix polarity....... Our results enhance our fundamental understanding of coherent dipole radiation and open a new vein of research based on glassy disordered dipolar composites that act as macroscopic antenna with cooperative action; furthermore, these results have important implications for new design rules of tailored...

Optical, electrical and mechanical properties of the tantalum oxynitride thin films deposited by pulsing reactive gas sputtering

International Nuclear Information System (INIS)

Le Dreo, H.; Banakh, O.; Keppner, H.; Steinmann, P.-A.; Briand, D.; Rooij, N.F. de

2006-01-01

Thin films of tantalum oxynitride were prepared by reactive magnetron sputtering using a Ta target and N 2 and O 2 as reactive gases. The nitrogen flow was kept constant while the oxygen flow was pulsed periodically. The film composition evolves progressively from TaO 0.25 N 1.51 to TaO 2.42 N 0.25 while increasing the oxygen pulse duty cycle without any abrupt change in the elemental content. The optical transmission spectra of the films deposited on glass show a 'blue shift' of the absorption edge with increasing oxygen content. X-ray diffraction (XRD) patterns of all films exhibit broad peaks typical for nanocrystalline materials. Cross-section film morphology is rather featureless and surface topography is smooth exhibiting very small grains, in agreement with the results obtained by XRD. The optical properties of the films are very sensitive to their chemical composition. All films exhibit semiconducting behaviour with an optical band gap changing from 1.85 to 4.0 eV with increasing oxygen content. In order to evaluate the potential of the tantalum oxynitride films for microelectronic applications some Ta-O-N films were integrated in a MOS structure. The results of the capacitance-voltage measurements of the system Al//Ta-O-N//p-Si are discussed with respect to the chemical composition of the Ta-O-N films

On the existence of europium aluminum oxynitrides with a magnetoplumbite or beta-alumina type structure

NARCIS (Netherlands)

Hintzen, H.T.J.M.; Hanssen, R.; Jansen, S.R.; Metselaar, R.

1999-01-01

In the literature confusion exists concerning the structure type, the valence of europium, and the amount of nitrogen incorporation of the compound europium aluminum oxynitride. By using X-ray diffraction and luminescence measurements, we show that europium aluminum oxynitride has the

Hydrogen distribution in oxynitride/oxide structures

NARCIS (Netherlands)

Oude Elferink, J.B.; Heide, U.A. van der; Arnold Bik, W.M.; Habraken, F.H.P.M.; Weg, W.F. van der

1987-01-01

Silicon oxynitride films with five different O/N ratios were deposited with low pressure chemical vapor deposition on a silicon substrate covered with an oxide. The films were subjected to subsequent post-deposition anneals in N2 and H2 at 1000°C, and a H plasma at 300°C to obtain information about

Effects of Xylem-Sap Composition on Glassy-Winged Sharpshooter (Hemiptera: Cicadellidae) Egg Maturation on High- and Low-Quality Host Plants.

Science.gov (United States)

Sisterson, Mark S; Wallis, Christopher M; Stenger, Drake C

2017-04-01

Glassy-winged sharpshooters must feed as adults to produce mature eggs. Cowpea and sunflower are both readily accepted by the glassy-winged sharpshooter for feeding, but egg production on sunflower was reported to be lower than egg production on cowpea. To better understand the role of adult diet in egg production, effects of xylem-sap chemistry on glassy-winged sharpshooter egg maturation was compared for females confined to cowpea and sunflower. Females confined to cowpea consumed more xylem-sap than females held on sunflower. In response, females held on cowpea produced more eggs, had heavier bodies, and greater lipid content than females held on sunflower. Analysis of cowpea and sunflower xylem-sap found that 17 of 19 amino acids were more concentrated in cowpea xylem-sap than in sunflower xylem-sap. Thus, decreased consumption of sunflower xylem-sap was likely owing to perceived lower quality, with decreased egg production owing to a combination of decreased feeding and lower return per unit volume of xylem-sap consumed. Examination of pairwise correlation coefficients among amino acids indicated that concentrations of several amino acids within a plant species were correlated. Principal component analyses identified latent variables describing amino acid composition of xylem-sap. For females held on cowpea, egg maturation was affected by test date, volume of excreta produced, and principal components describing amino acid composition of xylem-sap. Principal component analyses aided in identifying amino acids that were positively or negatively associated with egg production, although determining causality with respect to key nutritional requirements for glassy-winged sharpshooter egg production will require additional testing. Published by Oxford University Press on behalf of Entomological Society of America 2017. This work is written by US Government employees and is in the public domain in the US.

Neutron diffraction of γ-aluminium oxynitride

NARCIS (Netherlands)

Willems, H.X.; With, de G.; Metselaar, R.; Helmholdt, R.B.; Petersen, K.K.

1993-01-01

Neutron diffraction expts. were performed on Al oxynitride (Alon) powders with compns. corresponding to 67.5, 73 and 77.5 mol.% Al2O3. The 73 mol.% powder was produced by reacting Al2O3 and AlN powders for 3 h at 1750 Deg. After reaction the resultant powder was ground with a mortar and pestle to

Further studies on the lithium phosphorus oxynitride solid electrolyte

International Nuclear Information System (INIS)

Pichonat, Tristan; Lethien, Christophe; Tiercelin, Nicolas; Godey, Sylvie; Pichonat, Emmanuelle; Roussel, Pascal; Colmont, Marie; Rolland, Paul Alain

2010-01-01

First step in the way to the fabrication of an all-solid microbattery for autonomous wireless sensor node, amorphous thin solid films of lithium phosphorus oxynitride (LiPON) were prepared by radio-frequency sputtering of a mixture target of P 2 O 5 /Li 2 O in ambient nitrogen atmosphere. The morphology, composition, and ionic conductivity were characterized by scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, and A.C. impedance spectroscopy. With a thickness of 1.4 μm, the obtained LiPON amorphous layer provided an ionic conductivity close to 6 x 10 -7 S cm -1 at room temperature. MicroRaman UV spectroscopy study was successfully carried out for the first time on LiPON thin films to complete the characterization and bring further information on LiPON structure.

Oxynitrides decorated 316L SS for potential bioimplant application

Science.gov (United States)

Saravanan Kaliaraj, Gobi; Kumar, N.

2018-03-01

Titanium oxynitride (TiON) and zirconium oxynitride (ZrON) were deposited onto 316L stainless steel (316L SS) using reactive magnetron sputtering technique. The monoclinic and cubic phase of TiON and ZrON were obtained by x-ray diffraction (XRD). Nanoindentation and wear test analysis exhibited the better mechanical properties of TiON and ZrON films. Wettability studies showed hydrophilic nature on coated films; whereas bare 316L SS substrate was least hydrophilic. Drastic reduction of bacterial adhesion (Pseudomonas aeruginosa), as well as biofilm formation, was observed in both the films at different time duration. TiON and ZrON films were exhibited excellent hemocompatibility by preventing the platelet activation. Furthermore, the coated films exhibited corrosion protection in presence and absence of hydrogen peroxide (H2O2) in artificial blood plasma (ABP) solution.

Optical and electrical properties of negatively charged aluminium oxynitride films

Energy Technology Data Exchange (ETDEWEB)

Jang, Kyungsoo; Jung, Sungwook; Lee, Jeoungin; Lee, Kwangsoo; Kim, Jaehong; Son, Hyukjoo [School of information and communication Engineering, Sungkyunkwan University, 300 Chunchun-dong, Jangan-gu, Suwon, 440-746 (Korea, Republic of); Yi, Junsin [School of information and communication Engineering, Sungkyunkwan University, 300 Chunchun-dong, Jangan-gu, Suwon, 440-746 (Korea, Republic of)], E-mail: yi@yurim.ac.kr

2008-11-03

Aluminium oxynitride (AlON) thin films were deposited by Radio Frequency (RF) magnetron sputtering on n-type silicon (Si) substrate of (100) orientation using argon (Ar) and oxygen (O{sub 2}) gases at substrate temperature of 450 {sup o}C. To know the change in electrical properties with gases ratio, a deposition was carried out for 140 s with Ar:O{sub 2} ratio changed from 1:3 to 4:3. After that, electrical properties of Metal-Insulator-Semiconductor (MIS) structure with AlON was analyzed. For Ar:O{sub 2} ratios from 1:3 to 4:3, all samples showed characteristics of negative charge. In particular, when Ar:O{sub 2} were 2:3 and 3:3, the value of flatband voltage in normal C-V curve showed above 14 V. The composition of the AlON in the film was investigated using X-ray Photoelectron Spectroscopy (XPS). The flatband voltages (V{sub FB}) in C-V curves were found to depend on compositions. The characteristics of photon energy band gap were obtained by UV/VIS spectrum.

Electrical and physical characterizations of the effects of oxynitridation and wet oxidation at the interface of SiO2/4H-SiC(0001) and (000\\bar{1})

Science.gov (United States)

Shiomi, Hiromu; Kitai, Hidenori; Tsujimura, Masatoshi; Kiuchi, Yuji; Nakata, Daisuke; Ono, Shuichi; Kojima, Kazutoshi; Fukuda, Kenji; Sakamoto, Kunihiro; Yamasaki, Kimiyohi; Okumura, Hajime

2016-04-01

The effects of oxynitridation and wet oxidation at the interface of SiO2/4H-SiC(0001) and (000\\bar{1}) were investigated using both electrical and physical characterization methods. Hall measurements and split capacitance-voltage (C-V) measurements revealed that the difference in field-effect mobility between wet oxide and dry oxynitride interfaces was mainly attributed to the ratio of the mobile electron density to the total induced electron density. The surface states close to the conduction band edge causing a significant trapping of inversion carriers were also evaluated. High-resolution Rutherford backscattering spectroscopy (HR-RBS) analysis and high-resolution elastic recoil detection analysis (HR-ERDA) were employed to show the nanometer-scale compositional profile of the SiC-MOS interfaces for the first time. These analyses, together with cathode luminescence (CL) spectroscopy and transmission electron microscopy (TEM), suggested that the deviations of stoichiometry and roughness at the interface defined the effects of oxynitridation and wet oxidation at the interface of SiO2/4H-SiC(0001) and (000\\bar{1}).

Method of forming aluminum oxynitride material and bodies formed by such methods

Science.gov (United States)

Bakas, Michael P [Ammon, ID; Lillo, Thomas M [Idaho Falls, ID; Chu, Henry S [Idaho Falls, ID

2010-11-16

Methods of forming aluminum oxynitride (AlON) materials include sintering green bodies comprising aluminum orthophosphate or another sacrificial material therein. Such green bodies may comprise aluminum, oxygen, and nitrogen in addition to the aluminum orthophosphate. For example, the green bodies may include a mixture of aluminum oxide, aluminum nitride, and aluminum orthophosphate or another sacrificial material. Additional methods of forming aluminum oxynitride (AlON) materials include sintering a green body including a sacrificial material therein, using the sacrificial material to form pores in the green body during sintering, and infiltrating the pores formed in the green body with a liquid infiltrant during sintering. Bodies are formed using such methods.

Electronic structure simulation of chromium aluminum oxynitride by discrete variational-Xα method and X-ray photoelectron spectroscopy

International Nuclear Information System (INIS)

Choi, Youngmin; Chang, Hyunju; Lee, Jae Do; Kim, Eunah; No, Kwangsoo

2002-01-01

We use a first-principles discrete variational (DV)-Xα method to investigate the electronic structure of chromium aluminum oxynitride. When nitrogen is substituted for oxygen in the Cr-Al-O system, the N2p level appears in the energy range between O2p and Cr3d levels. Consequently, the valence band of chromium aluminum oxynitride becomes broader and the band gap becomes smaller than that of chromium aluminum oxide, which is consistent with the photoelectron spectra for the valence band using X-ray photoelectron spectroscopy (XPS) and ultraviolet photoelectron spectroscopy (UPS). We expect that this valence band structure of chromium aluminum oxynitride will modify the transmittance slope which is a requirement for photomask application. (author)

Computational study on oxynitride perovskites for CO_2 photoreduction

International Nuclear Information System (INIS)

Hafez, Ahmed M.; Zedan, Abdallah F.; AlQaradawi, Siham Y.; Salem, Noha M.; Allam, Nageh K.

2016-01-01

Highlights: • Oxynitride perovskites are investigated for photoelectrochemical CO_2 reduction. • They have small electron and hole effective masses, rendering higher mobility. • The effect of cation size on the band gap is investigated and discussed. • W-doping allowed the selection of specific CO_2 reduction products. - Abstract: The photocatalytic conversion of CO_2 into chemical fuels is an attractive route for recycling this greenhouse gas. However, the large scale application of such approach is limited by the low selectivity and activity of the currently used photocatalysts. Using first principles calculations, we report on the selection of optimum oxynitride perovskites as photocatalysts for photoelectrochemical CO_2 reduction. The results revealed six perovskites that perfectly straddle the carbon dioxide redox potential; namely, BaTaO_2N, SrTaO_2N, CaTaO_2N, LaTiO_2N, BaNbO_2N, and SrNbO_2N. The electronic structure and the effective mass of the selected candidates are discussed in details, the partial and total density of states illustrated the orbital hybridization and the contribution of each element in the valence and conduction band minima. The effect of cation size in the ABO_2N perovskites on the band gap is investigated and discussed. The optical properties of the selected perovskites are calculated to account for their photoactivity. Moreover, the effect of W doping on improving the selectivity of perovskites toward specific hydrocarbon product (methane) is discussed in details. This study reveals the promising optical and structural properties of oxynitride perovskite candidates for CO_2 photoreduction.

Electronic structure simulation of chromium aluminum oxynitride by discrete variational-X{alpha} method and X-ray photoelectron spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Choi, Youngmin; Chang, Hyunju; Lee, Jae Do [Korea Research Inst. of Chemical Technology, Taejon (Korea); Kim, Eunah; No, Kwangsoo [Korea Advanced Inst. of Science and Technology, Taejon (Korea)

2002-09-01

We use a first-principles discrete variational (DV)-X{alpha} method to investigate the electronic structure of chromium aluminum oxynitride. When nitrogen is substituted for oxygen in the Cr-Al-O system, the N2p level appears in the energy range between O2p and Cr3d levels. Consequently, the valence band of chromium aluminum oxynitride becomes broader and the band gap becomes smaller than that of chromium aluminum oxide, which is consistent with the photoelectron spectra for the valence band using X-ray photoelectron spectroscopy (XPS) and ultraviolet photoelectron spectroscopy (UPS). We expect that this valence band structure of chromium aluminum oxynitride will modify the transmittance slope which is a requirement for photomask application. (author)

Electrocatalytic reduction of oxygen at glassy carbon electrode modified by polypyrrole/anthraquinones composite film in various pH media

International Nuclear Information System (INIS)

Valarselvan, S.; Manisankar, P.

2011-01-01

Graphical abstract: The electrocatalytic reduction of dioxygen by one mono and four dihydroxy derivatives of 9,10-anthraquinone (AQ) incorporated in polypyrrole (PPy) matrix on glassy carbon electrode has been investigated. AQ and PPy composite film showed excellent electrocatalytic performance for the reduction of O 2 to H 2 O 2 . Highlights: → Hydroxyl derivatives of anthraquinones as electrocatalysts for dioxygen reduction. → AQ/PPy composite film on GC electrode exhibits potent electrocatalytic activity. → Substituent groups influence electrocatalytic dioxygen reduction. → Surface coverage varies the rate of electrocatalytic dioxygen reduction. - Abstract: The electrocatalytic reduction of dioxygen by one mono and four dihydroxy derivatives of 9,10-anthraquinone (AQ) incorporated in polypyrrole (PPy) matrix on glassy carbon electrode has been investigated. The electrochemical behaviour of the modified electrodes was examined in various pH media and both the formal potential of anthraquinones and reduction potential of dioxygen exhibited pH dependence. AQ and PPy composite film showed excellent electrocatalytic performance for the reduction of O 2 to H 2 O 2 . pH 6.0 was chosen as the most suitable medium to study the electrocatalysis by comparing the peak potential of oxygen reduction and enhancement in peak current for oxygen reduction. The diffusion coefficient values of AQ at the modified electrodes and the number of electrons involved in AQ reduction were evaluated by chronoamperometric and chronocoulometric techniques, respectively. In addition, hydrodynamic voltammetric studies showed the involvement of two electrons in O 2 reduction. The mass specific activity of AQ used, the diffusion coefficient of oxygen and the heterogeneous rate constants for the oxygen reduction at the surface of modified electrodes were also determined by rotating disk voltammetry.

Early stage oxynitridation process of Si(001) surface by NO gas: Reactive molecular dynamics simulation study

International Nuclear Information System (INIS)

Cao, Haining; Kim, Seungchul; Lee, Kwang-Ryeol; Srivastava, Pooja; Choi, Keunsu

2016-01-01

Initial stage of oxynitridation process of Si substrate is of crucial importance in fabricating the ultrathin gate dielectric layer of high quality in advanced MOSFET devices. The oxynitridation reaction on a relaxed Si(001) surface is investigated via reactive molecular dynamics (MD) simulation. A total of 1120 events of a single nitric oxide (NO) molecule reaction at temperatures ranging from 300 to 1000 K are statistically analyzed. The observed reaction kinetics are consistent with the previous experimental or calculation results, which show the viability of the reactive MD technique to study the NO dissociation reaction on Si. We suggest the reaction pathway for NO dissociation that is characterized by the inter-dimer bridge of a NO molecule as the intermediate state prior to NO dissociation. Although the energy of the inter-dimer bridge is higher than that of the intra-dimer one, our suggestion is supported by the ab initio nudged elastic band calculations showing that the energy barrier for the inter-dimer bridge formation is much lower. The growth mechanism of an ultrathin Si oxynitride layer is also investigated via consecutive NO reactions simulation. The simulation reveals the mechanism of self-limiting reaction at low temperature and the time evolution of the depth profile of N and O atoms depending on the process temperature, which would guide to optimize the oxynitridation process condition.

Early stage oxynitridation process of Si(001) surface by NO gas: Reactive molecular dynamics simulation study

Energy Technology Data Exchange (ETDEWEB)

Cao, Haining; Kim, Seungchul; Lee, Kwang-Ryeol, E-mail: krlee@kist.re.kr [Computational Science Research Center, Korea Institute of Science and Technology, 5, Hwarangno 14-gil, Seongbuk-gu, Seoul 02792 (Korea, Republic of); Department of Nanomaterial Science and Technology, Korea University of Science and Technology, 217 Gajeong-ro, Yuseong-gu, Daejeon 34113 (Korea, Republic of); Srivastava, Pooja; Choi, Keunsu [Computational Science Research Center, Korea Institute of Science and Technology, 5, Hwarangno 14-gil, Seongbuk-gu, Seoul 02792 (Korea, Republic of)

2016-03-28

Initial stage of oxynitridation process of Si substrate is of crucial importance in fabricating the ultrathin gate dielectric layer of high quality in advanced MOSFET devices. The oxynitridation reaction on a relaxed Si(001) surface is investigated via reactive molecular dynamics (MD) simulation. A total of 1120 events of a single nitric oxide (NO) molecule reaction at temperatures ranging from 300 to 1000 K are statistically analyzed. The observed reaction kinetics are consistent with the previous experimental or calculation results, which show the viability of the reactive MD technique to study the NO dissociation reaction on Si. We suggest the reaction pathway for NO dissociation that is characterized by the inter-dimer bridge of a NO molecule as the intermediate state prior to NO dissociation. Although the energy of the inter-dimer bridge is higher than that of the intra-dimer one, our suggestion is supported by the ab initio nudged elastic band calculations showing that the energy barrier for the inter-dimer bridge formation is much lower. The growth mechanism of an ultrathin Si oxynitride layer is also investigated via consecutive NO reactions simulation. The simulation reveals the mechanism of self-limiting reaction at low temperature and the time evolution of the depth profile of N and O atoms depending on the process temperature, which would guide to optimize the oxynitridation process condition.

Properties of zirconium silicate and zirconium-silicon oxynitride high-k dielectric alloys for advanced microelectronic applications: Chemical and electrical characterizations

Science.gov (United States)

Ju, Byongsun

2005-11-01

As the microelectronic devices are aggressively scaled down to the 1999 International Technology Roadmap, the advanced complementary metal oxide semiconductor (CMOS) is required to increase packing density of ultra-large scale integrated circuits (ULSI). High-k alternative dielectrics can provide the required levels of EOT for device scaling at larger physical thickness, thereby providing a materials pathway for reducing the tunneling current. Zr silicates and its end members (SiO2 and ZrO2) and Zr-Si oxynitride films, (ZrO2)x(Si3N 4)y(SiO2)z, have been deposited using a remote plasma-enhanced chemical vapor deposition (RPECVD) system. After deposition of Zr silicate, the films were exposed to He/N2 plasma to incorporate nitrogen atoms into the surface of films. The amount of incorporated nitrogen atoms was measured by on-line Auger electron spectrometry (AES) as a function of silicate composition and showed its local minimum around the 30% silicate. The effect of nitrogen atoms on capacitance-voltage (C-V) and leakage-voltage (J-V) were also investigated by fabricating metal-oxide-semiconductor (MOS) capacitors. Results suggested that incorporating nitrogen into silicate decreased the leakage current in SiO2-rich silicate, whereas the leakage increased in the middle range of silicate. Zr-Si oxynitride was a pseudo-ternary alloy and no phase separation was detected by x-ray photoelectron spectroscopy (XPS) analysis up to 1100°C annealing. The leakage current of Zr-Si oxynitride films showed two different temperature dependent activation energies, 0.02 eV for low temperature and 0.3 eV for high temperature. Poole-Frenkel emission was the dominant leakage mechanism. Zr silicate alloys with no Si3N4 phase were chemically separated into the SiO2 and ZrO2 phase as annealed above 900°C. While chemical phase separation in Zr silicate films with Si 3N4 phase (Zr-Si oxynitride) were suppressed as increasing the amount of Si3N4 phase due to the narrow bonding network m Si3

Modification of glassy carbon electrode with a polymer/mediator composite and its application for the electrochemical detection of iodate

International Nuclear Information System (INIS)

Li, Ta-Jen; Lin, Chia-Yu; Balamurugan, A.; Kung, Chung-Wei; Wang, Jen-Yuan; Hu, Chih-Wei; Wang, Chun-Chieh; Chen, Po-Yen; Vittal, R.; Ho, Kuo-Chuan

2012-01-01

Highlights: ► FAD and PEDOT are combined to modify the glassy carbon electrode for IO 3 − sensing. ► The doping of FAD into PEDOT matrix can almost be viewed as an irreversible process. ► The optimal cycle number for preparing the GCE/PEDOT/FAD electrode is found to be 9. ► The detection limit of the GCE/PEDOT/FAD electrode for IO 3 − is found to be 0.16 μM. ► The GCE/PEDOT/FAD electrode possesses enough selectivity toward IO 3 − . - Abstract: A modified glassy carbon electrode was prepared by depositing a composite of polymer and mediator on a glassy carbon electrode (GCE). The mediator, flavin adenine dinucleotide (FAD) and the polymer, poly(3,4-ethylenedioxythiophene) (PEDOT) were electrochemically deposited as a composite on the GCE by applying cyclic voltammetry (CV). This modified electrode is hereafter designated as GCE/PEDOT/FAD. FAD was found to significantly enhance the growth of PEDOT. Electrochemical quartz crystal microbalance (EQCM) analysis was performed to study the mass changes in the electrode during the electrodeposition of PEDOT, with and without the addition of FAD. The optimal cycle number for preparing the modified electrode was determined to be 9, and the corresponding surface coverage of FAD (Γ FAD ) was ca. 5.11 × 10 −10 mol cm −2 . The amperometric detection of iodate was performed in a 100 mM buffer solution (pH 1.5). The GCE/PEDOT/FAD showed a sensitivity of 0.78 μA μM −1 cm −2 , a linear range of 4–140 μM, and a limit of detection of 0.16 μM for iodate. The interference effects of 250-fold Na + , Mg 2+ , Ca 2+ , Zn 2+ , Fe 2+ , Cl − , NO 3 − , I − , SO 4 2− and SO 3 2− , with reference to the concentration of iodate were negligible. The long-term stability of GCE/PEDOT/FAD was also investigated. The GCE/PEDOT/FAD electrode retained 82% of its initial amperometric response to iodate after 7 days. The GCE/PEDOT/FAD was also applied to determine iodate in a commercial salt.

Characterization of silicon oxynitride films prepared by the simultaneous implantation of oxygen and nitrogen ions into silicon

International Nuclear Information System (INIS)

Hezel, R.; Streb, W.

1985-01-01

Silicon oxynitride films about 5 nm in thickness were prepared by simultaneously implanting 5 keV oxygen and nitrogen ions into silicon at room temperature up to saturation. These films with concentrations ranging from pure silicon oxide to silicon nitride were characterized using Auger electron spectroscopy, electron energy loss spectroscopy and depth-concentration profiling. The different behaviour of the silicon oxynitride films compared with those of silicon oxide and silicon nitride with regard to thermal stability and hardness against electron and argon ion irradiation is pointed out. (Auth.)

Ferromagnetic bulk glassy alloys

International Nuclear Information System (INIS)

Inoue, Akihisa; Makino, Akihiro; Mizushima, Takao

2000-01-01

This paper deals with the review on the formation, thermal stability and magnetic properties of the Fe-based bulk glassy alloys in as-cast bulk and melt-spun ribbon forms. A large supercooled liquid region over 50 K before crystallization was obtained in Fe-(Al, Ga)-(P, C, B, Si), Fe-(Cr, Mo, Nb)-(Al, Ga)-(P, C, B) and (Fe, Co, Ni)-Zr-M-B (M=Ti, Hf, V, Nb, Ta, Cr, Mo and W) systems and bulk glassy alloys were produced in a thickness range below 2 mm for the Fe-(Al, Ga)-(P, C, B, Si) system and 6 mm for the Fe-Co-(Zr, Nb, Ta)-(Mo, W)-B system by copper-mold casting. The ring-shaped glassy Fe-(Al, Ga)-(P, C, B, Si) alloys exhibit much better soft magnetic properties as compared with the ring-shaped alloy made from the melt-spun ribbon because of the formation of the unique domain structure. The good combination of high glass-forming ability and good soft magnetic properties indicates the possibility of future development as a new bulk glassy magnetic material

Properties of thermally oxidized and nitrided Zr-oxynitride thin film on 4H–SiC in diluted N2O ambient

International Nuclear Information System (INIS)

Wong, Yew Hoong; Cheong, Kuan Yew

2012-01-01

A systematic investigation on the structural, chemical, and electrical properties of thermally oxidized and nitrided sputtered Zr thin film in various N 2 O ambient (10–100%) at 500 °C for 15 min to form Zr-oxynitride on 4H–SiC substrate has been carried out. The chemical composition, depth profile analysis, and energy band alignment have been evaluated by X-ray photoelectron spectrometer. Zr-oxynitride layer and its interfacial layer comprised of compounds related to Zr–O, Zr–N, Zr–O–N, Si–N, and/or C–N were identified. A model related to the oxidation and nitridation mechanism has been suggested. Supportive results related to the model were obtained by energy filtered transmission electron microscopy, X-ray diffraction, and Raman analyses. A proposed crystal structure was employed to elucidate the surface roughness and topographies of the samples, which were characterized by atomic force microscopy. The electrical results revealed that 10% N 2 O sample has possessed the highest breakdown field and reliability. This was owing to the confinement of nitrogen-related compounds of Zr–O–N and/or Zr–N at or near interfacial layer region, smaller grain with finer structure on the surface, the lowest interface trap density, total interface trap density, and effective oxide charge, and highest barrier height between conduction band edge of oxide and semiconductor. -- Highlights: ► Zr-oxynitride as the gate oxide deposited on 4H–SiC substrate. ► Simultaneous oxidation and nitridation of sputtered Zr thin film on 4H–SiC using various concentrations of N 2 O gas. ► Presence of interfacial layer comprised of mixed compounds related to Zr–O, Zr–N, Zr–O–N, Si–N, and/or C–N. ► The highest electrical breakdown and highest reliability at diluted N 2 O of 10%.

Analysis of nitrogen species in titanium oxynitride ALD films

Energy Technology Data Exchange (ETDEWEB)

Sowińska, Małgorzata, E-mail: Malgorzata.Sowinska@b-tu.de [Brandenburgische Technische Universität Cottbus-Senftenberg, Angewandte Physik-Sensorik, Konrad-Wachsmann-Allee 17, 03046 Cottbus (Germany); Brizzi, Simone; Das, Chittaranjan [Brandenburgische Technische Universität Cottbus-Senftenberg, Angewandte Physik-Sensorik, Konrad-Wachsmann-Allee 17, 03046 Cottbus (Germany); Kärkkänen, Irina; Schneidewind, Jessica; Naumann, Franziska; Gargouri, Hassan [SENTECH Instruments GmbH, Schwarzschildstraße 2, 12489 Berlin (Germany); Henkel, Karsten; Schmeißer, Dieter [Brandenburgische Technische Universität Cottbus-Senftenberg, Angewandte Physik-Sensorik, Konrad-Wachsmann-Allee 17, 03046 Cottbus (Germany)

2016-09-15

Titanium oxynitride films are prepared by plasma enhanced atomic layer deposition method using two different precursors and nitrogen sources. Synchrotron radiation-based X-ray photoelectron spectroscopy and X-ray absorption spectroscopy are used to characterize the nitrogen species incorporated within these films depending on the deposition parameters. It is found that nitrogen atoms in these films are differently bonded. In particular, it can be distinguished between Ti−ON and Ti−N bonding configurations and molecular nitrogen species caused by precursor fragments.

Glassy slag: A complementary waste form to homogeneous glass for the implementation of MAWS in treating DOE low level/mixed wastes

International Nuclear Information System (INIS)

Feng, X.; Ordaz, G.; Krumrine, P.

1994-01-01

Glassy slag waste forms are being developed to complement glass waste forms in implementing the Minimum Additive Waste Stabilization (MAWS) Program for supporting DOE's environmental restoration efforts. These glassy slags are composed of various metal oxide crystalline phases embedded in an alumino-silicate glass phase. The slags are appropriate final waste forms for waste streams that contain large amounts of scrap metals and elements with low solubilities in glass, and that have low-flux contents. Homogeneous glass waste forms are appropriate for wastes with sufficient fluxes and low metal contents. Therefore, utilization of both glass and glassy slag waste forms will make vitrification technology applicable to the treatment of a much larger range of radioactive and mixed wastes. The MAWS approach was a plied to glassy slags by blending multiple waste streams to produce the final waste form, minimizing overall waste form volume and reducing costs. The crystalline oxide phases formed in the glassy slags can be specially formulated so that they are very durable and contain hazardous and radioactive elements in their lattice structures. The Structural Bond Strength (SBS) Model was used to predict the chemical durability of the product from the slag composition so that optimized slag compositions could be obtain with a limited number of crucible melts and testing

Deposition of silicon oxynitride films by low energy ion beam assisted nitridation at room temperature

Science.gov (United States)

Youroukov, S.; Kitova, S.; Danev, G.

2008-05-01

The possibility is studied of growing thin silicon oxynitride films by e-gun evaporation of SiO and SiO2 together with concurrent bombardment with low energy N2+ ions from a cyclotron resonance (ECR) source at room temperature of substrates. The degree of nitridation and oxidation of the films is investigated by means of X-ray spectroscopy. The optical characteristics of the films, their environmental stability and adhesion to different substrates are examined. The results obtained show than the films deposited are transparent. It is found that in the case of SiO evaporation with concurrent N2+ ion bombardment, reactive implantation of nitrogen within the films takes place at room temperature of the substrate with the formation of a new silicon oxynitride compound even at low ion energy (150-200 eV).

Glassy carbon coated graphite for nuclear applications

International Nuclear Information System (INIS)

Delpeux S; Cacciaguerra T; Duclaux L

2005-01-01

Taking into account the problems caused by the treatment of nuclear wastes, the molten salts breeder reactors are expected to a great development. They use a molten fluorinated salt (mixture of LiF, BeF 2 , ThF 4 , and UF 4 ) as fuel and coolant. The reactor core, made of graphite, is used as a neutrons moderator. Despite of its compatibility with nuclear environment, it appears crucial to improve the stability and inertness of graphite against the diffusion of chemicals species leading to its corrosion. One way is to cover the graphite surface by a protective impermeable deposit made of glassy carbon obtained by the pyrolysis of phenolic resin or polyvinyl chloride precursors. The main difficulty in the synthesis of glassy carbon is to create exclusively, in the primary pyrolysis product, a micro-porosity of about twenty Angstroms which closes later at higher temperature. Therefore, the evacuation of the volatile products occurring mainly between 330 and 600 C, must progress slowly to avoid the material to crack. In this study, the optimal parameters for the synthesis of glassy carbon as well as glassy carbon deposits on nuclear-type graphite pieces are discussed. Both thermal treatment of phenolic and PVC resins have been performed. The structure and micro-texture of glassy carbon have been investigated by X-ray diffraction, scanning and transmission electron microscopies and helium pycno-metry. Glassy carbon samples (obtained at 1200 C) show densities ranging from 1.3 to 1.55 g/cm 3 and closed pores with nano-metric size (∼ 5 to 10 nm) appear clearly on the TEM micrographs. Then, a thermal treatment to 2700 C leads to the shrinkage of the entangled graphene ribbons, in good agreement with the proposed texture model for glassy carbon. Glassy carbon deposits on nuclear graphite have been developed by an impregnation method. The uniformity of the deposit depends clearly on the surface texture and the chemistry of the graphite substrate. The deposit regions where

Glassy carbon coated graphite for nuclear applications

Energy Technology Data Exchange (ETDEWEB)

Delpeux, S.; Cacciaguerra, T.; Duclaux, L. [Orleans Univ., CRMD, CNRS, 45 (France)

2005-07-01

Taking into account the problems caused by the treatment of nuclear wastes, the molten salts breeder reactors are expected to a great development. They use a molten fluorinated salt (mixture of LiF, BeF{sub 2}, ThF{sub 4}, and UF{sub 4}) as fuel and coolant. The reactor core, made of graphite, is used as a neutrons moderator. Despite of its compatibility with nuclear environment, it appears crucial to improve the stability and inertness of graphite against the diffusion of chemicals species leading to its corrosion. One way is to cover the graphite surface by a protective impermeable deposit made of glassy carbon obtained by the pyrolysis of phenolic resin [1,2] or polyvinyl chloride [3] precursors. The main difficulty in the synthesis of glassy carbon is to create exclusively, in the primary pyrolysis product, a micro-porosity of about twenty Angstroms which closes later at higher temperature. Therefore, the evacuation of the volatile products occurring mainly between 330 and 600 C, must progress slowly to avoid the material to crack. In this study, the optimal parameters for the synthesis of glassy carbon as well as glassy carbon deposits on nuclear-type graphite pieces are discussed. Both thermal treatment of phenolic and PVC resins have been performed. The structure and micro-texture of glassy carbon have been investigated by X-ray diffraction, scanning and transmission electron microscopies and helium pycno-metry. Glassy carbon samples (obtained at 1200 C) show densities ranging from 1.3 to 1.55 g/cm{sup 3} and closed pores with nano-metric size ({approx} 5 to 10 nm) appear clearly on the TEM micrographs. Then, a thermal treatment to 2700 C leads to the shrinkage of the entangled graphene ribbons (Fig 1), in good agreement with the proposed texture model for glassy carbon (Fig 2) [4]. Glassy carbon deposits on nuclear graphite have been developed by an impregnation method. The uniformity of the deposit depends clearly on the surface texture and the chemistry

Corrosion resistance and biocompatibility of zirconium oxynitride thin film growth by RF sputtering

Energy Technology Data Exchange (ETDEWEB)

Cubillos, G. I.; Olaya, J. J.; Clavijo, D.; Alfonso, J. E. [Universidad Nacional de Colombia, Carrera 45 No. 26-85, AA 14490 Bogota D. C. (Colombia); Bethencourt, M., E-mail: jealfonsoo@unal.edu.co [Universidad de Cadiz, Centro Andaluz de Ciencia y Tecnologia Marinas, Departamento de Ciencia de los Materiales e Ingenieria Metalurgica y Quimica Inorganica, Av. Republica de Saharaui, Puerto Real, E-11510 Cadiz (Spain)

2012-07-01

Thin films of zirconium oxynitride were grown on common glass, silicon (100) and stainless steel 316 L substrates using the reactive RF magnetron sputtering technique. The films were analyzed through structural, morphological and biocompatibility studies. The structural analysis was carried out using X-ray diffraction (XRD), and the morphological analysis was carried out using scanning electron microscopy (Sem) and atomic force microscopy (AFM). These studies were done as a function of growth parameters, such as power applied to the target, substrate temperature, and flow ratios. The corrosion resistance studies were made on samples of stainless steel 316 L coated and uncoated with Zr{sub x}N{sub y}O films, through of polarization curves. The studies of biocompatibility were carried out on zirconium oxynitride films deposited on stainless steel 316 L through proliferation and cellular adhesion. The XRD analysis shows that films deposited at 623 K, with a flow ratio {Phi}N{sub 2}/{Phi}O{sub 2} of 1.25 and a total deposit time of 30 minutes grew preferentially oriented along the (111) plane of the zirconium oxynitride monoclinic phase. The Sem analyses showed that the films grew homogeneously, and the AFM studies indicated that the average rugosity of the film was 5.9 nm and the average particle size was 150 nm. The analysis of the corrosion resistant, shows that the stainless steel coated with the film was increased a factor 10. Finally; through the analysis of the biocompatibility we established that the films have a better surface than the substrate (stainless steel 316 L) in terms of the adhesion and proliferation of bone cells. (Author)

Glassy carbon electrode modified with horse radish peroxidase/organic nucleophilic-functionalized carbon nanotube composite for enhanced electrocatalytic oxidation and efficient voltammetric sensing of levodopa

Energy Technology Data Exchange (ETDEWEB)

Shoja, Yalda; Rafati, Amir Abbas, E-mail: aa_rafati@basu.ac.ir; Ghodsi, Javad

2016-01-01

A novel and selective enzymatic biosensor was designed and constructed for voltammetric determination of levodopa (L-Dopa) in aqueous media (phosphate buffer solution, pH = 7). Biosensor development was on the basis of to physically immobilizing of horse radish peroxidase (HRP) as electrochemical catalyst by sol–gel on glassy carbon electrode modified with organic nucleophilic carbon nanotube composite which in this composite p-phenylenediamine (pPDA) as organic nucleophile chemically bonded with functionalized MWCNT (MWCNT-COOH). The results of this study suggest that prepared bioorganic nucleophilic carbon nanotube composite (HRP/MWCNT-pPDA) shows fast electron transfer rate for electro oxidation of L-Dopa because of its high electrochemical catalytic activity toward the oxidation of L-Dopa, more −NH{sub 2} reactive sites and large effective surface area. Also in this work we measured L-Dopa in the presence of folic acid and uric acid as interferences. The proposed biosensor was characterized by scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX), FT-IR spectroscopy and cyclic voltammetry (CV). The differential pulse voltammetry (DPV) was used for determination of L-Dopa from 0.1 μM to 1.9 μM with a low detection limit of 40 nM (for S/N = 3) and sensitivity was about 35.5 μA/μM. Also this biosensor has several advantages such as rapid response, high stability and reproducibility. - Highlights: • Glassy carbon electrode modified by a novel composite in which pPDA as nucleophile is chemically attached to MWCNTs. • The developed biosensor exhibited excellent electrocatalytic activity in electrochemically determination of L-Dopa. • The biosensor showed acceptable sensitivity, reproducibility, detection limit, selectivity and stability. • MWCNT-pPDA provides a good electrical conductivity and large effective surface area for enzyme immobilization.

Methods of forming aluminum oxynitride-comprising bodies, including methods of forming a sheet of transparent armor

Science.gov (United States)

Chu, Henry Shiu-Hung [Idaho Falls, ID; Lillo, Thomas Martin [Idaho Falls, ID

2008-12-02

The invention includes methods of forming an aluminum oxynitride-comprising body. For example, a mixture is formed which comprises A:B:C in a respective molar ratio in the range of 9:3.6-6.2:0.1-1.1, where "A" is Al.sub.2O.sub.3, "B" is AlN, and "C" is a total of one or more of B.sub.2O.sub.3, SiO.sub.2, Si--Al--O--N, and TiO.sub.2. The mixture is sintered at a temperature of at least 1,600.degree. C. at a pressure of no greater than 500 psia effective to form an aluminum oxynitride-comprising body which is at least internally transparent and has at least 99% maximum theoretical density.

Detection of dopamine in non-treated urine samples using glassy carbon electrodes modified with PAMAM dendrimer-Pt composites

International Nuclear Information System (INIS)

Garcia, M.G.; Armendariz, G.M.E.; Godinez, Luis A.; Torres, J.; Sepulveda-Guzman, S.; Bustos, E.

2011-01-01

Composites of hydroxyl-terminated PAMAM dendrimers, generation 4.0 (64 peripheral OH groups) containing Pt nanoparticles were synthesized at different reaction times using a microwave reactor. The synthetic procedure resulted in dendrimer encapsulated nanoparticles of Pt (DENs-Pt) of 1.53 ± 0.17 nm diameter that was calculated from transmission electron microscopy, and the Pt nanoparticles had single crystal plane in (1 1 1) orientation determinate by selective area diffraction. Each composite was electrochemically immobilized on a pre-functionalized glassy carbon (GC) electrode that was incorporated as a flow injection amperometric (FIA) detector, for the selective detection and quantification of dopamine (DA) in untreated urine samples. Comparison of the analytical performance of the novel electrochemical detector revealed that the DENs-Pt modified GC electrode with the composite synthesized for 30 min in the microwave reactor, showed the best response for the detection of DA in samples of non-treated urine, being the detection and quantification limits smaller (19 and 9 ppb, respectively) than those corresponding to the naked a GC electrode (846 and 423 ppb, respectively) using the FIA detector. In addition, it was found that this electroanalytical approach suffers minimal matrix effects that arise in the analysis of DA in untreated samples of urine.

Detection of dopamine in non-treated urine samples using glassy carbon electrodes modified with PAMAM dendrimer-Pt composites

Energy Technology Data Exchange (ETDEWEB)

Garcia, M.G. [Laboratory of Bioelectrochemistry, Centro de Investigacion y Desarrollo Tecnologico en Electroquimica, S. C., Parque Tecnologico, Queretaro, Sanfandila, Pedro Escobedo 76703, Queretaro (Mexico); Department of Chemistry, Universidad de Guanajuato, Cerro de la Venada S/N Col. Pueblito de Rocha, 36040 Guanajuato, Gto (Mexico); Armendariz, G.M.E.; Godinez, Luis A.; Torres, J. [Laboratory of Bioelectrochemistry, Centro de Investigacion y Desarrollo Tecnologico en Electroquimica, S. C., Parque Tecnologico, Queretaro, Sanfandila, Pedro Escobedo 76703, Queretaro (Mexico); Sepulveda-Guzman, S. [Centro de Innovacion, Investigacion y Desarrollo en Ingenieria y Tecnologia, Facultad de Ingenieria Mecanica y Electrica, Universidad Autonoma de Nuevo Leon, Av. Universidad, San Nicolas de los Garza, Nuevo Leon, 66451 Nuevo Leon (Mexico); Bustos, E., E-mail: ebustos@cideteq.mx [Laboratory of Bioelectrochemistry, Centro de Investigacion y Desarrollo Tecnologico en Electroquimica, S. C., Parque Tecnologico, Queretaro, Sanfandila, Pedro Escobedo 76703, Queretaro (Mexico)

2011-09-01

Composites of hydroxyl-terminated PAMAM dendrimers, generation 4.0 (64 peripheral OH groups) containing Pt nanoparticles were synthesized at different reaction times using a microwave reactor. The synthetic procedure resulted in dendrimer encapsulated nanoparticles of Pt (DENs-Pt) of 1.53 {+-} 0.17 nm diameter that was calculated from transmission electron microscopy, and the Pt nanoparticles had single crystal plane in (1 1 1) orientation determinate by selective area diffraction. Each composite was electrochemically immobilized on a pre-functionalized glassy carbon (GC) electrode that was incorporated as a flow injection amperometric (FIA) detector, for the selective detection and quantification of dopamine (DA) in untreated urine samples. Comparison of the analytical performance of the novel electrochemical detector revealed that the DENs-Pt modified GC electrode with the composite synthesized for 30 min in the microwave reactor, showed the best response for the detection of DA in samples of non-treated urine, being the detection and quantification limits smaller (19 and 9 ppb, respectively) than those corresponding to the naked a GC electrode (846 and 423 ppb, respectively) using the FIA detector. In addition, it was found that this electroanalytical approach suffers minimal matrix effects that arise in the analysis of DA in untreated samples of urine.

Thermodynamic picture of the glassy state

NARCIS (Netherlands)

Nieuwenhuizen, T.M.

2000-01-01

A picture for the thermodynamics of the glassy state is introduced. It assumes that one extra parameter, the effective temperature, is needed to describe the glassy state. This explains the classical paradoxes concerning the Ehrenfest relations and the Prigogine-Defay ratio. As a second feature, the

Deposition of silicon oxynitride films by low energy ion beam assisted nitridation at room temperature

Energy Technology Data Exchange (ETDEWEB)

Youroukov, S; Kitova, S; Danev, G [Central Laboratory of Photoprocesses, Bulgarian Academy of Sciences, Acad. G. Bonchev Str., Bl. 109, 113 Sofia (Bulgaria)], E-mail: skitova@clf.bas.bg

2008-05-01

The possibility is studied of growing thin silicon oxynitride films by e-gun evaporation of SiO and SiO{sub 2} together with concurrent bombardment with low energy N{sub 2}{sup +} ions from a cyclotron resonance (ECR) source at room temperature of substrates. The degree of nitridation and oxidation of the films is investigated by means of X-ray spectroscopy. The optical characteristics of the films, their environmental stability and adhesion to different substrates are examined. The results obtained show than the films deposited are transparent. It is found that in the case of SiO evaporation with concurrent N{sub 2}{sup +} ion bombardment, reactive implantation of nitrogen within the films takes place at room temperature of the substrate with the formation of a new silicon oxynitride compound even at low ion energy (150-200 eV)

Activity and stability of a <> oxynitride in the dehydrogenation of isobutane

Energy Technology Data Exchange (ETDEWEB)

Delsarte, S.; Grange, P. [Univ. Catholique de Louvain (Belgium). Unite de Catalyse et Chimie des Materiaux Divises; Laurent, Y. [Lab. de Chimie des Materiaux, Univ. de Rennes 1, Rennes (France)

2000-07-01

Isobutane dehydrogenation was studied on platinum impregnated mixed aluminium gallium phosphorus oxide and oxynitride, in a continuous, flow micro-reactor at 500-550 C. Comparison of the <> and <> shows the importance of nitridation on the acido-basic properties of the catalyst. A deactivation of the catalyst, due to the deposition of carbonaceous species on the surface, was observed. As the properties of the oxynitride would be altered by a regeneration treatment at high temperature with flowing oxygen, the possibility of decreasing the deactivation rate by decreasing the reaction temperature and by adding hydrogen to the reactant mixture was explored. Catalytic tests, carried out at different hydrogen partial pressures, showed that the hydrogen inhibits the carbon deposition on the surface of the catalyst and thus increases the catalytic stability. (orig.)

Plasma enhanced chemical vapor deposition silicon oxynitride optimized for application in integrated optics

NARCIS (Netherlands)

Worhoff, Kerstin; Driessen, A.; Lambeck, Paul; Hilderink, L.T.H.; Linders, Petrus W.C.; Popma, T.J.A.

1999-01-01

Silicon Oxynitride layers are grown from SiH4/N2, NH3 and N2O by Plasma Enhanced Chemical Vapor Deposition. The process is optimized with respect to deposition of layers with excellent uniformity in the layer thickness, high homogeneity of the refractive index and good reproducibility of the layer

Comparison of glassy slag waste forms produced in laboratory crucibles and in a bench-scale plasma furnace

International Nuclear Information System (INIS)

Feng, X.; Wronkiewicz, D.J.; Brown, N.R.; Gong, M.; Whitworth, C.; Filius, K.; Battleson, D.

1994-01-01

Vitrification is currently the best demonstrated available technology for the disposal of high-level radioactive wastes. An innovative vitrification approach known as minimum additive waste stabilization (MAWS) is being developed. Both homogeneous glass and glassy slags have been used in implementing MAWS. Glassy slags (vitro-ceramics) are glass-crystal composites, and they are composed of various metal oxide crystalline phases embedded in an aluminosilicate glass matrix. Glassy slags with compositions developed in crucible melts at Argonne National Laboratory (ANL) were successfully produced in a bench-scale Retech plasma centrifugal furnace (PCF) by MSE, Inc. Detailed examinations of these materials showed that the crucible melts and the PCF produced similar glass and crystalline phases. The two sets of glassy slags exhibited similar chemical durability in terms of normalized releases of their major components. The slags produced in the PCF furnace using metals were usually less oxidized, although this had no effect on the corrosion behavior of the major components of the slags. However, the normalized release rate of cerium was initially lower for the PCF slags. This difference diminished with time as the redox sates of the metal oxides in slags began to be controlled by exposure to air in the tests. Thus, the deference in cerium release due to the differences in slag redox state may be transitory. The cerium solubility is a complex function of redox state and solution pH and Eh

Characterization of Nd{sub 2}AlO{sub 3}N and Sm{sub 2}AlO{sub 3}N oxynitrides synthesized by carbothermal reduction and nitridation

Energy Technology Data Exchange (ETDEWEB)

Chevire, Francois, E-mail: francois.chevire@univ-rennes1.fr [UMR CNRS 6226 ' Sciences Chimiques de Rennes' , Equipe Verres et Ceramiques, Groupe Materiaux Azotes et Ceramiques, Universite de Rennes 1, 35042 Rennes Cedex (France); Pallu, Arthur; Ray, Erwan; Tessier, Franck [UMR CNRS 6226 ' Sciences Chimiques de Rennes' , Equipe Verres et Ceramiques, Groupe Materiaux Azotes et Ceramiques, Universite de Rennes 1, 35042 Rennes Cedex (France)

2011-05-12

Research highlights: > Carbothermal reduction and nitridation leads to rare earth aluminum oxynitride starting from oxide mixture. > Absorption shifts towards visible in Nd{sub 2}AlO{sub 3}N (orange) and Sm{sub 2}AlO{sub 3}N (yellow). > Oxynitrides are stable up to 600 deg. C in air. > The so-called 'intermediate phase' phenomenon is evidenced in Sm{sub 2}AlO{sub 3}N. - Abstract: The Nd{sub 2}AlO{sub 3}N and Sm{sub 2}AlO{sub 3}N oxynitrides with the K{sub 2}NiF{sub 4}-type structure have been prepared from oxide mixture at 1250 deg. C using the carbothermal reduction and nitridation route (CRN). Optimization of the process is discussed to prevent surface oxidation of the oxynitrides during the synthesis. The absorption of Nd{sub 2}AlO{sub 3}N and Sm{sub 2}AlO{sub 3}N, orange and yellow respectively, has been characterized by diffuse reflectance as well as their thermal stability versus oxidation by thermogravimetric analyses.

Solar selective performance of metal nitride/oxynitride based magnetron sputtered thin film coatings: a comprehensive review

Science.gov (United States)

Ibrahim, Khalil; Taha, Hatem; Mahbubur Rahman, M.; Kabir, Humayun; Jiang, Zhong-Tao

2018-03-01

Since solar-thermal collectors are considered to be the most direct way of converting solar energy into usable forms, in the last few years growing attention has been paid to the development of transition metal nitride and metal oxynitride based thin film selective surfaces for solar-thermal collectors, in order to harvest more solar energy. A solar-thermal energy system, generally, shows very high solar absorption of incident solar radiation from the solar-thermal collectors in the visible range (0.3 to 2.5 μm) and extremely low thermal losses through emission (or high reflection) in the infrared region (≥2.5 μm). The efficiency of a solar-thermal energy conversion system can be improved by the use of solar selective surfaces consisting of novel metallic nanoparticles embedded in metal nitride/oxynitride systems. In order to enhance the effectiveness of solar-thermal devices, solar selective surfaces with high thermal stability are a prerequisite. Over the years, substantial efforts have been made in the field of solar selective surfaces to attain higher solar absorptance and lower thermal emittance in high temperature (above 400 °C) applications. In this article, we review the present state-of-the-art transition metal nitride and/or oxynitride based vacuum sputtered nanostructured thin film coatings, with respect to their optical and solar selective surface applications. We have also summarized the solar selectivity data from recently published investigations, including discussion on some potential applications for these materials.

Properties of thermally oxidized and nitrided Zr-oxynitride thin film on 4H-SiC in diluted N{sub 2}O ambient

Energy Technology Data Exchange (ETDEWEB)

Wong, Yew Hoong [Energy Efficient and Sustainable Semiconductor Research Group, School of Materials and Mineral Resources Engineering, Engineering Campus, Universiti Sains Malaysia, 14300, Nibong Tebal, Seberang Perai Selatan, Penang (Malaysia); Cheong, Kuan Yew, E-mail: cheong@eng.usm.my [Energy Efficient and Sustainable Semiconductor Research Group, School of Materials and Mineral Resources Engineering, Engineering Campus, Universiti Sains Malaysia, 14300, Nibong Tebal, Seberang Perai Selatan, Penang (Malaysia)

2012-10-15

A systematic investigation on the structural, chemical, and electrical properties of thermally oxidized and nitrided sputtered Zr thin film in various N{sub 2}O ambient (10-100%) at 500 Degree-Sign C for 15 min to form Zr-oxynitride on 4H-SiC substrate has been carried out. The chemical composition, depth profile analysis, and energy band alignment have been evaluated by X-ray photoelectron spectrometer. Zr-oxynitride layer and its interfacial layer comprised of compounds related to Zr-O, Zr-N, Zr-O-N, Si-N, and/or C-N were identified. A model related to the oxidation and nitridation mechanism has been suggested. Supportive results related to the model were obtained by energy filtered transmission electron microscopy, X-ray diffraction, and Raman analyses. A proposed crystal structure was employed to elucidate the surface roughness and topographies of the samples, which were characterized by atomic force microscopy. The electrical results revealed that 10% N{sub 2}O sample has possessed the highest breakdown field and reliability. This was owing to the confinement of nitrogen-related compounds of Zr-O-N and/or Zr-N at or near interfacial layer region, smaller grain with finer structure on the surface, the lowest interface trap density, total interface trap density, and effective oxide charge, and highest barrier height between conduction band edge of oxide and semiconductor. -- Highlights: Black-Right-Pointing-Pointer Zr-oxynitride as the gate oxide deposited on 4H-SiC substrate. Black-Right-Pointing-Pointer Simultaneous oxidation and nitridation of sputtered Zr thin film on 4H-SiC using various concentrations of N{sub 2}O gas. Black-Right-Pointing-Pointer Presence of interfacial layer comprised of mixed compounds related to Zr-O, Zr-N, Zr-O-N, Si-N, and/or C-N. Black-Right-Pointing-Pointer The highest electrical breakdown and highest reliability at diluted N{sub 2}O of 10%.

Titanium oxynitride thin films as high-capacity and high-rate anode materials for lithium-ion batteries

International Nuclear Information System (INIS)

Chiu, Kuo-Feng; Su, Shih-Hsuan; Leu, Hoang-Jyh; Hsia, Chen-Hsien

2015-01-01

Titanium oxynitride (TiO_xN_y) was synthesized by reactive magnetron sputtering in a mixed N_2/O_2/Ar gas at ambient temperature. TiO_xN_y thin films with various amounts of nitrogen contents were deposited by varying the N_2/O_2 ratios in the background gas. The synthesized TiO_xN_y films with different compositions (TiO_1_._8_3_7N_0_._0_6_0_, TiO_1_._8_9_0N_0_._0_6_8_, TiO_1_._8_6_5N_0_._0_7_3, and TiO_1_._8_8_2N_0_._1_6_3) all displayed anatase phase, except TiO_1_._8_8_2N_0_._1_6_3. The impedances and grain sizes showed obvious variations with the nitrogen contents. A wide potential window from 3.0 V to 0.05 V, high-rate charge–discharge testing, and long cycle testing were applied to investigate the performances of synthesized TiO_xN_y and pure TiO_2 as anodes for lithium-ion batteries. These TiO_xN_y anodes can be cycled under high rates of 125 μA/cm"2 (10 °C) because of the lower charge–transfer resistance compared with the TiO_2 anode. At 10 °C the discharge capacity of the optimal TiO_xN_y composition is 1.5 times higher than that of pure TiO_2. An unexpectedly large reversible capacity of ~ 300 μAh/cm"2 μm (~ 800 mAh/g) between 1.0 V and 0.05 V was recorded for the TiO_xN_y anodes. The TiO_xN_y anode was cycled (3.0 V to 0.05 V) at 10 °C over 300 times without capacity fading while delivering a capacity of ~ 150 μAh/cm"2 μm (~ 400 mAh/g). - Highlights: • Titanium oxynitride (TiO_xN_y) thin films as anode materials were studied. • TiO_xN_y thin films with various amounts of nitrogen contents were studied_. • High rate capability of TiO_xN_y was studied.

Study of the AlON-VN composite ceramic

Energy Technology Data Exchange (ETDEWEB)

Sainbaatar; Zhang Zuotai; Li Wenchao; Wang Xidong [Dept. of Physical Chemistry of Metallurgy, Univ. of Science and Technology Beijing, BJ (China)

2005-07-01

Aluminium oxynitride-vanadium nitride (AlON-VN) composite ceramic was fabricated based on thermodynamic analysis of V-Al-O-N systems. The results indicated that the VN dispersed homogeneously in AlON matrix and can reinforce AlON matrix. Oxidation behavior was studied and the results showed that it belongs to self-protective oxidation due to the good adherence of oxidation product. Therefore, AlON-VN composites have excellent oxidation resistance. (orig.)

Similar and dissimilar friction welding of Zr-Cu-Al bulk glassy alloys

International Nuclear Information System (INIS)

Shin, Hyung-Seop; Park, Jung-Soo; Jung, Yoon-Chul; Ahn, Jung-Ho; Yokoyama, Yoshihiko; Inoue, Akihisa

2009-01-01

The friction welding of three kinds of Zr-Cu-Al bulk glassy alloys (BGAs) which show eutectic or hypoeutectic compositions to similar and dissimilar BGAs and crystalline metals has been tried. The shape and volume of the protrusion formed at the weld interface were investigated. In order to characterize the friction welded interface, micrographic observation and X-ray diffraction analysis on the weld cross-section were carried out. A successful joining of Zr-Cu-Al bulk glassy alloys to similar and dissimilar BGAs was achieved without occurrence of crystallizations at the weld interface through the precise control of friction conditions. In addition, the joining of Zr 50 Cu 40 Al 10 BGA to crystalline alloys was tried, but it was only successful for specific material combinations. The residual strength after welding of dissimilar BGAs was evaluated by the four-point bending test.

Tuning the properties of visible-light-responsive tantalum (oxy)nitride photocatalysts by non-stoichiometric compositions: A first-principles viewpoint

KAUST Repository

Harb, Moussab

2014-01-01

Finding an ideal photocatalyst for achieving efficient overall water splitting still remains a great challenge. By applying accurate first-principles quantum calculations based on DFT with the screened non-local hybrid HSE06 functional, we bring rational insights at the atomic level into the influence of non-stoichiometric compositions on essential properties of tantalum (oxy)nitride compounds as visible-light-responsive photocatalysts for water splitting. Indeed, recent experiments show that such non-stoichiometry is inherent to the nitridation methods of tantalum oxide with unavoidable oxygen impurities. We considered here O-enriched Ta3N5 and N-enriched TaON materials. Although their structural parameters are found to be very similar to those of pure compounds and in good agreement with available experimental studies, their photocatalytic features for visible-light-driven overall water splitting reactions show different behaviors. Further partial nitration of TaON leads to a narrowed band gap, but partially oxidizing Ta3N5 causes only subtle changes in the gap. The main influence, however, is on the band edge positions relative to water redox potentials. The pure Ta3N5 is predicted to be a good candidate only for H+ reduction and H2 evolution, while the pure TaON is predicted to be a good candidate for water oxidation and O2 evolution. Non-stoichiometry has here a positive influence, since partially oxidized tantalum nitride, Ta(3-x)N(5-5x)O5x (for x ≥ 0.16) i.e. with a composition in between TaON and Ta3N5, reveals suitable band edge positions that correctly bracket the water redox potentials for visible-light-driven overall water splitting reactions. Among the various explored Ta(3-x)N(5-5x)O5x structures, a strong stabilization is obtained for the configuration displaying a strong interaction between the O-impurities and the created Ta-vacancies. In the lowest-energy structure, each created Ta-vacancy is surrounded by five O-impurity species substituting

On the phase formation of sputtered hafnium oxide and oxynitride films

International Nuclear Information System (INIS)

Sarakinos, K.; Music, D.; Mraz, S.; Baben, M. to; Jiang, K.; Nahif, F.; Braun, A.; Zilkens, C.; Schneider, J. M.; Konstantinidis, S.; Renaux, F.; Cossement, D.; Munnik, F.

2010-01-01

Hafnium oxynitride films are deposited from a Hf target employing direct current magnetron sputtering in an Ar-O 2 -N 2 atmosphere. It is shown that the presence of N 2 allows for the stabilization of the transition zone between the metallic and the compound sputtering mode enabling deposition of films at well defined conditions of target coverage by varying the O 2 partial pressure. Plasma analysis reveals that this experimental strategy facilitates control over the flux of the O - ions which are generated on the oxidized target surface and accelerated by the negative target potential toward the growing film. An arrangement that enables film growth without O - ion bombardment is also implemented. Moreover, stabilization of the transition sputtering zone and control of the O - ion flux without N 2 addition is achieved employing high power pulsed magnetron sputtering. Structural characterization of the deposited films unambiguously proves that the phase formation of hafnium oxide and hafnium oxynitride films with the crystal structure of HfO 2 is independent from the O - bombardment conditions. Experimental and theoretical data indicate that the presence of vacancies and/or the substitution of O by N atoms in the nonmetal sublattice favor the formation of the cubic and/or the tetragonal HfO 2 crystal structure at the expense of the monoclinic HfO 2 one.

Mechanical properties of silicon oxynitride thin films prepared by low energy ion beam assisted deposition

International Nuclear Information System (INIS)

Shima, Yukari; Hasuyama, Hiroki; Kondoh, Toshiharu; Imaoka, Yasuo; Watari, Takanori; Baba, Koumei; Hatada, Ruriko

1999-01-01

Silicon oxynitride (SiO x N y ) films (0.1-0.7 μm) were produced on Si (1 0 0), glass and 316L stainless steel substrates by ion beam assisted deposition (IBAD) using Si evaporation and the concurrent bombardment with a mixture of 200 eV N 2 and Ar, or O 2 and Ar ions. Adhesion was evaluated by pull-off tests. Film hardness was measured by a nanoindentation system with AFM. The measurement of internal stress in the films was carried out by the Stoney method. The film structure was examined by GXRD. XPS was employed to measure the composition of films and to analyze the chemical bonds. The dependence of mechanical properties on the film thickness and the processing temperature during deposition was studied. Finally, the relations between the mechanical properties of the films and the correlation with corrosion-protection ability of films are discussed and summarized

Synthesis and biological characterization of zirconium oxynitride thin film growth by radio-frequency sputtering

Energy Technology Data Exchange (ETDEWEB)

Cubillos, G.I. [Departamento de Química, Universidad Nacional de Colombia, AA 14490 Bogotá (Colombia); Olaya, J.J. [Facultad de Ingeniería, Universidad Nacional de Colombia, AA 14490 Bogotá (Colombia); Clavijo, D. [Facultad de Medicina, Universidad Nacional de Colombia, AA 14490 Bogotá (Colombia); Alfonso, J.E., E-mail: jealfonsoo@unal.edu.co [Grupo de materiales con Aplicaciones Tecnológicas, Universidad Nacional de Colombia, AA 14490 Bogotá (Colombia); Cardozo, C. [Instituto de Biotecnología, Universidad Nacional de Colombia, AA 14490 Bogotá (Colombia)

2013-02-01

Thin films of zirconium oxynitride were grown on common glass, silicon substrates (100) and on stainless steel 316L using the reactive RF magnetron sputtering technique. The films were analyzed through structural, morphological, and biocompatibility studies. The structural analysis was carried out using X-ray diffraction (XRD), and the morphological analysis was carried out using scanning electron microscopy (SEM) and atomic force microscopy (AFM). These studies were done as a function of growth parameters, such as power applied to the target, substrate temperature, and flow ratios. The studies of biocompatibility were carried out on zirconium oxynitride films deposited on stainless steel 316L through proliferation and cellular adhesion. The XRD analysis showed that films deposited at 623 K, with a flow ratio ΦN{sub 2}/ΦO{sub 2} of 1.25 and a total deposit time of 30 min grew preferentially oriented along the (111) plane of the zirconium oxynitride monoclinic phase. The SEM analyses showed that the films grew homogeneously, and the AFM studies indicated that the average rugosity of the film was 5.9 nm and the average particle size was 150 nm. Finally, through the analysis of the biocompatibility, we established that the films have a better surface than the substrate (stainless steel 316L) in terms of adhesion and proliferation of bone cells. - Highlights: ►ZrO{sub x}N{sub y} thin films were deposited using reactive radio-frequency magnetron sputtering. ►We studied the effect of deposition parameters on ZrO{sub x}N{sub y} thin films microstructure. ►We have been able to grow bone cells on ZrO{sub x}N{sub y} coated stainless steel 316L.

Deposition of silicon oxynitride at room temperature by Inductively Coupled Plasma-CVD

Energy Technology Data Exchange (ETDEWEB)

Zambom, Luis da Silva [MPCE-Faculdade de Tecnologia de Sao Paulo - CEETEPS, Pca Coronel Fernando Prestes, 30, Sao Paulo - CEP 01124-060 (Brazil)]. E-mail: zambom@lsi.usp.br; Verdonck, Patrick [PSI-LSI-Escola Politecnica da Universidade de Sao Paulo (Brazil)]. E-mail: patrick@lsi.usp.br

2006-10-25

Oxynitride thin films are used in important optical applications and as gate dielectric for MOS devices. Their traditional deposition processes have the drawbacks that high temperatures are needed, high mechanical stresses are induced and the deposition rate is low. Plasma assisted processes may alleviate these problems. In this study, oxynitride films were deposited at room temperature through the chemical reaction of silane, nitrogen and nitrous oxide (N{sub 2}O), in a conventional LPCVD furnace, which was modified into a high density Inductively Coupled Plasma (ICP) reactor. Deposition rates increased with applied coil power and were never lower than 10 nm/min, quite high for room temperature depositions. The films' refractive indexes and FTIR spectra indicate that for processes with low N{sub 2}O gas concentrations, when mixed together with N{sub 2} and SiH{sub 4}, nitrogen was incorporated in the film. This incorporation increased the resistivity, which was up to 70 G{omega} cm, increased the refractive index, from approximately 1.47 to approximately 1.50, and decreased the dielectric constant of these films, which varied in the 4-14 range. These characteristics are adequate for electric applications e.g. for TFT fabrication on glass or polymers which can not stand high temperature steps.

Plasma properties during magnetron sputtering of lithium phosphorous oxynitride thin films

DEFF Research Database (Denmark)

Christiansen, Ane Sælland; Stamate, Eugen; Thydén, Karl Tor Sune

2015-01-01

The nitrogen dissociation and plasma parameters during radio frequency sputtering of lithium phosphorus oxynitride thin films in nitrogen gas are investigated by mass appearance spectrometry, electrostatic probes and optical emission spectroscopy, and the results are correlated with electrochemical...... properties and microstructure of the films. Low pressure and moderate power are associated with lower plasma density, higher electron temperature, higher plasma potential and larger diffusion length for sputtered particles. This combination of parameters favors the presence of more atomic nitrogen, a fact...

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.

Physical properties evolution of sputtered zirconium oxynitride films: effects of the growth temperature

International Nuclear Information System (INIS)

Rizzo, A; Signore, M A; Mirenghi, L; Piscopiello, E; Tapfer, L

2009-01-01

Zirconium oxynitride (ZrNO) films were deposited by RF reactive magnetron sputtering in water vapour-nitrogen atmosphere varying the deposition temperature from RT to 600 0 C. Optical analysis, x-ray diffraction, x-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) are the employed characterization techniques to investigate the influence of the substrate temperature on the films physical properties. It was found that the variation of the substrate temperature from RT to 600 0 C caused a structural transition from cubic phase of Zr 2 ON 2 to ZrN one, as confirmed by TEM observations too. In particular, Forouhi-Bloomer dispersion equations for optical parameters (n and k) and deconvolution of XPS spectra allowed further chemical properties be elucidated. They also permitted identification of two oxynitride phases, γ phase (E g = 1.94 eV) and β phase (E g = 1.7 eV), and an over-stoichiometric nitride one. The use of [E c - E v ] values helped to confirm further the distinction between (γ, β)-phases and N-rich zirconium nitride compound, which is unachievable by using only E g values.

Physical properties evolution of sputtered zirconium oxynitride films: effects of the growth temperature

Energy Technology Data Exchange (ETDEWEB)

Rizzo, A; Signore, M A; Mirenghi, L; Piscopiello, E; Tapfer, L [ENEA, Department of Physical Technologies and New Materials, SS7, Appia, km 706, 72100 Brindisi (Italy)

2009-12-07

Zirconium oxynitride (ZrNO) films were deposited by RF reactive magnetron sputtering in water vapour-nitrogen atmosphere varying the deposition temperature from RT to 600 {sup 0}C. Optical analysis, x-ray diffraction, x-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) are the employed characterization techniques to investigate the influence of the substrate temperature on the films physical properties. It was found that the variation of the substrate temperature from RT to 600 {sup 0}C caused a structural transition from cubic phase of Zr{sub 2}ON{sub 2} to ZrN one, as confirmed by TEM observations too. In particular, Forouhi-Bloomer dispersion equations for optical parameters (n and k) and deconvolution of XPS spectra allowed further chemical properties be elucidated. They also permitted identification of two oxynitride phases, {gamma} phase (E{sub g} = 1.94 eV) and {beta} phase (E{sub g} = 1.7 eV), and an over-stoichiometric nitride one. The use of [E{sub c} - E{sub v}] values helped to confirm further the distinction between ({gamma}, {beta})-phases and N-rich zirconium nitride compound, which is unachievable by using only E{sub g} values.

ELECTROKINETIC PROPERTIES, IN VITRO DISSOLUTION, AND PROSPECTIVE HEMOAND BIOCOMPATIBILITY OF TITANIUM OXIDE AND OXYNITRIDE FILMS FOR CARDIOVASCULAR STENTS

Directory of Open Access Journals (Sweden)

I. A. Khlusov

2015-01-01

Full Text Available A state of titanium oxide and oxynitride coatings on L316 steel has been studied before and after their contact with model biological fluids. Electrokinetic investigation in 1 mmol potassium chloride showed significant (more than 10 times fall of magnitude of electrostatic potential of thin (200–300 nm titanium films at pH changing in the range of 5–9 units during 2 h. Nevertheless, zeta-potential of all samples had negative charge under pH > 6.5. Long-term (5 weeks contact of samples with simulated body fluid (SBF promoted steel corrosion and titanium oxide and oxynitride films dissolution. On the other hand, sodium and chloride ions precipitation and sodium chloride crystals formation occurred on the samples. Of positive fact is an absence of calcification of tested artificial surfaces in conditions of long-term being in SBF solution. It is supposed decreasing hazard of fast thrombosis and loss of materials functional properties. According to in vitro experiment conducted, prospective biocompatibility of materials tested before and after their contact with SBF lines up following manner: Ti–O–N (1/3 > Ti–O–N (1/1, TiO2 > Steel. It may be explained by: 1 the corrosion-preventive properties of thin titanium oxide and oxynitride films;2 a store of surface negative charge for Ti–O–N (1/3 film; 3 minor augmentation of mass and thickness of titanium films connected with speed of mineralization processes on the interface of solution/solid body. At the same time, initial (before SBF contact differences of samples wettability became equal. Modifying effect of model biological fluids on physicochemical characteristics of materials tested (roughness enhancement, a reduction or reversion of surface negative potential, sharp augmentation of surface hydrofilicity should took into account under titanium oxide and oxynitride films formation and a forecast of their optimal biological properties as the materials for cardiovascular stents.

Low temperature thermal conductivities of glassy carbons

International Nuclear Information System (INIS)

Anderson, A.C.

1979-01-01

The thermal conductivity of glassy carbon in the temperature range 0.1 to 100 0 K appears to depend only on the temperature at which the material was pyrolyzed. The thermal conductivity can be related to the microscopic structure of glassy carbon. The reticulated structure is especially useful for thermal isolation at cryogenic temperatures

Relationship between microstructure and tribological behavior of CFRC composites

Science.gov (United States)

de Souza, Maria Aparecida Miranda; Pardini, Luiz Claudio

2017-12-01

Carbon fiber reinforced carbon (CFRC) composites were initially introduced in spacecraft propulsion area and quickly started to be applied in aircraft braking systems, replacing conventional metallic systems, thanks to their excellent tribological properties. Each company develops their own CFRC composite production system, the information is unique to each manufacturer, and little is reported in the literature. In this work, tribological characterizations of three commercial CFRC composites are performed using a pin-on-disc tribometer. The results showed that the pairs assembled with pyrolytic matrix composites of rough or smooth laminar texture with graphitization index between 18 and 40% has an average COF between 0.15 and 0.25, while the pairs assembled with mixed pairs, pyrolytic matrix and glassy matrix, or pair of glassy matrix display average COF between 0.10 and 0.15. Wear which can reach a rate 9 times higher to the tribological pair of glassy composite when compared to a pyrolytic composite.

Growth Kinetics and Modeling of Direct Oxynitride Growth with NO-O2 Gas Mixtures

Energy Technology Data Exchange (ETDEWEB)

Everist, Sarah; Nelson, Jerry; Sharangpani, Rahul; Smith, Paul Martin; Tay, Sing-Pin; Thakur, Randhir

1999-05-03

We have modeled growth kinetics of oxynitrides grown in NO-O₂ gas mixtures from first principles using modified Deal-Grove equations. Retardation of oxygen diffusion through the nitrided dielectric was assumed to be the dominant growth-limiting step. The model was validated against experimentally obtained curves with good agreement. Excellent uniformity, which exceeded expected walues, was observed.

Treatment of early glassy cell carcinoma of uterine cervix

International Nuclear Information System (INIS)

Kim, Ok Bae; Kim, Jin Hee; Choi, Tae Jin

2006-01-01

The purpose of this study was to investigate the clinical findings, treatment, and outcome of patients with glassy cell carcinoma of cervix. We reviewed all cases of glassy cell carcinoma of the uterine cervix confirmed and treated at the Dongsan Medical Center, Keimyung University, between January 1993 and December 2005. There were 7 cases with histopathologically confirmed gassy cell carcinoma. A tumor was diagnosed as glassy cell carcinoma if over 50% of the tumor cell type displayed glassy cell features. Six patients with stage IB had radical hysterectomy and bilateral pelvic node dissection, and 2 of them received adjuvant external pelvic irradiation with concurrent chemotherapy. Remaining one patient with stage IIA had curative concurrent chemoradiotherapy with external pelvic irradiation and brachytherapy. There were 7 patients diagnosed as glassy cell carcinoma among the 3,745 (0.2%) patients of carcinoma of uterine cervix. The mean age of 7 patients was 44 years with range of 35 to 53 years of age. The most frequent symptom was vaginal bleeding (86%). By the punch biopsy undertaken before treatment of 7 cases, 2 only cases could diagnose as glassy cell carcinoma of uterine cervix, but remaining of them confirmed by surgical pathological examination. The mean follow up duration was 73 months with range of 13 to 150 months. All 7 patients were alive without disease after treatment. Glassy cell carcinoma of the uterine cervix is a distinct clinicopathologic entity that demonstrates an aggressive biologic behavior. However for early-stage disease, we may have more favorable clinical outcome with radical surgery followed by chemoradiotherapy

EDTA modified glassy carbon electrode: Preparation and characterization

International Nuclear Information System (INIS)

Ustuendag, Zafer; Solak, Ali Osman

2009-01-01

EDTA-phenoxyamide modified glassy carbon electrode (EDTA-GC) was prepared at a glassy carbon electrode by surface synthesis. In the first step, nitrophenyl was grafted to the glassy carbon (GC) surface via the electrochemical reduction of its tetraflouroborate diazonium salt. In the second step, nitrophenyl-modified electrode (NP-GC) was subjected to the cathodic potential scan to reduce the nitro to amine group. p-Aminophenyl modified glassy carbon electrode (AP-GC) was dipped into a EDTA solution containing 1-ethyl-3(3-(dimethlyamino)propyl)-carbodiimide (EDC) as an activating agent. Thus formed ((2-anilino-2-oxoethyl){2-[bis(carboxymethyl)amino]-ethyl}amino)acetic acid modified GC electrode was denoted as EDTA-GC and characterized by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), ellipsometry and X-ray photoelectron spectroscopy (XPS). Complexation of the EDTA-GC surface with Pb 2+ ions was investigated if this electrode could be used as a metal sensor.

Boron ion irradiation induced structural and surface modification of glassy carbon

International Nuclear Information System (INIS)

Kalijadis, Ana; Jovanović, Zoran; Cvijović-Alagić, Ivana; Laušević, Zoran

2013-01-01

The incorporation of boron into glassy carbon was achieved by irradiating two different types of targets: glassy carbon polymer precursor and carbonized glassy carbon. Targets were irradiated with a 45 keV B 3+ ion beam in the fluence range of 5 × 10 15 –5 × 10 16 ions cm −2 . For both types of targets, the implanted boron was located in a narrow region under the surface. Following irradiation, the polymer was carbonized under the same condition as the glassy carbon samples (at 1273 K) and examined by Raman spectroscopy, temperature programmed desorption, hardness and cyclic voltammetry measurements. Structural analysis showed that during the carbonization process of the irradiated polymers, boron is substitutionally incorporated into the glassy carbon structure, while for irradiated carbonized glassy carbon samples, boron irradiation caused an increase of the sp 3 carbon fraction, which is most pronounced for the highest fluence irradiation. Further analyses showed that different nature of boron incorporation, and thus changed structural parameters, are crucial for obtaining glassy carbon samples with modified mechanical, chemical and electrochemical properties over a wide range

Eu-doped barium aluminium oxynitride with the ß-alumina-type structure as new blue-emitting phosphor

NARCIS (Netherlands)

Jansen, S.R.; Migchels, J.M.; Hintzen, H.T.J.M.; Metselaar, R.

1999-01-01

Attractive new blue-emitting phosphors for use in low-pressure mercury gas discharge lamps are synthesized by Eu-substitution in the barium aluminum oxynitride host lattice with the -alumina-type structure. The emission spectra of these phosphors for 254 nm excitation show a band at about 450 nm

EDTA modified glassy carbon electrode: Preparation and characterization

Energy Technology Data Exchange (ETDEWEB)

Ustuendag, Zafer [Dumlupinar University, Faculty of Arts and Sciences, Department of Chemistry, Kuetahya (Turkey); Solak, Ali Osman [Ankara University, Faculty of Science, Department of Chemistry, Degol Street, Tandogan, 06100 Ankara (Turkey)], E-mail: osolak@science.ankara.edu.tr

2009-11-01

EDTA-phenoxyamide modified glassy carbon electrode (EDTA-GC) was prepared at a glassy carbon electrode by surface synthesis. In the first step, nitrophenyl was grafted to the glassy carbon (GC) surface via the electrochemical reduction of its tetraflouroborate diazonium salt. In the second step, nitrophenyl-modified electrode (NP-GC) was subjected to the cathodic potential scan to reduce the nitro to amine group. p-Aminophenyl modified glassy carbon electrode (AP-GC) was dipped into a EDTA solution containing 1-ethyl-3(3-(dimethlyamino)propyl)-carbodiimide (EDC) as an activating agent. Thus formed ((2-anilino-2-oxoethyl){l_brace}2-[bis(carboxymethyl)amino]-ethyl{r_brace}amino)acetic acid modified GC electrode was denoted as EDTA-GC and characterized by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), ellipsometry and X-ray photoelectron spectroscopy (XPS). Complexation of the EDTA-GC surface with Pb{sup 2+} ions was investigated if this electrode could be used as a metal sensor.

Titanium oxynitride thin films as high-capacity and high-rate anode materials for lithium-ion batteries

Energy Technology Data Exchange (ETDEWEB)

Chiu, Kuo-Feng [Department of Materials Science and Engineering, Feng Chia University, 100 Wenhwa Rd., Taichung 40724, Taiwan (China); Su, Shih-Hsuan, E-mail: minimono42@gmail.com [Department of Materials Science and Engineering, Feng Chia University, 100 Wenhwa Rd., Taichung 40724, Taiwan (China); Leu, Hoang-Jyh [Master' s Program of Green Energy Science and Technology, Feng Chia University, 100 Wenhwa Rd., Taichung 40724, Taiwan (China); Hsia, Chen-Hsien [Department of Materials Science and Engineering, Feng Chia University, 100 Wenhwa Rd., Taichung 40724, Taiwan (China)

2015-12-01

Titanium oxynitride (TiO{sub x}N{sub y}) was synthesized by reactive magnetron sputtering in a mixed N{sub 2}/O{sub 2}/Ar gas at ambient temperature. TiO{sub x}N{sub y} thin films with various amounts of nitrogen contents were deposited by varying the N{sub 2}/O{sub 2} ratios in the background gas. The synthesized TiO{sub x}N{sub y} films with different compositions (TiO{sub 1.837}N{sub 0.060,} TiO{sub 1.890}N{sub 0.068,} TiO{sub 1.865}N{sub 0.073}, and TiO{sub 1.882}N{sub 0.163}) all displayed anatase phase, except TiO{sub 1.882}N{sub 0.163}. The impedances and grain sizes showed obvious variations with the nitrogen contents. A wide potential window from 3.0 V to 0.05 V, high-rate charge–discharge testing, and long cycle testing were applied to investigate the performances of synthesized TiO{sub x}N{sub y} and pure TiO{sub 2} as anodes for lithium-ion batteries. These TiO{sub x}N{sub y} anodes can be cycled under high rates of 125 μA/cm{sup 2} (10 °C) because of the lower charge–transfer resistance compared with the TiO{sub 2} anode. At 10 °C the discharge capacity of the optimal TiO{sub x}N{sub y} composition is 1.5 times higher than that of pure TiO{sub 2}. An unexpectedly large reversible capacity of ~ 300 μAh/cm{sup 2} μm (~ 800 mAh/g) between 1.0 V and 0.05 V was recorded for the TiO{sub x}N{sub y} anodes. The TiO{sub x}N{sub y} anode was cycled (3.0 V to 0.05 V) at 10 °C over 300 times without capacity fading while delivering a capacity of ~ 150 μAh/cm{sup 2} μm (~ 400 mAh/g). - Highlights: • Titanium oxynitride (TiO{sub x}N{sub y}) thin films as anode materials were studied. • TiO{sub x}N{sub y} thin films with various amounts of nitrogen contents were studied{sub .} • High rate capability of TiO{sub x}N{sub y} was studied.

Plasma-enhanced chemical vapor deposited silicon oxynitride films for optical waveguide bridges for use in mechanical sensors

DEFF Research Database (Denmark)

Storgaard-Larsen, Torben; Leistiko, Otto

1997-01-01

In this paper the influence of RF power, ammonia flow, annealing temperature, and annealing time on the optical and mechanical properties of plasma-enhanced chemically vapor deposited silicon oxynitride films, is presented. A low refractive index (1.47 to 1.48) film having tensile stress has been...

New model system in radiation cryochemistry:. hyperquenched glassy water

Science.gov (United States)

Bednarek, Janusz; Plonka, Andrzej; Hallbrucker, Andreas; Mayer, Erwin

1999-08-01

Radicals generated by high-energy irradiation of liquid water, short-lived at ambient temperature, can be studied at cryogenic temperatures after irradiating water and dilute aqueous solutions in their glassy states which can be obtained by so-called hyperquenching of the liquids at cooling rates of ˜10 6-10 7 K s -1. In the glassy states of hyperquenched dilute aqueous solutions there is no problem with phase separation and radiolysis of glassy water is quite distinct from radiolysis of polycrystalline ice obtained from liquid water on slow-cooling in liquid nitrogen.

Manufacture and properties of AlON-TiN particulate composites

Energy Technology Data Exchange (ETDEWEB)

Zhang Zuotai; Wang Xidong; Zhang Mei; Li Wenchao [Dept. of Physical Chemistry of Metallurgy, Univ. of Science and Technology, Beijing, BJ (China)

2005-07-01

Dense aluminum oxynitride-titanium nitride (AlON-TiN) composites with 3{proportional_to}15 wt% TiN were fabricated by hot pressing technique. The effect of the content of a dispersion-toughening aid, TiN, on the mechanical properties, oxidation resistance and wear resistance were studied and related to the microstructure. The composites with a content of 15 wt% were characterized with the highest strength, 487 MPa, and the highest wear resistance properties. Oxidation behavior was studied and the results showed that AlON-TiN composites have excellent oxidation resistance. (orig.)

Glassy carbon based supercapacitor stacks

Energy Technology Data Exchange (ETDEWEB)

Baertsch, M; Braun, A; Koetz, R; Haas, O [Paul Scherrer Inst. (PSI), Villigen (Switzerland)

1997-06-01

Considerable effort is being made to develop electrochemical double layer capacitors (EDLC) that store relatively large quantities of electrical energy and possess at the same time a high power density. Our previous work has shown that glassy carbon is suitable as a material for capacitor electrodes concerning low resistance and high capacity requirements. We present the development of bipolar electrochemical glassy carbon capacitor stacks of up to 3 V. Bipolar stacks are an efficient way to meet the high voltage and high power density requirements for traction applications. Impedance and cyclic voltammogram measurements are reported here and show the frequency response of a 1, 2, and 3 V stack. (author) 3 figs., 1 ref..

10-fold enhancement in light-driven water splitting using niobium oxynitride microcone array films

KAUST Repository

Shaheen, Basamat

2016-03-26

We demonstrate, for the first time, the synthesis of highly ordered niobium oxynitride microcones as an attractive class of materials for visible-light-driven water splitting. As revealed by the ultraviolet photoelectron spectroscopy (UPS), photoelectrochemical and transient photocurrent measurements, the microcones showed enhanced performance (~1000% compared to mesoporous niobium oxide) as photoanodes for water splitting with remarkable stability and visible light activity. © 2016 Elsevier B.V. All rights reserved.

AlN and Al oxy-nitride gate dielectrics for reliable gate stacks on Ge and InGaAs channels

Energy Technology Data Exchange (ETDEWEB)

Guo, Y.; Li, H.; Robertson, J. [Engineering Department, Cambridge University, Cambridge CB2 1PZ (United Kingdom)

2016-05-28

AlN and Al oxy-nitride dielectric layers are proposed instead of Al{sub 2}O{sub 3} as a component of the gate dielectric stacks on higher mobility channels in metal oxide field effect transistors to improve their positive bias stress instability reliability. It is calculated that the gap states of nitrogen vacancies in AlN lie further away in energy from the semiconductor band gap than those of oxygen vacancies in Al{sub 2}O{sub 3}, and thus AlN might be less susceptible to charge trapping and have a better reliability performance. The unfavourable defect energy level distribution in amorphous Al{sub 2}O{sub 3} is attributed to its larger coordination disorder compared to the more symmetrically bonded AlN. Al oxy-nitride is also predicted to have less tendency for charge trapping.

Characterization of gate oxynitrides by means of time of flight secondary ion mass spectrometry and x-ray photoelectron spectroscopy. Quantification of nitrogen

International Nuclear Information System (INIS)

Ferrari, S.; Perego, M.; Fanciulli, M.

2002-01-01

We present a methodology for the quantitative estimation of nitrogen in ultrathin oxynitrides by means of time of flight secondary ion mass spectrometry (TOF-SIMS) and x-ray photoelectron spectroscopy (XPS). We consider an innovative approach to TOF-SIMS depth profiling, by elemental distribution of single species as sum of peaks containing such species. This approach is very efficient in overcoming matrix effect arising when quantifying elements were distributed in silicon and silicon oxide. We use XPS to calibrate TOF-SIMS and to obtain quantitative information on nitrogen distribution in oxynitride thin layers. In the method we propose we process TOF-SIMS and XPS data simultaneously to obtain a quantitative depth profile

Formation of a glassy phase in ceramic-like coatings

International Nuclear Information System (INIS)

Sazonova, M.V.; Gorbatova, G.N.

1986-01-01

The authors investigate the synthesis directly in coatings of a borosilicate melt that could fill the role of glassy matrix, thereby avoiding fusion and processing of the glassy material. The effect of added boron on the formation of coatings based on molybdenum disilicide and tungsten disilicide in air at 900 degrees C is presented. Without an additive no coating forms; there is no adhesion to the graphite and a continuous film does not form. As a result of boron oxidation an easily fused glassy matrix forms, which bonds the molybdenum disilicide or tungsten disilicide particles together and ensures adhesion to the graphite

The sorption induced glass transition in amorphous glassy polymers

NARCIS (Netherlands)

van der Vegt, N.F.A.; Wessling, Matthias; Strathmann, H.; Briels, Willem J.

1999-01-01

Sorption of CO2 in both the glassy and the rubbery state of an amorphous polyethylenelike polymer was investigated using molecular dynamics simulations. The temperature was chosen such that the system was in its glassy state at low solute concentrations and its rubbery state at large solute

Nanoindentation characterization of deformation and failure of aluminum oxynitride

Energy Technology Data Exchange (ETDEWEB)

Guo, J.J.; Wang, K.; Fujita, T. [WPI Advanced Institute for Materials Research, Tohoku University, Sendai 980-8577 (Japan); McCauley, J.W. [US Army Research Laboratory, Aberdeen Proving Ground, MD 21078 (United States); Singh, J.P. [US Army International Technology Center, Tokyo 106-0032 (Japan); Chen, M.W., E-mail: mwchen@wpi-aimr.tohoku.ac.jp [WPI Advanced Institute for Materials Research, Tohoku University, Sendai 980-8577 (Japan); Department of Mechanical Engineering, Johns Hopkins University, Baltimore, MD 21218 (United States)

2011-02-15

A systematic study of the mechanical deformation and failure of transparent ceramic aluminum oxynitride (AlON) has been conducted using a depth-sensitive nanoindentation technique combined with transmission electron microscopy (TEM) and Raman spectroscopy. Although discrete displacement bursts appear in the load-depth profiles at high applied forces, a detectable high-pressure phase transition has not been found by means of micro-Raman spectroscopy and TEM. Instead, a high density of dissociated <1 1 0> dislocations can be observed underneath the nanoindenters, suggesting that extensive plastic deformation takes place in the brittle ceramic at high contact pressures. Moreover, nanoindentation-induced micro-cracks oriented along well-defined crystallographic planes can also be observed, consistent with the low fracture toughness of AlON evaluated by an indentation method using Laugier's equation.

Electrical studies on silver based fast ion conducting glassy materials

International Nuclear Information System (INIS)

Rao, B. Appa; Kumar, E. Ramesh; Kumari, K. Rajani; Bhikshamaiah, G.

2014-01-01

Among all the available fast ion conductors, silver based glasses exhibit high conductivity. Further, glasses containing silver iodide enhances fast ion conducting behavior at room temperature. Glasses of various compositions of silver based fast ion conductors in the AgI−Ag 2 O−[(1−x)B 2 O 3 −xTeO 2 ] (x=0 to1 mol% in steps of 0.2) glassy system have been prepared by melt quenching method. The glassy nature of the compounds has been confirmed by X-ray diffraction. The electrical conductivity (AC) measurements have been carried out in the frequency range of 1 KHz–3MHz by Impedance Analyzer in the temperature range 303–423K. The DC conductivity measurements were also carried out in the temperature range 300–523K. From both AC and DC conductivity studies, it is found that the conductivity increases and activation energy decreases with increasing the concentration of TeO 2 as well as with temperature. The conductivity of the present glass system is found to be of the order of 10 −2 S/cm at room temperature. The ionic transport number of these glasses is found to be 0.999 indicating that these glasses can be used as electrolyte in batteries

Thermodynamic behavior of glassy state of structurally related compounds.

Science.gov (United States)

Kaushal, Aditya Mohan; Bansal, Arvind Kumar

2008-08-01

Thermodynamic properties of amorphous pharmaceutical forms are responsible for enhanced solubility as well as poor physical stability. The present study was designed to investigate the differences in thermodynamic parameters arising out of disparate molecular structures and associations for four structurally related pharmaceutical compounds--celecoxib, valdecoxib, rofecoxib, and etoricoxib. Conventional and modulated temperature differential scanning calorimetry were employed to study glass forming ability and thermodynamic behavior of the glassy state of model compounds. Glass transition temperature of four glassy compounds was in a close range of 327.6-331.8 K, however, other thermodynamic parameters varied considerably. Kauzmann temperature, strength parameter and fragility parameter showed rofecoxib glass to be most fragile of the four compounds. Glass forming ability of the compounds fared similar in the critical cooling rate experiments, suggesting that different factors were determining the glass forming ability and subsequent behavior of the compounds in glassy state. A comprehensive understanding of such thermodynamic facets of amorphous form would help in rationalizing the approaches towards development of stable glassy pharmaceuticals.

Glassy Dynamics

DEFF Research Database (Denmark)

Jensen, Henrik J.; Sibani, Paolo

2007-01-01

The term glassy dynamics is often used to refer to the extremely slow relaxation observed in several types of many component systems. The time span needed to reach a steady, time independent, state will typically be far beyond experimentally accessible time scales. When melted alloys are cooled...... down they typically do not enter a crystalline ordered state. Instead the atoms retain the amorphous arrangement characteristic of the liquid high temperature phase while the mobility of the molecules decreases very many orders of magnitude. This colossal change in the characteristic dynamical time...

Composition and structure variation for magnetron sputtered tantalum oxynitride thin films, as function of deposition parameters

Energy Technology Data Exchange (ETDEWEB)

Cristea, D.; Pătru, M.; Crisan, A.; Munteanu, D. [Department of Materials Science, Transilvania University, 500036 Brasov (Romania); Crăciun, D. [Laser Department, National Institute for Laser, Plasma, and Radiation Physics, Magurele (Romania); Barradas, N.P. [Centro de Ciências e Tecnologias Nucleares, Instituto Superior Técnico, Universidade de Lisboa, E.N. 10 ao km 139,7, 2695-066 Bobadela LRS (Portugal); Alves, E. [Instituto de Plasmas e Fusão Nuclear, Instituto Superior Técnico, Universidade de Lisboa, E.N. 10 ao km 139,7, 2695-066 Bobadela LRS (Portugal); Apreutesei, M. [Université de Lyon, Institut des Nanotechnologies de Lyon INL-UMR 5270, CNRS, Ecole Centrale de Lyon, Ecully F-69134 (France); MATEIS Laboratory-INSA de Lyon, Bât. B. Pascal, 7 Avenue Jean Capelle, 69621 Villeurbanne Cedex (France); Moura, C. [Center of Physics, University of Minho, Campus de Gualtar, 4710-057 Braga (Portugal); Cunha, L., E-mail: lcunha@fisica.uminho.pt [Center of Physics, University of Minho, Campus de Gualtar, 4710-057 Braga (Portugal)

2015-12-15

Highlights: • Structural evolution from β-Ta, to fcc-Ta(O,N), to amorphous Ta{sub 2}O{sub 5} with increasing P(N{sub 2} + O{sub 2}). • The substrate bias influences the N content, but does not influence the O content of the films. • The structural features of the films appear at lower P(N{sub 2} + O{sub 2}) when produced with grounded substrate. - Abstract: Tantalum oxynitride thin films were produced by magnetron sputtering. The films were deposited using a pure Ta target and a working atmosphere with a constant N{sub 2}/O{sub 2} ratio. The choice of this constant ratio limits the study concerning the influence of each reactive gas, but allows a deeper understanding of the aspects related to the affinity of Ta to the non-metallic elements and it is economically advantageous. This work begins by analysing the data obtained directly from the film deposition stage, followed by the analysis of the morphology, composition and structure. For a better understanding regarding the influence of the deposition parameters, the analyses are presented by using the following criterion: the films were divided into two sets, one of them produced with grounded substrate holder and the other with a polarization of −50 V. Each one of these sets was produced with different partial pressure of the reactive gases P(N{sub 2} + O{sub 2}). All the films exhibited a O/N ratio higher than the N/O ratio in the deposition chamber atmosphere. In the case of the films produced with grounded substrate holder, a strong increase of the O content is observed, associated to the strong decrease of the N content, when P(N{sub 2} + O{sub 2}) is higher than 0.13 Pa. The higher Ta affinity for O strongly influences the structural evolution of the films. Grazing incidence X-ray diffraction showed that the lower partial pressure films were crystalline, while X-ray reflectivity studies found out that the density of the films depended on the deposition conditions: the higher the gas pressure, the

Quantitative characterization of silicon- and aluminium oxynitride films produced by reactive dc-magnetron sputtering

International Nuclear Information System (INIS)

Dreer, S.

2000-05-01

The deposition of aluminum and silicon oxynitride films by reactive dc-magnetron sputtering was systematically planned by design of experiments, carried out and evaluated with the application of specialized statistics software. The influence of the deposition parameters on the resulting films was evaluated by multiple regression analysis. With the obtained data a model of the deposition process for the quantitative prediction of the deposition parameters necessary to obtain films with desired composition was built. This is also of technological importance, since the physical properties of the films strongly depend on their composition. Furthermore, the long term repeatability of the deposition process was implemented into the model. A precise and economic way for quantitative bulk analysis of silicon/aluminum, oxygen and nitrogen based on EPMA was presented and the use of data gained by the latter method is discussed for the calculation of relative sensitivity factors for SIMS and hf-SNMS. Advantages and disadvantages of SIMS, hf-SNMS, hf-GD-OES, and sputter AES were compared. The combination FT-IR/EPMA/SIMS at present offers the best possibility for a quantitative bulk and in depth distribution analysis of such films in the range of 20 to 1000 nm thickness. The films were also characterized by XRD and PAA. The refractive index and the growth rate of the films were determined by spectroscopic ellipsometry. With indentation by a nano hardness tester the hardness and the Young's modulus of the films were obtained. The results of these measurements were evaluated by statistical software. The dependencies of the physical properties on the deposition parameters and on the film thickness were evaluated and quantified. Furthermore, the dependencies of the physical properties on the film composition represented by the oxygen content were evaluated. (author)

Corrosion resistance of zirconium oxynitride coatings deposited via DC unbalanced magnetron sputtering and spray pyrolysis-nitriding

Energy Technology Data Exchange (ETDEWEB)

Cubillos, G.I., E-mail: gcubillos@unal.edu.co [Department of Chemistry, Group of Materials and Chemical Processes, Universidad Nacional de Colombia, Av. Cra. 30 No 45-03, Bogotá (Colombia); Bethencourt, M., E-mail: manuel.bethencourt@uca.es [Department of Materials Science, Metallurgy Engineering and Inorganic Chemistry, International Campus of Excellence of the Sea - CEI-MAR, University of Cadiz, Avda. República Saharaui s/n, 11510 Puerto Real, Cádiz (Spain); Olaya, J.J., E-mail: jjolayaf@unal.edu.co [Faculty of Engineering, Group of Materials and Chemical Processes, Universidad Nacional de Colombia, Av. Cra. 30 No 45-03, Bogotá (Colombia)

2015-02-01

Highlights: • New ZrO{sub x}N{sub y} films were deposited on stainless steel 316L using PSY-N and UBMS. • ZrO{sub x}N{sub y} rhombohedral polycrystalline film grew with PSY-N. • Zr{sub 2}ON{sub 2} crystalline structures, mostly oriented along the (2 2 2) plane, grew with UBMS. • Layers improved corrosion behavior in NaCl media, especially those deposited by UBMS. - Abstract: ZrO{sub x}N{sub y}/ZrO{sub 2} thin films were deposited on stainless steel using two different methods: ultrasonic spray pyrolysis-nitriding (SPY-N) and the DC unbalanced magnetron sputtering technique (UBMS). Using the first method, ZrO{sub 2} was initially deposited and subsequently nitrided in an anhydrous ammonia atmosphere at 1023 K at atmospheric pressure. For UBMS, the film was deposited in an atmosphere of air/argon with a Φair/ΦAr flow ratio of 3.0. Structural analysis was carried out through X-ray diffraction (XRD), and morphological analysis was done through scanning electron microscopy (SEM) and atomic force microscopy (AFM). Chemical analysis was carried out using X-ray photoelectron spectroscopy (XPS). ZrO{sub x}N{sub y} rhombohedral polycrystalline film was produced with spray pyrolysis-nitriding, whereas using the UBMS technique, the oxynitride films grew with cubic Zr{sub 2}ON{sub 2} crystalline structures preferentially oriented along the (2 2 2) plane. Upon chemical analysis of the surface, the coatings exhibited spectral lines of Zr3d, O1s, and N1s, characteristic of zirconium oxynitride/zirconia. SEM analysis showed the homogeneity of the films, and AFM showed morphological differences according to the deposition technique of the coatings. Zirconium oxynitride films enhanced the stainless steel's resistance to corrosion using both techniques. The protective efficacy was evaluated using electrochemical techniques based on linear polarization (LP). The results indicated that the layers provide good resistance to corrosion when exposed to chloride

Silicon oxynitride films deposited by reactive high power impulse magnetron sputtering using nitrous oxide as a single-source precursor

Energy Technology Data Exchange (ETDEWEB)

Hänninen, Tuomas, E-mail: tuoha@ifm.liu.se; Schmidt, Susann; Jensen, Jens; Hultman, Lars; Högberg, Hans [Thin Film Physics Division, Department of Physics, Chemistry, and Biology (IFM), Linköping University, Linköping SE-581 83 (Sweden)

2015-09-15

Silicon oxynitride thin films were synthesized by reactive high power impulse magnetron sputtering of silicon in argon/nitrous oxide plasmas. Nitrous oxide was employed as a single-source precursor supplying oxygen and nitrogen for the film growth. The films were characterized by elastic recoil detection analysis, x-ray photoelectron spectroscopy, x-ray diffraction, x-ray reflectivity, scanning electron microscopy, and spectroscopic ellipsometry. Results show that the films are silicon rich, amorphous, and exhibit a random chemical bonding structure. The optical properties with the refractive index and the extinction coefficient correlate with the film elemental composition, showing decreasing values with increasing film oxygen and nitrogen content. The total percentage of oxygen and nitrogen in the films is controlled by adjusting the gas flow ratio in the deposition processes. Furthermore, it is shown that the film oxygen-to-nitrogen ratio can be tailored by the high power impulse magnetron sputtering-specific parameters pulse frequency and energy per pulse.

Atmospheric pressure plasma treatment of glassy carbon for adhesion improvement

DEFF Research Database (Denmark)

Kusano, Yukihiro; Mortensen, Henrik Junge; Stenum, Bjarne

2007-01-01

density increased with the plasma treatments. Adhesion test of the treated glassy carbon covered with cured epoxy showed cohesive failure, indicating strong bonding after the treatments. This is in contrast to the adhesion tests of untreated samples where the epoxy readily peeled off the glassy carbon....

On the spherical nanoindentation creep of metallic glassy thin films at room temperature

Energy Technology Data Exchange (ETDEWEB)

Zhang, T.H.; Ye, J.H. [Institution of Micro/Nano-Mechanical Testing Technology & Application, College of Mechanical Engineering, Zhejiang University of Technology, Hangzhou 310014 (China); Feng, Y.H. [State Key Laboratory of Nonlinear Mechanics (LNM), Institute of Mechanics, Chinese Academy of Sciences, Beijing 100190 (China); Ma, Y., E-mail: may@zjut.edu.cn [Institution of Micro/Nano-Mechanical Testing Technology & Application, College of Mechanical Engineering, Zhejiang University of Technology, Hangzhou 310014 (China)

2017-02-08

Metallic glassy thin films with eight kind of compositions were successfully prepared on Si substrate by magnetron sputtering. The room-temperature creep tests were performed at plastic regions for each sample relying on spherical nanoindetation. The creep deformations were studied by recording the total creep displacement and strain after 2000 s holding. More pronounced creep deformation was observed in the sample with lower glass transition temperature (T{sub g}). Strain rate sensitivity (SRS) was then calculated from the steady-state creep and exhibited a negative correlation with increasing T{sub g}. It is suggested that creep mechanism of the nano-sized metallic glass was T{sub g}-dependent, according to the demarcation of SRS values. Based on the obtained SRS, shear transformation zone (STZ) size in each sample could be estimated. The results indicated that an STZ involves about 25–60 atoms for the employed eight samples and is strongly tied to T{sub g}. The characteristic of STZ size in metallic glassy thin films was discussed in terms of applied method and deformation modes.

Effects of composition and microstructure of Pd-Cu-Si metallic glassy alloy thin films on hydrogen absorbing properties

International Nuclear Information System (INIS)

Kajita, Susumu; Kohara, Shinji; Onodera, Yohei; Fukunaga, Toshiharu; Matsubara, Eiichiro

2011-01-01

Thin films of Pd-Cu-Si metallic glassy alloys for a hydrogen sensor were fabricated by a sputtering method. In order to find out the effect of the composition and the microstructure of them on the hydrogen absorbing property (the H 2 response), the structural parameters based on the short-range order (SRO) were measured. Additionally, the change of the structural parameters with hydrogen absorption was measured, and the correlations of the change with the H 2 response and the hydrogen induced linear expansion coefficient (LEC) were examined. The H 2 response decreased with increases in Si content and the structural parameters. These results can be explained by the positive effects of Si content and the structural parameters on the formation of a trigonal prism which is a structural unit of Pd-based amorphous alloys, and by the negative effect of the trigonal prism on absorbing hydrogen. From the observation of the elongation of the Pd-Pd atomic distance with absorbing hydrogen, H atoms are supposed to occupy the space between Pd atoms. The amount of the change in the Pd-Pd atomic distance showed the positive correlations with the H 2 response and the LEC. (author)

Electrochemical behavior and voltammetric determination of acetaminophen based on glassy carbon electrodes modified with poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite films.

Science.gov (United States)

Zhu, Wencai; Huang, Hui; Gao, Xiaochun; Ma, Houyi

2014-12-01

Poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite film modified glassy carbon electrodes (4-ABA/ERGO/GCEs) were fabricated by a two-step electrochemical method. The electrochemical behavior of acetaminophen at the modified electrode was investigated by means of cyclic voltammetry. The results indicated that 4-ABA/ERGO composite films possessed excellent electrocatalytic activity towards the oxidation of acetaminophen. The electrochemical reaction of acetaminophen at 4-ABA/ERGO/GCE is proved to be a surface-controlled process involving the same number of protons and electrons. The voltammetric determination of acetaminophen performed with the 4-ABA/ERGO modified electrode presents a good linearity in the range of 0.1-65 μM with a low detection limit of 0.01 μM (S/N=3). In the case of using the 4-ABA/ERGO/GCE, acetaminophen and dopamine can be simultaneously determined without mutual interference. Furthermore, the 4-ABA/ERGO/GCE has good reproducibility and stability, and can be used to determine acetaminophen in tablets. Copyright © 2014 Elsevier B.V. All rights reserved.

Niobium-aluminum oxynitride prepared by ammonolysis of oxide precursor obtained through the citrate route

Energy Technology Data Exchange (ETDEWEB)

Yamamoto, Shinichi; Ohashi, Yoshio; Masubuchi, Yuji; Takeda, Takashi; Motohashi, Teruki [Graduate School of Engineering, Hokkaido University, N13W8, Kita-ku, Sapporo 060-8628 (Japan); Kikkawa, Shinichi, E-mail: kikkawa@eng.hokudai.ac.j [Graduate School of Engineering, Hokkaido University, N13W8, Kita-ku, Sapporo 060-8628 (Japan)

2009-08-12

Oxynitrides in the (Nb{sub 1-x}Al{sub x})(O,N) quaternary system were prepared by ammonolysis of oxide precursor obtained through the citrate route. The products at 1000 deg. C were a mixture of Nb(N,O) and NbN{sub 0.95} at the niobium end (x = 0) and amorphous Al(O,N) at the aluminum end (x = 1). A new cubic compound (A) appeared mixed with Nb(N,O) in the compositional range 0.1 <= x <= 0.4. Its almost pure product was obtained at x = 0.5. The X-ray diffraction pattern was rock salt type (Nb{sub 0.56}Al{sub 0.44})(O{sub 0.38}N{sub 0.37}square{sub 025}) in F{sub m-3m} with a = 0.43481(1) nm. The product showed superconductivity with T{sub c} = 15 K. Its crystallinity was much improved and its superconducting volume fraction increased to 32% after its thermal annealing at 1100 deg. C in evacuated sealed tube. A second cubic compound (B), rock salt type Nb[(O,N){sub 0.85}square{sub 0.15}] with a = 0.434 nm, was observed mixed with amorphous Al(O,N) in the as-prepared products of the range 0.6 <= x <= 0.9.

Quasi-equilibrium in glassy dynamics: an algebraic view

International Nuclear Information System (INIS)

Franz, Silvio; Parisi, Giorgio

2013-01-01

We study a chain of identical glassy systems in a constrained equilibrium, where each bond of the chain is forced to remain at a preassigned distance to the previous one. We apply this description to mean-field glassy systems in the limit of a long chain where each bond is close to the previous one. We show that this construction defines a pseudo-dynamic process that in specific conditions can formally describe real relaxational dynamics for long times. In particular, in mean-field spin glass models we can recover in this way the equations of Langevin dynamics in the long time limit at the dynamical transition temperature and below. We interpret the formal identity as evidence that in these situations the configuration space is explored in a quasi-equilibrium fashion. Our general formalism, which relates dynamics to equilibrium, puts slow dynamics in a new perspective and opens the way to the computation of new dynamical quantities in glassy systems. (paper)

Structural analysis and characterization of layer perovskite oxynitrides made from Dion-Jacobson oxide precursors

International Nuclear Information System (INIS)

Schottenfeld, Joshua A.; Benesi, Alan J.; Stephens, Peter W.; Chen, Gugang; Eklund, Peter C.; Mallouk, Thomas E.

2005-01-01

A three-layer oxynitride Ruddlesden-Popper phase Rb 1+x Ca 2 Nb 3 O 10-x N x .yH 2 O (x=0.7-0.8, y=0.4-0.6) was synthesized by ammonialysis at 800 o C from the Dion-Jacobson phase RbCa 2 Nb 3 O 10 in the presence of Rb 2 CO 3 . Incorporation of nitrogen into the layer perovskite structure was confirmed by XPS, combustion analysis, and MAS NMR. The water content was determined by thermal gravimetric analysis and the rubidium content by ICP-MS. A similar layered perovskite interconversion occurred in the two-layer Dion-Jacobson oxide RbLaNb 2 O 7 to yield Rb 1+x LaNb 2 O 7-x N x .yH 2 O (x=0.7-0.8, y=0.5-1.0). Both compounds were air- and moisture-sensitive, with rapid loss of nitrogen by oxidation and hydrolysis reactions. The structure of the three-layer oxynitride Rb 1.7 Ca 2 Nb 3 O 9.3 N 0.7 .0.5H 2 O was solved in space group P4/mmm with a=3.887(3) and c=18.65(1)A, by Rietveld refinement of X-ray powder diffraction data. The two-layer oxynitride structure Rb 1.8 LaNb 2 O 6.3 N 0.7 .1.0H 2 O was also determined in space group P4/mmm with a=3.934(2) and c=14.697(2)A. GSAS refinement of synchrotron X-ray powder diffraction data showed that the water molecules were intercalated between a double layer of Rb+ ions in both the two- and three-layer Ruddlesden-Popper structures. Optical band gaps were measured by diffuse reflectance UV-vis for both materials. An indirect band gap of 2.51eV and a direct band gap of 2.99eV were found for the three-layer compound, while an indirect band gap of 2.29eV and a direct band gap of 2.84eV were measured for the two-layer compound. Photocatalytic activity tests of the three-layer compound under 380nm pass filtered light with AgNO 3 as a sacrificial electron acceptor gave a quantum yield of 0.025% for oxygen evolution

Synthesis and crystal structure of K{sub 2}NiF{sub 4}-type novel Gd{sub 1+x}Ca{sub 1−x}AlO{sub 4−x}N{sub x} oxynitrides

Energy Technology Data Exchange (ETDEWEB)

Masubuchi, Yuji, E-mail: yuji-mas@eng.hokudai.ac.jp; Hata, Tomoyuki; Motohashi, Teruki; Kikkawa, Shinichi

2014-01-05

Highlights: • Novel gadolinium calcium aluminum oxynitride was prepared by solid state reaction. • Crystal structure of the oxynitride was refined by using synchrotron X-ray diffraction. • Gd{sub 1.2}Ca{sub 0.8}AlO{sub 3.8}N{sub 0.2} has a layered K{sub 2}NiF{sub 4}-type structure with the I4mm space group. • Nitride ions preferentially occupy the apical site of aluminum octahedron. -- Abstract: Novel gadolinium calcium aluminum oxynitrides, Gd{sub 1+x}Ca{sub 1−x}AlO{sub 4−x}N{sub x}, were prepared in x = 0.15–0.25 by the solid state reaction of a nitrogen–rich mixture with AlN as an aluminum source; the mixture was sintered twice at 1500 °C for 5 h under 0.5 MPa of nitrogen gas. Shift in the optical absorption edge was observed in their diffuse reflectance spectra from 4.46 eV for the oxide (x = 0) to 2.94 eV for the oxynitride at x = 0.2. The crystal structure of Gd{sub 1.2}Ca{sub 0.8}AlO{sub 3.8}N{sub 0.2} at x = 0.2 was refined using a synchrotron X-ray diffraction data as a layered K{sub 2}NiF{sub 4}-type structure with the I4mm space group. Longer Al–O/N bond lengths in the oxynitride than those in GdCaAlO{sub 4} suggest that the nitride ions are in the apical site of aluminum polyhedron, similar to those in Nd{sub 2}AlO{sub 3}N.

Aryl Diazonium Chemistry for the Surface Functionalization of Glassy Biosensors.

Science.gov (United States)

Zheng, Wei; van den Hurk, Remko; Cao, Yong; Du, Rongbing; Sun, Xuejun; Wang, Yiyu; McDermott, Mark T; Evoy, Stephane

2016-03-14

Nanostring resonator and fiber-optics-based biosensors are of interest as they offer high sensitivity, real-time measurements and the ability to integrate with electronics. However, these devices are somewhat impaired by issues related to surface modification. Both nanostring resonators and photonic sensors employ glassy materials, which are incompatible with electrochemistry. A surface chemistry approach providing strong and stable adhesion to glassy surfaces is thus required. In this work, a diazonium salt induced aryl film grafting process is employed to modify a novel SiCN glassy material. Sandwich rabbit IgG binding assays are performed on the diazonium treated SiCN surfaces. Fluorescently labelled anti-rabbit IgG and anti-rabbit IgG conjugated gold nanoparticles were used as markers to demonstrate the absorption of anti-rabbit IgG and therefore verify the successful grafting of the aryl film. The results of the experiments support the effectiveness of diazonium chemistry for the surface functionalization of SiCN surfaces. This method is applicable to other types of glassy materials and potentially can be expanded to various nanomechanical and optical biosensors.

Aryl Diazonium Chemistry for the Surface Functionalization of Glassy Biosensors

Directory of Open Access Journals (Sweden)

Wei Zheng

2016-03-01

Full Text Available Nanostring resonator and fiber-optics-based biosensors are of interest as they offer high sensitivity, real-time measurements and the ability to integrate with electronics. However, these devices are somewhat impaired by issues related to surface modification. Both nanostring resonators and photonic sensors employ glassy materials, which are incompatible with electrochemistry. A surface chemistry approach providing strong and stable adhesion to glassy surfaces is thus required. In this work, a diazonium salt induced aryl film grafting process is employed to modify a novel SiCN glassy material. Sandwich rabbit IgG binding assays are performed on the diazonium treated SiCN surfaces. Fluorescently labelled anti-rabbit IgG and anti-rabbit IgG conjugated gold nanoparticles were used as markers to demonstrate the absorption of anti-rabbit IgG and therefore verify the successful grafting of the aryl film. The results of the experiments support the effectiveness of diazonium chemistry for the surface functionalization of SiCN surfaces. This method is applicable to other types of glassy materials and potentially can be expanded to various nanomechanical and optical biosensors.

Diffusion coefficients of tracers in glassy polymer systems prepared by gamma radiolysis

International Nuclear Information System (INIS)

Tonge, M.P.; Gilbert, R.G.

1996-01-01

Diffusion-controlled reactions are common in free radical polymerisation reactions, especially in glassy polymer matrices. Such reactions commonly have an important influence on the polymerisation process and final polymer properties. For example, the dominant growth-stopping event (bimolecular termination) is generally diffusion-controlled. In glassy polymer systems, where molecular mobility is very low, the chain growth mechanism (propagation) may become diffusion-controlled. At present, the mechanism for propagation in glassy polymers is poorly understood, but it is expected by the Smoluchowski expression applied to propagation to depend strongly on the diffusion coefficient of monomer. The objective of this study is to measure reliable diffusion coefficients of small tracer molecules in glassy polymers, and compare these with propagation rate coefficients in similar systems, by the prediction above. Samples were initially prepared in a sealed sampled cell containing monomer, inert diluent, and tracer dye. After irradiation for several days, complete conversion of monomer to polymer can be obtained. The diffusion coefficients for two tracer dyes have been measured as a function of weight fraction polymer glassy poly(methyl methacrylate) samples

Electrochemical Determination of Chlorpyrifos on a Nano-TiO₂Cellulose Acetate Composite Modified Glassy Carbon Electrode.

Science.gov (United States)

Kumaravel, Ammasai; Chandrasekaran, Maruthai

2015-07-15

A rapid and simple method of determination of chlorpyrifos is important in environmental monitoring and quality control. Electrochemical methods for the determination of pesticides are fast, sensitive, reproducible, and cost-effective. The key factor in electrochemical methods is the choice of suitable electrode materials. The electrode materials should have good stability, reproducibility, more sensitivity, and easy method of preparation. Mercury-based electrodes have been widely used for the determination of chlorpyrifos. From an environmental point of view mercury cannot be used. In this study a biocompatible nano-TiO2/cellulose acetate modified glassy carbon electrode was prepared by a simple method and used for the electrochemical sensing of chlorpyrifos in aqueous methanolic solution. Electroanalytical techniques such as cyclic voltammetry, differential pulse voltammetry, and amperometry were used in this work. This electrode showed very good stability, reproducibility, and sensitivity. A well-defined peak was obtained for the reduction of chlorpyrifos in cyclic voltammetry and differential pulse voltammetry. A smooth noise-free current response was obtained in amperometric analysis. The peak current obtained was proportional to the concentration of chlorpyrifos and was used to determine the unknown concentration of chlorpyrifos in the samples. Analytical parameters such as LOD, LOQ, and linear range were estimated. Analysis of real samples was also carried out. The results were validated through HPLC. This composite electrode can be used as an alternative to mercury electrodes reported in the literature.

Pressure-induced transformations in computer simulations of glassy water

Science.gov (United States)

Chiu, Janet; Starr, Francis W.; Giovambattista, Nicolas

2013-11-01

Glassy water occurs in at least two broad categories: low-density amorphous (LDA) and high-density amorphous (HDA) solid water. We perform out-of-equilibrium molecular dynamics simulations to study the transformations of glassy water using the ST2 model. Specifically, we study the known (i) compression-induced LDA-to-HDA, (ii) decompression-induced HDA-to-LDA, and (iii) compression-induced hexagonal ice-to-HDA transformations. We study each transformation for a broad range of compression/decompression temperatures, enabling us to construct a "P-T phase diagram" for glassy water. The resulting phase diagram shows the same qualitative features reported from experiments. While many simulations have probed the liquid-state phase behavior, comparatively little work has examined the transitions of glassy water. We examine how the glass transformations relate to the (first-order) liquid-liquid phase transition previously reported for this model. Specifically, our results support the hypothesis that the liquid-liquid spinodal lines, between a low-density and high-density liquid, are extensions of the LDA-HDA transformation lines in the limit of slow compression. Extending decompression runs to negative pressures, we locate the sublimation lines for both LDA and hyperquenched glassy water (HGW), and find that HGW is relatively more stable to the vapor. Additionally, we observe spontaneous crystallization of HDA at high pressure to ice VII. Experiments have also seen crystallization of HDA, but to ice XII. Finally, we contrast the structure of LDA and HDA for the ST2 model with experiments. We find that while the radial distribution functions (RDFs) of LDA are similar to those observed in experiments, considerable differences exist between the HDA RDFs of ST2 water and experiment. The differences in HDA structure, as well as the formation of ice VII (a tetrahedral crystal), are a consequence of ST2 overemphasizing the tetrahedral character of water.

Application of first-principles methods for the calculation of the crystal and electronic structure of oxynitrides

Energy Technology Data Exchange (ETDEWEB)

Fang, C.M.; Metselaar, R.; Hintzen, H.T.; With, G. de [Eindhoven Univ. of Technology (Netherlands). Lab. of Solid State and Materials Chemistry

2002-07-01

Theoretical simulations using density functional theory (DFT) within ab initio total-energy and molecular-dynamics method have been performed for several oxynitride materials. Examples dealt with are compounds in the Ta-O-N, Si-O-N and Al-O-N systems. Random or partially ordered distributions of the oxygen and nitrogen ions as well as other structural defects can be predicted very well by these methods. Local structure relaxation and its influence on the electronic properties are addressed. (orig.)

Electrochemical and microstructural characterization of platinum supported on glassy carbon

Directory of Open Access Journals (Sweden)

Terzić Sanja

2007-01-01

Full Text Available The effect of the electrochemical oxidation of glassy carbon on the deposition of platinum particles and the electrocatalytic activity of platinum supported on oxidized glassy carbon were studied for methanol oxidation in H2SO4 solution. Platinum was potentiostatically deposited from H2SO4 + 6mM H2PtCl6 solution. Glassy carbon was anodically polarized in 1 M NaOH at 1.41 V (SCE for 35 and 95 s and in 0.5 M H2SO4 at 2V (SCE for 35; 95 s and 2.25 V for 35 and 95 s. Electrochemical treatment of the GC support leads to a better distribution of platinum on the substrate and has remarkable effect on the activity. The activity of the Pt/GCox electrode for methanol oxidation is larger than that of polycrystalline Pt and by more than one order of magnitude larger than that of a Pt/GC electrode. This increase in activity indicates the pronounced role of the organic residues of the GC support on the properties of Pt particles deposited on glassy carbon.

Ionic conductivities of lithium phosphorus oxynitride glasses, polycrystals, and thin films

International Nuclear Information System (INIS)

Wang, B.; Bates, J.B.; Chakoumakos, B.C.; Sales, B.C.; Kwak, B.S.; Zuhr, R.A.; Robertson, J.D.

1994-11-01

Various lithium phosphorus oxynitrides have been prepared in the form of glasses, polycrystals, and thin films. The structures of these compounds were investigated by X-ray and neutron diffraction, X-ray photoelectron spectroscopy (XPS), and high-performance liquid chromatography (HPLC). The ac impedance measurements indicate a significant improvement of ionic conductivity as the result of incorporation of nitrogen into the structure. In the case of polycrystalline Li 2.88 PO 3.73 N 0.14 with the γ-Li 3 PO 4 structure, the conductivity increased by several orders of magnitude on small addition of nitrogen. The highest conductivities in the bulk glasses and thin films were found to be 3.0 x 10 -7 and 8.9 x 10 -7 S·cm -1 at 25 degrees C, respectively

Electrical properties of carbon nanotubes modified GaSe glassy system

Science.gov (United States)

Khan, Hana; Khan, Zubair M. S. H.; Islam, Shama; Rahman, Raja Saifu; Husain, M.; Zulfequar, M.

2018-05-01

In this paper we report the investigation of the effect of Carbon Nanotubes (CNT) addition on the electrical properties of GaSe Glassy system. Dielectric constant and dielectric loss of GaSe glassy system are found to increase on CNT addition. The conductivity of GaSe glasy systems is also found to increase on CNT addition. This behavior is attributed to the excellent conduction properties of Carbon Nanotube.

Grain-boundary, glassy-phase identification and possible artifacts

International Nuclear Information System (INIS)

Simpson, Y.K.; Carter, C.B.; Sklad, P.; Bentley, J.

1985-01-01

Specimen artifacts such as grain boundary grooving, surface damage of the specimen, and Si contamination are shown experimentally to arise from the ion milling used in the preparation of transmission electron microscopy specimens. These artifacts in polycrystalline, ceramic specimens can cause clean grain boundaries to appear to contain a glassy phase when the dark-field diffuse scattering technique, the Fresnel fringe technique, and analytical electron microscopy (energy dispersive spectroscopy) are used to identify glassy phases at a grain boundary. The ambiguity in interpreting each of these techniques due to the ion milling artifacts will be discussed from a theoretical view point and compared to experimental results obtained for alumina

Structure dependent resistivity and dielectric characteristics of tantalum oxynitride thin films produced by magnetron sputtering

Energy Technology Data Exchange (ETDEWEB)

Cristea, D., E-mail: daniel.cristea@unitbv.ro [Department of Materials Science, Transilvania University, 500036 Brasov (Romania); Crisan, A. [Department of Materials Science, Transilvania University, 500036 Brasov (Romania); Cretu, N. [Electrical Engineering and Applied Physics Department, Transilvania University, 500036 Brasov (Romania); Borges, J. [Centro de Física, Universidade do Minho, Campus de Gualtar, 4710 - 057 Braga (Portugal); Instituto Pedro Nunes, Laboratório de Ensaios, Desgaste e Materiais, Rua Pedro Nunes, 3030-199 Coimbra (Portugal); SEG-CEMUC, Mechanical Engineering Department, University of Coimbra, 3030-788 Coimbra (Portugal); Lopes, C.; Cunha, L. [Centro de Física, Universidade do Minho, Campus de Gualtar, 4710 - 057 Braga (Portugal); Ion, V.; Dinescu, M. [National Institute for Lasers, Plasma and Radiation Physics, Lasers Department, “Photonic Processing of Advanced Materials” Group, PO Box MG-16, RO 77125 Magurele-Bucharest (Romania); Barradas, N.P. [Centro de Ciências e Tecnologias Nucleares, Instituto Superior Técnico, Universidade de Lisboa, E.N. 10 ao km 139,7, 2695-066 Bobadela LRS (Portugal); Alves, E. [Instituto de Plasmas e Fusão Nuclear, Instituto Superior Técnico, Universidade de Lisboa, E.N. 10 ao km 139,7, 2695-066 Bobadela LRS (Portugal); Apreutesei, M. [MATEIS Laboratory-INSA de Lyon, 21 Avenue Jean Capelle, 69621 Villeurbanne cedex (France); Université de Lyon, Institut des Nanotechnologies de Lyon INL-UMR5270, CNRS, Ecole Centrale de Lyon, Ecully F-69134 (France); Munteanu, D. [Department of Materials Science, Transilvania University, 500036 Brasov (Romania)

2015-11-01

Highlights: • Tantalum oxynitride thin films have been deposited by magnetron sputtering, in various configurations. • The rising of the reactive gases mixture flow has the consequence of a gradual increase in the non-metallic content in the films, which results in a 10 orders of magnitude resistivity domain. • The higher resistivity films exhibit dielectric constants up to 41 and quality factors up to 70. - Abstract: The main purpose of this work is to present and to interpret the change of electrical properties of Ta{sub x}N{sub y}O{sub z} thin films, produced by DC reactive magnetron sputtering. Some parameters were varied during deposition: the flow of the reactive gases mixture (N{sub 2} and O{sub 2}, with a constant concentration ratio of 17:3); the substrate voltage bias (grounded, −50 V or −100 V) and the substrate (glass, (1 0 0) Si or high speed steel). The obtained films exhibit significant differences. The variation of the deposition parameters induces variations of the composition, microstructure and morphology. These differences cause variation of the electrical resistivity essentially correlated with the composition and structural changes. The gradual decrease of the Ta concentration in the films induces amorphization and causes a raise of the resistivity. The dielectric characteristics of some of the high resistance Ta{sub x}N{sub y}O{sub z} films were obtained in the samples with a capacitor-like design (deposited onto high speed steel, with gold pads deposited on the dielectric Ta{sub x}N{sub y}O{sub z} films). Some of these films exhibited dielectric constant values higher than those reported for other tantalum based dielectric films.

Effect of chain rigidity on network architecture and deformation behavior of glassy polymer networks

Science.gov (United States)

Knowles, Kyler Reser

Processing carbon fiber composite laminates creates molecular-level strains in the thermoset matrix upon curing and cooling which can lead to failures such as geometry deformations, micro-cracking, and other issues. It is known strain creation is attributed to the significant volume and physical state changes undergone by the polymer matrix throughout the curing process, though storage and relaxation of cure-induced strains remain poorly understood. This dissertation establishes two approaches to address the issue. The first establishes testing methods to simultaneously measure key volumetric properties of a carbon fiber composite laminate and its polymer matrix. The second approach considers the rigidity of the polymer matrix in regards to strain storage and relaxation mechanisms which ultimately control composite performance throughout manufacturing and use. Through the use of a non-contact, full-field strain measurement technique known as digital image correlation (DIC), we describe and implement useful experiments which quantify matrix and composite parameters necessary for simulation efforts and failure models. The methods are compared to more traditional techniques and show excellent correlation. Further, we established relationships which represent matrix-fiber compatibility in regards to critical processing constraints. The second approach involves a systematic study of epoxy-amine networks which are chemically-similar but differ in chain segment rigidity. Prior research has investigated the isomer effect of glassy polymers, showing sizeable differences in thermal, volumetric, physical, and mechanical properties. This work builds on these themes and shows the apparent isomer effect is rather an effect of chain rigidity. Indeed, it was found that structurally-dissimilar polymer networks exhibit very similar properties as a consequence of their shared average network rigidity. Differences in chain packing, as a consequence of chain rigidity, were shown to

Thermonuclear reactor materials composed of glassy carbons

International Nuclear Information System (INIS)

Kazumata, Yukio.

1979-01-01

Purpose: To improve the durability to plasma radiation by the use of glassy carbon as the structural materials for the first wall and the blanket in thermonuclear devices. Constitution: The glassy carbon (glass-like carbon) is obtained by forming specific organic substances into a predetermined configuration and carbonizing them by heat decomposition under special conditions. They are impermeable carbon material of 1.40 - 1.70 specific gravity, less graphitizable and being almost in isotropic crystal forms in which isotropic structure such as in graphite is scarcely observed. They have an extremely high hardness, are less likely to be damaged when exposed to radiation and have great strength and corrosion resistance. Accordingly, the service life of the reactor walls and the likes can remarkably be increased by using the materials. (Horiuchi, T.)

Positron annihilation study of graphite, glassy carbon and C60/C70 fullerene

International Nuclear Information System (INIS)

Hasegawa, Masayuki; Kajino, Masahiro; Yamaguchi, Sadae; Iwata, Tadao; Kuramoto, Eiichi; Takenaka, Minoru.

1992-01-01

ACAR (Angular Correlation of Annihilation Radiation) and positron lifetime measurements have been made on, HOPG (Highly Oriented Pyrolytic Graphite), isotropic fine-grained graphite, glassy carbons and C 60 /C 70 powder. HOPG showed marked bimodality along the c-axis and anisotropy in ACAR momentum distribution, which stem from characteristic annihilation between 'interlayer' positrons and π-electrons in graphite. ACAR curves of the isotropic graphite and glassy carbons are even narrower than that of HOPG perpendicular to the c-axis. Positron lifetime of 420 and 390 - 480 psec, much longer than that of 221 psec in HOPG, were observed for the isotropic graphite and glassy carbons respectively, which are due to positron trapping in structural voids in them. Positron lifetime and ACAR width (FWHM) can be well correlated to void sizes (1.7 to 5.0 nm) of glassy carbons which have been determined by small angle neutron (SAN) scattering measurements. ACAR curves and positron lifetime of C 60 /C 70 powder agree well with those of glassy carbons. This shows that positron wave functions extend, as in the voids of glassy carbons, much wider than open spaces of the octahedral interstices of the face-centered cubic (FCC) structure of C 60 crystal and strongly suggests positron trapping in the 'soccer ball' vacancy. Possible positron states in the carbon materials are discussed with a simple model of void volume-trapping. Preliminary results on neutron irradiation damage in HOPG are also presented. (author)

The electrocatalytical reduction of m-nitrophenol on palladium nanoparticles modified glassy carbon electrodes

International Nuclear Information System (INIS)

Shi Qiaofang; Diao Guowang

2011-01-01

Highlights: ► The deposition of palladium on a GC electrode was performed by cyclic voltammetry. ► SEM images showed palladium nanoparticles deposited on a glassy carbon (GC) electrode. ► The Pd/GC electrode can effectively catalyze m-nitrophenol in aqueous media. ► The reduction of m-nitrophenol on the Pd/GC electrode depended on potential and pH. ► XPS spectra of the Pd/GC electrodes demonstrated the presence of palladium. - Abstract: Palladium nanoparticles modified glassy carbon electrodes (Pd/GC) were prepared via the electrodeposition of palladium on a glassy carbon (GC) electrode using cyclic voltammetry in different sweeping potential ranges. The scanning electron microscope images of palladium particles on the GC electrodes indicate that palladium particles with diameters of 20–50 nm were homogeneously dispersed on the GC electrode at the optimal deposition conditions, which can effectively catalyze the reduction of m-nitrophenol in aqueous solutions, but their catalytic activities are strongly related to the deposition conditions of Pd. The X-ray photoelectron spectroscopy spectra of the Pd/GC electrode confirmed that 37.1% Pd was contained in the surface composition of the Pd/GC electrode. The cyclic voltammograms of the Pd/GC electrode in the solution of m-nitrophenol show that the reduction peak of m-nitrophenol shifts towards the more positive potentials, accompanied with an increase in the peak current compared to the bare GC electrode. The electrocatalytic activity of the Pd/GC electrode is affected by pH values of the solution. In addition, the electrolysis of m-nitrophenol under a constant potential indicates that the reduction current of m-nitrophenol on the Pd/GC electrode is approximately 20 times larger than that on the bare GC electrode.

Study of short range order in alloy of glassy metals and effect of neutron irradiation on them

International Nuclear Information System (INIS)

Habibi, S.; Banaee, N.; Salman, M.; Gupta, A.; Principi, G.

2000-04-01

In this paper, we have studied a series of glassy metals with composition Fe 78-x Ni x Si 8 B 14 with x=0, 15, 25,38,53, 58. We have used Moessbauer spectroscopy to get information about short range order and local structure in these alloys. The specimens are exposed to neutron irradiation to perturb local structure and their short range order. The hyperfine parameters obtained from spectra before and after n-irradiation and are compared

Ionic conductivities of lithium phosphorus oxynitride glasses, polycrystals, and thin films

Energy Technology Data Exchange (ETDEWEB)

Wang, B.; Bates, J.B.; Chakoumakos, B.C.; Sales, B.C.; Kwak, B.S.; Zuhr, R.A. [Oak Ridge National Lab., TN (United States); Robertson, J.D. [Univ. of Kentucky, Lexington, KY (United States). Dept. of Chemistry

1994-11-01

Various lithium phosphorus oxynitrides have been prepared in the form of glasses, polycrystals, and thin films. The structures of these compounds were investigated by X-ray and neutron diffraction, X-ray photoelectron spectroscopy (XPS), and high-performance liquid chromatography (HPLC). The ac impedance measurements indicate a significant improvement of ionic conductivity as the result of incorporation of nitrogen into the structure. In the case of polycrystalline Li{sub 2.88}PO{sub 3.73}N{sub 0.14} with the {gamma}-Li{sub 3}PO{sub 4} structure, the conductivity increased by several orders of magnitude on small addition of nitrogen. The highest conductivities in the bulk glasses and thin films were found to be 3.0 {times} 10{sup -7} and 8.9 {times} 10{sup -7} S{center_dot}cm{sup -1} at 25{degrees}C, respectively.

Resistivity and Passivity Characterization of Ni-Base Glassy Alloys in NaOH Media

Directory of Open Access Journals (Sweden)

Khadijah M. Emran

2018-01-01

Full Text Available Resistivity and passivation behavior of two Ni-base bulk metallic glasses, with the nominal composition of Ni70Cr21Si0.5B0.5P8C ≤ 0.1Co ≤ 1Fe ≤ 1 (VZ1 and Ni72.65Cr7.3-Si6.7B2.15C ≤ 0.06Fe8.2Mo3 (VZ2, in various concentrations of NaOH solutions were studied. The investigations involved cyclic polarization (CP, electrochemical impedance spectroscopy (EIS, and electrochemical frequency modulation (EFM methods. Cyclic polarization measurements showed spontaneous passivation for both Ni-base glassy alloys at all alkaline concentrations, due to the presence of chromium as an alloying element that formed an oxide film on the alloy surface. The EIS analysis showed that the passive layers grown on the two Ni-base glassy alloy surfaces are formed by a double oxide layer structure. Scanning electron microscope (SEM examinations of the electrode surface showed Cr, Ni, Fe, and O rich corrosion products that reduced the extent of corrosion damage. Atomic force microscopy (AFM imaging technique was used to evaluate the topographic and morphologic features of surface layers formed on the surface of the alloys.

Electrocatalytical oxidation and sensitive determination of acetaminophen on glassy carbon electrode modified with graphene–chitosan composite

International Nuclear Information System (INIS)

Zheng, Meixia; Gao, Feng; Wang, Qingxiang; Cai, Xili; Jiang, Shulian; Huang, Lizhang; Gao, Fei

2013-01-01

The electrochemical behaviors of acetaminophen (ACOP) on a graphene–chitosan (GR–CS) nanocomposite modified glassy carbon electrode (GCE) were investigated by cyclic voltammetry (CV), chronocoulometry (CC) and differential pulse voltammetry (DPV). Electrochemical characterization showed that the GR–CS nanocomposite had excellent electrocatalytic activity and surface area effect. As compared with bare GCE, the redox signal of ACOP on GR–CS/GCE was greatly enhanced. The values of electron transfer rate constant (k s ), diffusion coefficient (D) and the surface adsorption amount (Γ ⁎ ) of ACOP on GR–CS/GCE were determined to be 0.25 s −1 , 3.61 × 10 −5 cm 2 s −1 and 1.09 × 10 −9 mol cm −2 , respectively. Additionally, a 2e − /2H + electrochemical reaction mechanism of ACOP was deduced based on the acidity experiment. Under the optimized conditions, the ACOP could be quantified in the range from 1.0 × 10 −6 to 1.0 × 10 −4 M with a low detection limit of 3.0 × 10 −7 M based on 3S/N. The interference and recovery experiments further showed that the proposed method is acceptable for the determination of ACOP in real pharmaceutical preparations. Highlights: ► A chitosan–graphene nanocomposite modified glassy carbon electrode was prepared. ► The modified electrode was electrochemically characterized by CV and EIS. ► Electro-oxidation of acetaminophen was examined on the modified electrode. ► Sensing analysis of the modified electrode toward acetaminophen was studied

Voltammetric quantitation of nitazoxanide by glassy carbon electrode

Directory of Open Access Journals (Sweden)

Rajeev Jain

2013-12-01

Full Text Available The present study reports voltammetric reduction of nitazoxanide in Britton–Robinson (B–R buffer by cyclic and square-wave voltammetry at glassy carbon electrode. A versatile fully validated voltammetric method for quantitative determination of nitazoxanide in pharmaceutical formulation has been proposed. A squrewave peak current was linear over the nitazoxanide concentration in the range of 20–140 µg/mL. The limit of detection (LOD and limit of quantification (LOQ was calculated to be 5.23 μg/mL and 17.45 μg/mL, respectively. Keywords: Nitazoxanide, Squarewave voltammetry, Glassy carbon electrode, Pharmaceutical formulation

Fabrication and nano-imprintabilities of Zr-, Pd- and Cu-based glassy alloy thin films

International Nuclear Information System (INIS)

Takenaka, Kana; Saidoh, Noriko; Nishiyama, Nobuyuki; Inoue, Akihisa

2011-01-01

With the aim of investigating nano-imprintability of glassy alloys in a film form, Zr 49 Al 11 Ni 8 Cu 32 , Pd 39 Cu 29 Ni 13 P 19 and Cu 38 Zr 47 Al 9 Ag 6 glassy alloy thin films were fabricated on Si substrate by a magnetron sputtering method. These films exhibit a very smooth surface, a distinct glass transition phenomenon and a large supercooled liquid region of about 80 K, which are suitable for imprinting materials. Moreover, thermal nano-imprintability of these obtained films is demonstrated by using a dot array mold with a dot diameter of 90 nm. Surface observations revealed that periodic nano-hole arrays with a hole diameter of 90 nm were successfully imprinted on the surface of these films. Among them, Pd-based glassy alloy thin film indicated more precise pattern imprintability, namely, flatter residual surface plane and sharper hole edge. It is said that these glassy alloy thin films, especially Pd-based glassy alloy thin film, are one of the promising materials for fabricating micro-machines and nano-devices by thermal imprinting.

Comparing the mechanism of water condensation and evaporation in glassy aerosol.

Science.gov (United States)

Bones, David L; Reid, Jonathan P; Lienhard, Daniel M; Krieger, Ulrich K

2012-07-17

Atmospheric models generally assume that aerosol particles are in equilibrium with the surrounding gas phase. However, recent observations that secondary organic aerosols can exist in a glassy state have highlighted the need to more fully understand the kinetic limitations that may control water partitioning in ambient particles. Here, we explore the influence of slow water diffusion in the condensed aerosol phase on the rates of both condensation and evaporation, demonstrating that significant inhibition in mass transfer occurs for ultraviscous aerosol, not just for glassy aerosol. Using coarse mode (3-4 um radius) ternary sucrose/sodium chloride/aqueous droplets as a proxy for multicomponent ambient aerosol, we demonstrate that the timescale for particle equilibration correlates with bulk viscosity and can be ≫10(3) s. Extrapolation of these timescales to particle sizes in the accumulation mode (e.g., approximately 100 nm) by applying the Stokes-Einstein equation suggests that the kinetic limitations imposed on mass transfer of water by slow bulk phase diffusion must be more fully investigated for atmospheric aerosol. Measurements have been made on particles covering a range in dynamic viscosity from  10(13) Pa s. We also retrieve the radial inhomogeneities apparent in particle composition during condensation and evaporation and contrast the dynamics of slow dissolution of a viscous core into a labile shell during condensation with the slow percolation of water during evaporation through a more homogeneous viscous particle bulk.

Immobilization of DNA at Glassy Ccarbon Electrodes: A Critical Study of Adsorbed Layer

Directory of Open Access Journals (Sweden)

G. A. Rivas

2005-11-01

Full Text Available In this work we present a critical study of the nucleic acid layer immobilized atglassy carbon electrodes. Different studies were performed in order to assess the nature of theinteraction between DNA and the electrode surface. The adsorption and electrooxidation of DNAdemonstrated to be highly dependent on the surface and nature of the glassy carbon electrode. TheDNA layer immobilized at a freshly polished glassy carbon electrode was very stable even afterapplying highly negative potentials. The electron transfer of potassium ferricyanide, catechol anddopamine at glassy carbon surfaces modified with thin (obtained by adsorption under controlledpotential conditions and thick (obtained by casting the glassy carbon surface with highly concentratedDNA solutions DNA layers was slower than that at the bare glassy carbon electrode, although thiseffect was dependent on the thickness of the layer and was not charge selective. Raman experimentsshowed an important decrease of the vibrational modes assigned to the nucleobases residues,suggesting a strong interaction of these residues with the electrode surface. The hybridization ofoligo(dG21 and oligo(dC21 was evaluated from the guanine oxidation signal and the reduction of theredox indicator Co(phen33+ . In both cases the chronopotentiometric response indicated that thecompromise of the bases in the interaction of DNA with the electrode surface is too strong, preventingfurther hybridization. In summary, glassy carbon is a useful electrode material to detect DNA in adirect and very sensitive way, but not to be used for the preparation of biorecognition layers by directadsorption of the probe sequence on the electrode surface for detecting the hybridization event.

Composition and microstructure of a furnace ash deposit from a coal-fired utility boiler

Energy Technology Data Exchange (ETDEWEB)

Fessler, R R

1980-07-01

An exploratory study of the structure and composition of furnace-ash deposits was carried out using optical metallography, electron microprobe analysis, scanning electron microscopy, and energy-dispersive X-ray analysis. The results of these analyses were supplemented by studies of particulate melting temperature using hot-stage microscopy to measure melting temperature, and energy-dispersive X-ray analyses to measure composition of melted particles. It was found that the general structure of the ash deposit was a matrix of glassy, spherical particles having a wide range of composition in which unfused particles containing iron oxide and calcium oxide were dispersed. At the imprint of the tube surface a considerable concentration of calcium, sulphur and iron was found. Near the fused outer surface of the deposit, the glassy materials had melted into a porous, glassy slag containing spherical globules of iron oxide combined with other materials. There were no systematic compositional gradients from the tube surface to the fused outer layer except for the sulfur layer found only at the tube surface. However, there were significant differences in composition from particle to particle and these differences were similar to those found in the coal mineral matter as isolated by low-temperature ashing. Single particles of low-temperature ash were found having low fusion temperatures, in the range of fusion temperatures for particles in furnance has. Thus, the glassy spheres found in furnace deposits could originate from single coal particles, without the need of interactions among coal particles or ash particles.

Voltammetric determination of the endocrine disruptor diethylstilbestrol by using a glassy carbon electrode modified with a composite consisting of platinum nanoparticles and multiwalled carbon nanotubes

International Nuclear Information System (INIS)

Hu, Xiaobin; Zhang, Rongfei

2016-01-01

A nanocomposite consisting of multi-walled carbon nanotubes (MWCNTs) decorated with Pt nanoparticles (Pt-NPs) was synthesized via an ionic liquid-assisted method. The composite was characterized by transmission electron microscopy, X-ray diffraction patterns, and X-ray photo-electron spectroscopy. The results showed the Pt-NPs to be evenly deposited on the surface of the MWCNTs, with diameters ranging from about 2 nm to 3 nm. The nanocomposite was used to modify a glassy carbon electrode which then revealed a substantial catalytic activity for the oxidation of diethylstilbestrol (DES), best at a working potential of 0.73 V (vs. Ag/AgCl) at pH 7. The electrochemical oxidation mechanism is discussed. The peak current in square wave voltammetry is linearly related to the concentration of DES in the 0.1 to 25 μM range. The limit of detection (at an SNR of 3) is 12 nM. (author)

Prediction of Process-Induced Distortions in L-Shaped Composite Profiles Using Path-Dependent Constitutive Law

Science.gov (United States)

Ding, Anxin; Li, Shuxin; Wang, Jihui; Ni, Aiqing; Sun, Liangliang; Chang, Lei

2016-10-01

In this paper, the corner spring-in angles of AS4/8552 L-shaped composite profiles with different thicknesses are predicted using path-dependent constitutive law with the consideration of material properties variation due to phase change during curing. The prediction accuracy mainly depends on the properties in the rubbery and glassy states obtained by homogenization method rather than experimental measurements. Both analytical and finite element (FE) homogenization methods are applied to predict the overall properties of AS4/8552 composite. The effect of fiber volume fraction on the properties is investigated for both rubbery and glassy states using both methods. And the predicted results are compared with experimental measurements for the glassy state. Good agreement is achieved between the predicted results and available experimental data, showing the reliability of the homogenization method. Furthermore, the corner spring-in angles of L-shaped composite profiles are measured experimentally and the reliability of path-dependent constitutive law is validated as well as the properties prediction by FE homogenization method.

Spatially heterogeneous ages in glassy dynamics

International Nuclear Information System (INIS)

Castillo, Horacio E.; Chamon, Claudio Chamon; Cugliandolo, Leticia F.; Iguain, Jose Luis; Kennett, Malcolm P.

2003-09-01

We construct a framework for the study of fluctuations in the nonequilibrium relaxation of glassy systems with and without quenched disorder. We study two types of two-time local correlators with the aim of characterizing the heterogeneous evolution in these systems: in one case we average the local correlators over histories of the thermal noise, in the other case we simply coarse-grain the local correlators obtained for a given noise realization. We explain why the noise-averaged correlators describe the fingerprint of quenched disorder when it exists, while the coarse-grained correlators are linked to noise-induced mesoscopic fluctuations. We predict constraints on the distribution of the fluctuations of the coarse-grained quantities. In particular, we show that locally defined correlations and responses are connected by a generalized local out-of-equilibrium fluctuation-dissipation relation. We argue that large size heterogeneities in the age of the system survive in the long-time limit. A symmetry of the underlying theory, namely invariance under reparametrizations of the time coordinates, underlies these results. We establish a connection between the probabilities of spatial distributions of local coarse-grained quantities and the theory of dynamic random manifolds. We define, and discuss the behavior of, a two-time dependent correlation length from the spatial decay of the fluctuations in the two-time local functions. We characterize the fluctuations in the system in terms of their fractal properties. For concreteness, we present numerical tests performed on disordered spin models in finite and infinite dimensions. Finally, we explain how these ideas can be applied to the analysis of the dynamics of other glassy systems that can be either spin models without disorder or atomic and molecular glassy systems. (author)

Dielectric relaxation in glassy Se75In25− xPbx alloys

Indian Academy of Sciences (India)

In this paper we report the effect of Pb incorporation in the dielectric properties of a-Se75In25 glassy alloy. The temperature and frequency dependence of the dielectric constants and the dielectric losses in glassy Se75In25−Pb ( = 0, 5, 10 and 15) alloys in the frequency range (1 kHz–5 MHz) and temperature range ...

Temperature and frequency response of conductivity in Ag2S doped chalcogenide glassy semiconductor

Science.gov (United States)

Ojha, Swarupa; Das, Anindya Sundar; Roy, Madhab; Bhattacharya, Sanjib

2018-06-01

The electric conductivity of chalcogenide glassy semiconductor xAg2S-(1-x)(0.5S-0.5Te) has been presented here as a function of temperature and frequency. Formation of different nanocrystallites has been confirmed from X-ray diffraction study. It is also noteworthy that average size of nanocrystallites decreases with the increase of dislocation density. Dc conductivity data have been interpreted using Mott's model and Greaves's model in low and high temperature regions respectively. Ac conductivity above the room temperature has been analyzed using Meyer-Neldel (MN) conduction rule. It is interestingly noted that Correlated Barrier Hopping (CBH) model is the most appropriate conduction mechanism for x = 0.35, where pairs of charge carrier are considered to hop over the potential barrier between the sites via thermal activation. To interpret experimental data for x = 0.45, modified non-overlapping small polaron tunnelling (NSPT) model is supposed to be appropriate model due to tunnelling through grain boundary. The conductivity spectra at various temperatures have been analyzed using Almond-West Formalism (power law model). Scaling of conductivity spectra reveals that electrical relaxation process of charge carriers (polaron) is temperature independent but depends upon the composition of the present chalcogenide glassy system.

Potentiometric application of boron- and phosphorus-doped glassy carbon electrodes

Directory of Open Access Journals (Sweden)

ZORAN V. LAUSEVIC

2001-03-01

Full Text Available Acomparative study was carried out of the potentiometric application of boronand phosphorus-doped and undoped glassy carbon samples prepared at the same heat treatment temperature (HTT 1000°C. The electrochemical activities of the obtained electrode materials were investigated on the example of argentometric titrations. It was found that the electrochemical behaviour of the doped glassy carbon samples are very similar to a Sigri (undoped glassy carbon sample (HTT 2400°C. The experiments showed that the potentiometric response depends on the polarization mode, the nature of the sample, the pretreatment of the electrode surface, and the nature of the supporting electrolyte. The amounts of iodide, bromide, and of chloridewere determined to be 1.27 mg, 0.80 mg and 0.54 mg, respectively, with a maximum relative standard deviation of less than 1.1%. The obtained results are in good agreement with the results of comparative potentiometric titrations using a silver indicator electrode. The titrationmethod was applied to the indirect determination of pyridoxine hydrochloride, i.e., vitamin B6.

Voltammetric pH sensing using carbon electrodes: glassy carbon behaves similarly to EPPG.

Science.gov (United States)

Lu, Min; Compton, Richard G

2014-09-21

Developing and building on recent work based on a simple sensor for pH determination using unmodified edge plane pyrolytic graphite (EPPG) electrodes, we present a voltammetric method for pH determination using a bare unmodified glassy carbon (GC) electrode. By exploiting the pH sensitive nature of quinones present on carbon edge-plane like sites within the GC, we show how GC electrodes can be used to measure pH. The electro-reduction of surface quinone groups on the glassy carbon electrode was characterised using cyclic voltammetry (CV) and optimised with square-wave voltammetry (SWV) at 298 K and 310 K. At both temperatures, a linear correlation was observed, corresponding to a 2 electron, 2 proton Nernstian response over the aqueous pH range 1.0 to 13.1. As such, unmodified glassy carbon electrodes are seen to be pH dependent, and the Nernstian response suggests its facile use for pH sensing. Given the widespread use of glassy carbon electrodes in electroanalysis, the approach offers a method for the near-simultaneous measurement and monitoring of pH during such analyses.

Electrochemical behavior and voltammetric determination of acetaminophen based on glassy carbon electrodes modified with poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite films

International Nuclear Information System (INIS)

Zhu, Wencai; Huang, Hui; Gao, Xiaochun; Ma, Houyi

2014-01-01

Poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite film modified glassy carbon electrodes (4-ABA/ERGO/GCEs) were fabricated by a two-step electrochemical method. The electrochemical behavior of acetaminophen at the modified electrode was investigated by means of cyclic voltammetry. The results indicated that 4-ABA/ERGO composite films possessed excellent electrocatalytic activity towards the oxidation of acetaminophen. The electrochemical reaction of acetaminophen at 4-ABA/ERGO/GCE is proved to be a surface-controlled process involving the same number of protons and electrons. The voltammetric determination of acetaminophen performed with the 4-ABA/ERGO modified electrode presents a good linearity in the range of 0.1–65 μM with a low detection limit of 0.01 μM (S/N = 3). In the case of using the 4-ABA/ERGO/GCE, acetaminophen and dopamine can be simultaneously determined without mutual interference. Furthermore, the 4-ABA/ERGO/GCE has good reproducibility and stability, and can be used to determine acetaminophen in tablets. - Highlights: • The 4-ABA/ERGO/GCE was fabricated by a two-step electrochemical method. • Electrochemical behavior of acetaminophen at the 4-ABA/ERGO/GCE was investigated. • The electrochemical sensor exhibited a low detection limit and good selectivity. • This sensor was applied to the detection of acetaminophen in commercial tablets

Electrochemical behavior and voltammetric determination of acetaminophen based on glassy carbon electrodes modified with poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite films

Energy Technology Data Exchange (ETDEWEB)

Zhu, Wencai [Key Laboratory for Colloid and Interface Chemistry of State Education Ministry, School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China); School of Chemistry and Chemical Engineering, Qilu Normal University, Jinan 250013 (China); Huang, Hui; Gao, Xiaochun [Key Laboratory for Colloid and Interface Chemistry of State Education Ministry, School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China); Ma, Houyi, E-mail: hyma@sdu.edu.cn [Key Laboratory for Colloid and Interface Chemistry of State Education Ministry, School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China)

2014-12-01

Poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite film modified glassy carbon electrodes (4-ABA/ERGO/GCEs) were fabricated by a two-step electrochemical method. The electrochemical behavior of acetaminophen at the modified electrode was investigated by means of cyclic voltammetry. The results indicated that 4-ABA/ERGO composite films possessed excellent electrocatalytic activity towards the oxidation of acetaminophen. The electrochemical reaction of acetaminophen at 4-ABA/ERGO/GCE is proved to be a surface-controlled process involving the same number of protons and electrons. The voltammetric determination of acetaminophen performed with the 4-ABA/ERGO modified electrode presents a good linearity in the range of 0.1–65 μM with a low detection limit of 0.01 μM (S/N = 3). In the case of using the 4-ABA/ERGO/GCE, acetaminophen and dopamine can be simultaneously determined without mutual interference. Furthermore, the 4-ABA/ERGO/GCE has good reproducibility and stability, and can be used to determine acetaminophen in tablets. - Highlights: • The 4-ABA/ERGO/GCE was fabricated by a two-step electrochemical method. • Electrochemical behavior of acetaminophen at the 4-ABA/ERGO/GCE was investigated. • The electrochemical sensor exhibited a low detection limit and good selectivity. • This sensor was applied to the detection of acetaminophen in commercial tablets.

Thermodynamic Modeling of Gas Transport in Glassy Polymeric Membranes.

Science.gov (United States)

Minelli, Matteo; Sarti, Giulio Cesare

2017-08-19

Solubility and permeability of gases in glassy polymers have been considered with the aim of illustrating the applicability of thermodynamically-based models for their description and prediction. The solubility isotherms are described by using the nonequilibrium lattice fluid (NELF) (model, already known to be appropriate for nonequilibrium glassy polymers, while the permeability isotherms are described through a general transport model in which diffusivity is the product of a purely kinetic factor, the mobility coefficient, and a thermodynamic factor. The latter is calculated from the NELF model and mobility is considered concentration-dependent through an exponential relationship containing two parameters only. The models are tested explicitly considering solubility and permeability data of various penetrants in three glassy polymers, PSf, PPh and 6FDA-6FpDA, selected as the reference for different behaviors. It is shown that the models are able to calculate the different behaviors observed, and in particular the permeability dependence on upstream pressure, both when it is decreasing as well as when it is increasing, with no need to invoke the onset of additional plasticization phenomena. The correlations found between polymer and penetrant properties with the two parameters of the mobility coefficient also lead to the predictive ability of the transport model.

X-ray absorption investigation of titanium oxynitride nanoparticles obtained from laser pyrolysis

International Nuclear Information System (INIS)

Simon, Pardis; March, Katia; Stéphan, Odile; Leconte, Yann; Reynaud, Cécile; Herlin-Boime, Nathalie; Flank, Anne-Marie

2013-01-01

Highlights: • Original Ti(O,N) nanoparticles with a TiO FCC structure were synthesized by laser pyrolysis. • EELS and XAS allows to demonstrate that the nanoparticles are a solid solution of N and O in Ti. • Upon heat treatment, oxidation occurs from the surface with survival of FCC contribution till 400 °C. • Optical properties (absorption in the visible range) can be adjusted through the control of oxidation state. - Abstract: This work presents a structural study by X-ray Absorption Spectroscopy (XAS) and Electron Energy-Loss Spectroscopy (EELS) of complex titanium oxynitride nanoparticles (Ti(O,N)), synthesized by laser pyrolysis from titanium tetraisopropoxide and ammonia as precursors. Previous structural characterizations obtained by XRD and XPS have shown that the nanoparticles present a TiO type face-centered cubic (FCC) structure but with three different oxidation degree for titanium. The synthesis of this kind of titanium oxide or oxynitride nanoparticles is very unusual. Moreover, their properties are highly dependent of their structure. EELS spectrum-imaging data were therefore used for mapping the different chemical species. These measurements reveal that the nanoparticles are composed of a FCC solid solution of nitrogen and oxygen in titanium. The local structure around Ti was then studied. XANES measurements show an absorption threshold corresponding to a global valence state between Ti 3+ and Ti 4+ , with a pre-edge structure characteristic of a mix between a face-centered cubic (FCC) structure and a disordered TiO 2 structure whereas the EXAFS signal is dominated by the contribution of the FCC structure. Oxidative heat-treatments have been performed from 250 to 450 °C in order to follow the transition towards the dioxide phase. EELS measurements show that the oxidation occurs from the surface of the nanoparticles. XAS show that this transition does not involve any other crystallographic phase than TiO 2 , mainly in its anatase form, and

Relation between time-temperature transformation and continuous heating transformation diagrams of metallic glassy alloys

International Nuclear Information System (INIS)

Louzguine-Luzgin, Dmitri V.; Inoue, Akihisa

2005-01-01

The time-temperature transformation (TTT) diagrams for the onset of devitrification of the Ge-Ni-La and Cu-Hf-Ti glassy alloys were calculated from the isothermal differential calorimetry data using an Arrhenius equation. The continuous heating transformation (CHT) diagrams for the onset of devitrification of the glassy alloys were subsequently recalculated from TTT diagrams. The recalculation method used for conversion of the TTT into CHT diagrams produces reasonable results and is not sensitive to the type of the devitrification reaction (polymorphous or primary transformation). The diagrams allow to perform a comparison of the stabilities of glassy alloys on a long-term scale. The relationship between these diagrams is discussed

Impedimetric Salmonella aptasensor using a glassy carbon electrode modified with an electrodeposited composite consisting of reduced graphene oxide and carbon nanotubes

International Nuclear Information System (INIS)

Jia, Fei; Dai, Ruitong; Duan, Nuo; Wu, Shijia; Wang, Zhouping; Li, Xingmin

2016-01-01

We describe a Salmonella biosensor that was obtained by electrochemical immobilization of a nanocomposite consisting of reduced graphene oxide (rGO) and carboxy-modified multi-walled carbon nanotubes (MWCNTs) directly on the surface of a glassy carbon electrode (GCE). An amino-modified aptamer specific for Salmonella was covalently bound to the rGO-MWCNT composite via amide bonds. The morphology of the rGO-MWCNT nanocomposite was characterized by transmission electron microscopy and scanning electron microscopy. Cyclic voltammetry and electrochemical impedance spectroscopy were used to monitor all steps during assembly. When exposed to samples containing Salmonella, the anti-Salmonella aptamer on the electrode captures its target. Hence, electron transfer is blocked, and this results in a large increase in impedance. Salmonella can be quantified by this aptasensor, typically operated at a working voltage of 0.2 V (vs. Ag/AgCl), in the range from 75 to 7.5 × 10 5 cfu⋅mL −1 and detection limit of 25 cfu⋅mL −1 (at an S/N of 3). The method is perceived to have a wide scope in that other bacteria may be detected by analogy to this approach and with very low limits of detection by applying respective analyte-specific aptamers. (author)

Playback interference of glassy-winged sharp shooter communication

Science.gov (United States)

Animal communication is vital to reproduction, particularly for securing a mate. Insects commonly communicate by exchanging vibrational signals that are transmitted through host plants. The glassy-winged sharpshooter (GWSS), Homalodisca vitripennis, is an important vector of Xylella fastidiosa, a pl...

Glassy selenium at high pressure: Le Chatelier's principle still works

Science.gov (United States)

Brazhkin, V. V.; Tsiok, O. B.

2017-10-01

Selenium is the only easily vitrified elementary substance. Numerous experimental studies of glassy Se (g -Se) at high pressures show a large spread in the data on the compressibility and electrical resistivity of g -Se. Furthermore, H. Liu et al. [Proc. Natl. Acad. Sci. USA 105, 13229 (2008), 10.1073/pnas.0806857105] have arrived at the surprising conclusion that the volume of glass increases during pressure-induced crystallization. We have performed high-precision measurements of the specific volume and electrical resistivity of glassy selenium (g -Se) at high hydrostatic pressures up to 9 GPa. The measured bulk modulus at normal pressure is B =(9.0 5 ±0.15 ) GPa and its pressure derivative is BP'=6.4 ±0.2 . In the pressure range P <3 GPa, glassy selenium has an anomalously large negative second derivative of the bulk modulus. The electrical resistivity of g -Se decreases almost exponentially with increasing pressure and reaches 20 Ω cm at a pressure of 8.75 GPa. The inelastic behavior and weak relaxation of the volume for g -Se begin at pressures above 3.5 GPa; the volume and logarithm of the electrical resistivity relax significantly (logarithmically with the time) at pressures above 8 GPa. Bulk measurements certainly indicate that the volume of g -Se glass in the crystallization pressure range is larger than the volumes of both appearing crystalline phases (by 2% and 4%). Therefore, the "volume expansion phenomenon" suggested in [H. Liu et al., Proc. Natl. Acad. Sci. USA 105, 13229 (2008), 10.1073/pnas.0806857105] is not observed, and the pressure-induced crystallization of glassy selenium is consistent with the laws of thermodynamics.

Hansen solubility parameters for a carbon fiber/epoxy composite

DEFF Research Database (Denmark)

Launay, Helene; Hansen, Charles M.; Almdal, Kristoffer

2007-01-01

In this study, the physical affinity between an epoxy matrix and oxidized, unsized carbon fibers has been evaluated using Hansen solubility (cohesion) parameters (HSP). A strong physical compatibility has been shown, since their respective HSP are close. The use of a glassy carbon substrate...... as a model for unsized carbon fiber has been demonstrated as appropriate for the study of interactions between the materials in composite carbon fiber-epoxy systems. The HSP of glassy carbon are similar to those of carbon fibers and epoxy matrix. (C) 2007 Elsevier Ltd. All rights reserved....

Very sensitive electrochemical determination of diuron on glassy carbon electrode modified with reduced graphene oxide-gold nanoparticle-Nafion composite film.

Science.gov (United States)

Zarei, K; Khodadadi, A

2017-10-01

In this work, a very sensitive electrochemical sensor based on glassy carbon electrode (GCE) modified with reduced graphene oxide-gold nanoparticles/Nafion (rGO-AuNPs/Nafion) composite film was applied to determine diuron. Synthesized GO was characterized using X-ray diffraction (XRD) and UV-visible spectroscopy. The surface morphology of the rGO-AuNPs/Nafion film was also characterized using scanning electron microscopy and electrochemical impedance spectroscopy. Cyclic voltammetry (CV) and adsorptive differential pulse voltammetry (AdDPV) were applied to investigate the electrochemical response of the diuron on the modified electrode. The electrode showed a linear response at 1.0×10 -9 -1.0×10 -7 M and a detection limit of 0.3nM under the optimized conditions. The effect of some other species on the determination of diuron was investigated and the sensor showed good selectivity for determination of diuron. The constructed sensor was applied to determine diuron in enriched samples of orange juice, mineral and tap water which statistical t-test showed accuracy of method. Also the sensor was applied to obtain diuron content in the tea sample. The reliability of the proposed sensor was confirmed after comparing the results with those obtained using high performance liquid chromatography (HPLC) as a comparative method. Copyright © 2017 Elsevier Inc. All rights reserved.

Annealing effects on the migration of ion-implanted cadmium in glassy carbon

Energy Technology Data Exchange (ETDEWEB)

Hlatshwayo, T.T., E-mail: thulani.hlatshwayo@up.ac.za [Physics Department, University of Pretoria, Pretoria (South Africa); Sebitla, L.D. [Physics Department, University of Pretoria, Pretoria (South Africa); Physics Department, University of Botswana, Gaborone (Botswana); Njoroge, E.G.; Mlambo, M.; Malherbe, J.B. [Physics Department, University of Pretoria, Pretoria (South Africa)

2017-03-15

The migration behaviour of cadmium (Cd) implanted into glassy carbon and the effects of annealing on radiation damage introduced by ion implantation were investigated. The glassy carbon substrates were implanted with Cd at a dose of 2 × 10{sup 16} ions/cm{sup 2} and energy of 360 keV. The implantation was performed at room temperature (RT), 430 °C and 600 °C. The RT implanted samples were isochronally annealed in vacuum at 350, 500 and 600 °C for 1 h and isothermally annealed at 350 °C up to 4 h. The as-implanted and annealed samples were characterized by Raman spectroscopy and Rutherford backscattering spectrometry (RBS). Raman results revealed that implantation at room temperature amorphized the glassy carbon structure while high temperature implantations resulted in slightly less radiation damage. Isochronal annealing of the RT implanted samples resulted in some recrystallization as a function of increasing temperature. The original glassy carbon structure was not achieved at the highest annealing temperature of 600 °C. Diffusion of Cd in glassy carbon was already taking place during implantation at 430 °C. This diffusion of Cd was accompanied by significant loss from the surface during implantation at 600 °C. Isochronal annealing of the room temperature implanted samples at 350 °C for 1 h caused Cd to diffuse towards the bulk while isothermal annealing at 500 and 600 °C resulted in the migration of implanted Cd toward the surface accompanied by a loss of Cd from the surface. Isothermal annealing at 350 °C for 1 h caused Cd to diffuse towards the bulk while for annealing time >1 h Cd diffused towards the surface. These results were interpreted in terms of trapping and de-trapping of implanted Cd by radiation damage.

How Glassy States Affect Brown Carbon Production?

Science.gov (United States)

Liu, P.; Li, Y.; Wang, Y.; Bateman, A. P.; Zhang, Y.; Gong, Z.; Gilles, M. K.; Martin, S. T.

2015-12-01

Secondary organic material (SOM) can become light-absorbing (i.e. brown carbon) via multiphase reactions with nitrogen-containing species such as ammonia and amines. The physical states of SOM, however, potentially slow the diffusion of reactant molecules in organic matrix under conditions that semisolids or solids prevail, thus inhibiting the browning reaction pathways. In this study, the physical states and the in-particle diffusivity were investigated by measuring the evaporation kinetics of both water and organics from aromatic-derived SOMs using a quartz-crystal-microbalance (QCM). The results indicate that the SOMs derived from aromatic precursors toluene and m-xylene became solid (glassy) and the in particle diffusion was significantly impeded for sufficiently low relative humidity ( toluene-derived SOM after ammonia exposure at varied RHs. The results suggest that the production of light-absorbing nitrogen-containing compounds from multiphase reactions with ammonia was kinetically limited in the glassy organic matrix, which otherwise produce brown carbon. The results of this study have significant implications for production and optical properties of brown carbon in urban atmospheres that ultimately influence the climate and tropospheric photochemistry.

Shear-transformation-zone theory of linear glassy dynamics.

Science.gov (United States)

Bouchbinder, Eran; Langer, J S

2011-06-01

We present a linearized shear-transformation-zone (STZ) theory of glassy dynamics in which the internal STZ transition rates are characterized by a broad distribution of activation barriers. For slowly aging or fully aged systems, the main features of the barrier-height distribution are determined by the effective temperature and other near-equilibrium properties of the configurational degrees of freedom. Our theory accounts for the wide range of relaxation rates observed in both metallic glasses and soft glassy materials such as colloidal suspensions. We find that the frequency-dependent loss modulus is not just a superposition of Maxwell modes. Rather, it exhibits an α peak that rises near the viscous relaxation rate and, for nearly jammed, glassy systems, extends to much higher frequencies in accord with experimental observations. We also use this theory to compute strain recovery following a period of large, persistent deformation and then abrupt unloading. We find that strain recovery is determined in part by the initial barrier-height distribution, but that true structural aging also occurs during this process and determines the system's response to subsequent perturbations. In particular, we find by comparison with experimental data that the initial deformation produces a highly disordered state with a large population of low activation barriers, and that this state relaxes quickly toward one in which the distribution is dominated by the high barriers predicted by the near-equilibrium analysis. The nonequilibrium dynamics of the barrier-height distribution is the most important of the issues raised and left unresolved in this paper.

Morphological and compositional engineering of Ni/carbon ...

Indian Academy of Sciences (India)

Ni/multi-walled carbon nanotubes (MWCNTs) composite films were deposited on the glassy carbon electrode (GCE) by a Ni plating bath containing homogeneously dispersed MWCNTs using polyvinylpyrrolidone (PVP) as dispersion additive. Incorporation of MWCNTs into Ni matrix was greatly enhanced by the application ...

Electrochemical oxidation of niclosamide at a glassy carbon ...

African Journals Online (AJOL)

Cyclic voltammetry, square-wave voltammetry and controlled potential electrolysis have been used to study the electrochemical oxidation behaviour of niclosamide at a glassy carbon electrode. The number of electrons transferred, the wave characteristics, the diffusion coefficient and reversibility of the reactions have been ...

Glassy carbon supercapacitor: 100,000 cycles demonstrated

Energy Technology Data Exchange (ETDEWEB)

Baertsch, M; Braun, A; Schnyder, B; Koetz, R [Paul Scherrer Inst. (PSI), Villigen (Switzerland)

1999-08-01

A 5 V glassy carbon capacitor stack was built consisting of four bipolar and two end-plate electrodes. More than 100,000 charging/discharging cycles were applied to test the stability of the double-layer capacitor. Low and high frequency resistances were measured as a function of the number of cycles. (author) 2 figs., 1 ref.

Observation of glassy state relaxation during annealing of frozen sugar solutions by X-ray computed tomography.

Science.gov (United States)

Nakagawa, Kyuya; Tamiya, Shinri; Do, Gabsoo; Kono, Shinji; Ochiai, Takaaki

2018-06-01

Glassy phase formation in a frozen product determines various properties of the freeze-dried products. When an aqueous solution is subjected to freezing, a glassy phase forms as a consequence of freeze-concentration. During post-freezing annealing, the relaxation of the glassy phase and the ripening of ice crystals (i.e. Ostwald ripening) spontaneously occur, where the kinetics are controlled by the annealing and glass transition temperatures. This study was motivated to observe the progress of glassy state relaxation separate from ice coarsening during annealing. X-ray computed tomography (CT) was used to observe a frozen and post-freezing annealed solutions by using monochromatized X-ray from the synchrotron radiation. CT images were successfully obtained, and the frozen matrix were analyzed based on the gray level values that were equivalent to the linear X-ray attenuation coefficients of the observed matters. The CT images obtained from rapidly frozen sucrose and dextrin solutions with different concentrations gave clear linear relationships between the linear X-ray attenuation coefficients values and the solute concentrations. It was confirmed that the glassy state relaxation progressed as increasing annealing time, and this trend was larger in the order of the glass transition temperature of the maximally freeze-concentrated phase. The sucrose-water system required nearly 20 h of annealing time at -5 °C for the completion of the glassy phase relaxation, whereas dextrin-water systems required much longer periods because of their higher glass transition temperatures. The trends of ice coarsening, however, did not perfectly correspond to the trends of the relaxation, suggesting that the glassy phase relaxation and Ostwald ripening would jointly control the ice crystal growth/ripening kinetics, and the dominant mechanism differed by the annealing stage. Copyright © 2018 Elsevier B.V. All rights reserved.

A novel sensor made of Antimony Doped Tin Oxide-silica composite sol on a glassy carbon electrode modified by single-walled carbon nanotubes for detection of norepinephrine.

Science.gov (United States)

Wang, Zhao; Wang, Kai; Zhao, Lu; Chai, Shigan; Zhang, Jinzhi; Zhang, Xiuhua; Zou, Qichao

2017-11-01

In this study, we designed a novel molecularly imprinted polymer (MIP), Antimony Doped Tin Oxide (ATO)-silica composite sol, which was made using a sol-gel method. Then a sensitive and selective imprinted electrochemical sensor was constructed with the ATO-silica composite sol on a glassy carbon electrode modified by single-walled carbon nanotubes (SWNTs). The introduction of SWNTs increased the sensitivity of the MIP sensor. The surface morphology of the MIP and MIP/SWNTs were characterized by scanning electron microscopy (SEM), and the optimal conditions for detection were determined. The oxidative peak current increased linearly with the concentration of norepinephrine in the range of 9.99×10 -8 M to 1.50×10 -5 M, as detected by cyclic voltammetry (CV), the detection limit was 3.33×10 -8 M (S/N=3). In addition, the proposed electrochemical sensors were successfully applied to detect the norepinephrine concentration in human blood serum samples. The recoveries of the sensors varied from 99.67% to 104.17%, indicating that the sensor has potential for the determination of norepinephrine in clinical tests. Moreover, the imprinted electrochemical sensor was used to selectively detect norepinephrine. The analytical application was conducted successfully and yielded accurate and precise results. Copyright © 2017. Published by Elsevier B.V.

SUPERNOVA SHOCK-WAVE-INDUCED CO-FORMATION OF GLASSY CARBON AND NANODIAMOND

Energy Technology Data Exchange (ETDEWEB)

Stroud, Rhonda [Naval Research Laboratory, Washington, D.C.; Chisholm, Matthew F [ORNL; Heck, Phillipp [The Field Museum, Chicago, IL; Alexander, Conel [Carnegie Institution of Washington; Nittler, Larry [Carnegie Institution of Washington

2011-01-01

Nanodiamond (ND) was the first extrasolar dust phase to be identified in meteorites. However, the 2 nm average size of the NDs precludes isotopic analysis of individual particles, and thus their origin(s) remains controversial. Using electron microscopy with subnanometer resolution, we show that ND separates from the Allende and Murchison meteorites are actually a two-phase mixture of ND and glassy carbon. This phase mixture is likely the product of supernova shock-wave transformation of pre-formed organics in the interstellar medium (ISM). The glassy carbon ND mixture is also a plausible contributor to the 2175 extinction feature in the diffuse ISM.

Band gap determination of thin praseodymium oxide layers on aluminium oxynitride films

Energy Technology Data Exchange (ETDEWEB)

Bergholz, Matthias; Schmeisser, Dieter [Brandenburgische Technische Universitaet, Cottbus (Germany). Angewandte Physik - Sensorik

2008-07-01

High-k dielectrics are important as never before in semiconductor industry. We investigate Pr{sub 2}O{sub 3} as one representative of this group on silicon and silicon-aluminium oxynitride substrates. In earlier work we observed the positive influence of this AlO{sub x}N{sub y} intermediate layer on the electrical properties of the Pr{sub 2}O{sub 3} layer. Now we present in-situ EELS, XPS and UPS measurements of gradually grown thin Pr{sub 2}O{sub 3} on AlO{sub x}N{sub y}. From these measurements we determine the band structure and find a very fast change of the band gap for the first few A, coupled with n-type behaviour for the Pr{sub 2}O{sub 3} film. These results are compared with RIXS measurements of a 5 nm Pr{sub 2}O{sub 3} on a 1 nm thick AlO{sub x}N{sub y} layer.

Solvated electron structure in glassy matrices

International Nuclear Information System (INIS)

Kevan, L.

1981-01-01

Current knowledge of the detailed geometrical structure of solvated electrons in aqueous and organic media is summarized. The geometry of solvated electrons in glassy methanol, ethanol, and 2-methyltetrahydrofuran is discussed. Advanced electron magnetic resonance methods and development of new methods of analysis of electron spin echo modulation patterns, second moment line shapes, and forbidden photon spin-flip transitions for paramagnetic species in these disordered systems are discussed. 66 references are cited

A glassy lava flow from Toconce volcano and its relation with the Altiplano-Puna Magma Body in Central Andes

Science.gov (United States)

Godoy, B.; Rodriguez, I.; Aguilera, F.

2012-12-01

Toconce is a composite stratovolcano located at the San Pedro - Linzor volcanic chain (SPLVC). This volcanic chain distributes within the Altiplano-Puna region (Central Andes) which is characterized by extensive rhyodacitic-to-rhyolitic ignimbritic fields, and voluminous domes of dacitic-to-rhyolitic composition (de Silva, 1989). The felsic melts that gave origin to ignimbrites and domes at this area were generated by mixing of mantle-derived magmas and anatectic melts assimilated during their ascent through the thick crust. Thus, partially molten layers exist in the upper crust below the APVC (de Silva et al., 2006). Evidence of large volumes of such melts has been also proposed by geophysical methods (i.e. the Altiplano-Puna Magma Body; Chmielowsky et al., 1999) In this work, petrography and whole rock, mineralogical and melt inclusions geochemistry of a glassy lava flow of Toconce volcano are presented. Petrographically, this lava flow shows a porphyric texture, with euhdral to subhedral plagioclase, ortho- and clino-pyroxene phenocrysts immersed in a glassy groundmass. Geochemically, the lava flow has 64.7% wt. SiO2. The glassy groundmass (~70% wt. SiO2) is more felsic than all the lavas in the volcanic chain (47-68% wt., Godoy et al., 2011). Analyzed orthopyroxene-hosted melt inclusions show an even higher SiO2 content (72-75% wt.), and a decreasing on Al2O3, Na2O, and CaO content with differentiation. Crystallization pressures of this lava flow, obtained using Putirka's two-pyroxene and clinopyroxene-liquid models (Putirka, 2008), range between 6 and 9 kbar. According to crystallization pressures, and major element composition, a felsic source located at shallow crustal pressures - where plagioclase is a stable mineralogical phase - originated the inclusions. This could be related to the presence of the Altiplano-Puna Magma Body (APMB) located below SPLVC. On the other hand, glassy groundmass, and disequilibrium textures in minerals of this lava flow could

High temperature flow behaviour of SiC reinforced lithium ...

Indian Academy of Sciences (India)

Unknown

Verdier (1996) explored the effect of SiC particulate rein- forcements in oxynitride glasses. Like in silicate compo- sites, non-Newtonian behaviour was observed in oxynitride glasses but instead of shear thinning they observed shear thickening. This was attributed to change in composition of grain boundary glass coupled ...

Graphene oxide-mediated electrochemistry of glucose oxidase on glassy carbon electrodes.

Science.gov (United States)

Castrignanò, Silvia; Valetti, Francesca; Gilardi, Gianfranco; Sadeghi, Sheila J

2016-01-01

Glucose oxidase (GOD) was immobilized on glassy carbon electrodes in the presence of graphene oxide (GO) as a model system for the interaction between GO and biological molecules. Lyotropic properties of didodecyldimethylammonium bromide (DDAB) were used to stabilize the enzymatic layer on the electrode surface resulting in a markedly improved electrochemical response of the immobilized GOD. Transmission electron microscopy images of the GO with DDAB confirmed the distribution of the GO in a two-dimensional manner as a foil-like material. Although it is known that glassy carbon surfaces are not ideal for hydrogen peroxide detection, successful chronoamperometric titrations of the GOD in the presence of GO with β-d-glucose were performed on glassy carbon electrodes, whereas no current response was detected upon β-d-glucose addition in the absence of GO. The GOD-DDAB-GO system displayed a high turnover efficiency and substrate affinity as a glucose biosensor. The simplicity and ease of the electrode preparation procedure of this GO/DDAB system make it a good candidate for immobilizing other biomolecules for fabrication of amperometric biosensors. © 2015 International Union of Biochemistry and Molecular Biology, Inc.

Optical emission spectroscopy during fabrication of indium-tin-oxynitride films by RF-sputtering

International Nuclear Information System (INIS)

Koufaki, M.; Sifakis, M.; Iliopoulos, E.; Pelekanos, N.; Modreanu, M.; Cimalla, V.; Ecke, G.; Aperathitis, E.

2006-01-01

Indium-tin-oxide (ITO) and indium-tin-oxynitride (ITON) films have been deposited on glass by rf-sputtering from an ITO target, using Ar plasma and N 2 plasma, respectively, and different rf-power. Optical emission spectroscopy (OES) was employed to identify the species present in the plasma and to correlate them with the properties of the ITO and ITON thin films. Emission lines of ionic In could only be detected in N 2 plasma, whereas in the Ar plasma additional lines corresponding to atomic In and InO, were detected. The deposition rate of thin films was correlated with the In species, rather than the nitrogen species, emission intensity in the plasma. The higher resistivity and lower carrier concentration of the ITON films, as compared to the respective properties of the ITO films, were attributed to the incorporation of nitrogen, instead of oxygen, in the ITON structure

How mechanical behavior of glassy polymers enables us to characterize melt deformation: elastic yielding in glassy state after melt stretching?

Science.gov (United States)

Wang, Shi-Qing; Zhao, Zhichen; Tsige, Mesfin; Zheng, Yexin

Fast melt deformation well above the glass transition temperature Tg is known to produce elastic stress in an entangled polymer due to the chain entropy loss at the length scale of the network mesh size. Here chains of high molecular weight are assumed to form an entanglement network so that such a polymer behaves transiently like vulcanized rubber capable of affine deformation. We consider quenching a melt-deformed glassy polymer to well below Tg to preserve the elastic stress. Upon heating such a sample to Tg, the sample can return to the shape it took before melt deformation. This is the basic principle behind the design of all polymer-based shape-memory materials. This work presents intriguing evidence based on both experiment and computer simulation that the chain network, deformed well above Tg, can drive the glassy polymer to undergo elastic yielding. Our experimental systems include polystyrene, poly(methyl methacrylate) and polycarbonate; the molecular dynamics simulation is based on Kremer-Grest bead-spring model. National Science Foundation (DMR-1444859 and DMR-1609977).

SUPERNOVA SHOCK-WAVE-INDUCED CO-FORMATION OF GLASSY CARBON AND NANODIAMOND

International Nuclear Information System (INIS)

Stroud, Rhonda M.; Chisholm, Matthew F.; Heck, Philipp R.; Alexander, Conel M. O'D.; Nittler, Larry R.

2011-01-01

Nanodiamond (ND) was the first extrasolar dust phase to be identified in meteorites. However, the 2 nm average size of the NDs precludes isotopic analysis of individual particles, and thus their origin(s) remains controversial. Using electron microscopy with subnanometer resolution, we show that ND separates from the Allende and Murchison meteorites are actually a two-phase mixture of ND and glassy carbon. This phase mixture is likely the product of supernova shock-wave transformation of pre-formed organics in the interstellar medium (ISM). The glassy carbon-ND mixture is also a plausible contributor to the 2175 A extinction feature in the diffuse ISM.

A novel electrochemical sensor of bisphenol A based on stacked graphene nanofibers/gold nanoparticles composite modified glassy carbon electrode

International Nuclear Information System (INIS)

Niu, Xiuli; Yang, Wu; Wang, Guoying; Ren, Jie; Guo, Hao; Gao, Jinzhang

2013-01-01

In this paper, a novel and convenient electrochemical sensor based on stacked graphene nanofibers (SGNF) and gold nanoparticles (AuNPs) composite modified glassy carbon electrode (GCE) was developed for the determination of bisphenol A (BPA). The AuNPs/SGNF modified electrode showed an efficient electrocatalytic role for the oxidation of BPA, and the oxidation overpotentials of BPA were decreased significantly and the peak current increased greatly compared with bare GCE and other modified electrode. The transfer electron number (n) and the charge transfer coefficient (α) were calculated with the result as n = 4, α = 0.52 for BPA, which indicated the electrochemical oxidation of BPA on AuNPs/SGNF modified electrode was a four-electron and four-proton process. The effective surface areas of AuNPs/SGNF/GCE increased for about 1.7-fold larger than that of the bare GCE. In addition, the kinetic parameters of the modified electrode were calculated and the apparent heterogeneous electron transfer rate constant (k s ) was 0.51 s −1 . Linear sweep voltammetry was applied as a sensitive analytical method for the determination of BPA and a good linear relationship between the peak current and BPA concentration was obtained in the range from 0.08 to 250 μM with a detection limit of 3.5 × 10 −8 M. The modified electrode exhibited a high sensitivity, long-term stability and remarkable reproducible analytical performance and was successfully applied for the determination of BPA in baby bottles with satisfying results

Identifying glass compositions in fly ash

Directory of Open Access Journals (Sweden)

Katherine eAughenbaugh

2016-01-01

Full Text Available In this study, four Class F fly ashes were studied with a scanning electron microscope; the glassy phases were identified and their compositions quantified using point compositional analysis with k-means clustering and multispectral image analysis. The results showed that while the bulk oxide contents of the fly ashes were different, the four fly ashes had somewhat similar glassy phase compositions. Aluminosilicate glasses (AS, calcium aluminosilicate glasses (CAS, a mixed glass, and, in one case, a high iron glass were identified in the fly ashes. Quartz and iron crystalline phases were identified in each fly ash as well. The compositions of the three main glasses identified, AS, CAS, and mixed glass, were relatively similar in each ash. The amounts of each glass were varied by fly ash, with the highest calcium fly ash containing the most of calcium-containing glass. Some of the glasses were identified as intermixed in individual particles, particularly the calcium-containing glasses. Finally, the smallest particles in the fly ashes, with the most surface area available to react in alkaline solution, such as when mixed with portland cement or in alkali-activated fly ash, were not different in composition than the large particles, with each of the glasses represented. The method used in the study may be applied to a fly ash of interest for use as a cementing material in order to understand its potential for reactivity.

Mechanical properties of Fe-Ni-Cr-Si-B bulk glassy alloy

International Nuclear Information System (INIS)

Lee, Kee Ahn; Kim, Yong Chan; Kim, Jung Han; Lee, Chong Soo; Namkung, Jung; Kim, Moon Chul

2007-01-01

The mechanical properties and crystallization behavior of new Fe-Ni-Cr-Si-B-based bulk glassy alloys were investigated. The suitability of the continuous roll casting method for the production of bulk metallic glass (BMG) sheets in such alloy systems was also examined. BMG samples (Fe-Ni-Cr-Si-B, Fe-Ni-Zr-Cr-Si-B, Fe-Ni-Zr-Cr-W-Si-B) in amorphous strip, cylindrical, and sheet forms were prepared through melt spinning, copper mold casting, and twin roll strip casting, respectively. Fe-Ni-Cr-Si-B alloy exhibited compressive strength of up to 2.93 GPa and plastic strain of about 1.51%. On the other hand, the Fe-Ni-Zr-Cr-Si-B, composite-type bulk sample with diameter of 2.0 mm showed remarkable compressive plastic strain of about 4.03%. The addition of zirconium was found to enhance the homogeneous precipitation of nanocrystalline less than 7 nm and to develop a hybrid-composite microstructure with increasing sample thickness. Twin roll strip casting was successfully applied to the fabrication of sheets in Fe-Ni-Cr-Si-B-based BMGs. The combined characteristics of high mechanical properties and ease of microstructure control proved to be promising in terms of the future progress of structural bulk amorphous alloys

Mechanical properties of Fe-Ni-Cr-Si-B bulk glassy alloy

Energy Technology Data Exchange (ETDEWEB)

Lee, Kee Ahn [School of Advanced Materials Engineering, Andong National University, Andong 760-749 (Korea, Republic of)]. E-mail: keeahn@andong.ac.kr; Kim, Yong Chan [New Metals Research Team, RIST, Pohang 790-330 (Korea, Republic of); Kim, Jung Han [Center for Advanced Aerospace materials, POSTECH, Pohang 790-784 (Korea, Republic of); Lee, Chong Soo [Center for Advanced Aerospace materials, POSTECH, Pohang 790-784 (Korea, Republic of); Namkung, Jung [New Metals Research Team, RIST, Pohang 790-330 (Korea, Republic of); Kim, Moon Chul [New Metals Research Team, RIST, Pohang 790-330 (Korea, Republic of)

2007-03-25

The mechanical properties and crystallization behavior of new Fe-Ni-Cr-Si-B-based bulk glassy alloys were investigated. The suitability of the continuous roll casting method for the production of bulk metallic glass (BMG) sheets in such alloy systems was also examined. BMG samples (Fe-Ni-Cr-Si-B, Fe-Ni-Zr-Cr-Si-B, Fe-Ni-Zr-Cr-W-Si-B) in amorphous strip, cylindrical, and sheet forms were prepared through melt spinning, copper mold casting, and twin roll strip casting, respectively. Fe-Ni-Cr-Si-B alloy exhibited compressive strength of up to 2.93 GPa and plastic strain of about 1.51%. On the other hand, the Fe-Ni-Zr-Cr-Si-B, composite-type bulk sample with diameter of 2.0 mm showed remarkable compressive plastic strain of about 4.03%. The addition of zirconium was found to enhance the homogeneous precipitation of nanocrystalline less than 7 nm and to develop a hybrid-composite microstructure with increasing sample thickness. Twin roll strip casting was successfully applied to the fabrication of sheets in Fe-Ni-Cr-Si-B-based BMGs. The combined characteristics of high mechanical properties and ease of microstructure control proved to be promising in terms of the future progress of structural bulk amorphous alloys.

Irradiation-induced defects in graphite and glassy carbon studied by positron annihilation

International Nuclear Information System (INIS)

Hasegawa, M.; Kajino, M.; Kuwahara, H.; Yamaguchi, S.; Kuramoto, E.; Takenaka, M.

1992-01-01

ACAR and positron lifetime measurements have been made on, HOPG, isotropic fine-grained graphites, glassy carbons and C 60 /C 70 . HOPG showed a marked bimodal ACAR distribution along the c-axis. By irradiation of 1.0 X 10 19 fast neutrons/cm 2 remarkable narrowing in the ACAR curves and disappearance of the bimodal distribution were observed. Lifetime in HOPG increased from 225 psec to 289 psec (positron-lifetime in vacancies and their small clusters) by the irradiation. The irradiation on isotropic graphites and glassy carbons, however, gave slight narrowing in ACAR curves and decrease in lifetimes (360 psec → 300psec). This suggests irradiation-induced vacancy trapping in crystallites. In C 60 /C 70 powder two lifetime components were detected: τ 1 =177psec, τ 2 =403psec (I 2 =58%). The former is less than the bulk lifetime of HOPG, while the latter being very close to lifetimes in the isotropic graphites and glassy carbons. This and recent 2D-ACAR study of HOPG surface [15] strongly suggest free and defect surface states around ''soccer ball'' cages

Electrochemical pre anodization of glassy carbon electrode and application to determine chloramphenicol

International Nuclear Information System (INIS)

Truc, Nguyen Minh; Mortensen, John; Anh, Nguyen Ba Hoai

2008-01-01

This paper suggested a method to enhance the performance of carbon electrodes for the determination of chloramphenicol (CAP). The sensitivity and the reproducibility of the carbon electrodes could be enhanced easily by electrochemical pretreatment. Some kinds of carbon material were studied including glassy carbon, graphite carbon and pyrolytic carbon. Numerous kinds of supporting electrolyte have been tried. For glassy carbon electrode, the acidic solution, H 2 SO 4 5 mM, resulted in best performance at pretreated voltage of +2.1V (vs. Ag/ AgCl) in duration of 250 second. However, for graphite and pyrolytic carbon electrodes, the phosphate buffer solution pH 6.0 gave the best performance at +1.7V (vs. Ag/ AgCl) in duration of 20 seconds. The detection limit could be at very low concentration of CAP: 0.8 ng/ ml for glassy carbon electrode, 3.5 ng/ ml for graphite carbon electrode. The method was successful applied to aqua-agriculture water sample and milk sample with simple extraction as well as direct ointment sample analysis. (author)

Permeation of Mixed Penetrants through Glassy Polymer Membranes.

Science.gov (United States)

1985-03-15

and LOPE. Also, ESCA was used in conjunction with plasma etching to determine the effects of the gas phase fluorine concentration and fluorination...at 35 3C. ARD-AISS5 65 PERMEATION OF MIXED PENETRANTS THROUGH GLASSY POLYMER 213 MENBRANES (U) NORTH CAROLINA STATE UNIV AT RALEIGH R T CHERN ET AL. 15

Mechanical Behaviour of Glassy Composite Seals for IT-SOFC Application

DEFF Research Database (Denmark)

Nielsen, Karsten Agersted; Solvang, Mette; Nielsen, Sofie Birkedal Lund

2007-01-01

Glass-based sealants have been developed with emphasis on filler material and surface treatment of the sealing components in order to optimise their mechanical and functional behaviour during the initial sealing process as well as during thermal cycling of the SOFC-stack after exposure to operating...... conditions. The bonding strength and microstructure of the interfaces between composite seals and interconnect materials were investigated as a function of surface treatment of the sealing surfaces, glass matrix composition, sealing pressure and temperature. The initial sealing performance and resistance...... to thermal cycling were then investigated on selected combinations of materials after ageing. Strongest bonding between sodium aluminosilicate glass composite and steel surfaces was obtained for sealing at 850°C. For the strongest interface, having shear strength of 2.35 MPa, rupture occurred in the glass...

Effects of nymphal diet and adult feeding on allocation of resources to glassy-winged sharpshooter egg production

Science.gov (United States)

The glassy-winged sharpshooter is an invasive insect capable of transmitting the bacterial pathogen Xylella fastidiosa. Pre-oviposition periods of laboratory reared glassy-winged sharpshooters are variable. Here, two questions were addressed: does nymphal diet affect pre-oviposition period and how d...

Formation of glassy carbon structure and its change under neutron irradiation

Energy Technology Data Exchange (ETDEWEB)

Kurolenkin, E.I.; Lopato, Yu.S.; Virgil' ev, Yu.S.; Khakimova, D.K.; Aksenov, S.I.

1981-01-01

The changes of glassy carbon structure, which is prepared of phenol-formaldehyde and furfurol-phenol-formaldehyde resins in the process of irradiation with 5.3x10/sup 20/ cm/sup -2/ neutron fluence with the energy E>0.18 MeV in the temperature range of 90-540 deg C are studied. It is established the irradiation results in the shrinkage of the samples. The compression of the samples increases with the irradiation temperature and neutron fluence. The thermal annealing does not result in the restoration of the volume of samples. The sample shrinkage, caused by more compact package of globular structures and the destruction of film structures, decrease gas permeability of glassy carbon.

Stressing effects on the charge trapping of silicon oxynitride prepared by thermal oxidation of LPCVD Si-rich silicon nitride

International Nuclear Information System (INIS)

Choi, H.Y.; Wong, H.; Filip, V.; Sen, B.; Kok, C.W.; Chan, M.; Poon, M.C.

2006-01-01

It was recently found that the silicon oxynitride prepared by oxidation of silicon-rich silicon nitride (SRN) has several important features. The high nitrogen and extremely low hydrogen content of this material allows it to have a high dielectric constant and a low trap density. The present work investigates in further detail the electrical reliability of this kind of gate dielectric films by studying the charge trapping and interface state generation induced by constant current stressing. Capacitance-voltage (C-V) measurements indicate that for oxidation temperatures of 850 and 950 deg. C, the interface trap generation is minimal because of the high nitrogen content at the interface. At a higher oxidation temperature of 1050 deg. C, a large flatband shift is found for constant current stressing. This observation can be explained by the significant reduction of the nitrogen content and the phase separation effect at this temperature as found by X-ray photoelectron spectroscopy study. In addition to the high nitrogen content, the Si atoms at the interface exist in the form of random bonding to oxygen and nitrogen atoms for samples oxidized at 850 and 950 deg. C. This structure reduces the interface bonding constraint and results in the low interface trap density. For heavily oxidized samples the trace amount of interface nitrogen atoms exist in the form of a highly constraint SiN 4 phase and the interface oxynitride layer is a random mixture of SiO 4 and SiN 4 phases, which consequently reduces the reliability against high energy electron stressing

Voltammetric Determination of Codeine on Glassy Carbon Electrode Modified with Nafion/MWCNTs

Directory of Open Access Journals (Sweden)

Robert Piech

2015-01-01

Full Text Available A glassy carbon electrode modified with a Nafion/MWCNTs composite is shown to enable the determination of codeine using differential pulse voltammetry in phosphate buffer of pH 3.0. At a preconcentration time of 15 s, the calibration graph is linear in the 0.5 µM (0.15 mg·L−1 to 15 µM (4.5 mg·L−1 concentration range with a correlation coefficient of 0.998. The detection limit at a preconcentration time of 120 s is as low as 4.5 μg·L−1. The repeatability of the method at a 0.6 μg·L−1 concentration level, expressed as the RSD, is 3.7% (for n=5. The method was successfully applied and validated by analyzing codeine in drug, human plasma, and urine samples.

Room temperature ferromagnetism and CH{sub 4} gas sensing of titanium oxynitride induced by milling and annealing

Energy Technology Data Exchange (ETDEWEB)

Bolokang, Amogelang S., E-mail: Sylvester.Bolokang@transnet.net [DST/CSIR National Centre for Nano-Structured Materials, Council for Scientific and Industrial Research, Pretoria, 0001 (South Africa); Transnet Engineering, Product Development, Private Bag X 528, Kilnerpark, 0127 (South Africa); Tshabalala, Zamaswazi P. [DST/CSIR National Centre for Nano-Structured Materials, Council for Scientific and Industrial Research, Pretoria, 0001 (South Africa); Malgas, Gerald F. [Department of Physics, University of the Western Cape, Private Bag X17, Bellville, 7535 (South Africa); Kortidis, Ioannis [DST/CSIR National Centre for Nano-Structured Materials, Council for Scientific and Industrial Research, Pretoria, 0001 (South Africa); West Virginia University, Department of Mechanical & Aerospace Engineering, Evansdale Campus, Morgantown, WV, 26506 (United States); Swart, Hendrik C. [Department of Physics, University of the Free State, P.O. Box 339, Bloemfontein, ZA9300 (South Africa); Motaung, David E., E-mail: dmotaung@csir.co.za [DST/CSIR National Centre for Nano-Structured Materials, Council for Scientific and Industrial Research, Pretoria, 0001 (South Africa)

2017-06-01

We report on the room temperature ferromagnetism and CH{sub 4} gas sensing of titanium oxynitride prepared by milling and annealing at 1100 °C in a nitrogen gas environment. Structural analyses revealed a metastable orthorhombic TiO{sub 2} phase after milling for 120 h. The 120 h milled TiO{sub 2} particles and subsequently annealed in nitrogen gas at 1100 °C showed the formation of titanium oxynitride (TiO{sub x}N{sub y}) with a tetragonal crystal structure. An FCC metastable TiO{sub x}N{sub y} phase was also observed with a lattice parameter a = 4.235 Å. The vibrating sample magnetometer and electron paramagnetic analyses showed that the milled and TiO{sub x}N{sub y} samples possess room temperature ferromagnetism. Gas sensing measurements were carried out toward CH{sub 4} and H{sub 2} gases. The TiO{sub x}N{sub y} nanostructures demonstrated higher sensing response and selectivity to CH{sub 4} gas at room temperature. The enhanced response of 1010 and sensitivity of 50.12 ppm{sup -1} at a concentration of 20 ppm CH{sub 4} are associated with higher surface area, pore diameter and surface defects such as oxygen vacancies and Ti{sup 3+}, as evidenced from the Brunauer–Emmet–Teller, photoluminescence, electron paramagnetic resonance and x-ray photoelectron analyses. - Highlights: • Ball milled of TiO{sub 2} structure revealed metastable orthorhombic phase. • Upon nitridation tetragonal and FCC TiO{sub x}N{sub y} crystal structures were induced. • The magnetic properties of TiO{sub 2} nanoparticles was transformed by milling. • TiO{sub x}N{sub y} sensing response for CH{sub 4} gas at room temperature was high.

Polyenergy ion beam synthesis of buried oxynitride layer in silicon

Energy Technology Data Exchange (ETDEWEB)

Barabanenkov, M.Yu. E-mail: barab@ipmt-hpm.ac.ru; Agafonov, Yu.A.; Mordkovich, V.N.; Pustovit, A.N.; Vyatkin, A.F.; Zinenko, V.I

2000-11-01

The efficiency of silicon oxynitride synthesis in silicon crystals implanted with substoichiometric doses of oxygen and nitrogen ions is investigated both experimentally and theoretically. Si crystals are implanted with oxygen and nitrogen ions with doses of 1.5 and 4.5x10{sup 17} cm{sup -2}, respectively, at fixed oxygen ion energy of 150 keV and nitrogen ion energies varied from 80 to 180 keV. The samples annealed at 1200 deg C for 2 h were analysed by secondary ion mass spectroscopy (SIMS). Theoretically, a `diffusion-alternative sinks' model is applied to the annealing stage of ion beam synthesis of a buried layer of a new phase in solids. It is shown that the maximum of the ternary phase production is attained when nitrogen ions are implanted deeper than oxygen ions. An explanation of this fact is given in terms of that (i) the segregation of oxygen and nitrogen species on the surface of oxide nuclei removes the kinetic restriction of nuclei growth, characteristic of oxide growth, at the expense of only oxygen atoms, and (ii) the higher the implantation energy the smoother the shape of ion range distribution in the target, which, in its turn, causes the predominance of the impurity sink over the impurity diffusion.

Polyenergy ion beam synthesis of buried oxynitride layer in silicon

International Nuclear Information System (INIS)

Barabanenkov, M.Yu.; Agafonov, Yu.A.; Mordkovich, V.N.; Pustovit, A.N.; Vyatkin, A.F.; Zinenko, V.I.

2000-01-01

The efficiency of silicon oxynitride synthesis in silicon crystals implanted with substoichiometric doses of oxygen and nitrogen ions is investigated both experimentally and theoretically. Si crystals are implanted with oxygen and nitrogen ions with doses of 1.5 and 4.5x10 17 cm -2 , respectively, at fixed oxygen ion energy of 150 keV and nitrogen ion energies varied from 80 to 180 keV. The samples annealed at 1200 deg C for 2 h were analysed by secondary ion mass spectroscopy (SIMS). Theoretically, a `diffusion-alternative sinks' model is applied to the annealing stage of ion beam synthesis of a buried layer of a new phase in solids. It is shown that the maximum of the ternary phase production is attained when nitrogen ions are implanted deeper than oxygen ions. An explanation of this fact is given in terms of that (i) the segregation of oxygen and nitrogen species on the surface of oxide nuclei removes the kinetic restriction of nuclei growth, characteristic of oxide growth, at the expense of only oxygen atoms, and (ii) the higher the implantation energy the smoother the shape of ion range distribution in the target, which, in its turn, causes the predominance of the impurity sink over the impurity diffusion

Charge trapping and carrier transport mechanism in silicon-rich silicon oxynitride

International Nuclear Information System (INIS)

Yu Zhenrui; Aceves, Mariano; Carrillo, Jesus; Lopez-Estopier, Rosa

2006-01-01

The charge-trapping and carrier transport properties of silicon-rich silicon oxynitride (SRO:N) were studied. The SRO:N films were deposited by low pressure chemical vapor deposition. Infrared (IR) and transmission electron microscopic (TEM) measurements were performed to characterize their structural properties. Capacitance versus voltage and current versus voltage measurements (I-V) were used to study the charge-trapping and carrier transport mechanism. IR and TEM measurements revealed the existence of Si nanodots in SRO:N films. I-V measurements revealed that there are two conduction regimes divided by a threshold voltage V T . When the applied voltage is smaller than V T , the current is dominated by the charge transfer between the SRO:N and substrate; and in this regime only dynamic charging/discharging of the SRO:N layer is observed. When the voltage is larger than V T , the current increases rapidly and is dominated by the Poole-Frenkel mechanism; and in this regime, large permanent trapped charge density is obtained. Nitrogen incorporation significantly reduced the silicon nanodots or defects near the SRO:N/Si interface. However, a significant increase of the density of silicon nanodot in the bulk of the SRO:N layer is obtained

Ice cloud processing of ultra-viscous/glassy aerosol particles leads to enhanced ice nucleation ability

Directory of Open Access Journals (Sweden)

R. Wagner

2012-09-01

Full Text Available The ice nucleation potential of airborne glassy aqueous aerosol particles has been investigated by controlled expansion cooling cycles in the AIDA aerosol and cloud chamber of the Karlsruhe Institute of Technology at temperatures between 247 and 216 K. Four different solutes were used as proxies for oxygenated organic matter found in the atmosphere: raffinose, 4-hydroxy-3-methoxy-DL-mandelic acid (HMMA, levoglucosan, and a multi-component mixture of raffinose with five dicarboxylic acids and ammonium sulphate. Similar to previous experiments with citric acid aerosols, all particles were found to nucleate ice heterogeneously before reaching the homogeneous freezing threshold provided that the freezing cycles were started well below the respective glass transition temperatures of the compounds; this is discussed in detail in a separate article. In this contribution, we identify a further mechanism by which glassy aerosols can promote ice nucleation below the homogeneous freezing limit. If the glassy aerosol particles are probed in freezing cycles started only a few degrees below their respective glass transition temperatures, they enter the liquid regime of the state diagram upon increasing relative humidity (moisture-induced glass-to-liquid transition before being able to act as heterogeneous ice nuclei. Ice formation then only occurs by homogeneous freezing at elevated supersaturation levels. When ice forms the remaining solution freeze concentrates and re-vitrifies. If these ice cloud processed glassy aerosol particles are then probed in a second freezing cycle at the same temperature, they catalyse ice formation at a supersaturation threshold between 5 and 30% with respect to ice. By analogy with the enhanced ice nucleation ability of insoluble ice nuclei like mineral dusts after they nucleate ice once, we refer to this phenomenon as pre-activation. We propose a number of possible explanations for why glassy aerosol particles that have re

Understanding the Composition Dependence of the Fragility of AgI-Ag2O-MxOy Glassy Systems

International Nuclear Information System (INIS)

Aniya, M

2011-01-01

It has been reported that the fragility in the AgI-Ag 2 O-M x O y (M = B, Ge, P, Mo) system is determined by Ag 2 O-M x O y and does not depend on the amount of AgI. This is an interesting result and provides a hint to understand the nature of the glassy state of these materials. However, the origin of such behavior has not been sufficiently discussed. In the present report a model for the above behavior is presented. According to the model, the behavior arises from the solid like nature of the network formed by Ag 2 O-M x O y and the liquid like AgI which flow between the networks. The model is consistent with the structural model of superionic glasses proposed previously.

Study and Electrochemical Determination of Tyrosine at Graphene Nanosheets Composite Film Modified Glassy Carbon Electrode

Directory of Open Access Journals (Sweden)

M. Behpour

2013-06-01

Full Text Available A graphene nanosheets (GNS film coated glassy carbon electrode (GCE was fabricated for sensitive determination of tyrosine (Tyr. The GNS-based sensor was characterized by scanning electron microscope and electrochemical impedance spectroscopy. The voltammetric techniques were employed to study electro-oxidation of Tyr. The results revealed that the modified electrode showed an electrocatalytic activity toward the anodic oxidation of Tyr by a marked enhancement in the current intensity and the shift in the oxidation potential to lower values (50 mV in comparison with the bare GCE. Some kinetic parameters such as the electron transfer coefficient (α were also determined for the Tyr oxidation. The detection limit  for Tyr was found to be 2.0×10-8 M (n=9, and the peak current increases linearly with the Tyr concentration within the molar concentration ranges of 5.0 ×10-6 to 1.2 ×10-4 M. The modified electrode shows good sensitivity, selectivity and stability. The prepared electrode was applied for the determination of Tyr in real sample.

Glassy slags as novel waste forms for remediating mixed wastes with high metal contents

International Nuclear Information System (INIS)

Feng, X.; Wronkiewicz, D.J.; Bates, J.K.; Brown, N.R.; Buck, E.C.; Gong, M.; Ebert, W.L.

1994-01-01

Argonne National Laboratory (ANL) is developing a glassy slag final waste form for the remediation of low-level radioactive and mixed wastes with high metal contents. This waste form is composed of various crystalline and metal oxide phases embedded in a silicate glass phase. This work indicates that glassy slag shows promise as final waste form because (1) it has similar or better chemical durability than high-level nuclear waste (HLW) glasses, (2) it can incorporate large amounts of metal wastes, (3) it can incorporate waste streams having low contents of flux components (boron and alkalis), (4) it has less stringent processing requirements (e.g., viscosity and electric conductivity) than glass waste forms, (5) its production can require little or no purchased additives, which can result in greater reduction in waste volume and overall treatment costs. By using glassy slag waste forms, minimum additive waste stabilization approach can be applied to a much wider range of waste streams than those amenable only to glass waste forms

Phase separation and structure formation in gadolinium based liquid and glassy metallic alloys

International Nuclear Information System (INIS)

Han, Junhee

2014-01-01

tailored both at microscopic and macroscopic length scales. This includes either droplet-like or interconnected microstructures at the microscopic level and glass-glass or glass-crystalline composites at the macroscopic level. Essential parameter for the quenched in microstructure is the temperature dependence of liquid-liquid phase separation, which is determined by the chemical composition of the alloy: on the one hand, earlier and/or later stages of spinodal decomposition or almost homogeneous glassy states are obtained if the critical temperature of miscibility gap T c is close to the glass transition temperature T g ; and on the one hand, coarsening and secondary precipitations of the liquids are obtained if T c is much higher than T g . Finally, the influence of the microstructure developed by phase separation on their magnetic properties had been investigated. The saturation magnetization σ S depends on the overall amount of Gd atoms in the alloys and is not remarkably affected by phase separation processes. The Curie temperature T Curie of the magnetic transition is influenced by the changed chemical composition of the Gd-rich glassy phases compared to that of monolithic Gd-Co-Al glasses.

Die-cast heterophase composites with AlSi13Mg1CuNi matrix

Directory of Open Access Journals (Sweden)

M. Dyzia

2010-01-01

Full Text Available On the basis of the performed tests, an advantageous interaction of glassy carbon particles in a couple consisting of a heterophase composite and a spheroidal cast iron has been corroborated. It was found that, the presence of glassy carbon in the heterophase composite (SiC+C affects the stabilization of the friction coefficient value as a function of the friction distance and reduces the intensity of the wearing-in stage of the interacting surfaces. Both a decrease of the friction coefficient and the wear of the heterophase composites may be connected with the carbon particles' chipping effect and the deposition of its fragments on the surface of the interacting components of the friction couple, which forms a kind of a solid lubricating agent in the system. This should allow applying of this material to the composite piston - cylinder sleeve system in piston air-compressors. Further works will concern the selection of the matrix alloy composition with the purpose of reducing the phenomenon of particles chipping during machining. It seems that one of the possibilities is the application of a more plastic matrix and optimizing the fraction of reinforcing phases and their gradient distribution in the casting.

Local structure, composition, and crystallization mechanism of a model two-phase “composite nanoglass”

Energy Technology Data Exchange (ETDEWEB)

Chattopadhyay, Soma; Shibata, Tomohiro [CSRRI-IIT, MRCAT, Sector 10, Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Kelly, S. D. [EXAFS Analysis, Bolingbrook, Illinois 60440 (United States); Balasubramanian, M. [Sector 20 XOR, Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Srinivasan, S. G.; Du, Jincheng; Banerjee, Rajarshi [Department of Materials Science and Engineering, University of North Texas, Denton, Texas 76203-5017 (United States); Ayyub, Pushan, E-mail: pushan@tifr.res.in [Department of Condensed Matter Physics and Materials Science, Tata Institute of Fundamental Research, Mumbai 400005 (India)

2016-02-14

We report a detailed study of the local composition and structure of a model, bi-phasic nanoglass with nominal stoichiometry Cu{sub 55}Nb{sub 45}. Three dimensional atom probe data suggest a nanoscale-phase-separated glassy structure having well defined Cu-rich and Nb-rich regions with a characteristic length scale of ≈3 nm. However, extended x-ray absorption fine structure analysis indicates subtle differences in the local environments of Cu and Nb. While the Cu atoms displayed a strong tendency to cluster and negligible structural order beyond the first coordination shell, the Nb atoms had a larger fraction of unlike neighbors (higher chemical order) and a distinctly better-ordered structural environment (higher topological order). This provides the first experimental indication that metallic glass formation may occur due to frustration arising from the competition between chemical ordering and clustering. These observations are complemented by classical as well as ab initio molecular dynamics simulations. Our study indicates that these nanoscale phase-separated glasses are quite distinct from the single phase nanoglasses (studied by Gleiter and others) in the following three respects: (i) they contain at least two structurally and compositionally distinct, nanodispersed, glassy phases, (ii) these phases are separated by comparatively sharp inter-phase boundaries, and (iii) thermally induced crystallization occurs via a complex, multi-step mechanism. Such materials, therefore, appear to constitute a new class of disordered systems that may be called a composite nanoglass.

Dielectric relaxation and AC conductivity studies of Se90Cd10−xInx glassy alloys

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Nitesh Shukla

2016-06-01

Full Text Available Chalcogenide glassy alloys of Se90Cd10−xInx (x = 2, 4, 6, 8 are synthesized by melt quench technique. The prepared glassy alloys have been characterized by techniques such as differential scanning calorimetry (DSC, scanning electron microscopy (SEM and energy dispersive X-ray (EDAX. Dielectric properties of Se90Cd10−xInx (x = 2, 4, 6, 8 chalcogenide glassy system have been studied using impedance spectroscopic technique in the frequency range 42 Hz to 5 MHz at room temperature. It is found that the dielectric constants ɛ′, dielectric loss factor ɛ″ and loss angle Tan δ depend on frequency. ɛ′, ɛ″ and loss angle Tan δ are found to be decreasing with the In content in Se90Cd10−xInx glassy system. AC conductivity of the prepared sample has also been studied. It is found that AC conductivity increases with frequency where as it has decreasing trend with increasing In content in Se–Cd matrix. The semicircles observed in the Cole–Cole plots indicate a single relaxation process.

Effect of glassy carbon properties on the electrochemical deposition of platinum nano-catalyst and its activity for methanol oxidation

Directory of Open Access Journals (Sweden)

SANJA TERZIC

2007-02-01

Full Text Available The effects of the properties of glassy carbon on the deposition of platinum particles and the electrocatalytic activity of platinum supported on glassy carbon (GC/Pt for methanol oxidation in alkaline and acidic solutions were studied. Platinum was potentiostatically deposited on two glassy carbon samples, thermally treated at different temperatures, which were either polished or anodicaly polarised in acid (GCOX-AC/Pt and in alkali (GCOX-AL/Pt. Anodic polarisation of glassy carbon, either in alkaline or acidic solution, enhances the activity of both types of GC/Pt electrodes for methanol oxidation. The activity of the catalysts follows the change in the properties of the glassy carbon support upon anodic treatment. The specific activity of the GCOX-AL/Pt electrode for this reaction in alkali is increased only a few times in comparison with the activity of the GC/Pt one. On the other hand, the specific activity of the GCOX-AC/Pt electrode for methanol oxidation in acid is about one order of magnitude higher than that of the GC/Pt electrode. The role of the substrate on the properties of catalyst is discussed in detail.

Connection between NMR and electrical conductivity in glassy chalcogenide fast ionic conductors

International Nuclear Information System (INIS)

Kim, K.H.

1995-01-01

The work documented in this thesis follows the traditional order. In this chapter a general discussion of ionic conduction and of glassy materials are followed by a brief outline of the experimental techniques for the investigation of fast ionic conduction in glassy materials, including NMR and impedance spectroscopy techniques. A summary of the previous and present studies is presented in the last section of this introductory chapter. The details of the background theory and models are found in the Chapter II, followed by the description of the experimental details in Chapter III. Chapter IV of the thesis describes the experimental results and the analysis of the experimental observations followed by the conclusions in chapter V

Orbital physics in sulfur spinels: ordered, liquid and glassy ground states

International Nuclear Information System (INIS)

Buettgen, N; Hemberger, J; Fritsch, V; Krimmel, A; Muecksch, M; Nidda, H-A Krug von; Lunkenheimer, P; Fichtl, R; Tsurkan, V; Loidl, A

2004-01-01

Measurements of magnetization M(T, H), heat capacity C(T), NMR lineshift K(T) and linewidth Δ(T), neutron scattering S(Q, ω, T) and broadband dielectric spectroscopy ε(ω, T) provide experimental evidence of the different orbital ground states in the cubic sulfur spinels under investigation. In all compounds, the tetrahedrally coordinated Jahn-Teller ions Fe 2+ are characterized by a degeneracy of the orbital degrees of freedom. Particularly, we found a long-range orbital ordering in polycrystalline (PC) FeCr 2 S 4 , and a glassy freezing of the orbital degrees of freedom in FeCr 2 S 4 (single crystals) (SCs). In contrast, FeSc 2 S 4 belongs to the rare class of spin-orbital liquids, where quantum fluctuations accompanying the glassy freezing of the orbitals suppress long-range magnetic order

Glassy behavior in the layered perovskites La2−xSrxCoO4(1.1≤x≤1.3)

International Nuclear Information System (INIS)

Mukherjee, S.; Mukherjee, Rajarshi; Banerjee, S.; Ranganathan, R.; Kumar, Uday

2012-01-01

The glassy behavior of the phase segregated state in the layered cobaltite La 2−x Sr x CoO 4 has been studied. The role of the inter-cluster interactions as well as the disordered spins at the paramagnetic–ferromagnetic interface, behind the observed glassy behavior have been investigated. The disordered spins at the interface appear to be strongly pinned, and they contribute little to the observed glassy behavior. On the other hand, the inter-cluster interactions play the key role. Both the Co 4+ and Co 3+ ions are in the intermediate spin state. - Highlights: ► Phase segregated state of cobaltite La 2−x Sr x CoO 4 for (1.1≤x≤1.3) to find the origin of the observed glassy behavior. ► Result of the frequency dependent ac susceptibility measurement excludes the possibility of any spin glass phase, hints strong inter-cluster interactions. ► Relaxation experiments confirm the system to be a collection of clusters with two preferred sizes. ► The glassy behavior originates from strong inter-cluster interactions.

Glassy slag from rotary hearth vitrification

International Nuclear Information System (INIS)

Eschenbach, R.C.; Simpson, M.D.; Paulson, W.S.; Whitworth, C.G.

1995-01-01

Use of a Plasma Arc Centrifugal Treatment (PACT) system for treating mixed wastes containing significant quantities of soil results in formation of a glassy slag which melts at significantly higher temperatures than the borosilicate glasses. The slag typically contains mostly crystalline material, frequently in an amorphous matrix, thus the appellation open-quotes glassy slag.close quotes Details of the PACT process are given. The process will be used for treating buried wastes from Pit 9 at the Idaho National Engineering Laboratory and low-level mixed wastes from nuclear power plants in Switzerland. Properties of the slag after cooling to room temperature are reported, in particular the Product Consistency Test, for a number of different feedstocks. In almost all cases, the results compare favorably with conventional borosilicate glasses. In the PACT system, a transferred arc carries current from the plasma torch to a rotating molten bed of slag, which is the material being heated. Thus this transferred arc adds energy where it is needed - at and near the surface of the molten bath. Material is fed into the furnace through a sealed feeder, and falls into a rotating tub which is heated by the arc. Any organic material is quickly vaporized into the space above the slag bed and burned by the oxygen in the furnace. Metal oxides in the charge are melted into the slag. Metal in the feed tends to melt and collect as a separate phase underneath the slag, but can be oxidized if desired. When oxidized, it unites with other constituents forming a homogeneous slag

Generation of fine hydromagmatic ash by growth and disintegration of glassy rinds

Science.gov (United States)

Mastin, L.G.

2007-01-01

The deposits of mafic hydromagmatic eruptions are more fine grained and variable in vesicularity than dry magmatic deposits. Blocky, equant shapes of many hydromagmatic clasts also contrast with droplet, thread, and bubble wall morphology of dry magmatic fragments. Small (disintegration of glassy rinds on pyroclast surfaces as they deform within turbulent flows. This process, termed "turbulent shedding", may occur during the expansion phase of vapor explosions or during turbulent but nonexplosive mixing of magma with water, steam, or water sprays. The occurrence of turbulent shedding and the resulting fragment sizes depend on the timescale for rind growth and the timescale between disturbances that remove or disintegrate glassy rinds. Turbulent shedding is directly observable in some small littoral jets at Kilauea. Calculations suggest that, in the presence of liquid water or water sprays, glassy rinds having a thickness of microns to millimeters should form in milliseconds to seconds. This is similar to the timescale between turbulent velocity fluctuations that can shred lava globules and remove such rinds. The fraction of a deposit consisting of fine ash should increase with the duration of this process: Large-scale Surtseyan jets generate hundreds or thousands of shedding events; bubble bursts or tephra jets at Kilauea's coast may produce only a few.

Protection of nuclear graphite toward fluoride molten salt by glassy carbon deposit

International Nuclear Information System (INIS)

Bernardet, V.; Gomes, S.; Delpeux, S.; Dubois, M.; Guerin, K.; Avignant, D.; Renaudin, G.; Duclaux, L.

2009-01-01

Molten salt reactor represents one of the promising future Generation IV nuclear reactors families where the fuel, a liquid molten fluoride salt, is circulating through the graphite reactor core. The interactions between nuclear graphite and fluoride molten salt and also the graphite surface protection were investigated in this paper by powder X-ray diffraction, micro-Raman spectroscopy and scanning electron microscopy coupled with X-ray microanalysis. Nuclear graphite discs were covered by two kinds of protection deposit: a glassy carbon coating and a double coating of pyrolitic carbon/glassy carbon. Different behaviours have been highlighted according to the presence and the nature of the coated protection film. Intercalation of molten salt between the graphite layers did not occur. Nevertheless the molten salt adhered more or less to the surface of the graphite disc, filled more or less the graphite surface porosity and perturbed more or less the graphite stacking order at the disc surface. The behaviour of unprotected graphite was far to be satisfactory after two days of immersion of graphite in molten salt at 500 deg. C. The best protection of the graphite disc surface, with the maximum of inertness towards molten salt, has been obtained with the double coating of pyrolitic carbon/glassy carbon

Electrocatalytic Determination of Isoniazid by a Glassy Carbon Electrode Modified with Poly (Eriochrome Black T)

OpenAIRE

Karim Asadpour-Zeynali; Venus Baghalabadi

2017-01-01

In this work poly eriochrome black T (EBT) was electrochemically synthesized on the glassy carbon electrode as electrode modifier. On the modified electrode, voltammetric behavior of isoniazid (INH) was investigated. The poly (EBT)-modified glassy carbon electrode has excellent electrocatalytic ability for the electrooxidation of isoniazid. This fact was appeared as a reduced overpotential of INH oxidation in a wide operational pH range from 2 to 13. It has been found that the catalytic peak ...

Electrochemical Determination of Caffeine Content in Ethiopian Coffee Samples Using Lignin Modified Glassy Carbon Electrode

OpenAIRE

Amare, Meareg; Aklog, Senait

2017-01-01

Lignin film was deposited at the surface of glassy carbon electrode potentiostatically. In contrast to the unmodified glassy carbon electrode, an oxidative peak with an improved current and overpotential for caffeine at modified electrode showed catalytic activity of the modifier towards oxidation of caffeine. Linear dependence of peak current on caffeine concentration in the range 6 ? 10?6 to 100 ? 10?6?mol?L?1 with determination coefficient and method detection limit (LoD = 3?s/slope) of 0....

Sensitive stripping voltammetric determination of Cd(II) and Pb(II) by a Bi/multi-walled carbon nanotube-emeraldine base polyaniline-Nafion composite modified glassy carbon electrode

International Nuclear Information System (INIS)

Zhao, Guo; Yin, Yuan; Wang, Hui; Liu, Gang; Wang, Zhiqiang

2016-01-01

Highlights: • A MWCNT-EBP-NA composite film modified GCE was fabricated and characterized. • The GCE modified with the MWCNT-EBP-NA composite film exhibited excellent performance in the analysis of Cd(II) and Pb(II) by SWASV. • The Cd(II) and Pb(II) detection limits of the developed electrode were approximately 0.06 μg/L and 0.08 μg/L, respectively. • Bi/MWCNT-EBP-NA/GCE was successfully used to determine metal ions in soil samples. - Abstract: In this study, a multi-walled carbon nanotube (MWCNT)-emeraldine base polyaniline (EBP)-Nafion (NA) composite modified glassy carbon electrode (MWCNT-EBP-NA/GCE) was prepared and used for the sensitive detection of trace Pb(II) and Cd(II), with a detection limit of 0.06 μg/L for Cd(II) and 0.08 μg/L for Pb(II) (S/N = 3), by square wave anodic stripping voltammetry (SWASV). A bismuth film was prepared through the in situ plating of bismuth on the MWCNT-EBP-NA/GCE. The morphologies and electrochemical properties of the modified electrode were characterized by SWASV, scanning electron microscopy (SEM), electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). The parameters affecting the stripping current response were investigated and optimized. The formed MWCNTs in the composite film enlarged the specific surface area of the electrode and significantly promoted electron transferring, and the formed polyaniline (PANI) enhanced the ion-exchange capacity and prevented the macromolecules in real samples from absorbing onto the surface of the electrode. The presence of NA effectively increased the stability and adhesion of the composite film, enhanced the cation-exchange capacity and improved the ability to preconcentrate metal ions. Under the optimized conditions, a linear range of 1.0 to 50.0 μg/L was achieved for both metal ions, with a detection limit of 0.06 μg/L for Cd(II) and 0.08 μg/L for Pb(II) (S/N = 3), offering good repeatability. Finally, the Bi/MWCNT-EBP-NA/GCE was used for the

Theoretical and Experimental Investigations into Novel Oxynitride Discovery in the GaN-TiO2 System at High Pressure

Directory of Open Access Journals (Sweden)

Alwin James

2018-01-01

Full Text Available We employed ab initio evolutionary algorithm USPEX to speed up the discovery of a novel oxynitride in the binary system of GaN-TiO2 using high-pressure synthesis. A 1:2 mixture of GaN and nanocrystalline TiO2 (anatase was reacted under 1 GPa of pressure and at 1200 °C in a piston cylinder apparatus to produce a mixture of TiO2 (rutile and an unknown phase. From the initial analysis of high resolution neutron and X-ray diffraction data, it is isomorphic with monoclinic V2GaO5 with a unit cell composition of Ga10Ti8O28N2 with the following parameters: monoclinic, space group C2/m, a = 17.823(1 Å, b = 2.9970(1 Å, c = 9.4205(5 Å, β = 98.446(3°; Volume = 497.74(3 Å3. Further, a joint rietveld refinement revealed two distinct regimes—A Ti-rich block and a Ga-rich block. The Ti-rich block consists of four edge-shared octahedra and contains a site which is about 60% occupied by N; this site is bonded to four Ti. The remainder of the block consists of edge linked Ti-octahedral chains linked to the TiN/TiO fragments at octahedral corners partially occupied by nitrogen. The Ga-block contains two symmetry independent octahedral sites, occupied mostly by Ga, and a pure Ga-centered tetrahedral site bonded mostly to oxygen.

Relook on fitting of viscosity with undercooling of glassy liquids

Indian Academy of Sciences (India)

Department of Materials Science and Engineering, Indian Institute of Technology, Kanpur ... The present approach is on the modification of viscosity fitting of undercooled liquid as a function of ... behaviour of glassy alloys and organic and ionic compounds ...... the present method is applied to calculate the analytical solu-.

Metal-Catalyst-Free Synthesis and Characterization of Single-Crystalline Silicon Oxynitride Nanowires

Directory of Open Access Journals (Sweden)

Shuang Xi

2012-01-01

Full Text Available Large quantities of single-crystal silicon oxynitride nanowires with high N concentration have been synthesized directly on silicon substrate at 1200°C without using any metal catalyst. The diameter of these ternary nanowires is ranging from 10 to 180 nm with log-normal distribution, and the length of these nanowires varies from a few hundreds of micrometers to several millimeters. A vapor-solid mechanism was proposed to explain the growth of the nanowires. These nanowires are grown to form a disordered mat with an ultrabright white nonspecular appearance. The mat demonstrates highly diffusive reflectivity with the optical reflectivity of around 80% over the whole visible wavelength, which is comparable to the most brilliant white beetle scales found in nature. The whiteness might be resulted from the strong multiscattering of a large fraction of incident light on the disordered nanowire mat. These ultra-bright white nanowires could form as reflecting surface to meet the stringent requirements of bright-white light-emitting-diode lighting for higher optical efficiency. They can also find applications in diverse fields such as sensors, cosmetics, paints, and tooth whitening.

Electrical resistivity in Zr48Nb8Cu12Fe8Be24 glassy and crystallized alloys

Science.gov (United States)

Bai, H. Y.; Tong, C. Z.; Zheng, P.

2004-02-01

The electrical resistivity of Zr48Nb8Cu12Fe8Be24 bulk metallic glassy and crystallized alloys in the temperature range of 4.2-293 K is investigated. It is found that the resistivity in glassy and crystallized states shows opposite temperature coefficients. For the metallic glass, the resistivity shows a negative logarithmic dependence at temperatures below 16 K, whereas it has more normal behavior for the crystallized alloy. At higher temperatures, the resistivity in both glassy and crystallized alloys shows dependence upon both T and T2, but the signs of the T and T2 terms are opposite. The results are interpreted in terms of scattering from two-level tunneling states in glasses and the generalized Ziman diffraction model.

Studies of PVC/ENR blends: blend compositions

International Nuclear Information System (INIS)

Chantara Thevy Ratnam; Khairul Zaman Mohd Dahlan; Nasir, M.; Baharin, A.

2002-01-01

Blends of poly(vinyl chloride/epoxidized natural rubber (PVC/ENR) were prepared by using Bra bender Plasticorder at compositions ranging from 0-100% PVC. They were blended at 150 degree C mixing temperature, 50 rpm rotor speed and 10 minutes mixing time. The blends were characterized for tensile strength , elongation at break, glass transition temperatures and Fourier transform infra red spectroscopy (FTIR). Results revealed that as the PVC content increases the blend behaviour changes from elastomeric to glassy. However the blends found to be compatible at all compositions. (Author)

Outstanding resistance and passivation behaviour of new Fe-Co metal-metal glassy alloys in alkaline media.

Directory of Open Access Journals (Sweden)

Khadijah M Emran

Full Text Available The electrochemical behavior of the oxide layers on two metal-metal glassy alloys, Fe78Co9Cr10Mo2Al1 (VX9and Fe49Co49V2 (VX50 (at.%, were studied using electrochemical techniques including electrochemical frequency modulation (EFM, electrochemical impedance spectroscopy (EIS and cyclic polarization (CP measurements. The morphology and composition of the alloy surfaces were investigated using X-ray photoelectron spectroscopy (XPS, scanning electron microscopy (SEM and atomic force microscopy (AFM. The corrosion rate and surface roughness of both alloys increased as the concentration of NaOH in aqueous solution was raised. The presence of some protective elements in the composition of the alloys led to the formation of a spontaneous passive layer on the alloy surface. The higher resistance values of both alloys were associated with the magnitude of the dielectric properties of the passive films formed on their surfaces. Both alloys are classified as having outstanding resistance to corrosion, which results from the formation of a passive film that acts as an efficient barrier to corrosion in alkaline solution.

Electrochemical functionalization of glassy carbon electrode by reduction of diazonium cations in protic ionic liquid

International Nuclear Information System (INIS)

Shul, Galyna; Ruiz, Carlos Alberto Castro; Rochefort, Dominic; Brooksby, Paula A.; Bélanger, Daniel

2013-01-01

Protic ionic liquid based on 2-methoxypyridine and trifluoroacetic acid was used as electrolyte for the functionalization of a glassy carbon electrode surface by electrochemical reduction of in situ generated 4-chlorobenzene diazonium and 4-nitrobenzene diazonium cations. The diazonium cations were synthesized in an electrochemical cell by reaction of the corresponding amines with NaNO 2 dissolved in protic ionic liquid. The resulting electrografted organic layers exhibit similar properties to those layers obtained by the derivatization from isolated diazonium salts dissolved in protic ionic liquid. Functionalized glassy carbon electrode surfaces were characterized by cyclic voltammetry, Fourier transform infrared and X-ray photoelectron spectroscopies. Atomic force microscopy thickness measurements revealed that, in our experimental conditions, the use of protic ionic liquid led to the formation of film with a thickness of about 1.5 nm. It is also demonstrated that the nitrobenzene chemisorbed on glassy carbon electrode or dissolved in protic ionic liquid undergoes electrochemical conversion to hydroxyaminobenzene

Some Recent Developments in Structure and Glassy Behavior of Proteins

Science.gov (United States)

Hu, Chin-Kun

2012-02-01

We have used ARVO developed by us to find that the ratio of volume and surface area of proteins in Protein Data Bank distributed in a very narrow region [1]. Such result is useful for the determination of protein 3D structures. It has been widely known that a spin glass model can be used to understand the slow relaxation behavior of a glass at low temperatures [2]. We have used molecular dynamics and simple models of polymer chains to study relaxation and aggregation of proteins under various conditions and found that polymer chains with neighboring monomers connected by rigid bonds can relax very slowly and show glassy behavior [3]. We have also found that native collagen fibrils show glassy behavior at room temperatures [4]. The results of [3] and [4] about the glassy behavior of polymers or proteins are useful for understanding the mechanism for a biological system to maintain in a non-equilibrium state, including the ancient seed [5], which can maintain in a non-equilibrium state for a very long time. (1) M.-C. Wu, M. S. Li, W.-J. Ma, M. Kouza, and C.-K. Hu, EPL, in press (2011); (2) C. Dasgupta, S.-K. Ma, and C.-K. Hu. Phys. Rev. B 20, 3837-3849 (1979); (3) W.-J. Ma and C.-K. Hu, J. Phys. Soc. Japan 79, 024005, 024006, 054001, and 104002 (2010), C.-K. Hu and W.-J. Ma, Prog. Theor. Phys. Supp. 184, 369 (2010); S. G. Gevorkian, A. E. Allahverdyan, D. S. Gevorgyan and C.-K. Hu, EPL 95, 23001 (2011); S. Sallon, et al. Science 320, 1464 (2008).

A glassy carbon electrode modified with a composite consisting of reduced graphene oxide, zinc oxide and silver nanoparticles in a chitosan matrix for studying the direct electron transfer of glucose oxidase and for enzymatic sensing of glucose

International Nuclear Information System (INIS)

Li, Zhenjiang; Sheng, Liying; Xie, Cuicui; Meng, Alan; Zhao, Kun

2016-01-01

The authors describe the fabrication of a nanocomposite consisting of reduced graphene oxide, zinc oxide and silver nanoparticles by microwave-assisted synthesis. The composite was further reduced in-situ with hydrazine hydrate and then placed, along with the enzyme glucose oxidase, on a glassy carbon electrode. The synergistic effect of the materials employed in the nanocomposite result in excellent electrocatalytic activity. The Michaelis-Menten constant of the adsorbed GOx is 0.25 mM, implying a remarkable affinity of the GOx for glucose. The amperometric response of the modified GCE is linearly proportional to the concentration of glucose in 0.1 to 12.0 mM concentration range, and the detection limit is 10.6 µM. The biosensor is highly selective, well reproducible and stable. (author)

Vapor annealing synthesis of non-epitaxial MgB2 films on glassy carbon

Science.gov (United States)

Baker, A. A.; Bayu Aji, L. B.; Bae, J. H.; Stavrou, E.; Steich, D. J.; McCall, S. K.; Kucheyev, S. O.

2018-05-01

We describe the fabrication and characterization of 25–800 nm thick MgB2 films on glassy carbon substrates by Mg vapor annealing of sputter-deposited amorphous B films. Results demonstrate a critical role of both the initial B film thickness and the temperature–time profile on the microstructure, elemental composition, and superconducting properties of the resultant MgB2 films. Films with thicknesses of 55 nm and below exhibit a smooth surface, with a roughness of 1.1 nm, while thicker films have surface morphology consisting of elongated nano-crystallites. The suppression of the superconducting transition temperature for thin films scales linearly with the oxygen impurity concentration and also correlates with the amount of lattice disorder probed by Raman scattering. The best results are obtained by a rapid (12 min) anneal at 850 °C with large temperature ramp and cooling rates of ∼540 °C min‑1. Such fast processing suppresses the deleterious oxygen uptake.

Wetting of a Charged Surface of Glassy Carbon by Molten Alkali-Metal Chlorides

Science.gov (United States)

Stepanov, V. P.

2018-03-01

Values of the contact angle of wetting of a surface of glassy carbon by molten chlorides of lithium, sodium, potassium, and cesium are measured by the meniscus weight method to determine the common factors of wettability of solid surfaces by ionic melts upon a change in the salt phase composition and a jump in electric potential. It is found that with a potential shift in the positive direction the shape of the curve of the contact angle's dependence on the potential varies upon substitution of one salt by another: the angle of wetting shrinks monotonously in lithium chloride but remains constant in molten cesium chloride. This phenomenon is explained by the hypothesis that the nature of the halide anion adsorption on the positively charged surface of an electrode is chemical and not electrostatic. It is shown that the adsorption process is accompanied by charge transfer through the interface, with covalent bonding between the adsorbent and adsorbate.

Multilayered nanoclusters of platinum and gold: insights on electrodeposition pathways, electrocatalysis, surface and bulk compositional properties

CSIR Research Space (South Africa)

Mkwizu, TS

2013-06-01

Full Text Available Electrochemical, surface and bulk compositional properties of multilayered nanoclusters of Pt and Au, electrochemically deposited on glassy carbon under conditions involving sequential surface–limited redox–replacement reactions (performed at open...

Equation-free dynamic renormalization in a glassy compaction model

International Nuclear Information System (INIS)

Chen, L.; Kevrekidis, I. G.; Kevrekidis, P. G.

2006-01-01

Combining dynamic renormalization with equation-free computational tools, we study the apparently asymptotically self-similar evolution of void distribution dynamics in the diffusion-deposition problem proposed by Stinchcombe and Depken [Phys. Rev. Lett. 88, 125701 (2002)]. We illustrate fixed point and dynamic approaches, forward as well as backward in time; these can be used to accelerate simulators of glassy dynamic phenomena

Equation-free dynamic renormalization in a glassy compaction model

Science.gov (United States)

Chen, L.; Kevrekidis, I. G.; Kevrekidis, P. G.

2006-07-01

Combining dynamic renormalization with equation-free computational tools, we study the apparently asymptotically self-similar evolution of void distribution dynamics in the diffusion-deposition problem proposed by Stinchcombe and Depken [Phys. Rev. Lett. 88, 125701 (2002)]. We illustrate fixed point and dynamic approaches, forward as well as backward in time; these can be used to accelerate simulators of glassy dynamic phenomena.

New anode material for lithium-ion cells produced by catalytic graphitization of glassy carbon at 1000 degrees C

Energy Technology Data Exchange (ETDEWEB)

Skowronski, J.M. [Poznan Univ. of Technology, Poznan (Poland). Inst. of Chemistry and Technical Electrochemistry; Central Lab. of Batteries and Cells, Poznan (Poland); Knofczynski, K. [Central Lab. of Batteries and Cells, Poznan (Poland)

2006-10-15

This study investigated the conversion of glassy carbon into graphite at relatively low temperature of 1000 degrees C under ambient pressure using iron powder as the catalyst. The composite product of reaction was a graphite and turbostratic carbon whose use was then examined in terms of application in lithium-ion cells. Glassy, hard carbon spheres of 10 to 15 {iota}m were prepared from phenolic resin in a nitrogen atmosphere and then subjected to heat treatment with an iron powder mixture. After cooling down to ambient temperature, the carbon/iron mixture was treated with diluted HCl solution to remove metallic additives. The modified carbon was then washed with distilled water until chloride ions disappeared in a filtrate. All samples were characterized using XRD analysis. Working electrodes for electrochemical measurements were made by mixing carbons with PVDF. Cyclic voltammograms recorded for unmodified and modified carbons were consistent with XRD measurements. SEM analysis revealed that the process of graphitization begins at the external regions of glassy carbon spheres where erosion occurs when the carbon reacts with iron particles. The surface destruction of carbon spheres progresses into the interior of the spheres, resulting in their collapse followed by the transformation into pallets resembling a stack of graphite sheets. It was noted that not all unorganized carbon was conversed to graphite. Rather, only 50 per cent of turbostratic carbon existed in the product of heat treatment. The product of graphitization appeared to be a promising material for the preparation of anodes for lithium-ion cells. The discharge capacity for carbon produced by catalytic treatment was found to be approximately 5 times higher, while the discharge/charge reversibility was 23 per cent higher than values obtained for untreated carbon. The study showed that the uptake of lithium ions by the original carbon depends on the insertion/deinsertion mechanism of hard carbon as well

A study of nanostructured gold modified glassy carbon electrode for ...

Indian Academy of Sciences (India)

A nanostructured gold modified glassy carbon electrode (Aunano/GCE) was employed for the determination of trace chromium(VI). To prepare Aunano/GCE, the GCE was immersed into KAuCl4 solution and electrodeposition was conducted at the potential of -0.4 V (vs Ag/AgCl) for 600 s. Scanning electron microscopy ...

Gold nanoparticles directly modified glassy carbon electrode for non-enzymatic detection of glucose

Energy Technology Data Exchange (ETDEWEB)

Chang, Gang; Shu, Honghui; Ji, Kai [Ministry-of-Education Key Laboratory for the Green Preparation and Application of Functional Materials, Faculty of Materials Science and Engineering, Hubei University, No. 368 Youyi Avenue, Wuchang, Wuhan 430062 (China); Oyama, Munetaka [Department of Material Chemistry, Graduate School of Engineering, Kyoto University, Nishikyo-ku, Kyoto 615-8520 (Japan); Liu, Xiong [Ministry-of-Education Key Laboratory for the Green Preparation and Application of Functional Materials, Faculty of Materials Science and Engineering, Hubei University, No. 368 Youyi Avenue, Wuchang, Wuhan 430062 (China); He, Yunbin, E-mail: ybhe@hubu.edu.cn [Ministry-of-Education Key Laboratory for the Green Preparation and Application of Functional Materials, Faculty of Materials Science and Engineering, Hubei University, No. 368 Youyi Avenue, Wuchang, Wuhan 430062 (China)

2014-01-01

This work describes controllable preparation of gold nanoparticles on glassy carbon electrodes by using the seed mediated growth method, which contains two steps, namely, nanoseeds attachment and nanocrystals growth. The size and the dispersion of gold nanoparticles grown on glassy carbon electrodes could be easily tuned through the growth time based on results of field-emission scanning electron microscopy. Excellent electrochemical catalytic characteristics for glucose oxidation were observed for the gold nanoparticles modified glassy carbon electrodes (AuNPs/GC), resulting from the extended active surface area provided by the dense gold nanoparticles attached. It exhibited a wide linear range from 0.1 mM to 25 mM with the sensitivity of 87.5 μA cm{sup −2} mM{sup −1} and low detection limit down to 0.05 mM for the sensing of glucose. The common interfering species such as chloride ion, ascorbic acid, uric acid and 4-acetamidophenol were verified having no interference effect on the detection of glucose. It is demonstrated that the seed mediated method is one of the facile approaches for fabricating Au nanoparticles modified substrates, which could work as one kind of promising electrode materials for the glucose nonenzymatic sensing.

Ultrathin silicon oxynitride layer on GaN for dangling-bond-free GaN/insulator interface.

Science.gov (United States)

Nishio, Kengo; Yayama, Tomoe; Miyazaki, Takehide; Taoka, Noriyuki; Shimizu, Mitsuaki

2018-01-23

Despite the scientific and technological importance of removing interface dangling bonds, even an ideal model of a dangling-bond-free interface between GaN and an insulator has not been known. The formation of an atomically thin ordered buffer layer between crystalline GaN and amorphous SiO 2 would be a key to synthesize a dangling-bond-free GaN/SiO 2 interface. Here, we predict that a silicon oxynitride (Si 4 O 5 N 3 ) layer can epitaxially grow on a GaN(0001) surface without creating dangling bonds at the interface. Our ab initio calculations show that the GaN/Si 4 O 5 N 3 structure is more stable than silicon-oxide-terminated GaN(0001) surfaces. The electronic properties of the GaN/Si 4 O 5 N 3 structure can be tuned by modifying the chemical components near the interface. We also propose a possible approach to experimentally synthesize the GaN/Si 4 O 5 N 3 structure.

Perovskite oxynitride LaTiOxNy thin films: Dielectric characterization in low and high frequencies

International Nuclear Information System (INIS)

Lu, Y.; Ziani, A.; Le Paven-Thivet, C.; Benzerga, R.; Le Gendre, L.; Fasquelle, D.; Kassem, H.

2011-01-01

Lanthanum titanium oxynitride (LaTiO x N y ) thin films are studied with respect to their dielectric properties in low and high frequencies. Thin films are deposited by radio frequency magnetron sputtering on different substrates. Effects of nitrogen content and crystalline quality on dielectric properties are investigated. In low-frequency range, textured LaTiO x N y thin films deposited on conductive single crystal Nb–STO show a dielectric constant ε′ ≈ 140 with low losses tanδ = 0.012 at 100 kHz. For the LaTiO x N y polycrystalline films deposited on conductive silicon substrates with platinum (Pt/Ti/SiO 2 /Si), the tunability reached up to 57% for a weak electric field of 50 kV/cm. In high-frequency range, epitaxial LaTiO x N y films deposited on MgO substrate present a high dielectric constant with low losses (ε′ ≈ 170, tanδ = 0.011, 12 GHz).

Evolution of Shock Melt Compositions in Lunar Agglutinates

Science.gov (United States)

Vance, A. M.; Christoffersen, R.; Keller, L. P.

2015-01-01

Lunar agglutinates are aggregates of regolith grains fused together in a glassy matrix of shock melt produced during smaller-scale (mostly micrometeorite) impacts. Agglutinate formation is a key space weathering process under which the optically-active component of nanophase metallic Fe (npFe(sup 0)) is added to the lunar regolith. Here we have used energy-dispersive X-ray (EDX) compositional spectrum imaging in the SEM to quantify the chemical homogeneity of agglutinitic glass, correlate its homogeneity to its parent soil maturity, and identify the principle chemical components contributing to the shock melt compositional variations.

Free volume and elastic properties changes in Cu-Zr-Ti-Pd bulk glassy alloy on heating

International Nuclear Information System (INIS)

Louzguine-Luzgin, Dmitri V.; Yavari, Alain Reza; Fukuhara, Mikio; Ota, Katsumi; Xie, Guoqiang; Vaughan, Gavin; Inoue, Akihisa

2007-01-01

The variation of free volume and elastic properties of the Cu 55 Zr 30 Ti 10 Pd 5 glassy alloy on heating was studied. The structure changes on heating were studied by synchrotron X-ray diffraction, differential scanning and isothermal calorimetries. The studied glassy alloy shows a rather high Poisson's ratio exceeding 0.42 which is maintained after the structure relaxation and primary devitrification. Young's and Shear modules decrease upon primary devitrification while Bulk modulus exhibits a maximum after structural relaxation

Occurrence of particle debris field during focused Ga ion beam milling of glassy carbon

Energy Technology Data Exchange (ETDEWEB)

Hu Qin [Centre for Industrial Photonics, Institute for Manufacturing, Department of Engineering, University of Cambridge, Alan Reece Building, 17 Charles Babbage Road, Cambridge, CB3 0FS (United Kingdom); O' Neill, William, E-mail: wo207@eng.cam.ac.uk [Centre for Industrial Photonics, Institute for Manufacturing, Department of Engineering, University of Cambridge, Alan Reece Building, 17 Charles Babbage Road, Cambridge, CB3 0FS (United Kingdom)

2010-08-01

To explore the machining characteristics of glassy carbon by focused ion beam (FIB), particles induced by FIB milling on glassy carbon have been studied in the current work. Nano-sized particles in the range of tens of nanometers up to 400 nm can often be found around the area subject to FIB milling. Two ion beam scanning modes - slow single scan and fast repetitive scan - have been tested. Fewer particles are found in single patterns milled in fast repetitive scan mode. For a group of test patterns milled in a sequence, it was found that a greater number of particles were deposited around sites machined early in the sequence. In situ EDX analysis of the particles showed that they were composed of C and Ga. The formation of particles is related to the debris generated at the surrounding areas, the low melting point of gallium used as FIB ion source and the high contact angle of gallium on glassy carbon induces de-wetting of Ga and the subsequent formation of Ga particles. Ultrasonic cleaning can remove over 98% of visible particles. The surface roughness (R{sub a}) of FIB milled areas after cleaning is less than 2 nm.

Occurrence of particle debris field during focused Ga ion beam milling of glassy carbon

International Nuclear Information System (INIS)

Hu Qin; O'Neill, William

2010-01-01

To explore the machining characteristics of glassy carbon by focused ion beam (FIB), particles induced by FIB milling on glassy carbon have been studied in the current work. Nano-sized particles in the range of tens of nanometers up to 400 nm can often be found around the area subject to FIB milling. Two ion beam scanning modes - slow single scan and fast repetitive scan - have been tested. Fewer particles are found in single patterns milled in fast repetitive scan mode. For a group of test patterns milled in a sequence, it was found that a greater number of particles were deposited around sites machined early in the sequence. In situ EDX analysis of the particles showed that they were composed of C and Ga. The formation of particles is related to the debris generated at the surrounding areas, the low melting point of gallium used as FIB ion source and the high contact angle of gallium on glassy carbon induces de-wetting of Ga and the subsequent formation of Ga particles. Ultrasonic cleaning can remove over 98% of visible particles. The surface roughness (R a ) of FIB milled areas after cleaning is less than 2 nm.

Electrochemical investigations of Pu(IV)/Pu(III) redox reaction using graphene modified glassy carbon electrodes and a comparison to the performance of SWCNTs modified glassy carbon electrodes

International Nuclear Information System (INIS)

Gupta, Ruma; Gamare, Jayashree; Sharma, Manoj K.; Kamat, J.V.

2016-01-01

Highlights: • First report of aqueous electrochemistry of Plutonium on graphene modified electrode. • Graphene is best electrocatalytic material for Pu(IV)/Pu(III) redox couple among the reported modifiers viz. reduced graphene oxide (rGO) and SWCNT’s. • The electrochemical reversibility of Pu(IV)/Pu(III) redox couple improves significantly on graphene modified electrode compared to previously reported rGO & SWCNTs modified electrodes • Donnan interaction between plutonium species and graphene surface offers a possibility for designing a highly sensitive sensor for plutonium • Graphene modified electrode shows higher sensitivity for the determination of plutonium compared to glassy carbon and single walled carbon nanotube modified electrode - Abstract: The work reported in this paper demonstrates for the first time that graphene modified glassy carbon electrode (Gr/GC) show remarkable electrocatalysis towards Pu(IV)/Pu(III) redox reaction and the results were compared with that of single-walled carbon nanotubes modified GC (SWCNTs/GC) and glassy carbon (GC) electrodes. Graphene catalyzes the exchange of current of the Pu(IV)/Pu(III) couple by reducing both the anodic and cathodic overpotentials. The Gr/GC electrode shows higher peak currents (i p ) and smaller peak potential separation (ΔE p ) values than the SWCNTs/GC and GC electrodes. The heterogeneous electron transfer rate constants (k s ), charge transfer coefficients (α) and the diffusion coefficients (D) involved in the electrocatalytic redox reaction were determined. Our observations show that graphene is best electrocatalytic material among both the SWCNTs and GC to study Pu(IV)/Pu(III) redox reaction.

Determination of Volatility and Element Fractionation in Glassy Fallout Debris by SIMS

Energy Technology Data Exchange (ETDEWEB)

Williamson, Todd L. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Tenner, Travis Jay [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Bonamici, Chloe Elizabeth [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Kinman, William Scott [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Pollington, Anthony Douglas [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Steiner, Robert Ernest [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

2016-05-10

The purpose of this report is to characterize glassy fallout debris using the Trinity Test and then characterize the U-isotopes of U₃O₈ reference materials that contain weaponized debris.

Physical ageing in the above-bandgap photoexposured glassy arsenic selenides

Energy Technology Data Exchange (ETDEWEB)

Kozdras, A [Faculty of Physics of Opole University of Technology, 75, Ozimska str., Opole, PL-45370 (Poland); Golovchak, R [Lviv Scientific Research Institute of Materials of SRC ' Carat' , 202, Stryjska str., Lviv, UA-79031 (Ukraine); Shpotyuk, O [Lviv Scientific Research Institute of Materials of SRC ' Carat' , 202, Stryjska str., Lviv, UA-79031 (Ukraine)

2007-08-15

Physical ageing induced by above-bandgap light illumination is studied in glassy As-Se using differential scanning calorimetry. It is shown that measurable effect like to known short-term physical ageing is observed only in Se-rich glasses. The kinetics of this effect is compared with that caused by natural storage in a dark.

Physical ageing in the above-bandgap photoexposured glassy arsenic selenides

International Nuclear Information System (INIS)

Kozdras, A; Golovchak, R; Shpotyuk, O

2007-01-01

Physical ageing induced by above-bandgap light illumination is studied in glassy As-Se using differential scanning calorimetry. It is shown that measurable effect like to known short-term physical ageing is observed only in Se-rich glasses. The kinetics of this effect is compared with that caused by natural storage in a dark

Co-based soft magnetic bulk glassy alloys optimized for glass ...

Indian Academy of Sciences (India)

diameter of 5 mm by conventional copper mould casting method. It reveals ... For example, Co43Fe20Ta5.5B31.5 glassy alloy with a ... coercive force (Hc) of 0.25 A m. −1 ..... [7] Lu Z P, Liu C T, Thompson J R and Porter W D 2004 Phys. Rev.

A low-temperature synthesis of electrochemical active Pt nanoparticles and thin films by atomic layer deposition on Si(111) and glassy carbon surfaces

Energy Technology Data Exchange (ETDEWEB)

Liu, Rui [Joint Center for Artificial Photosynthesis, California Institute of Technology, Pasadena, CA 91125 (United States); Han, Lihao [Joint Center for Artificial Photosynthesis, California Institute of Technology, Pasadena, CA 91125 (United States); Photovoltaic Materials and Devices (PVMD) Laboratory, Delft University of Technology, P.O. Box 5031, GA Delft 2600 (Netherlands); Huang, Zhuangqun; Ferrer, Ivonne M. [Joint Center for Artificial Photosynthesis, California Institute of Technology, Pasadena, CA 91125 (United States); Division of Chemistry and Chemical Engineering, California Institute of Technology, 210 Noyes Laboratory 127-72, Pasadena, CA 91125 (United States); Smets, Arno H.M.; Zeman, Miro [Photovoltaic Materials and Devices (PVMD) Laboratory, Delft University of Technology, P.O. Box 5031, GA Delft 2600 (Netherlands); Brunschwig, Bruce S., E-mail: bsb@caltech.edu [Beckman Institute, California Institute of Technology, Pasadena, CA 91125 (United States); Lewis, Nathan S., E-mail: nslewis@caltech.edu [Joint Center for Artificial Photosynthesis, California Institute of Technology, Pasadena, CA 91125 (United States); Beckman Institute, California Institute of Technology, Pasadena, CA 91125 (United States); Division of Chemistry and Chemical Engineering, California Institute of Technology, 210 Noyes Laboratory 127-72, Pasadena, CA 91125 (United States); Kavli Nanoscience Institute, California Institute of Technology, Pasadena, CA 91125 (United States)

2015-07-01

Atomic layer deposition (ALD) was used to deposit nanoparticles and thin films of Pt onto etched p-type Si(111) wafers and glassy carbon discs. Using precursors of MeCpPtMe{sub 3} and ozone and a temperature window of 200–300 °C, the growth rate was 80–110 pm/cycle. X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), and scanning electron microscopy (SEM) were used to analyze the composition, structure, morphology, and thickness of the ALD-grown Pt nanoparticle films. The catalytic activity of the ALD-grown Pt for the hydrogen evolution reaction was shown to be equivalent to that of e-beam evaporated Pt on glassy carbon electrode. - Highlights: • Pure Pt films were grown by atomic layer deposition (ALD) using MeCpPtMe3 and ozone. • ALD-grown Pt thin films had high growth rates of 110 pm/cycle. • ALD-grown Pt films were electrocatalytic for hydrogen evolution from water. • Electrocatalytic activity of the ALD Pt films was equivalent to e-beam deposited Pt. • No carbon species were detected in the ALD-grown Pt films.

A low-temperature synthesis of electrochemical active Pt nanoparticles and thin films by atomic layer deposition on Si(111) and glassy carbon surfaces

International Nuclear Information System (INIS)

Liu, Rui; Han, Lihao; Huang, Zhuangqun; Ferrer, Ivonne M.; Smets, Arno H.M.; Zeman, Miro; Brunschwig, Bruce S.; Lewis, Nathan S.

2015-01-01

Atomic layer deposition (ALD) was used to deposit nanoparticles and thin films of Pt onto etched p-type Si(111) wafers and glassy carbon discs. Using precursors of MeCpPtMe 3 and ozone and a temperature window of 200–300 °C, the growth rate was 80–110 pm/cycle. X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), and scanning electron microscopy (SEM) were used to analyze the composition, structure, morphology, and thickness of the ALD-grown Pt nanoparticle films. The catalytic activity of the ALD-grown Pt for the hydrogen evolution reaction was shown to be equivalent to that of e-beam evaporated Pt on glassy carbon electrode. - Highlights: • Pure Pt films were grown by atomic layer deposition (ALD) using MeCpPtMe3 and ozone. • ALD-grown Pt thin films had high growth rates of 110 pm/cycle. • ALD-grown Pt films were electrocatalytic for hydrogen evolution from water. • Electrocatalytic activity of the ALD Pt films was equivalent to e-beam deposited Pt. • No carbon species were detected in the ALD-grown Pt films

Definition and preparation of glassy matrices by innovating processes to confine radioactive wastes and industrial toxic materials

International Nuclear Information System (INIS)

Moncouyoux, J.P.

1995-01-01

The confinement by vitrification of high-level radioactive wastes is studied in the CEA for fifteen years. These studies have lead to the preparation of glassy matrices by innovating processes. These processes can be applied to non-radioactive toxic materials treatment too. In this work are more particularly described the glassy matrix long-dated behaviour and the different vitrification processes used (by direct induction in cold crucible, by transferred arc plasma). (O.L.). 1 tab

Impedimetric PSA aptasensor based on the use of a glassy carbon electrode modified with titanium oxide nanoparticles and silk fibroin nanofibers.

Science.gov (United States)

Benvidi, Ali; Banaei, Maryam; Tezerjani, Marzieh Dehghan; Molahosseini, Hosein; Jahanbani, Shahriar

2017-12-14

This article describes an impedimetric aptasensor for the prostate specific antigen (PSA), a widely accepted prostate cancer biomarker. A glassy carbon electrode (GCE) was modified with titanium oxide nanoparticles (TiO 2 ) and silk fibroin nanofiber (SF) composite. The aptasensor was obtained by immobilizing a PSA-binding aptamer on the AuNP-modified with 6-mercapto-1-hexanol. The single fabrication steps were characterized by cyclic voltammetry and electrochemical impedance spectroscopy. The assay has two linear response ranges (from 2.5 fg.mL -1 to 25 pg.mL -1 , and from 25 pg.mL -1 to 25 ng.mL -1 ) and a 0.8 fg.mL -1 detection limit. After optimization of experimental conditions, the sensor is highly selective for PSA over bovine serum albumin and lysozyme. It was successfully applied to the detection of PSA in spiked serum samples. Graphical abstract Schematic of the fabrication of an aptasensor for the prostate specific antigen (PSA). It is based on the use of a glassy carbon electrode modified with gold nanoparticles and titanium oxide-silk fibroin. The immobilization process of aptamer and interaction with PSA were followed by electrochemical impedance spectroscopy technique.

Dielectric relaxation studies in super-cooled liquid and glassy phases of anti-cancerous alkaloid: Brucine

Science.gov (United States)

Afzal, Aboothahir; Shahin Thayyil, M.; Sulaiman, M. K.; Kulkarni, A. R.

2018-05-01

Brucine has good anti-tumor effects, on both liver cancer and breast cancer. It has bioavailability of 40.83%. Since the bioavailability of the drug is low, an alternative method to increase its bioavailability and solubility is by changing the drug into glassy form. We used Differential Scanning Calorimetry (DSC) for studying the glass forming ability of the drug. Brucine was found to be a very good glass former glass transition temperature 365 K. Based on the DSC analysis we have used broadband dielectric spectroscopy (BDS) for studying the drug in the super cooled and glassy state. BDS is an effective tool to probe the molecular dynamics in the super cooled and glassy state. Molecular mobility is found to be present even in the glassy state of this active pharmaceutical ingredient (API) which is responsible for the instability. Our aim is to study the factors responsible for instability of this API in amorphous form. Cooling curves for dielectric permittivity and dielectric loss revealed the presence of structural (α) and secondary relaxations (β and γ). Temperature dependence of relaxation time is fitted by Vogel-Fulcher-Tammann equation and found the values of activation energy of the α relaxation, fragility and glass transition temperature. Paluch's anti correlation is also verified, that the width of the α-loss peak at or near the glass transition temperature Tg is strongly anticorrelated with the polarity of the molecule. The larger the dielectric relaxation strength Δɛ (Tg) of the system, the narrower is the α-loss peak (higher value of βKWW).

On the electronic nature of silicon and germanium based oxynitrides and their related mechanical, optical and vibrational properties as obtained from DFT and DFPT

KAUST Repository

Goumri-Said, Souraya

2012-02-01

Electronic structure, bonding and optical properties of the orthorhombic oxynitrides Si 2N 2O and Ge 2N 2O are studied using the density function theory as implemented in pseudo-potential plane wave and full-potential (linearized) augmented plane wave plus local orbitals methods. Generalized gradient approximation is employed in order to determine the band gap energy. Indeed, the Si 2N 2O exhibits a large direct gap whereas Ge 2N 2O have an indirect one. Bonding is analyzed via the charge densities and Mulliken population, where the role of oxygen is investigated. The analysis of the elastic constants show the mechanical stability of both oxynitrides. Their bulk and shear modulus are slightly smaller than those reported on nitrides semiconductors due to the oxygen presence. The optical properties, namely the dielectric function, optical reflectivity, refractive index and electron energy loss, are reported for radiation up to 30 eV. The phonon dispersion relation, zone-center optical mode frequency, density of phonon states are calculated using the density functional perturbed theory. Thermodynamic properties of Si 2N 2O and Ge 2N 2O, such as heat capacity and Debye temperature, are given for reference. Our study suggests that Si 2N 2O and Ge 2N 2O could be a promising potential materials for applications in the microelectronics and optoelectronics areas of research. © 2011 Elsevier B.V. All rights reserved.

Electrocatalytic oxidation of hydrazine at overoxidized polypyrrole film modified glassy carbon electrode

Energy Technology Data Exchange (ETDEWEB)

Majidi, Mir Reza [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz 51664 (Iran, Islamic Republic of); Jouyban, Abolghasem [Faculty of Pharmacy and Drug Applied Research Center, Tabriz University of Medical Sciences, Tabriz 51664 (Iran, Islamic Republic of); Asadpour-Zeynali, Karim [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz 51664 (Iran, Islamic Republic of)]. E-mail: asadpour@tabrizu.ac.ir

2007-06-20

Electrocatalytic oxidation of hydrazine (HZ) was studied on an overoxidized polypyrrole (OPPy) modified glassy carbon electrode using cyclic voltammetry and chronoamperometry techniques. The OPPy-modified glassy carbon electrode has very high catalytic ability for electrooxidation of HZ, which appeared as a reduced overpotential in a wide operational pH range of 5-10. The overall numbers of electrons involved in the catalytic oxidation of HZ, the number of electrons involved in the rate-determining and diffusion coefficient of HZ were estimated using cyclic voltammetry and chronoamperometry. It has been shown that using the OPPy-modified electrode, HZ can be determined by cyclic voltammetry and amperometry with limit of detection 36 and 3.7 {mu}M, respectively. The results of the analysis suggest that the proposed method promises accurate results and could be employed for the routine determination of HZ.

Physical and electrical characteristics of silicon oxynitride films with various refractive indices

Energy Technology Data Exchange (ETDEWEB)

Liao, Jeng-Hwa; Hsieh, Jung-Yu; Lin, Hsing-Ju; Tang, Wei-Yao; Chiang, Chun-Ling; Yang, Ling-Wu; Yang, Tahone; Chen, Kuang-Chao; Lu, Chih-Yuan [Macronix International Co. Ltd, No 16, Li-Hsin Road, Hsinchu Science Park, Hsinchu 300, Taiwan (China); Lo, Yun-Shan; Wu, Tai-Bor, E-mail: jhliao@mxic.com.t [Department of Materials Science and Engineering, National Tsing Hua University, Hsinchu 300, Taiwan (China)

2009-09-07

This study explores the relationship between both the physical and the electrical characteristics of silicon oxynitride (SiON) films and the refractive index. The single wafer rapid thermal process modules were used for low pressure chemical vapour deposition of SiON films. A series of SiON films with refractive index between 1.50 and 1.83 were fabricated. Fourier transform infrared absorption spectroscopy and x-ray photoelectron spectroscopy identified the chemical bonding configurations of different SiON films: the Si-N bonds are replaced by Si-O bonds as the refractive index of the SiON films declines. Moreover, the Si atomic ratio is kept between 35% and 40% while the oxygen atomic ratio increases and the nitrogen atomic ratio decreases as the refractive index of the SiON film declines. The electrical characteristics of different SiON-based silicon-oxide-nitride-oxide-silicon (SONOS) devices suggest that (1) the dielectric constant increases with increasing refractive index of the SiON film and (2) the charge-trap density is inversely proportional to the oxygen concentration in the SiON film. Based on these results, the SiON films with various refractive indices can provide a wider application for silicon-based devices, such as SONOS and MOS devices.

Physical and electrical characteristics of silicon oxynitride films with various refractive indices

International Nuclear Information System (INIS)

Liao, Jeng-Hwa; Hsieh, Jung-Yu; Lin, Hsing-Ju; Tang, Wei-Yao; Chiang, Chun-Ling; Yang, Ling-Wu; Yang, Tahone; Chen, Kuang-Chao; Lu, Chih-Yuan; Lo, Yun-Shan; Wu, Tai-Bor

2009-01-01

This study explores the relationship between both the physical and the electrical characteristics of silicon oxynitride (SiON) films and the refractive index. The single wafer rapid thermal process modules were used for low pressure chemical vapour deposition of SiON films. A series of SiON films with refractive index between 1.50 and 1.83 were fabricated. Fourier transform infrared absorption spectroscopy and x-ray photoelectron spectroscopy identified the chemical bonding configurations of different SiON films: the Si-N bonds are replaced by Si-O bonds as the refractive index of the SiON films declines. Moreover, the Si atomic ratio is kept between 35% and 40% while the oxygen atomic ratio increases and the nitrogen atomic ratio decreases as the refractive index of the SiON film declines. The electrical characteristics of different SiON-based silicon-oxide-nitride-oxide-silicon (SONOS) devices suggest that (1) the dielectric constant increases with increasing refractive index of the SiON film and (2) the charge-trap density is inversely proportional to the oxygen concentration in the SiON film. Based on these results, the SiON films with various refractive indices can provide a wider application for silicon-based devices, such as SONOS and MOS devices.

Study of electrical properties of glassy Se100–xTex alloys

Indian Academy of Sciences (India)

Unknown

can be successfully explained by correlated barrier hopping (CBH) model. ... The results show that bipolaron hopping dominates over single-polaron hopping in this glassy system. This .... where ∆E is the activation energy and σ0 is called the.

Silicon oxynitrides of KCC-1, SBA-15 and MCM-41 for CO 2 capture with excellent stability and regenerability

KAUST Repository

Patil, Umesh

2012-01-01

We report the use of silicon oxynitrides as novel adsorbents for CO 2 capture. Three series of functionalized materials based on KCC-1, SBA-15 and MCM-41 with Si-NH 2 groups were prepared using a simple one-step process via thermal ammonolysis using ammonia gas, and they demonstrated excellent CO 2 capture capabilities. These materials overcome several limitations of conventional amine-grafted mesoporous silica. They offer good CO 2 capture capacity, faster adsorption-desorption kinetics, efficient regeneration and reuse, more crucially excellent thermal and mechanical stability even in oxidative environments, and a clean and green synthesis route, which allows the overall CO 2 capture process to be practical and sustainable. This journal is © The Royal Society of Chemistry 2012.

Correlation between nanostructural and electrical properties of barium titanate-based glass-ceramic nano-composites

Energy Technology Data Exchange (ETDEWEB)

Al-Assiri, M.S., E-mail: msassiri@kku.edu.sa [Department of Physics, King Khaled University, P.O. Box 9003, Abha (Saudi Arabia); El-Desoky, M.M., E-mail: mmdesoky@gmail.com [Department of Physics, King Khaled University, P.O. Box 9003, Abha (Saudi Arabia); Department of Physics, Faculty of Science, Suez Canal University, Suez (Egypt)

2011-09-08

Highlights: > Glasses have been transformed into nanomaterials by annealing at crystallization temperature. > Glass-ceramic nano-composites are important because of their new physical. > Grain sizes are the most significant structural parameter in electronic nanocrystalline phases. > These phases are very high electrical conductivity. > Hence, glass-ceramic nanocrystals are expected to be used, as gas sensors. - Abstract: Glasses in the system BaTiO{sub 3}-V{sub 2}O{sub 5}-Bi{sub 2}O{sub 3} have been transformed into glass-ceramic nano-composites by annealing at crystallization temperature T{sub cr} determined from DSC thermograms. After annealing they consist of small crystallites embedded in glassy matrix. The crystallization temperature T{sub cr} increases with increasing BaTiO{sub 3} content. XRD and TEM of the glass-ceramic nano-composites show that nanocrystals were embedded in the glassy matrix with an average grain size of 25 nm. The resulting materials exhibit much higher electrical conductivity than the initial glasses. It was postulated that the major role in the conductivity enhancement of these nanomaterials is played by the developed interfacial regions between crystalline and amorphous phases, in which the concentration of V{sup 4+}-V{sup 5+} pairs responsible for electron hopping, has higher than values that inside the glassy matrix. The experimental results were discussed in terms of a model proposed in this work and based on a 'core-shell' concept. From the best fits, reasonable values of various small polaron hopping (SPH) parameters were obtained. The conduction was attributed to non-adiabatic hopping of small polaron.

Cooperative strings and glassy interfaces.

Science.gov (United States)

Salez, Thomas; Salez, Justin; Dalnoki-Veress, Kari; Raphaël, Elie; Forrest, James A

2015-07-07

We introduce a minimal theory of glass formation based on the ideas of molecular crowding and resultant string-like cooperative rearrangement, and address the effects of free interfaces. In the bulk case, we obtain a scaling expression for the number of particles taking part in cooperative strings, and we recover the Adam-Gibbs description of glassy dynamics. Then, by including thermal dilatation, the Vogel-Fulcher-Tammann relation is derived. Moreover, the random and string-like characters of the cooperative rearrangement allow us to predict a temperature-dependent expression for the cooperative length ξ of bulk relaxation. Finally, we explore the influence of sample boundaries when the system size becomes comparable to ξ. The theory is in agreement with measurements of the glass-transition temperature of thin polymer films, and allows quantification of the temperature-dependent thickness hm of the interfacial mobile layer.

A glassy carbon electrode modified with an iron N4-macrocycle and reduced graphene oxide for voltammetric sensing of dissolved oxygen

International Nuclear Information System (INIS)

Silva, Saimon M.; Aguiar, Lucas F.; Carvalho, Rita M. S.; Tanaka, Auro A.; Damos, Flavio S.; Luz, Rita C. S.

2016-01-01

The authors describe a platform for the electrochemical reduction of oxygen. It is based on the use of a glassy carbon electrode (GCE) that was modified in a single-step microwave assisted reaction with a N4-macrocycle containing iron(III) (FeN4) and with reduced graphene oxide. The FeN4/rGO composite was characterized by cyclic voltammetry, differential pulse voltammetry, and scanning electrochemical microscopy (SECM). Cyclic voltammetry showed the composite to enable efficient reduction of O_2 at a very low overpotential (−0.05 V vs. Ag/AgCl). SECM measurements were carried out to map (in the redox competition mode) the activity of a GCE microelectrode modified with FeN4/rGO. Under optimized conditions, the response to dissolved O_2 ranges from 0.8 up to 25 mg⋅L"-"1, and the limit of detection is 0.2 mg⋅L"-"1. (author)

Glassy behavior in the layered perovskites La{sub 2-x}Sr{sub x}CoO{sub 4}(1.1{<=}x{<=}1.3)

Energy Technology Data Exchange (ETDEWEB)

Mukherjee, S., E-mail: sanseb68@yahoo.co.in [Department of Physics, University of Burdwan, Burdwan 713104 (India); Mukherjee, Rajarshi [Department .of Physics, University of Burdwan, Burdwan 713104 (India); Banerjee, S.; Ranganathan, R. [Saha Institute of Nuclear Physics, Kolkata 700 064 (India); Kumar, Uday [Department of Physical Sciences, Indian Institute of Science Education and Research - Kolkata, Mohonpur 741252 (India)

2012-03-15

The glassy behavior of the phase segregated state in the layered cobaltite La{sub 2-x}Sr{sub x}CoO{sub 4} has been studied. The role of the inter-cluster interactions as well as the disordered spins at the paramagnetic-ferromagnetic interface, behind the observed glassy behavior have been investigated. The disordered spins at the interface appear to be strongly pinned, and they contribute little to the observed glassy behavior. On the other hand, the inter-cluster interactions play the key role. Both the Co{sup 4+} and Co{sup 3+} ions are in the intermediate spin state. - Highlights: Black-Right-Pointing-Pointer Phase segregated state of cobaltite La{sub 2-x}Sr{sub x}CoO{sub 4} for (1.1{<=}x{<=}1.3) to find the origin of the observed glassy behavior. Black-Right-Pointing-Pointer Result of the frequency dependent ac susceptibility measurement excludes the possibility of any spin glass phase, hints strong inter-cluster interactions. Black-Right-Pointing-Pointer Relaxation experiments confirm the system to be a collection of clusters with two preferred sizes. Black-Right-Pointing-Pointer The glassy behavior originates from strong inter-cluster interactions.

Characterization of glassy phase at the surface of alumina ceramics substrate and its effect on laser cutting

Energy Technology Data Exchange (ETDEWEB)

Fu Renli [School of Mechanical-Electronic and Materials Engineering, China Univ. of Mining and Technology, Xuzhou, JS (China); Dept. of Ceramics and Glass Engineering, CICECO, Univ. of Aveiro, Aveiro (Portugal); Li Yanbo [School of Mechanical-Electronic and Materials Engineering, China Univ. of Mining and Technology, Xuzhou, JS (China); Xu Xin; Ferreira, J.M.F. [Dept. of Ceramics and Glass Engineering, CICECO, Univ. of Aveiro, Aveiro (Portugal)

2004-07-01

Nowadays alumina ceramic substrates are widely used for high precision applications in electronic devices, such as hybrid integrated circuits (HIC). Usually, the alumina ceramic substrates are shaped through tape casting method and sintered in continuous slab kilns. The sintering aids used to enhance densification during sintering give rise to the formation of an alumino-silicate liquid phase, which is of crucial importance in pressureless and low-temperature sintering (<1600 C) of alumina ceramics. The preferential migration of liquid phase to the surface of alumina substrates under the capillary action and its transformation into glassy phase during cooling affects the subsequent processing steps of HIC. A smoothening effect on surface with its enrichment in glassy phase is accompanied by a decrease of the surface toughness. On the other hand, the accumulated glassy phase onto the surface has a great effect on laser cutting. The high temperatures developed during laser cutting turn the superficial glassy phase into liquid again, while rapid solidification will occur after removing laser beam. The fast cooling of the liquid phase causes formation of extensive network of cracks on the surface of alumina substrate. Apparently, the presence of such faults degrades mechanical strength and thermal shock resistance of alumina substrates. Meanwhile, the recast layers and spatter deposits at the periphery of the hole has been observed. (orig.)

Modification of glassy carbon surfaces by atmospheric pressure cold plasma torch

DEFF Research Database (Denmark)

Mortensen, Henrik Junge; Kusano, Yukihiro; Leipold, Frank

2006-01-01

The effect of plasma treatment on glassy carbon (GC) surfaces was studied with adhesion improvement in mind. A newly constructed remote plasma source was used to treat GC plates. Pure He and a dilute NH3/He mixture were used as feed gases. Optical emission spectroscopy was performed for plasma to...

Direct electron transfer from glucose oxidase immobilized on a nano-porous glassy carbon electrode

International Nuclear Information System (INIS)

Haghighi, Behzad; Tabrizi, Mahmoud Amouzadeh

2011-01-01

Highlights: → A direct electron transfer reaction of glucose oxidase was observed on the surface of a nano-porous glassy carbon electrode. → A pair of well-defined and reversible redox peaks was observed at the formal potential of approximately -0.439 V. → The apparent electron transfer rate constant was measured to be 5.27 s -1 . → A mechanism for the observed direct electron transfer reaction was proposed, which consists of a two-electron and a two-proton transfer. - Abstract: A pair of well-defined and reversible redox peaks was observed for the direct electron transfer (DET) reaction of an immobilized glucose oxidase (GOx) on the surface of a nano-porous glassy carbon electrode at the formal potential (E o ') of -0.439 V versus Ag/AgCl/saturated KCl. The electron transfer rate constant (k s ) was calculated to be 5.27 s -1 . The dependence of E o ' on pH indicated that the direct electron transfer of the GOx was a two-electron transfer process, coupled with two-proton transfer. The results clearly demonstrate that the nano-porous glassy carbon electrode is a cost-effective and ready-to-use scaffold for the fabrication of a glucose biosensor.

Direct electron transfer from glucose oxidase immobilized on a nano-porous glassy carbon electrode

Energy Technology Data Exchange (ETDEWEB)

Haghighi, Behzad, E-mail: haghighi@iasbs.ac.ir [Department of Chemistry, Institute for Advanced Studies in Basic Sciences, P.O. Box 45195-1159, Gava Zang, Zanjan (Iran, Islamic Republic of); Tabrizi, Mahmoud Amouzadeh [Department of Chemistry, Institute for Advanced Studies in Basic Sciences, P.O. Box 45195-1159, Gava Zang, Zanjan (Iran, Islamic Republic of)

2011-11-30

Highlights: > A direct electron transfer reaction of glucose oxidase was observed on the surface of a nano-porous glassy carbon electrode. > A pair of well-defined and reversible redox peaks was observed at the formal potential of approximately -0.439 V. > The apparent electron transfer rate constant was measured to be 5.27 s{sup -1}. > A mechanism for the observed direct electron transfer reaction was proposed, which consists of a two-electron and a two-proton transfer. - Abstract: A pair of well-defined and reversible redox peaks was observed for the direct electron transfer (DET) reaction of an immobilized glucose oxidase (GOx) on the surface of a nano-porous glassy carbon electrode at the formal potential (E{sup o}') of -0.439 V versus Ag/AgCl/saturated KCl. The electron transfer rate constant (k{sub s}) was calculated to be 5.27 s{sup -1}. The dependence of E{sup o}' on pH indicated that the direct electron transfer of the GOx was a two-electron transfer process, coupled with two-proton transfer. The results clearly demonstrate that the nano-porous glassy carbon electrode is a cost-effective and ready-to-use scaffold for the fabrication of a glucose biosensor.

Voltammetric behavior of sedative drug midazolam at glassy carbon electrode in solubilized systems

Directory of Open Access Journals (Sweden)

Rajeev Jain

2012-04-01

Full Text Available Redox behavior of midazolam was studied at a glassy carbon electrode in various buffer systems, supporting electrolytes and pH using differential pulse, square-wave and cyclic voltammetry. Based on its reduction behavior, a direct differential pulse voltammetric method has been developed and validated for the determination of midazolam in parenteral dosage. Three well-defined peaks were observed in 0.1% SLS, Britton–Robinson (BR buffer of pH 2.5. The effect of surfactants like sodium lauryl sulfate (SLS, cetyl trimethyl ammonium bromide (CTAB and Tween 20 was studied. Among these surfactants SLS showed significant enhancement in reduction peak. The cathodic peak currents were directly proportional to the concentration of midazolam with correlation coefficient of 0.99. Keywords: Midazolam, Voltammetry, Surfactant, Glassy carbon electrode, Parenteral dosage form

ELECTROCHEMICAL DETERMINATION OF ETHANOL, 2- PROPANOL AND 1-BUTANOL ON GLASSY CARBON ELECTRODE MODIFIED WITH NICKEL OXIDE FILM

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A. Benchettara

2014-12-01

Full Text Available In this work, we present the modification of a glassy carbon electrode with nickel oxide film which is performed in two successive steps. In the first one, the electrochemical deposition of metallic nickel on the glassy carbon electrode (GCE is achieved in 0.1M boric acid; in the second step, the metallic deposit is anodically oxidized in 0.1M NaOH. These two operations were carried out in a three electrode cell with a filiform platinum auxiliary electrode, a SCE as potential reference and a working microelectrode of modified glassy carbon with nickel oxides. This electrode is characterized by several electrochemical techniques and is used for the catalytic determination of ethanol, 2-propanol and 1-butanol in 0.1 M NaOH. The proposed chemical mechanism shows that NiO2 acts as a mediator.

ELECTROCHEMICAL DETERMINATION OF ETHANOL, 2- PROPANOL AND 1-BUTANOL ON GLASSY CARBON ELECTRODE MODIFIED WITH NICKEL OXIDE FILM

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A. Benchettara

2015-07-01

Full Text Available In this work, we present the modification of a glassy carbon electrode with nickel oxide film which is performed in two successive steps. In the first one, the electrochemical deposition of metallic nickel on the glassy carbon electrode (GCE is achieved in 0.1M boric acid; in the second step, the metallic deposit is anodically oxidized in 0.1M NaOH. These two operations were carried out in a three electrode cell with a filiform platinum auxiliary electrode, a SCE as potential reference and a working microelectrode of modified glassy carbon with nickel oxides. This electrode is characterized by several electrochemical techniques and is used for the catalytic determination of ethanol, 2-propanol and 1-butanol in 0.1 M NaOH. The proposed chemical mechanism shows that NiO2 acts as a mediator.

Electrochemically modified sulfisoxazole nanofilm on glassy carbon for determination of cadmium(II) in water samples

International Nuclear Information System (INIS)

Gupta, Vinod Kumar; Yola, Mehmet Lütfi; Atar, Necip; Solak, Ali Osman; Uzun, Lokman; Üstündağ, Zafer

2013-01-01

Highlights: • Sulfisoxazole was grafted onto glassy carbon electrode. • The electrode was characterized by spectroscopic and electrochemical methods. • It has been used for the determination of Cd(II) ions in real samples in very low concentrations. -- Abstract: Sulfisoxazole (SO) was grafted to glassy carbon electrode (GCE) via the electrochemical oxidation of SO in acetonitrile solution containing 0.1 M tetrabutylammoniumtetra-fluoroborate (TBATFB). The prepared electrode was characterized by using cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), reflection–absorption infrared spectroscopy (RAIRS) and X-ray photoelectron spectroscopy (XPS). The ellipsometric thickness of SO nanofilm at the glassy carbon surface was obtained as 14.48 ± 0.11 nm. The stability of the SO modified GCE was studied. The SO modified GCE was also utilized for the determination of Cd(II) ions in water samples in the presence of Pb(II) and Fe(II) by adsorptive stripping voltammetry. The linearity range and the detection limit of Cd(II) ions were 1.0 × 10 −10 to 5.0 × 10 −8 M and 3.3 × 10 −11 M (S/N = 3), respectively

Electrochemical Glucose Oxidation Using Glassy Carbon Electrodes Modified with Au-Ag Nanoparticles: Influence of Ag Content

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Nancy Gabriela García-Morales

2015-01-01

Full Text Available This paper describes the application of glassy carbon modified electrodes bearing Aux-Agy nanoparticles to catalyze the electrochemical oxidation of glucose. In particular, the paper shows the influence of the Ag content on this oxidation process. A simple method was applied to prepare the nanoparticles, which were characterized by transmission electron microscopy, Ultraviolet-Visible spectroscopy, X-ray diffraction spectroscopy, and cyclic voltammetry. These nanoparticles were used to modify glassy carbon electrodes. The effectiveness of these electrodes for electrochemical glucose oxidation was evaluated. The modified glassy carbon electrodes are highly sensitive to glucose oxidation in alkaline media, which could be attributed to the presence of Aux-Agy nanoparticles on the electrode surface. The voltammetric results suggest that the glucose oxidation speed is controlled by the glucose diffusion to the electrode surface. These results also show that the catalytic activity of the electrodes depends on the Ag content of the nanoparticles. Best results were obtained for the Au80-Ag20 nanoparticles modified electrode. This electrode could be used for Gluconic acid (GA production.

Adsorptive Stripping Voltammetric Determination of Hydroquinone using an Electrochemically Pretreated Glassy Carbon Electrode

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Abdul Niaz1,

2008-12-01

Full Text Available A simple and efficient adsorptive stripping voltammetric (AdSV method was developed for the determination of hydroquinone at an electrochemically pretreated glassy carbon (GC electrode in waste water. Various parameters such as solvent system, accumulation potential, accumulation time and scan rate were optimized. The electrochemically pretreated GC electrode showed good response towards hydroquinone determination by using AdSV. Under the optimized conditions the peak current showed good linear relationship with the hydroquinone concentration in the range of 0.5-4.0mg L-1 and 5-30mg L-1. The 60/40 methanol/water composition was found to be the best solvent system and 0.05mol L-1 H2SO4 was found as useful supporting electrolyte concentration. The accumulation time was 60 s and the detection limit was 50µg L-1. The developed method was successfully applied for the determination of hydroquinone in polymeric industrial discharge samples waste photographic developer solution and cream sample without any significant effect of surface fouling.

Elastic properties of aspirin in its crystalline and glassy phases studied by micro-Brillouin scattering

Science.gov (United States)

Ko, Jae-Hyeon; Lee, Kwang-Sei; Ike, Yuji; Kojima, Seiji

2008-11-01

The acoustic waves propagating along the direction perpendicular to the (1 0 0) cleavage plane of aspirin crystal were investigated using micro-Brillouin spectroscopy from which C11, C55 and C66 were obtained. The temperature dependence of the longitudinal acoustic waves could be explained by normal anharmonic lattice models, while the transverse acoustic waves showed an abnormal increase in the hypersonic attenuation at low temperatures indicating their coupling to local remnant dynamics. The sound velocity as well as the attenuation of the longitudinal acoustic waves of glassy aspirin showed a substantial change at ˜235 K confirming a transition from glassy to supercooled liquid state in vitreous aspirin.

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

Radiation-induced structural transitions in composite materials with strong interaction of polymer components

International Nuclear Information System (INIS)

Zaikin, Yu.A.; Koztaeva, U.P.

2002-01-01

In earlier papers the internal friction (IF) method was applied to studies of structural relaxation in different types of polymer-based composite materials (glass-cloth, paper-based and foiled laminates impregnated by epoxy and phenolic resins) irradiated by 2 MeV electrons in the dose range of 0.1-50.0 MGy. Selectivity and high sensibility of the internal friction method allowed to distinguish glassy transitions in different structural components of the composites. The relaxation processes observed were identified and attributed to structural alterations in the polymer filler, the binder and the boundary layers. It was shown that changes in the parameters of relaxation maximums during irradiation can be considered as quantitative characteristics for the degree of radiation-induced degradation or cross-linking of polymer molecules. This paper deals with specific features of IF spectra in paper-based laminates where both the filler fibers and the binder are strongly interacting polymers. Anisotropy of viscous and elastic properties is very weak for this kind of materials, so that IF measurements give nearly the same result independently on the filler fiber orientation in the sample. The main reasons for it are the rigid chain structure of fillers (polyethylene-terephthalate and cellulose) and the good adhesion strengthened by diffusion of the epoxy or phenolic binder to defect regions of the filler.The IF temperature dependence observed in paper-based laminates is represented by superposition of two very broad relaxation maximums associated with transitions from glassy to high-elastic state in structural components, each based on one of the polymers. The inflection points characteristic for IF temperature dependence in paper-based laminates give a reason to treat them as a superposition of α-peaks associated with transitions from glassy to high-elastic state in structural components of a composite based on the binder and the filler, respectively. Another

Fabrication of Al-based composites reinforced with in situ devitrified Al{sub 84}Ni{sub 8.4}Y{sub 4.8}La{sub 1.8}Co{sub 1} particles by hot pressing consolidation

Energy Technology Data Exchange (ETDEWEB)

Yang, Qing, E-mail: buaayq00@gmail.com; Zhang, Yitan; Zhang, Haiping; Zheng, Ruixiao; Xiao, Wenlong; Ma, Chaoli, E-mail: machaoli@buaa.edu.cn

2015-11-05

In this study, Al{sub 84}Ni{sub 8.4}Y{sub 4.8}La{sub 1.8}Co{sub 1} particles reinforced Al-based composites were prepared by hot pressing sintering and subsequent hot extrusion. The glassy powders were produced by gas atomization and then employed to mechanical milling. After hot pressing sintering, the nano-scale intermetallic compounds precipitated from metallic glass matrix due to higher temperature than super-cooled liquid region. The mechanical properties of 2024 alloy were improved by addition of glassy particles. The ultimate compressive stress increased from 482 MPa for 2024 alloy to 545 MPa, 627 MPa and 735 MPa for composites with 20 w.t.% 40 w.t.% and 60 w.t.% glassy powders addition, respectively, together with considerable fracture strain ranging between 2.9% and 13.6%. And the mechanical properties could be predicted by using the Rule of Mixture, which predicts the mechanical properties of the bulks from the volume weighed average of the constituent properties. - Highlights: • The composites are fabricate by hot pressing and extrusion. • The single phase of amorphous alloy is obtained by sieving. • The nano-scale compounds precipitates from glassy matrix. • The compressive strength reaches to the value of 735 MPa. • The strength can fit well with rule of mixture.

Highly improved sensing of dopamine by using glassy carbon electrode modified with MnO2, graphene oxide, carbon nanotubes and gold nanoparticles

International Nuclear Information System (INIS)

Rao, Dejiang; Zhang, Xinjin; Sheng, Qinglin; Zheng, Jianbin

2016-01-01

A composite material obtained by ultrasonication of graphene oxide (GO) and multi-walled carbon nanotubes (MWCNTs) was loaded with manganese dioxide (MnO 2 ), poly(diallyldimethylammonium chloride) and gold nanoparticles (AuNPs), and the resulting multilayer hybrid films were deposited on a glassy carbon electrode (GCE). The microstructure, composition and electrochemical behavior of the composite and the modified GCE were characterized by transmission electron microscopy, Raman spectra, energy-dispersive X-ray spectroscopy, electrochemical impedance spectroscopy and cyclic voltammetry. The electrode induces efficient electrocatalytic oxidation of dopamine at a rather low working voltage of 0.22 V (vs. SCE) at neutral pH values. The response is linear in the 0.5 μM to 2.5 mM concentration range, the sensitivity is 233.4 μA·mM -1 ·cm -2 , and the detection limit is 0.17 μM at an SNR of 3. The sensor is well reproducible and stable. It displays high selectivity over ascorbic acid, uric acid and glucose even if these are present in comparable concentrations. (author)

Diazonium Chemistry for the Bio-Functionalization of Glassy Nanostring Resonator Arrays

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Wei Zheng

2015-07-01

Full Text Available Resonant glassy nanostrings have been employed for the detection of biomolecules. These devices offer high sensitivity and amenability to large array integration and multiplexed assays. Such a concept has however been impaired by the lack of stable and biocompatible linker chemistries. Diazonium salt reduction-induced aryl grafting is an aqueous-based process providing strong chemical adhesion. In this work, diazonium-based linker chemistry was performed for the first time on glassy nanostrings, which enabled the bio-functionalization of such devices. Large arrays of nanostrings with ultra-narrow widths down to 10 nm were fabricated employing electron beam lithography. Diazonium modification was first developed on SiCN surfaces and validated by X-ray photoelectron spectroscopy. Similarly modified nanostrings were then covalently functionalized with anti-rabbit IgG as a molecular probe. Specific enumeration of rabbit IgG was successfully performed through observation of downshifts of resonant frequencies. The specificity of this enumeration was confirmed through proper negative control experiments. Helium ion microscopy further verified the successful functionalization of nanostrings.

Diazonium Chemistry for the Bio-Functionalization of Glassy Nanostring Resonator Arrays.

Science.gov (United States)

Zheng, Wei; Du, Rongbing; Cao, Yong; Mohammad, Mohammad A; Dew, Steven K; McDermott, Mark T; Evoy, Stephane

2015-07-30

Resonant glassy nanostrings have been employed for the detection of biomolecules. These devices offer high sensitivity and amenability to large array integration and multiplexed assays. Such a concept has however been impaired by the lack of stable and biocompatible linker chemistries. Diazonium salt reduction-induced aryl grafting is an aqueous-based process providing strong chemical adhesion. In this work, diazonium-based linker chemistry was performed for the first time on glassy nanostrings, which enabled the bio-functionalization of such devices. Large arrays of nanostrings with ultra-narrow widths down to 10 nm were fabricated employing electron beam lithography. Diazonium modification was first developed on SiCN surfaces and validated by X-ray photoelectron spectroscopy. Similarly modified nanostrings were then covalently functionalized with anti-rabbit IgG as a molecular probe. Specific enumeration of rabbit IgG was successfully performed through observation of downshifts of resonant frequencies. The specificity of this enumeration was confirmed through proper negative control experiments. Helium ion microscopy further verified the successful functionalization of nanostrings.

Electro-oxidation nitrite based on copper calcined layered double hydroxide and gold nanoparticles modified glassy carbon electrode

Energy Technology Data Exchange (ETDEWEB)

Cui Lin; Meng Xiaomeng; Xu Minrong; Shang Kun [College of Chemistry and Material Science, Shandong Agricultural University, Taian 271018, Shandong (China); Ai Shiyun, E-mail: ashy@sdau.edu.cn [College of Chemistry and Material Science, Shandong Agricultural University, Taian 271018, Shandong (China); Liu Yinping [College of Chemistry and Material Science, Shandong Agricultural University, Taian 271018, Shandong (China)

2011-11-30

Highlights: > A nitrite sensor fabricated based on copper calcined layered double hydroxides and gold nanoparticles modified electrode. > This sensor exhibited excellent electrocatalytic oxidation to nitrite. > This nitrite sensor exhibited very good analytical performance with low cost, convenient preparation and rapid detection. - Abstract: In this paper, a novel nitrite sensor was constructed based on electrodeposition of gold nanoparticles (AuNPs) on a copper calcined layered double hydroxide (Cu-CLDH) modified glassy carbon electrode. Electrochemical experiments showed that AuNPs/CLDH composite film exhibited excellent electrocatalytic oxidation activity with nitrite due to the synergistic effect of the Cu-CLDH with AuNPs. The fabricated sensor exhibited excellent performance for nitrite detection within a wide concentration interval of 1-191 {mu}M and with a detection limit of 0.5 {mu}M. The superior electrocatalytic response to nitrite was mainly attributed to the large surface area, minimized diffusion resistance, and enhanced electron transfer of the Cu-CLDH and AuNPs composition film. This platform offers a novel route for nitrite sensing with wide analytical applications and will supply the practical applications for a variety of simple, robust, and easy-to-manufacture analytical approaches in the future.

Electro-oxidation nitrite based on copper calcined layered double hydroxide and gold nanoparticles modified glassy carbon electrode

International Nuclear Information System (INIS)

Cui Lin; Meng Xiaomeng; Xu Minrong; Shang Kun; Ai Shiyun; Liu Yinping

2011-01-01

Highlights: → A nitrite sensor fabricated based on copper calcined layered double hydroxides and gold nanoparticles modified electrode. → This sensor exhibited excellent electrocatalytic oxidation to nitrite. → This nitrite sensor exhibited very good analytical performance with low cost, convenient preparation and rapid detection. - Abstract: In this paper, a novel nitrite sensor was constructed based on electrodeposition of gold nanoparticles (AuNPs) on a copper calcined layered double hydroxide (Cu-CLDH) modified glassy carbon electrode. Electrochemical experiments showed that AuNPs/CLDH composite film exhibited excellent electrocatalytic oxidation activity with nitrite due to the synergistic effect of the Cu-CLDH with AuNPs. The fabricated sensor exhibited excellent performance for nitrite detection within a wide concentration interval of 1-191 μM and with a detection limit of 0.5 μM. The superior electrocatalytic response to nitrite was mainly attributed to the large surface area, minimized diffusion resistance, and enhanced electron transfer of the Cu-CLDH and AuNPs composition film. This platform offers a novel route for nitrite sensing with wide analytical applications and will supply the practical applications for a variety of simple, robust, and easy-to-manufacture analytical approaches in the future.

Dynamics and Geometry of Icosahedral Order in Liquid and Glassy Phases of Metallic Glasses

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Masato Shimono

2015-07-01

Full Text Available The geometrical properties of the icosahedral ordered structure formed in liquid and glassy phases of metallic glasses are investigated by using molecular dynamics simulations. We investigate the Zr-Cu alloy system as well as a simple model for binary alloys, in which we can change the atomic size ratio between alloying components. In both cases, we found the same nature of icosahedral order in liquid and glassy phases. The icosahedral clusters are observed in liquid phases as well as in glassy phases. As the temperature approaches to the glass transition point Tg, the density of the clusters rapidly grows and the icosahedral clusters begin to connect to each other and form a medium-range network structure. By investigating the geometry of connection between clusters in the icosahedral network, we found that the dominant connecting pattern is the one sharing seven atoms which forms a pentagonal bicap with five-fold symmetry. From a geometrical point of view, we can understand the mechanism of the formation and growth of the icosahedral order by using the Regge calculus, which is originally employed to formulate a theory of gravity. The Regge calculus tells us that the distortion energy of the pentagonal bicap could be decreased by introducing an atomic size difference between alloying elements and that the icosahedral network would be stabilized by a considerably large atomic size difference.

"Non-equilibrium" block copolymer micelles with glassy cores: a predictive approach based on theory of equilibrium micelles.

Science.gov (United States)

Nagarajan, Ramanathan

2015-07-01

Micelles generated in water from most amphiphilic block copolymers are widely recognized to be non-equilibrium structures. Typically, the micelles are prepared by a kinetic process, first allowing molecular scale dissolution of the block copolymer in a common solvent that likes both the blocks and then gradually replacing the common solvent by water to promote the hydrophobic blocks to aggregate and create the micelles. The non-equilibrium nature of the micelle originates from the fact that dynamic exchange between the block copolymer molecules in the micelle and the singly dispersed block copolymer molecules in water is suppressed, because of the glassy nature of the core forming polymer block and/or its very large hydrophobicity. Although most amphiphilic block copolymers generate such non-equilibrium micelles, no theoretical approach to a priori predict the micelle characteristics currently exists. In this work, we propose a predictive approach for non-equilibrium micelles with glassy cores by applying the equilibrium theory of micelles in two steps. In the first, we calculate the properties of micelles formed in the mixed solvent while true equilibrium prevails, until the micelle core becomes glassy. In the second step, we freeze the micelle aggregation number at this glassy state and calculate the corona dimension from the equilibrium theory of micelles. The condition when the micelle core becomes glassy is independently determined from a statistical thermodynamic treatment of diluent effect on polymer glass transition temperature. The predictions based on this "non-equilibrium" model compare reasonably well with experimental data for polystyrene-polyethylene oxide diblock copolymer, which is the most extensively studied system in the literature. In contrast, the application of the equilibrium model to describe such a system significantly overpredicts the micelle core and corona dimensions and the aggregation number. The non-equilibrium model suggests ways to

A neutron-X-ray, NMR and calorimetric study of glassy Probucol synthesized using containerless techniques

International Nuclear Information System (INIS)

Weber, J.K.R.; Benmore, C.J.; Tailor, A.N.; Tumber, S.K.; Neuefeind, J.; Cherry, B.; Yarger, J.L.; Mou, Q.; Weber, W.; Byrn, S.R.

2013-01-01

Highlights: • Acoustic levitation was used to make phase-pure glassy forms of pharmaceutical compounds. • Neutrons, X-rays and NMR were used to characterize the glasses. • The glass comprised of slightly distorted molecules packed in a random network. • Potential for new drug synthesis routes is discussed. - Abstract: Acoustic levitation was used to trap 1–3 mm diameter drops of Probucol and other pharmaceutical materials in containerless conditions. Samples were studied in situ using X-ray diffraction and ex situ using neutron diffraction, NMR and DSC techniques. The materials were brought into non-equilibrium states by supersaturating solutions or by supercooling melts. The glass transition and crystallization temperatures of glassy Probucol were 29 ± 1 and 71 ± 1 °C respectively. The glassy form was stable with a shelf life of at least 8 months. A neutron/X-ray difference function of the glass showed that while molecular sub-groups remain rigid, many of the hydrogen correlations observed in the crystal become smeared out in the disordered material. The glass is principally comprised of slightly distorted Form I Probucol molecules with disordered packing rather than large changes in the individual molecular structure. Avoiding surface contact-induced nucleation provided access to highly non-equilibrium phases and enabled synthesis of phase-pure glasses

A neutron-X-ray, NMR and calorimetric study of glassy Probucol synthesized using containerless techniques

Energy Technology Data Exchange (ETDEWEB)

Weber, J.K.R., E-mail: rweber@anl.gov [Materials Development, Inc., Arlington Heights, IL 60004 (United States); Argonne National Laboratory, Argonne, IL 60439 (United States); Benmore, C.J. [Argonne National Laboratory, Argonne, IL 60439 (United States); Department of Physics, Arizona State University, AZ 85287 (United States); Tailor, A.N.; Tumber, S.K. [Materials Development, Inc., Arlington Heights, IL 60004 (United States); Neuefeind, J. [Oak Ridge National Laboratory, Oak Ridge, TN 37831 (United States); Cherry, B. [Magnetic Resonance Research Center, Arizona State University, AZ 85287 (United States); Department of Chemistry and Biochemistry, Arizona State University, AZ 85287 (United States); Yarger, J.L. [Department of Physics, Arizona State University, AZ 85287 (United States); Magnetic Resonance Research Center, Arizona State University, AZ 85287 (United States); Department of Chemistry and Biochemistry, Arizona State University, AZ 85287 (United States); Mou, Q. [Magnetic Resonance Research Center, Arizona State University, AZ 85287 (United States); Department of Chemistry and Biochemistry, Arizona State University, AZ 85287 (United States); Weber, W. [Department of Physics, Arizona State University, AZ 85287 (United States); Department of Chemistry and Biochemistry, Arizona State University, AZ 85287 (United States); Byrn, S.R. [Department of Industrial and Physical Pharmacy, Purdue University, IN 47907 (United States)

2013-10-16

Highlights: • Acoustic levitation was used to make phase-pure glassy forms of pharmaceutical compounds. • Neutrons, X-rays and NMR were used to characterize the glasses. • The glass comprised of slightly distorted molecules packed in a random network. • Potential for new drug synthesis routes is discussed. - Abstract: Acoustic levitation was used to trap 1–3 mm diameter drops of Probucol and other pharmaceutical materials in containerless conditions. Samples were studied in situ using X-ray diffraction and ex situ using neutron diffraction, NMR and DSC techniques. The materials were brought into non-equilibrium states by supersaturating solutions or by supercooling melts. The glass transition and crystallization temperatures of glassy Probucol were 29 ± 1 and 71 ± 1 °C respectively. The glassy form was stable with a shelf life of at least 8 months. A neutron/X-ray difference function of the glass showed that while molecular sub-groups remain rigid, many of the hydrogen correlations observed in the crystal become smeared out in the disordered material. The glass is principally comprised of slightly distorted Form I Probucol molecules with disordered packing rather than large changes in the individual molecular structure. Avoiding surface contact-induced nucleation provided access to highly non-equilibrium phases and enabled synthesis of phase-pure glasses.

Violation of the fluctuation-dissipation theorem in glassy systems: basic notions and the numerical evidence

International Nuclear Information System (INIS)

Crisanti, A; Ritort, F

2003-01-01

This review reports on the research done during past years on violations of the fluctuation-dissipation theorem (FDT) in glassy systems. It is focused on the existence of a quasi-fluctuation-dissipation theorem (QFDT) in glassy systems and the current supporting knowledge gained from numerical simulation studies. It covers a broad range of non-stationary aging and stationary driven systems such as structural glasses, spin glasses, coarsening systems, ferromagnetic models at criticality, trap models, models with entropy barriers, kinetically constrained models, sheared systems and granular media. The review is divided into four main parts: (1) an introductory section explaining basic notions related to the existence of the FDT in equilibrium and its possible extension to the glassy regime (QFDT), (2) a description of the basic analytical tools and results derived in the framework of some exactly solvable models, (3) a detailed report of the current evidence in favour of the QFDT and (4) a brief digression on the experimental evidence in its favour. This review is intended for inexpert readers who want to learn about the basic notions and concepts related to the existence of the QFDT as well as for the more expert readers who may be interested in more specific results. (topical review)

Deposition of lead-silicate glassy thin coatings by RF magnetron sputtering: Correlation between deposition parameters and electrical and structural properties

International Nuclear Information System (INIS)

Rigato, V.; Maggioni, G.; Boscarino, D.; Della Mea, G.; Univ. di Trento, Mesiano

1996-01-01

Lead-silicate glassy thin films produced by means of Reactive Radio Frequency Magnetron Sputtering have found recent application in the development of MicroStrip Gas Chambers radiation detectors. Here, thin films (100--400 nm) of lead silicate glass have been deposited by RF magnetron sputtering in Ar plasma at different discharge conditions. The interaction of the sputtered species with the gas atoms during the transport process through the discharge region and the kinetics of growth of the films have been investigated as a function of the target composition and of the substrate temperature. This study demonstrates the possibility of controlling the surface electrical resistance of the films in a wide range of values ranging from 10 12 to 10 17 Ω/□ during the film growth

Topological structure and mechanics of glassy polymer networks.

Science.gov (United States)

Elder, Robert M; Sirk, Timothy W

2017-11-22

The influence of chain-level network architecture (i.e., topology) on mechanics was explored for unentangled polymer networks using a blend of coarse-grained molecular simulations and graph-theoretic concepts. A simple extension of the Watts-Strogatz model is proposed to control the graph properties of the network such that the corresponding physical properties can be studied with simulations. The architecture of polymer networks assembled with a dynamic curing approach were compared with the extended Watts-Strogatz model, and found to agree surprisingly well. The final cured structures of the dynamically-assembled networks were nearly an intermediate between lattice and random connections due to restrictions imposed by the finite length of the chains. Further, the uni-axial stress response, character of the bond breaking, and non-affine displacements of fully-cured glassy networks were analyzed as a function of the degree of disorder in the network architecture. It is shown that the architecture strongly affects the network stability, flow stress, onset of bond breaking, and ultimate stress while leaving the modulus and yield point nearly unchanged. The results show that internal restrictions imposed by the network architecture alter the chain-level response through changes to the crosslink dynamics in the flow regime and through the degree of coordinated chain failure at the ultimate stress. The properties considered here are shown to be sensitive to even incremental changes to the architecture and, therefore, the overall network architecture, beyond simple defects, is predicted to be a meaningful physical parameter in the mechanics of glassy polymer networks.

Read/write characteristics of a new type of bit-patterned-media using nano-patterned glassy alloy

International Nuclear Information System (INIS)

Takenaka, Kana; Saidoh, Noriko; Nishiyama, Nobuyuki; Ishimaru, Manabu; Futamoto, Masaaki; Inoue, Akihisa

2012-01-01

The paper reports a feasibility study of new type bit-patterned-media using a nano-patterned glassy alloy template for ultra-high density hard disk applications. The prototype bit-patterned-media was prepared using a nano-hole array pattern fabricated on a Pd-based glassy alloy thin film and a Co/Pd multilayered film filled in the nano-holes. The prepared prototype bit-patterned-media had a smooth surface and isolated Co/Pd multilayer magnetic dots, where the average dot diameter, the average dot pitch and the average dot height were 30, 60 and 19 nm, respectively. MFM (magnetic force microscope) observation revealed that each dot was magnetized in a perpendicular direction and the magnetization could reverse when an opposite magnetic field was applied. Static read/write tester measurements showed that repeated writing and reading on isolated magnetic dots were possible in combination with conventional magnetic heads and high-accuracy positioning technologies. The present study indicates that the new type of bit-patterned-media composed of nano-hole arrays fabricated on glassy alloy film template and Co/Pd multilayer magnetic dots are promising for applications to next generation ultra-high density hard disk drives. - Highlights: ► Prototype BPM using a nano-hole array pattern of imprinted Pd-based glassy alloy thin film and Co/Pd multilayered film was set. ► The prototype BPM has smooth surface and isolated Co/Pd multilayer magnetic dots with an average dot diameter of 30 nm. ► Dots acted as perpendicular magnetic dot and were able to read, erase and write in a row by a usual perpendicular magnetic head.

Effect of high-order multicomponent on formation and properties of Zr-based bulk glassy alloys

Energy Technology Data Exchange (ETDEWEB)

Inoue, A., E-mail: ainouebmg@yahoo.co.jp [International Institute of Green Materials, Josai International University, Togane 283-8555 (Japan); School of Materials Science and Engineering, Tianjin University, Tianjin 300072 (China); Department of Physics, King Abdulaziz University, Jeddah 22254 (Saudi Arabia); Wang, Z.; Louzguine-Luzgin, D.V. [WPI Advanced Institute for Materials Research, Tohoku University, Sendai 980-8577 (Japan); Han, Y. [School of Materials Science and Engineering, Tianjin University, Tianjin 300072 (China); Kong, F.L. [International Institute of Green Materials, Josai International University, Togane 283-8555 (Japan); Shalaan, E.; Al-Marzouki, F. [Department of Physics, King Abdulaziz University, Jeddah 22254 (Saudi Arabia)

2015-07-25

Highlights: • A multicomponent Zr{sub 55}Al{sub 10}Fe{sub 6}Co{sub 6}Ni{sub 6}Cu{sub 6}Pd{sub 6}Ag{sub 5} bulk glassy alloy was formed. • The high-order multiplication suppression of the decrease in mechanical strength. • The BGAs show good corrosion resistance and slow growth rate of primary precipitates. - Abstract: We examined the formation, thermal stability, mechanical properties and corrosion behavior of a multicomponent Zr{sub 55}Al{sub 10}Fe{sub 6}Co{sub 6}Ni{sub 6}Cu{sub 6}Pd{sub 6}Ag{sub 5} bulk glassy alloy, with the aim of clarifying the effect of high-order multiplication of the number of components on their properties. The bulk glassy alloy rods of 2 and 6 mm in diameter were formed by suction casting even at the low total content of typical glass-forming 3-d late transition metals like Co, Ni and Cu. The Vickers hardness is different in the center region and in the outer surface region. The difference seems to reflect the relaxation level of glassy structure. The Young’s modulus and the compressive fracture strength are nearly the same for the base Zr{sub 55}Al{sub 10}Ni{sub 5}Cu{sub 30} alloy in spite of the existence of immiscible atomic pairs. Moreover, the multicomponent alloy exhibits better corrosion resistance than that for the base alloy. The glassy phase changes to a supercooled liquid state at 720 K and then starts to crystallize at 754 K with a single exothermic peak, in contrast to the appearance of a wide supercooled liquid region for the base alloy. The primary crystalline phase precipitates with very short incubation time and very low growth rate, which are different from those for the base alloy. The extremely low growth rate of the crystallites is presumably due to the reduction of diffusivity of late transition metal elements resulting from multiplication. Thus, the high-order multiplication has the features of (1) the maintenance of high glass-forming ability even at the lower Co, Ni and Cu content and in the absence of

Evolution of Shock Melt Compositions in Lunar Regoliths

Science.gov (United States)

Vance, A. M.; Christoffersen, R.; Keller, L. P.; Berger, E. L.; Noble, S. K.

2016-01-01

Space weathering processes - driven primarily by solar wind ion and micrometeorite bombardment, are constantly changing the surface regoliths of airless bodies, such as the Moon. It is essential to study lunar soils in order to fully under-stand the processes of space weathering, and how they alter the optical reflectance spectral properties of the lunar surface relative to bedrock. Lunar agglutinates are aggregates of regolith grains fused together in a glassy matrix of shock melt produced during micrometeorite impacts into the lunar regolith. The formation of the shock melt component in agglutinates involves reduction of Fe in the target material to generate nm-scale spherules of metallic Fe (nanophase Fe0 or npFe0). The ratio of elemental Fe, in the form of npFe0, to FeO in a given bulk soil indicates its maturity, which increases with length of surface exposure as well as being typically higher in the finer-size fraction of soils. The melting and mixing process in agglutinate formation remain poorly understood. This includes incomplete knowledge regarding how the homogeneity and overall compositional trends of the agglutinate glass portions (agglutinitic glass) evolve with maturity. The aim of this study is to use sub-micrometer scale X-ray compositional mapping and image analysis to quantify the chemical homogeneity of agglutinitic glass, correlate its homogeneity to its parent soil maturity, and identify the principal chemical components contributing to the shock melt composition variations. An additional focus is to see if agglutinitic glass contains anomalously high Fe sub-micron scale compositional domains similar to those recently reported in glassy patina coatings on lunar rocks.

Cap casting and enveloped casting techniques for Zr55Cu30Ni5Al10 glassy alloy rod with 32 mm in diameter

International Nuclear Information System (INIS)

Yokoyama, Yoshihiko; Inoue, Akihisa; Mund, Enrico; Schultz, Ludwig

2009-01-01

In order to produce centimetre-sized bulk glassy alloys (BMGs), various cast techniques have been developed. We succeed in the development of cap casting and enveloped casting technique to accomplish the fabrication of centimetre sized BMGs. The former has an advantage to increase cooling rate and the later has an advantage to joint another materials instead of welding. This paper presents the production of a glassy Zr 55 Cu 30 Ni 5 Al 10 alloy rod with a diameter of 32 mm and joined glassy Zr 55 Cu 30 Ni 5 Al 10 alloy parts with another materials for industrial applications.

Self-organized nickel nanoparticles on nanostructured silicon substrate intermediated by a titanium oxynitride (TiNxOy) interface

Science.gov (United States)

Morales, M.; Droppa, R., Jr.; de Mello, S. R. S.; Figueroa, C. A.; Zanatta, A. R.; Alvarez, F.

2018-01-01

In this work we report an experimental approach by combining in situ sequential top-down and bottom-up processes to induce the organization of nanosized nickel particles. The top-down process consists in xenon ion bombardment of a crystalline silicon substrate to generate a pattern, followed by depositing a ˜15 nm titanium oxynitride thin film to act as a metallic diffusion barrier. Then, metallic nanoparticles are deposited by argon ion sputtering a pure nickel target, and the sample is annealed to promote the organization of the nickel nanoparticles (a bottom-up process). According to the experimental results, the surface pattern and the substrate biaxial surface strain are the driving forces behind the alignment and organization of the nickel nanoparticles. Moreover, the ratio between the F of metallic atoms arriving at the substrate relative to its surface diffusion mobility determines the nucleation regime of the nickel nanoparticles. These features are presented and discussed considering the existing technical literature on the subject.

Different glassy states, as indicated by a violation of the generalized Cauchy relation

Energy Technology Data Exchange (ETDEWEB)

Krueger, J K [Laboratoire Europeen de Recherche Universitaire Saarland-Lorraine (LERUSL), Universitaet des Saarlandes, Fakultaet fuer Physik und Elektrotechnik 7.2, Gebaeude 38, D-66041 Saarbruecken (Germany); Britz, T [Laboratoire Europeen de Recherche Universitaire Saarland-Lorraine (LERUSL), Universitaet des Saarlandes, Fakultaet fuer Physik und Elektrotechnik 7.2, Gebaeude 38, D-66041 Saarbruecken (Germany); Coutre, A le [Laboratoire Europeen de Recherche Universitaire Saarland-Lorraine (LERUSL), Universitaet des Saarlandes, Fakultaet fuer Physik und Elektrotechnik 7.2, Gebaeude 38, D-66041 Saarbruecken (Germany); Baller, J [Laboratoire Europeen de Recherche Universitaire Saarland-Lorraine (LERUSL), Universitaet des Saarlandes, Fakultaet fuer Physik und Elektrotechnik 7.2, Gebaeude 38, D-66041 Saarbruecken (Germany); Possart, W [Universitaet des Saarlandes, Fakultaet fuer Chemie, Pharmazie und Werkstoffwissenschaften 8.15, Gebaeude 22, D-66041 Saarbruecken (Germany); Alnot, P [Laboratoire Europeen de Recherche Universitaire Saarland-Lorraine (LERUSL), Universitaet des Saarlandes, Fakultaet fuer Physik und Elektrotechnik 7.2, Gebaeude 38, D-66041 Saarbruecken (Germany); Sanctuary, R [Centre Universitaire de Luxembourg, Departement des Sciences, Laboratoire 1.19, 162a Avenue de la Faiencerie, L-1511, Luxembourg (Luxembourg)

2003-07-01

Using Brillouin spectroscopy as a probe for high-frequency clamped acoustic properties, a shear modulus c{sub 44}{sup {infinity}} can be measured in addition to the longitudinal modulus c{sub 11}{sup {infinity}} already well above the thermal glass transition. On slow cooling of the liquid through the thermal glass transition temperature T{sub g}, both moduli show a kink-like behaviour and the function c{sub 11}{sup {infinity}} = c{sub 11}{sup {infinity}}(c{sub 44}{sup {infinity}}) follows a generalized Cauchy relation (gCR) defined by the linear relation c{sub 11}{sup {infinity}} = 3c{sub 44}{sup {infinity}} + constant, which completely hides the glass transition. In this work we show experimentally that on fast cooling this linear transformation becomes violated within the glassy state, but that thermal ageing drives the elastic coefficients towards the gCR, i.e. towards a unique glassy state.

Luminescent properties of the potassium zinc phosphates of composition K1-xTlxZn(PO3)3

International Nuclear Information System (INIS)

El Abiad, A.; Mesnaoui, M.; Maazaz, M.; Parent, C.; Le Flem, G.

2003-01-01

Crystalline and glassy K 1-x Tl x Zn(PO 3 ) 3 polyphosphates have been synthesized and characterized. UV-visible spectroscopy was systematically used in order to analyze the optical properties of Tl + ions both in crystalline and glassy forms with the similar compositions. The investigated polyphosphates can be considered as a model system since the spectroscopic properties of Tl + ions in the glasses could be deduced by comparison with those in crystals. From structural point of view, in the crystalline forms the thallium ions are six-fold coordinated in a dissymmetrical oxygenated sites. Three luminescences (α, A X , A T ) have been then observed and were attributed to the isolated Tl + ions. In the glassy forms, an additional luminescence (D) has been detected in the low-energy range and was assigned to the Tl + pairs formation. The relationship between the Tl + site symmetry and its optical properties is discussed in the context of the Fukuda's model

Characterization of cell lines developed from the glassy-winged sharpshooter, Homalodisca coagulata (Hemiptera: Cicadellidae).

Science.gov (United States)

Kamita, Shizuo G; Do, Zung N; Samra, Aman I; Hagler, James R; Hammock, Bruce D

2005-01-01

Four continuous cell lines were established from the embryos of the glassy-winged sharpshooter, Homalodisca coagulata (Say), an economically important insect vector of bacterial pathogens of grape, almond, citrus, oleander, and other agricultural and ornamental plantings. The cell lines were designated GWSS-Z10, GWSS-Z15, GWSS-G3, and GWSS-LH. The GWSS-Z10, GWSS-Z15, and GWSS-G3 lines were cultured in Ex-Cell 401 medium supplemented with 10% fetal bovine serum (FBS), whereas the GWSS-LH line was cultured in LH medium supplemented with 20% FBS. The cell lines were characterized in terms of their morphology, growth, protein composition, and polymerase chain reaction- amplification patterns of their chromosomal deoxyribonucleic acid. The population doubling times of GWSS-Z10, GWSS-Z15, GWSS-G3, and GWSS-LH were 46.2, 90.9, 100.3, and 60.2 h, respectively. These lines should be useful for the study of insect-pathogenic viruses of leafhoppers, aphids, treehoppers, and other related insects as well as plant-pathogenic viruses that are transmitted by these insects.

Dielectric relaxation in glassy Se75In25−xPbx alloys

Indian Academy of Sciences (India)

to their atomic percentages and were sealed in quartz ampoules (length ~5 cm and internal dia. ~8 mm) in vacuum ... samples were taken out by breaking the quartz ampoules. The glassy nature of the ... measured with the help of a calibrated copper–constantan thermocouple mounted very near to the sample, which could ...

Dynamical singularities of glassy systems in a quantum quench.

Science.gov (United States)

Obuchi, Tomoyuki; Takahashi, Kazutaka

2012-11-01

We present a prototype of behavior of glassy systems driven by quantum dynamics in a quenching protocol by analyzing the random energy model in a transverse field. We calculate several types of dynamical quantum amplitude and find a freezing transition at some critical time. The behavior is understood by the partition-function zeros in the complex temperature plane. We discuss the properties of the freezing phase as a dynamical chaotic phase, which are contrasted to those of the spin-glass phase in the static system.

Gas Permeation Related to the Moisture Sorption in Films of Glassy Hydrophilic Polymers

NARCIS (Netherlands)

Laksmana, F. L.; Kok, P. J. A. Hartman; Frijlink, H. W.; Vromans, H.; Maarschalk, K. Van Der Voort

2010-01-01

The purpose of this article is to elucidate the effect of integral sorption of moisture on gas permeation in glassy hydrophilic polymers. The oxygen and the simultaneous moisture sorption into various hydroxypropyl methylcellulose (HPMC) films were measured under a wide range of relative humidities

A TPD-MS study of glassy carbon surfaces oxidized by CO2 and O2

Directory of Open Access Journals (Sweden)

MILA D. LAUSEVIC

2002-11-01

Full Text Available The temperature-programmed desorption (TPD method combined with mass spectrometric (MS analysis has been applied to investigate the surface properties of carbon materials. The apparatus consisting of a temperature-programmed furnace and a quadrupole mass spectrometer was constructed in order to characterize the surface of differently treated glassy carbon samples. In this work, samples of glassy carbon exposed to air, CO2 and O2 were examined. The desorption of H2O, CO and CO2, as major products, indicated the presence of different oxide groups. The amount of these groups for all samples was calculated. It is concluded that oxidation affects the nature and the amount of the surface oxide groups and contributes to their increased stability.

Novel electroanalysis of hydroxyurea at glassy carbon and gold electrode surfaces

Directory of Open Access Journals (Sweden)

Keerti M. Naik

2014-09-01

Full Text Available A simple and a novel electroanalysis of hydroxyurea (HU drug at glassy carbon and gold electrode was investigated for the first time using cyclic, linear sweep and differential pulse voltammetric techniques. The oxidation of HU was irreversible and exhibited a diffusion controlled process on both electrodes. The oxidation mechanism was proposed. The dependence of the current on pH, the concentration, nature of buffer, and scan rate was investigated to optimize the experimental conditions for the determination of HU. It was found that the optimum buffer pH was 7.0, a physiological pH. In the range of 0.01 to 1.0 mM, the current measured by differential pulse voltammetry showed a linear relationship with HU concentration with limit of detection of 0.46 µM for glassy carbon electrode and 0.92 µM for gold electrode. In addition, reproducibility, precision and accuracy of the method were checked as well. The developed method was successfully applied to HU determination in pharmaceutical formulation and human biological fluids. The method finds its applications in quality control laboratories and pharmacokinetics.

Two-phase quasi-equilibrium in β-type Ti-based bulk metallic glass composites

Science.gov (United States)

Zhang, L.; Pauly, S.; Tang, M. Q.; Eckert, J.; Zhang, H. F.

2016-01-01

The microstructural evolution of cast Ti/Zr-based bulk metallic glass composites (BMGCs) containing β-Ti still remains ambiguous. This is why to date the strategies and alloys suitable for producing such BMGCs with precisely controllable volume fractions and crystallite sizes are still rather limited. In this work, a Ti-based BMGC containing β-Ti was developed in the Ti-Zr-Cu-Co-Be system. The glassy matrix of this BMGC possesses an exceptional glass-forming ability and as a consequence, the volume fractions as well as the composition of the β-Ti dendrites remain constant over a wide range of cooling rates. This finding can be explained in terms of a two-phase quasi-equilibrium between the supercooled liquid and β-Ti, which the system attains on cooling. The two-phase quasi-equilibrium allows predicting the crystalline and glassy volume fractions by means of the lever rule and we succeeded in reproducing these values by slight variations in the alloy composition at a fixed cooling rate. The two-phase quasi-equilibrium could be of critical importance for understanding and designing the microstructures of BMGCs containing the β-phase. Its implications on the nucleation and growth of the crystalline phase are elaborated. PMID:26754315

Gold nanoparticle/multi-walled carbon nanotube modified glassy carbon electrode as a sensitive voltammetric sensor for the determination of diclofenac sodium.

Science.gov (United States)

Afkhami, Abbas; Bahiraei, Atousa; Madrakian, Tayyebeh

2016-02-01

A simple and highly sensitive sensor for the determination of diclofenac sodium based on gold nanoparticle/multi-walled carbon nanotube modified glassy carbon electrode is reported. Scanning electron microscopy along with energy dispersive X-ray spectroscopy, electrochemical impedance spectroscopy, cyclic voltammetry and square wave voltammetry was used to characterize the nanostructure and performance of the sensor and the results were compared with those obtained at the multi-walled carbon nanotube modified glassy carbon electrode and bare glassy carbon electrode. Under the optimized experimental conditions diclofenac sodium gave linear response over the range of 0.03-200μmolL(-1). The lower detection limits were found to be 0.02μmolL(-1). The effect of common interferences on the current response of DS was investigated. The practical application of the modified electrode was demonstrated by measuring the concentration of diclofenac sodium in urine and pharmaceutical samples. This revealed that the gold nanoparticle/multiwalled carbon nanotube modified glassy carbon electrode shows excellent analytical performance for the determination of diclofenac sodium in terms of a very low detection limit, high sensitivity, very good accuracy, repeatability and reproducibility. Copyright © 2015 Elsevier B.V. All rights reserved.

New model system in radiation cryochemistry. Hyperquenched glassy water

International Nuclear Information System (INIS)

Plonka, A.

1998-01-01

Complete text of publication follows. Since the radical generated by high-energy irradiation of liquid water are short-lived at ambient temperature, they are often studied at cryogenic temperatures after irradiating either crystalline ice or highly concentrated aqueous electrolyte solution glasses. While these studies provided a wealth of information, they also bear disadvantages in that further reactions of these radicals may not be those occurring in liquid water because of formation of other radicals from the solute in the case of the electrolyte solution glass and/or perturbation of the water structure by the solute. Furthermore, in slow-cooled aqueous solutions where ice is formed and phase separation of the solute occurs, the radicals trapped in the ice compartments are unable to interact with solutes because these are dissolved in the 'freeze-concentration' regions. These problems can in principle be overcome by investigating water and dilute aqueous solutions in their glassy states which can be obtained by rapid quenching of the liquids. Glassy water can now routinely be made in gram-quantities by so-called 'hyperquenching' of micrometer-sized water droplets on a solid cryoplate. The cooling rates are of the order of 10 6 - 10 7 K s -1 . Our results show that indeed in the hyperquenched dilute aqueous solutions there is no problem with phase separation and radiolysis of hyperquenched water is quite distinct from radiolysis of polycrystalline ice obtained from liquid water quenched in the liquid nitrogen

Studies on Photodarkening Effect in Glassy As2S3 Using High Field NMR

Science.gov (United States)

Hari, Parameswar; Su, Tining; Taylor, Craig; Reyes, Arneil; Kuhns, Phil; Moulton, William; Sullivan, N. S.

2001-03-01

Photodarkening, or the shift of the optical absorption edge to smaller energies after excitation with light whose energy is near that of the optical band edge, has been studied in many chalcogenide glasses for many years. Recently we have conducted nuclear magnetic resonance (NMR) studies of 75As in glassy As2S3 at 17T . We compared the 75As NMR lineshape in glassy As2S3 before and after irradiation at 77K. After irradiation at 514.5 nm for 230 hours with 170 mW/cm2 there is a subtle change in the NMR lineshape. This change is reversible on annealing at 200 C for 1.75 hours. We will discuss the implications of this result based on NMR lineshape analysis using an exact solution of the spin 3/2 Hamiltonian

Nitric Oxide Detection with Glassy Carbon Electrodes Coated with Charge-different Polymer Films

Directory of Open Access Journals (Sweden)

Jianping Lei

2005-04-01

Full Text Available Trace amounts of nitric oxide (NO have been determined in aqueous phosphate buffersolutions (pH=7.4 by using a glassy carbon electrode coated with three charge-different polymerfilms. The glassy carbon electrode was coated first with negatively charged Nafion film containingtetrakis(pentafluorophenylporphyrin iron(III chloride (Fe(IIITPFPP as the NO oxidation catalyst,and then with positively charged poly(acrylamide-co-diallyldimethylammonium chloride (PADDAand with neutral poly(dimethylsiloxane (silicone at the outermost layer. This polymer-coatedelectrode showed an excellent selectivity towards NO against possible concomitants in blood such asnitrite, ascorbic acid, uric acid, and dopamine. All current ratios between each concomitant and NOat the cyclic voltammogram was in 10-3 ~ 10-4. This type of electrode showed a detection limit of80 nM for NO. It was speculated from the electrochemical study in methanol that high-valent oxoiron(IV of Fe(TPFPP participated in the catalytic oxidation of NO.

Calix[6]arene mono-diazonium salt synthesis and covalent immobilization onto glassy carbon electrodes

International Nuclear Information System (INIS)

Cannizzo, Caroline; Jasmin, Jean-Philippe; Vautrin-Ul, Christine; Chausse, Annie; Wagner, Mathieu; Doizi, Denis; Lamouroux, Christine

2014-01-01

This Letter describes the fast synthesis of a mono-aminated calix[6]arene. The immobilization of this macrocycle onto glassy carbon electrodes via diazonium salt chemistry and the electrochemical characterization of the grafted organic layer are also reported. (authors)

Positronics of radiation-induced effects in chalcogenide glassy semiconductors

International Nuclear Information System (INIS)

Shpotyuk, O.; Kozyukhin, S. A.; Shpotyuk, M.; Ingram, A.; Szatanik, R.

2015-01-01

Using As 2 S 3 and AsS 2 glasses as an example, the principal possibility of using positron annihilation spectroscopy methods for studying the evolution of the free volume of hollow nanoobjects in chalcogenide glassy semiconductors exposed to radiation is shown. The results obtained by measurements of the positron annihilation lifetime and Doppler broadening of the annihilation line in reverse chronological order are in full agreement with the optical spectroscopy data in the region of the fundamental absorption edge, being adequately described within coordination defect-formation and physical-aging models

Positronics of radiation-induced effects in chalcogenide glassy semiconductors

Energy Technology Data Exchange (ETDEWEB)

Shpotyuk, O. [Scientific Research Company “Carat” (Ukraine); Kozyukhin, S. A., E-mail: sergkoz@igic.ras.ru [Russian Academy of Sciences, Kurnakov Institute of General and Inorganic Chemistry (Russian Federation); Shpotyuk, M. [Scientific Research Company “Carat” (Ukraine); Ingram, A. [Opole Technical University (Poland); Szatanik, R. [Opole University (Poland)

2015-03-15

Using As{sub 2}S{sub 3} and AsS{sub 2} glasses as an example, the principal possibility of using positron annihilation spectroscopy methods for studying the evolution of the free volume of hollow nanoobjects in chalcogenide glassy semiconductors exposed to radiation is shown. The results obtained by measurements of the positron annihilation lifetime and Doppler broadening of the annihilation line in reverse chronological order are in full agreement with the optical spectroscopy data in the region of the fundamental absorption edge, being adequately described within coordination defect-formation and physical-aging models.

Emergence of Griffiths phase and glassy mixed phase in Sm0.5Ca0.5MnO3 nanomanganites

International Nuclear Information System (INIS)

Giri, S.K.; Yusuf, S.M.; Mukadam, M.D.; Nath, T.K.

2014-01-01

Graphical abstract: A detailed investigation on the effect of grain size on formation of Griffiths phase, and glassy mixed phase in CE-type antiferromagnetic Sm 0.5 Ca 0.5 MnO 3 manganite are carried out. A rigorous measurement of linear and non-linear ac magnetic susceptibilities, time dependent relaxation and aging phenomena in Sm 0.5 Ca 0.5 MnO 3 nanomanganite confirm the existence of a glassy mixed phase in the low temperature regime. The signature of Griffiths phase in nanosized manganite has been confirmed from the detailed ac and dc magnetization studies. The existence of Griffiths phase is verified through the anomalous behavior of the low field temperature dependent an inverse ac and dc magnetic susceptibility. Based on experimental results, the glassy phase of nanomanganites has been attributed to the phase separation effect and interaction between the ferromagnetic clusters. A phenomenological core/shell model has also been proposed based on the surface disorder to explain the observed Griffiths phase in these nanosized manganites. Fig. 1: (Left) The plot of inverse of ac susceptibility χ ac -1 measured at f = 1 Hz and H ac = 2 Oe as a function of temperature for S750 sample. Inset shows the same for S550 sample. (Right) A schematic of the proposed model to describe the magnetic state of the Sm 0.5 Ca 0.5 MnO 3 system at different average sizes. Highlights: • Effect of grain size on Griffiths phase and glassy mixed phase is discussed. • GP is confirmed by dc, linear and non-linear ac magnetization in nanomanganites. • Glassy mixed phase is discussed by time dependent relaxation and aging phenomena. • The existence of GP is verified through an inverse ac and dc magnetic susceptibility. • A phenomenological core/shell model has been proposed based on surface disorder. -- Abstract: A detailed investigation on the effect of grain size on formation of Griffiths phase (GP), and glassy mixed phase in CE-type antiferromagnetic Sm 0.5 Ca 0.5 MnO 3

Evaluation of diffusion barrier and electrical properties of tantalum oxynitride thin films for silver metallization

International Nuclear Information System (INIS)

Misra, E.; Wang, Y.; Theodore, N.D.; Alford, T.L.

2004-01-01

The thermal stability and the diffusion barrier properties of DC reactively sputtered tantalum oxynitride (Ta-O-N) thin films, between silver (Ag) and silicon (Si) p + n diodes were investigated. Both materials characterization (X-ray diffraction analysis, Rutherford backscattering spectrometry (RBS), Auger depth profiling) and electrical measurements (reverse-biased junction leakage current-density) were used to evaluate diffusion barrier properties of the thin films. The leakage current density of p + n diodes with the barrier (Ta-O-N) was approximately four orders of magnitude lower than those without barriers after a 30 min, 400 deg. C back contact anneal. The Ta-O-N barriers were stable up to 500 deg. C, 30 min anneals. However, this was not the case for the 600 deg. C anneal. RBS spectra and cross-sectional transmission electron microscopy of as-deposited and vacuum annealed samples of Ag/barrier (Ta-O-N)/Si indicate the absence of any interfacial interaction between the barrier and substrate (silicon). The failure of the Ta-O-N barriers has been attributed to thermally induced stresses, which cause the thin film to crack at elevated temperatures

Characterization of the Young's modulus and residual stresses for a sputtered silicon oxynitride film using micro-structures

International Nuclear Information System (INIS)

Dong, Jian; Du, Ping; Zhang, Xin

2013-01-01

Silicon oxynitride (SiON) is an important material to fabricate micro-electro-mechanical system (MEMS) devices due to its composition-dependent tunability in electronic and mechanical properties. In this work, the SiON film with 41.45% silicon, 32.77% oxygen and 25.78% nitrogen content was deposited by RF magnetron sputtering. Two types of optimized micro-structures including micro-cantilevers and micro-rotating-fingers were designed and fabricated using MEMS surface micromachining technology. The micro-cantilever bending tests were conducted using a nanoindenter to characterize the Young's modulus of the SiON film. Owing to the elimination of the residual stress effect on the micro-cantilever structure, higher accuracy in the Young's modulus was achieved from this technique. With the information of Young's modulus of the film, the residual stresses were characterized from the deflection of the micro-rotating-fingers. This structure was able to locally measure a large range of tensile or compressive residual stresses in a thin film with sufficient sensitivities. The results showed that the Young's modulus of the SiON film was 122 GPa and the residual stresses of the SiON film were 327 MPa in the crystallographic orientation of the wafer and 334 MPa in the direction perpendicular to the crystallographic orientation, both in compression. This work presents a comprehensive methodology to measure the Young's modulus and residual stresses of a thin film with improved accuracy, which is promising for applications in mechanical characterization of MEMS devices. - Highlight: • We measured the Young's modulus and residual stress of SiON film by microstructure. • Micro cantilever structure improved the Young's modulus' measurement accuracy. • We explored the reason for the deviations of residual stress value of SiON film

Development of ΔE-E telescope ERDA with 40 MeV {sup 35}Cl{sup 7+} beam at MALT in the University of Tokyo optimized for analysis of metal oxynitride thin films

Energy Technology Data Exchange (ETDEWEB)

Harayama, I.; Nagashima, K. [Graduate School of Pure and Applied Sciences, University of Tsukuba, Tennodai 1-1-1, Tsukuba, Ibaraki 305-8573 (Japan); Hirose, Y. [Graduate School of Science, The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-0033 (Japan); CREST, Japan Science and Technology Agency, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-0033 (Japan); Matsuzaki, H. [School of Engineering, The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-8656 (Japan); Sekiba, D., E-mail: sekiba@tac.tsukuba.ac.jp [Graduate School of Pure and Applied Sciences, University of Tsukuba, Tennodai 1-1-1, Tsukuba, Ibaraki 305-8573 (Japan); Tandem Accelerator Complex, University of Tsukuba, Tennodai 1-1-1, Tsukuba, Ibaraki 305-8577 (Japan)

2016-10-01

We have developed a compact ΔE-E telescope elastic recoil detection analysis (ERDA) system, for the first time at Micro Analysis Laboratory, Tandem Accelerator (MALT) in the University of Tokyo, which consists of a gas ionization chamber and solid state detector (SSD) for the quantitative analysis of light elements. The gas ionization chamber is designed to identify the recoils of O and N from metal oxynitrides thin films irradiated with 40 MeV {sup 35}Cl{sup 7+}. The length of the electrodes along the beam direction is 50 mm optimized to sufficiently separate energy loss of O and N recoils in P10 gas at 6.0 × 10{sup 3} Pa. The performance of the gas ionization chamber was examined by comparing the ERDA results on the SrTaO{sub 2}N thin films with semi-empirical simulation and the chemical compositions previously determined by nuclear reaction analysis (NRA) and Rutherford backscattering spectrometry (RBS). We also confirmed availability of the gas ionization chamber for identifying not only the recoils of O and N but also those of lithium, carbon and fluorine.

Egg maturation by the glassy-winged sharpshooter (Hemiptera: Cicadellidae); a vector of Xylella fastidiosa

Science.gov (United States)

Rates of spread of insect-transmitted plant pathogens are a function of vector abundance. Despite this, factors affecting population growth rates of insects that transmit plant pathogens have received limited attention. The glassy-winged sharpshooter (Homalodisca vitripennis) feeds on xylem-sap and ...

Composite with a metallic matrix Al-AlN: from the powder to the material; Composite a matrice metallique A1-A1N: de la poudre au materiau

Energy Technology Data Exchange (ETDEWEB)

Troadec, C.

1996-05-09

Two types of powders are used: a `composite` powder synthesized by direct nitridation of aluminium by nitrogen, and a `mixed` powder obtained by a mixture of Al and AlN powders. These two powders types are crushed in a high energetic planetary crusher under an Ar atmosphere, then they are sintered under solid phase hot pressure. Microstructure of these materials, studied by Tem and XED, is relatively heterogenous, with high density polycrystalline area and high porous nano-crystals area. Size of these porous area are higher in `mixed` powders, and is linked to AlN percentage and to the crushing time. High density area are composed of Al grains surrounded by AlN nano-crystals with Al{sub 2}O{sub 3} needles and few aluminium oxynitride crystals. Physicochemical and mechanical properties, wear and corrosion comportment differ in function of the initial powders (`mixed` or `composite`) and with the AlN percentage. These new materials have, at similar reinforcement concentration, equivalent properties to Al/SiC or Al/Al{sub 2}O{sub 3} materials. (A.B.) 112 refs.

Effect of cooling rate on microstructure and deformation behavior of Ti-based metallic glassy/crystalline powders

Energy Technology Data Exchange (ETDEWEB)

Wang, D.J. [State Key Laboratory of Advanced Welding Production Technology, Harbin Institute of Technology, Harbin 150001 (China); School of Mechanical and Mining Engineering, University of Queensland, Brisbane, QLD 4072 (Australia); Huang, Y.J. [State Key Laboratory of Advanced Welding Production Technology, Harbin Institute of Technology, Harbin 150001 (China); Shen, J., E-mail: junshen@hit.edu.cn [State Key Laboratory of Advanced Welding Production Technology, Harbin Institute of Technology, Harbin 150001 (China); Wu, Y.Q.; Huang, H. [School of Mechanical and Mining Engineering, University of Queensland, Brisbane, QLD 4072 (Australia); Zou, J., E-mail: j.zou@uq.edu.au [School of Mechanical and Mining Engineering, University of Queensland, Brisbane, QLD 4072 (Australia); Centre for Microscopy and Microanalysis, University of Queensland, Brisbane, QLD 4072 (Australia)

2010-08-20

The microstructures and deformation behavior of Ti-based metallic powders were comprehensively investigated. It has been found that, with increasing the powder size, the phase constituent alters from pure glassy to glassy with crystalline phases (face centered cubic structured NiSnZr and hexagonal structured Ti{sub 3}Sn phases). Our results suggest that the synergetic effect of the thermodynamics and kinetics determines the subsequent characteristics of the crystalline precipitations. Through comparative nanoindentation tests, it was found that the small powders exhibit more pop-in events and a larger pile-up ratio, suggesting that the plastic deformation of the metallic powders is governed by the combined effects of the free volume and the crystallization, which are determined by the cooling rate.

Structural characterization and aging of glassy pharmaceuticals made using acoustic levitation.

Science.gov (United States)

Benmore, Chris J; Weber, J K R; Tailor, Amit N; Cherry, Brian R; Yarger, Jeffery L; Mou, Qiushi; Weber, Warner; Neuefeind, Joerg; Byrn, Stephen R

2013-04-01

Here, we report the structural characterization of several amorphous drugs made using the method of quenching molten droplets suspended in an acoustic levitator. (13) C NMR, X-ray, and neutron diffraction results are discussed for glassy cinnarizine, carbamazepine, miconazole nitrate, probucol, and clotrimazole. The (13) C NMR results did not find any change in chemical bonding induced by the amorphization process. High-energy X-ray diffraction results were used to characterize the ratio of crystalline to amorphous material present in the glasses over a period of 8 months. All the glasses were stable for at least 6 months except carbamazepine, which has a strong tendency to crystallize within a few months. Neutron and X-ray pair distribution function analyses were applied to the glassy materials, and the results were compared with their crystalline counterparts. The two diffraction techniques yielded similar results in most cases and identified distinct intramolecular and intermolecular correlations. The intramolecular scattering was calculated based on the crystal structure and fit to the measured X-ray structure factor. The resulting intermolecular pair distribution functions revealed broad-nearest and next-nearest neighbor molecule-molecule correlations. © 2013 Wiley Periodicals, Inc. and the American Pharmacists Association J Pharm Sci 102:1290-1300, 2013. Copyright © 2013 Wiley Periodicals, Inc.

Crystal-like nature of acoustic excitations in glassy ethanol

International Nuclear Information System (INIS)

Matic, A.; Engberg, D.; Boerjesson, L.; Masciovecchio, C.; Santucci, S.C.; Monaco, G.; Verbeni, R.

2004-01-01

We report on inelastic x-ray scattering experiments on crystalline and glassy phases of ethanol in order to directly compare the influence of disorder on high frequency acoustic excitations. We find that both the dispersion and the line-width of the longitudinal acoustic excitations in the glass are the same as in the polycrystal in the reciprocal space portion covering the 1st and 2nd Brillouin zones. The structural disorder is found to play little role apart from an intrinsic angular averaging, and the nature of these excitations must essentially be the same in both glass and poly crystal

Modified positron annihilation model for glassy-like As2Se3

International Nuclear Information System (INIS)

Kozdras, A.; Shpotyuk, O.; Kovalskiy, A.; Filipecki, J.

2005-01-01

An approach to structural characterization of chalcogenide glasses based on the study of void distribution is discussed. The results of positron annihilation lifetime spectra measurements for glassy As 2 Se 3 are compared with nano-void distribution data obtained from Monte Carlo simulation. In this consideration perspectives to involve the parameters of nano-voids calculated from the first sharp diffraction peak in the frame work of known Elliott's model are analyzed. (author)

Formation and Applications of Bulk Glassy Alloys in Late Transition Metal Base System

International Nuclear Information System (INIS)

Inoue, Akihisa; Shen Baolong

2006-01-01

This paper reviews our recent results of the formation, fundamental properties, workability and applications of late transition metal (LTM) base bulk glassy alloys (BGAs) developed since 1995. The BGAs were obtained in Fe-(Al,Ga)-(P,C,B,Si), Fe-(Cr,Mo)-(C,B), Fe-(Zr,Hf,Nb,Ta)-B, Fe-Ln-B(Ln=lanthanide metal), Fe-B-Si-Nb and Fe-Nd-Al for Fe-based alloys, Co-(Ta,Mo)-B and Co-B-Si-Nb for Co-based alloys, Ni-Nb-(Ti,Zr)-(Co,Ni) for Ni-based alloys, and Cu-Ti-(Zr,Hf), Cu-Al-(Zr,Hf), Cu-Ti-(Zr,Hf)-(Ni,Co) and Cu-Al-(Zr,Hf)-(Ag,Pd) for Cu-based alloys. These BGAs exhibit useful properties of high mechanical strength, large elastic elongation and high corrosion resistance. In addition, Fe- and Co-based glassy alloys have good soft magnetic properties which cannot be obtained for amorphous and crystalline type magnetic alloys. The Fe- and Ni-based BGAs have already been used in some application fields. These LTM base BGAs are promising as new metallic engineering materials

De-chlorination and solidification of radioactive LiCl waste salt by using SiO_2-Al_2O_3-P_2O_5 (SAP) inorganic composite including B_2O_3 component

International Nuclear Information System (INIS)

Lee, Ki Rak; Park, Hwan-Seo; Cho, In-Hak; Choi, Jung-Hoon; Eun, Hee-Chul; Lee, Tae-Kyo; Han, Seung Youb; Ahn, Do-Hee

2017-01-01

SAP (SiO_2-Al_2O_3-P_2O_5) composite has been recently studied in KAERI to deal with the immobilization of radioactive salt waste, one of the most problematic wastes in the pyro-chemical process. Highly unstable salt waste was successfully converted into stable compounds by the dechlorination process with SAPs, and then a durable waste form with a high waste loading was produced when adding glassy materials to dechlorination product. In the present study, U-SAP composite which is SAP bearing glassy component (Boron) was synthesized to remove the adding and mixing steps of glassy materials for a monolithic wasteform. With U-SAPs prepared by a sol-gel process, a series of wasteforms were fabricated to identify a proper reaction condition. Physical and chemical properties of dechlorination products and U-SAP wasteforms were characterized by XRD, DSC, SEM, TGA and PCT-A. A U-SAP wasteform showed suitable properties as a radioactive wasteform such as dense surface morphology, high waste loading, and high durability at the optimized U-SAP/salt ratio 2.

Application of nondestructive ion beam analysis to measure variations in the elemental composition of armor materials

Energy Technology Data Exchange (ETDEWEB)

Pallone, Arthur. E-mail: art.pallone@murraystate.edu; Demaree, John; Adams, Jane. E-mail: jadams@arl.army.mil

2004-06-01

Lightweight, state-of-the-art armors rely on ceramics for their enhanced performance. One goal of the United States Army is to expand the industrial base of companies that provide the armors. A systematic study of armor performance as a function of ceramic stoichiometry will result in a better understanding of the fundamental relations between composition and mechanical performance. One ceramic of interest is aluminum oxynitride (AlON). The stoichiometries of representative samples of AlON were investigated with the nondestructive techniques of Rutherford backscattering spectrometry and resonant nuclear reaction analysis. Future tests of the performance of the AlON samples are to be correlated with the stoichiometries, and hence will lead to optimum, standardized processes for the manufacture of the AlON.

Playback of natural vibrational signals in vineyard trellis for mating disruption of glassy-winged sharpshooter

Science.gov (United States)

The glassy-winged sharpshooter, Homalodisca vitripennis (Germar) (Hemiptera: Cicadellidae), is a vector of Xylella fastidiosa, an important bacterial pathogen of several crops in the Americas and Europe. Mating communication of this and many other cicadellid pests involves the exchange of substrate-...

Luminescence properties of Eu2+ - activated alkaline-earth silicon-oxynitride MSi2O2-deltaN2+2/3delta (M = Ca, Sr, Ba) : A promising class of novel LED conversion phosphors

NARCIS (Netherlands)

Li, Y.Q.; Delsing, A.C.A.; With, de G.; Hintzen, H.T.J.M.

2005-01-01

The luminescence properties of Eu2+-activated alk.-earth Si-oxynitrides were studied. In the BaO-SiO2-Si3N4 system, a new BaSi2O2N2 compd. was obtained having the monoclinic structure with lattice parameters a 14.070(4), b 7.276(2), c 13.181(3) .ANG., b 107.74(6)°. All MSi2O2-dN2+2/3d:Eu2+ (M = Ca,

Glucose biosensor based on a glassy carbon electrode modified with polythionine and multiwalled carbon nanotubes.

Directory of Open Access Journals (Sweden)

Wenwei Tang

Full Text Available A novel glucose biosensor was fabricated. The first layer of the biosensor was polythionine, which was formed by the electrochemical polymerisation of the thionine monomer on a glassy carbon electrode. The remaining layers were coated with chitosan-MWCNTs, GOx, and the chitosan-PTFE film in sequence. The MWCNTs embedded in FAD were like "conductive wires" connecting FAD with electrode, reduced the distance between them and were propitious to fast direct electron transfer. Combining with good electrical conductivity of PTH and MWCNTs, the current response was enlarged. The sensor was a parallel multi-component reaction system (PMRS and excellent electrocatalytic performance for glucose could be obtained without a mediator. The glucose sensor had a working voltage of -0.42 V, an optimum working temperature of 25°C, an optimum working pH of 7.0, and the best percentage of polytetrafluoroethylene emulsion (PTFE in the outer composite film was 2%. Under the optimised conditions, the biosensor displayed a high sensitivity of 2.80 µA mM(-1 cm(-2 and a low detection limit of 5 µM (S/N = 3, with a response time of less than 15 s and a linear range of 0.04 mM to 2.5 mM. Furthermore, the fabricated biosensor had a good selectivity, reproducibility, and long-term stability, indicating that the novel CTS+PTFE/GOx/MWCNTs/PTH composite is a promising material for immobilization of biomolecules and fabrication of third generation biosensors.

Memristive behaviour of Si-Al oxynitride thin films: the role of oxygen and nitrogen vacancies in the electroforming process

Science.gov (United States)

Blázquez, O.; Martín, G.; Camps, I.; Mariscal, A.; López-Vidrier, J.; Ramírez, J. M.; Hernández, S.; Estradé, S.; Peiró, F.; Serna, R.; Garrido, B.

2018-06-01

The resistive switching properties of silicon-aluminium oxynitride (SiAlON) based devices have been studied. Electrical transport mechanisms in both resistance states were determined, exhibiting an ohmic behaviour at low resistance and a defect-related Poole‑Frenkel mechanism at high resistance. Nevertheless, some features of the Al top-electrode are generated during the initial electroforming, suggesting some material modifications. An in-depth microscopic study at the nanoscale has been performed after the electroforming process, by acquiring scanning electron microscopy and transmission electron microscopy images. The direct observation of the devices confirmed features on the top electrode with bubble-like appearance, as well as some precipitates within the SiAlON. Chemical analysis by electron energy loss spectroscopy has demonstrated that there is an out-diffusion of oxygen and nitrogen ions from the SiAlON layer towards the electrode, thus forming silicon-rich paths within the dielectric layer and indicating vacancy change to be the main mechanism in the resistive switching.

Mechanical measurements on lithium phosphorous oxynitride coated silicon thin film electrodes for lithium-ion batteries during lithiation and delithiation

Energy Technology Data Exchange (ETDEWEB)

Al-Obeidi, Ahmed, E-mail: alobeidi@mit.edu; Thompson, Carl V., E-mail: reiner.moenig@kit.edu, E-mail: cthomp@mit.edu [Department of Materials Science and Engineering, Massachusetts Institute of Technology, 77 Massachusetts Avenue, Cambridge, Massachusetts 02139 (United States); Kramer, Dominik, E-mail: dominik.kramer@kit.edu; Mönig, Reiner, E-mail: reiner.moenig@kit.edu, E-mail: cthomp@mit.edu [Institute for Applied Materials, Karlsruhe Institute of Technology, Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Helmholtz Institute Ulm for Electrochemical Energy Storage (HIU), Helmholtzstraße 11, 89081 Ulm (Germany); Boles, Steven T., E-mail: steven.t.boles@polyu.edu.hk [Institute for Applied Materials, Karlsruhe Institute of Technology, Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Hong Kong Polytechnic University, 11 Yuk Choi Rd, Hung Hom (Hong Kong)

2016-08-15

The development of large stresses during lithiation and delithiation drives mechanical and chemical degradation processes (cracking and electrolyte decomposition) in thin film silicon anodes that complicate the study of normal electrochemical and mechanical processes. To reduce these effects, lithium phosphorous oxynitride (LiPON) coatings were applied to silicon thin film electrodes. Applying a LiPON coating has two purposes. First, the coating acts as a stable artificial solid electrolyte interphase. Second, it limits mechanical degradation by retaining the electrode's planar morphology during cycling. The development of stress in LiPON-coated electrodes was monitored using substrate curvature measurements. LiPON-coated electrodes displayed highly reproducible cycle-to-cycle behavior, unlike uncoated electrodes which had poorer coulombic efficiency and exhibited a continual loss in stress magnitude with continued cycling due to film fracture. The improved mechanical stability of the coated silicon electrodes allowed for a better investigation of rate effects and variations of mechanical properties during electrochemical cycling.

Fatigue damage and fracture behavior of tungsten fiber reinforced Zr-based metallic glassy composite

Energy Technology Data Exchange (ETDEWEB)

Zhang, H. [Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, 72 Wenhua Road, Shenyang 110016 (China); Zhang, Z.F. [Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, 72 Wenhua Road, Shenyang 110016 (China)]. E-mail: zhfzhang@imr.ac.cn; Wang, Z.G. [Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, 72 Wenhua Road, Shenyang 110016 (China); Qiu, K.Q. [Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, 72 Wenhua Road, Shenyang 110016 (China); Zhang, H.F. [Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, 72 Wenhua Road, Shenyang 110016 (China); Zang, Q.S. [Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, 72 Wenhua Road, Shenyang 110016 (China); Hu, Z.Q. [Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, 72 Wenhua Road, Shenyang 110016 (China)

2006-02-25

The fatigue life, damage and fracture behavior of tungsten fiber reinforced metallic glass Zr{sub 41.25}Ti{sub 13.75}Ni{sub 10}Cu{sub 12.5}Be{sub 22.5} composites are investigated under cyclic push-pull loading. It is found that the fatigue life of the composite increases with increasing the volume fraction of tungsten fibers. Similar to crystalline metals, the regions of crack initiation, propagation and overload fracture can be discerned on the fracture surface of the specimen. Fatigue crack normally initiates in the metallic glass matrix at the outer surface of the composite specimen and propagates predominantly in the matrix. Different crack front profile around the tungsten fibers and fiber pullout demonstrate that fatigue crack may propagate around the fiber, leading to bridging of the crack faces by the unbroken fiber and hence improved fatigue crack-growth resistance. Locally decreased effective stiffness in the region where fiber distribution is sparse may provide preferential crack path in the composite. A proposed model was exercised to elucidate different tungsten fiber fracture morphologies in the fatigue crack propagation and overload fracture regions in the light of Poisson's ratio effect during fatigue loading.

Fatigue damage and fracture behavior of tungsten fiber reinforced Zr-based metallic glassy composite

International Nuclear Information System (INIS)

Zhang, H.; Zhang, Z.F.; Wang, Z.G.; Qiu, K.Q.; Zhang, H.F.; Zang, Q.S.; Hu, Z.Q.

2006-01-01

The fatigue life, damage and fracture behavior of tungsten fiber reinforced metallic glass Zr 41.25 Ti 13.75 Ni 10 Cu 12.5 Be 22.5 composites are investigated under cyclic push-pull loading. It is found that the fatigue life of the composite increases with increasing the volume fraction of tungsten fibers. Similar to crystalline metals, the regions of crack initiation, propagation and overload fracture can be discerned on the fracture surface of the specimen. Fatigue crack normally initiates in the metallic glass matrix at the outer surface of the composite specimen and propagates predominantly in the matrix. Different crack front profile around the tungsten fibers and fiber pullout demonstrate that fatigue crack may propagate around the fiber, leading to bridging of the crack faces by the unbroken fiber and hence improved fatigue crack-growth resistance. Locally decreased effective stiffness in the region where fiber distribution is sparse may provide preferential crack path in the composite. A proposed model was exercised to elucidate different tungsten fiber fracture morphologies in the fatigue crack propagation and overload fracture regions in the light of Poisson's ratio effect during fatigue loading

Formulation of thermodynamics for the glassy state : Configurational energy as a modest source of energy

NARCIS (Netherlands)

Nieuwenhuizen, T.M.

2001-01-01

Glass is an under-cooled liquid that very slowly relaxes towards the equilibrium crystalline state. Its energy balance is ill understood, since it is widely believed that the glassy state cannot be described thermodynamically. However, the classical paradoxes involving the Ehrenfest relations and

Chemical attachment of functionalized multiwalled carbon nanotubes on glassy carbon electrode for electrocatalytic application

International Nuclear Information System (INIS)

Rajalakshmi, K.; Abraham John, S.

2015-01-01

Highlights: • FMWCNTs were covalently attached on GC surface with the aid of alkyldiamine. • The attached FMWCNTs were stable for a wide potential window due to the robust C−N bond. • The composite electrode was prepared by electropolymerizing thiadiazole on FMWCNTs. • The detection limit of 0.27 μM (S/N = 3) of GMP was achieved using composite modified electrode. - Abstract: The covalent attachment of acid functionalized multiwalled carbon nanotubes (FMWCNTs) on glassy carbon (GC) electrode using 1,8-octanediamine (OD) as a linker via carbodiimide chemistry was described. The attachment of FMWCNTs on GC electrode were confirmed by attenuated total reflectance Fourier transform infra-red (ATR-FT-IR) spectroscopy, Raman, scanning electron microscopy (SEM) and electrochemical impedance studies. Raman spectrum of FMWCNTs modified surface shows the characteristic G and D bands at 1563 cm −1 and 1340 cm −1 , respectively. This confirmed the successful attachment of FMWCNTs on the OD modified GC surface. Further, the attachment of FMWCNTs on OD modified surface via amide linkage was confirmed from the observed characteristic peak at 1681 cm −1 in the ATR-FT-IR spectrum. The SEM images showed that the covalently attached FMWCNTs retained their morphology similar to powder and the average diameter of them was found to be 58 nm. Unlike modification of FMWCNTs on gold substrates with the aid of conventional thiol linkers (Au−S bond), modification of them by the present method was stable for a wide positive potential window due to the robust C−N bond. To demonstrate the electrochemical stability of the MWCNTs modified electrode at more positive potential, guanosine 5′-monophosphate (GMP) was selected as a representative probe because its oxidation occurs at more than 1 V. It was found that the FMWCNTs modified electrode not only showed a stable signal for GMP but also enhanced its oxidation current when compared to bare GC electrode. Further, the

Evidence for a glassy state in strongly driven carbon

International Nuclear Information System (INIS)

Brown, C.R.D.; Gericke, D.O.; Wunsch, K.; Cammarata, M.; Fritz, D.; Glenzer, S.H.; Heimann, P.; Lee, H.J.; Lemke, H.; Nagler, B.; Zhu, D.; Galtier, E.; Moinard, A.; Rosmej, F.B.

2014-01-01

Here, we report results of an experiment creating a transient, highly correlated carbon state using a combination of optical and x-ray lasers. Scattered x-rays reveal a highly ordered state with an electrostatic energy significantly exceeding the thermal energy of the ions. Strong Coulomb forces are predicted to induce nucleation into a crystalline ion structure within a few picoseconds. However, we observe no evidence of such phase transition after several tens of picoseconds but strong indications for an over-correlated fluid state. The experiment suggests a much slower nucleation and points to an intermediate glassy state where the ions are frozen close to their original positions in the fluid. (authors)

Detection and typing of Xylella fastidiosa from glassy-winged sharpshooter for Pierce’s disease epidemiology

Science.gov (United States)

Epidemiology of Pierce’s disease of grape, caused by the bacterial pathogen Xylella fastidiosa (Xf), is largely dependent on populations of insect vectors such as the invasive glassy-winged sharpshooter (GWSS) (Homalodisca vitripennis). In the grape-growing regions of the southern San Joaquin Valley...

Micromechanical modeling of tungsten-based bulk metallic glass matrix composites

Energy Technology Data Exchange (ETDEWEB)

Li Hao [Department of Mechanical Engineering-Engineering Mechanics, Michigan Technological University, 1400 Townsend Drive, Houghton, MI 49931 (United States); Li Ke [Department of Mechanical Engineering, Texas A and M University, TAMU 3123, College Station, TX 77843 (United States)]. E-mail: keli@tamu.edu; Subhash, Ghatu [Department of Mechanical Engineering-Engineering Mechanics, Michigan Technological University, 1400 Townsend Drive, Houghton, MI 49931 (United States); Kecskes, Laszlo J. [Weapons and Materials Research Directorate, US Army Research Laboratory, Aberdeen Proving Ground, MD 21005 (United States); Dowding, Robert J. [Weapons and Materials Research Directorate, US Army Research Laboratory, Aberdeen Proving Ground, MD 21005 (United States)

2006-08-15

Micromechanics models are developed for tungsten (W)-based bulk metallic glass (BMG) matrix composites employing the Voronoi tessellation technique and the finite element (FE) method. The simulation results indicate that the computed elastic moduli are close to those measured in the experiments. The predicted stress-strain curves agree well with their experimentally obtained counterparts in the early stage of the plastic deformation. An increase in the W volume fraction leads to a decrease in the yield stress and an increase in the Young's modulus of the composite. In addition, contours of equivalent plastic strain for increasing applied strains provide an explanation why shear bands were observed in the glassy phase, along the W/BMG interface, and in the W phase of failed W/BMG composite specimens.

EIS study of the redox reaction of Fe(CN)63-/4- at glassy carbon electrode via diazonium reduction in aqueous and acetonitrile solutions

Energy Technology Data Exchange (ETDEWEB)

Khoshroo, M.; Rostami, A. [Mazandaran Univ., Babolsar (Iran, Islamic Republic of). Dept. of Physical Chemistry

2008-07-01

This paper reported on a study that characterized soluble electroactive species by cyclic voltammetry to investigate the presence of grafted films and their blocking properties. In particular, the authority of the glassy carbon electrode modification conditions on the cyclic voltammetric response of Fe(CN)63-/4- oxido-reduction was examined for 2 layers grafted by electrochemical reduction of diazonium salts in acetonitrile and aqueous solutions. PAA and Fast Black K modified glassy carbon electrodes exhibited a significant blocking behaviour for oxidation and reduction reactions of the Fe(CN)63-/4- redox system in aqueous and acetonitrile solutions. The study showed that the blocking effect increased which changes in time and concentration of diazonium salts in acetonitrile solution. Electrochemical impedance spectroscopy (EIS) measurements showed that the physical barrier of grafted layers prevent the access of Fe(CN)63-/4- to the underlying glassy carbon electrode. Therefore the RCT resistance increases during the modification treatment. The substituted phenyl layers are much more compact and less permeable in a nonaqueous solvent than with an aqueous solvent. Electrochemical impedance measurements indicate that the kinetics of electron transfer slow down when the time and the concentration used to modify the glassy carbon electrode increase. 4 refs., 1 fig.

Statistics of energy levels and zero temperature dynamics for deterministic spin models with glassy behaviour

NARCIS (Netherlands)

Degli Esposti, M.; Giardinà, C.; Graffi, S.; Isola, S.

2001-01-01

We consider the zero-temperature dynamics for the infinite-range, non translation invariant one-dimensional spin model introduced by Marinari, Parisi and Ritort to generate glassy behaviour out of a deterministic interaction. It is argued that there can be a large number of metastable (i.e.,

Preparing microspheres of actinide nitrides from carbon containing oxide sols

International Nuclear Information System (INIS)

Triggiani, L.V.

1975-01-01

A process is given for preparing uranium nitride, uranium oxynitride, and uranium carboxynitride microspheres and the microspheres as compositions of matter. The microspheres are prepared from carbide sols by reduction and nitriding steps. (Official Gazette)

Glass-forming ability and crystallization behavior of some binary and ternary Ni-based glassy alloys

International Nuclear Information System (INIS)

Louzguine-Luzgin, Dmitri V.; Louzguina-Luzgina, Larissa V.; Xie Guoqiang; Li Song; Zhang Wei; Inoue, Akihisa

2008-01-01

The purpose of the current paper is to study the influence of Ti, V, Nb, Al, Sn and Pd additions on the glass-forming ability, formation of a supercooled liquid region and a devitrification process of some Ni-Zr glassy alloys as well as to compare the results with those obtained for similar Cu-based alloys studied earlier. The Ni-based glassy alloys were investigated by using X-ray diffraction, differential scanning and isothermal calorimetries. Although the studied Ni-based alloys showed high values of the reduced glass-transition temperature of about 0.6, their glass-forming ability is quite low. This fact may be explained by low stability of the supercooled liquid against crystallization and formation of the equilibrium intermetallic compounds with a high growth rate compared to those observed in similar Cu-based alloys studied earlier. Relatively low thermal conductivity of Ni-based alloys is also found to be another factor limiting their glass-forming ability

Destruction-polymerization transformations as a source of radiation-induced extended defects in chalcogenide glassy semiconductors

International Nuclear Information System (INIS)

Shpotyuk, Oleh; Filipecki, Jacek; Shpotyuk, Mykhaylo

2013-01-01

Long-wave shift of the optical transmission spectrum in the region of fundamental optical absorption edge is registered for As 2 S 3 chalcogenide glassy semiconductors after γ-irradiation. This effect is explained in the frameworks of the destruction-polymerization transformations concept by accepting the switching of the heteropolar As-S covalent bonds into homopolar As-As ones. It is assumed that (As 4 + ; S 1 - ) defect pairs are created under such switching. Formula to calculate content of the induced defects in chalcogenide glassy semiconductors is proposed. It is assumed that defects concentration depends on energy of broken covalent bond, bond-switching energy balance, correlation energy, optical band-gap and energy of excitation light. It is shown that theoretically calculated maximally possible content of radiation-induced defects in As 2 S 3 is about 1.6% while concentration of native defects is negligible. (copyright 2013 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

Influence of thermal history on the photostructural changes in glassy As15S85 studied by Raman scattering and ab initio calculations

International Nuclear Information System (INIS)

Kolar, J.; Strizik, L.; Kohoutek, T.; Wagner, T.; Voyiatzis, G. A.; Chrissanthopoulos, A.; Yannopoulos, S. N.

2013-01-01

Photostructural changes—the hallmark of non-crystalline chalcogenides—are in essence the basis of a number of photoinduced effects, i.e., changes of their physical properties, which are exploited in a variety of applications, especially in photonics and optoelectronics. Despite the vast number of investigations of photostructural changes, there is currently lack of systematic studies on how the thermal history, which affects glass structure, modifies the extent of photostructural changes. In this article, we study the role of thermal history on photostructural changes in glassy As 15 S 85 . This particular sulfur-rich composition has been chosen based on the colossal photostructural response it exhibits under near-band gap light irradiation, which inherently originates from its nanoscale phase-separated nature. To control the thermal history, the glass was quenched to various temperatures and each of these quenched products was annealed under four different conditions. Off-resonant Raman scattering was used to study the equilibrium study of each product. Structural changes of interest involve changes of the sulfur atoms participating into S 8 rings and S n chains. Their ratio was found to depend on quenching/annealing conditions. Near-band gap light was used to perturb the rings-to-chain ratio and at the same time to record these changes through Raman scattering, revealing an intricate behavior of photostructural changes. Ab initio calculations were employed to determine the stability of various sulfur clusters/molecules thus aiding the correlation of the particular photo-response of glassy As 15 S 85 with its structural constituents

Solute induced relaxation in glassy polymers: Experimental measurements and nonequilibrium thermodynamic model

International Nuclear Information System (INIS)

Minelli, Matteo; Doghieri, Ferruccio

2014-01-01

Data for kinetics of mass uptake from vapor sorption experiments in thin glassy polymer samples are here interpreted in terms of relaxation times for volume dilation. To this result, both models from non-equilibrium thermodynamics and from mechanics of volume relaxation contribute. Different kind of sorption experiments have been considered in order to facilitate the direct comparison between kinetics of solute induced volume dilation and corresponding data from process driven by pressure or temperature jumps

A glassy carbon electrode modified with β-cyclodextin, multiwalled carbon nanotubes and graphene oxide for sensitive determination of 1,3-dinitrobenzene

International Nuclear Information System (INIS)

Li, Junhua; Feng, Haibo; Liu, Jinlong; Liu, Youcai; Jiang, Jianbo; Feng, Yonglan; Qian, Dong

2014-01-01

We are presenting a host-guest electrochemical platform for sensing the pollutant 1,3-dinitrobenzene. The method is based on the use of a glassy carbon electrode (GCE) covered with a composite made from multiwalled carbon nanotubes and graphene oxide, and functionalized with β-cyclodextrin (β-CD). The resultant composite was characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, thermogravimetric analysis and electrochemical techniques. The modified GCE was used for the sensitive detection of 1,3-dinitrobenzene (DNB) at working voltages of −355 mV and −483 mV. Due to the specific recognition property of β-CD and the excellent electronic properties of the carbon nanomaterials, the electrode exhibits outstanding supramolecular recognition and enhanced electrochemical response to DNB compared to more conventional electrodes. Under optimum conditions, the peak currents vary linearly with the DNB concentrations in the range from 0.02 to 30.0 μM, and the detection limit is 5.0 nM (at an S/N of 3). The electrode exhibits long-term stability and has been successfully applied to the determination of DNB in spiked soil and water samples. (author)

Temperature-dependent microindentation data of an epoxy composition in the glassy region

Czech Academy of Sciences Publication Activity Database

Minster, Jiří; Králík, V.

2015-01-01

Roč. 19, č. 1 (2015), s. 75-85 ISSN 1385-2000 R&D Projects: GA ČR(CZ) GAP105/12/0824 Institutional support: RVO:68378297 Keywords : mechanical properties * viscoelasticity * glass transition * microindentation * time-temperature superposition Subject RIV: JI - Composite Materials Impact factor: 1.120, year: 2015 http://link.springer.com/article/10.1007/s11043-014-9252-6

Glass composite waste forms for iodine confined in bismuth-embedded SBA-15

Energy Technology Data Exchange (ETDEWEB)

Yang, Jae Hwan [Nuclear Fuel Cycle Process Development Division, Korea Atomic Energy Research Institute, 989-111 Daeduk-daero, Yuseong-gu, Daejeon, 305-353 (Korea, Republic of); Department of Nuclear and Quantum Engineering, Korea Advanced Institute of Science and Technology, 291 Daehak-ro, Yuseong-gu, Daejeon, 305-701 (Korea, Republic of); Park, Hwan Seo; Ahn, Do-Hee [Nuclear Fuel Cycle Process Development Division, Korea Atomic Energy Research Institute, 989-111 Daeduk-daero, Yuseong-gu, Daejeon, 305-353 (Korea, Republic of); Yim, Man-Sung, E-mail: msyim@kaist.ac.kr [Department of Nuclear and Quantum Engineering, Korea Advanced Institute of Science and Technology, 291 Daehak-ro, Yuseong-gu, Daejeon, 305-701 (Korea, Republic of)

2016-11-15

The aim of this study was to stabilize bismuth-embedded SBA-15 that captured iodine gas by fabrication of monolithic waste forms. The iodine containing waste was mixed with Bi{sub 2}O{sub 3} (a stabilizing additive) and low-temperature sintering glass followed by pelletizing and the sintering process to produce glass composite materials. Iodine volatility during the sintering process was significantly affected by the ratio of Bi{sub 2}O{sub 3} and the glass composition. It was confirmed that BiI{sub 3}, the main iodine phase within bismuth-embedded SBA-15, was effectively transformed to the mixed phases of Bi{sub 5}O{sub 7}I and BiOI. The initial leaching rates of iodine from the glass composite waste forms ranged 10{sup −3}–10{sup −2} g/m{sup 2} day, showing the stability of the iodine phases encapsulated by the glassy networks. It was also observed that common groundwater anions (e.g., chloride, carbonate, sulfite, and fluoride) elevated the iodine leaching rate by anion exchange reactions. The present results suggest that the glass composite waste form of bismuth-embedded SBA-15 could be a candidate material for stable storage of {sup 129}I. - Highlights: • Glass composite waste forms were developed to stabilize iodine confined in Bi-embedded SBA-15. • BiI{sub 3} within Bi-embedded SBA-15 was transformed to BiOI and Bi{sub 5}O{sub 7}I during sintering process. • Iodine volatility was significantly affected by glass composition and Bi{sub 2}O{sub 3} additive. • Iodine leaching rates were 10{sup −3}–10{sup −2} g/m{sup 2} day due to the stable iodine phases encapsulated by glassy networks. • Glass composite waste form of Bi-embedded SBA-15 is expected to be a candidate material for stable storage of {sup 129}I.

Fabrication and modification of metal nanocluster composites using ion and laser beams

International Nuclear Information System (INIS)

Haglund, R.F. Jr.; Osborne, D.H. Jr.; Magruder, R.H. III; White, C.W.; Zuhr, R.A.; Townsend, P.D.; Hole, D.E.; Leuchtner, R.E.

1994-12-01

Metal nanocluster composites have attractive properties for applications in nonlinear optics. However, traditional fabrication techniques -- using melt-glass substrates -- are severely constrained by equilibrium thermodynamics and kinetics. This paper describes the fabrication of metal nanoclusters in both crystalline and glassy hosts by ion implantation and pulsed laser deposition. The size and size distribution of the metal nanoclusters can be modified by controlling substrate temperature during implantation, by subsequent thermal annealing, or by laser irradiation. The authors have characterized the optical response of the composites by absorption and third-order nonlinear-optical spectroscopies; electron and scanning-probe microscopies have been used to benchmark the physical characteristics of the composites. The outlook for controlling the structure and nonlinear optical response properties of these nanophase materials appears increasingly promising

Physical and chemical analysis of glass beads and glassy slag from Iron Age sites in northeast Thailand : preliminary findings

International Nuclear Information System (INIS)

Saitowitz, S.J.; Reid, D.L.

2001-01-01

Substantial numbers of glass beads have been found at the Iron Age site of Noen U-Loke (ca. 850 BC to AD 500) in northeast Thailand. Typological classification of the beads, using standardised procedures, together with specialized analytical data show that while distinctly different bead-making techniques were used to produce the beads, the chemical composition of the glass was very similar. This information suggests the possibility of multiple craftsmen, at varied levels of expertise, using glass made at a single source or using raw materials found within a specific region. These findings allow for more detailed physical and chemical analysis of the beads, so as to quantify the spatial and temporal variability of different bead types. A fragment of glassy slag, excavated at Noen U-Loke, was analysed to distinguish whether it could be associated with a glass making process. However, the results were unable to confirm whether it was used to make glass suitable for beads. (author). 30 refs., 12 figs., 2 tabs

Amperometric nitrite sensor based on a glassy carbon electrode modified with multi-walled carbon nanotubes and poly(toluidine blue)

International Nuclear Information System (INIS)

Dai, Juan; Deng, Fei; He, Shuang; Deng, Dongli; Yuan, Yali; Zhang, Jinzhong

2016-01-01

An amperometric nitrite sensor modified with multi-walled carbon nanotubes (MWCNTs) and poly(toluidine blue) (PTB) on glassy carbon electrode was constructed. The surface morphology of the composite- modified electrode was characterized by scanning electron microscopy, and the electrochemical response behavior and electrocatalytic oxidation mechanism of nitrite were investigated by cyclic voltammetry. The high surface-to-volume ratio of MWCNTs and PTB brings the electrochemical sensing unit and nitrite in full contact. This renders the electrochemical response extremely sensitive to nitrite. Under the optimal measurement conditions and a working voltage of 0.73 V (vs. SCE), a linear relationship is obtained between the oxidation peak current and nitrite concentration in the range of 39 nM–1.1 mM, and the limit of detection is lowered to 19 nM (at an S/N ratio of 3). The sensor was successfully applied to the determination of nitrite in greenhouse soils. (author)

Norepinephrine-modified glassy carbon electrode for the simultaneous determination of ascorbic acid and uric acid

International Nuclear Information System (INIS)

Zare, H.R.; Memarzadeh, F.; Ardakani, M. Mazloum; Namazian, M.; Golabi, S.M.

2005-01-01

The oxidation of norepinephrine (NE) on a preactivated glassy carbon electrode leads to the formation of a deposited layer of about 4.2 x 10 -10 mol cm -2 at the surface of the electrode. The electron transfer rate constant, k s , and charge transfer coefficient, α, for electron transfer between the electrode and immobilized NE film were calculated as 44 s -1 and 0.46, respectively. The NE-modified glassy carbon electrode exhibited good electrocatalytic properties towards ascorbic acid (AA) oxidation in phosphate buffer (pH 7.0) with an overpotential of about 475 mV lower than that of the bare electrode. The electrocatalytic response was evaluated by cyclic voltammetry, chronoamperometry, amperometry and rotating disk voltammetry. The overall number of electrons involved in the catalytic oxidation of AA and the number of electrons involved in the rate-determining step are 2 and 1, respectively. The rate constant for the catalytic oxidation of AA was evaluated by RDE voltammetry and an average value of k h was found to be 8.42 x 10 3 M -1 s -1 . Amperometric determination of AA in stirred solution exhibits a linear range of 2.0-1300.0 μM (correlation coefficient 0.9999) and a detection limit of 0.076 μM. The precision of amperometry was found to be 1.9% for replicate determination of a 49.0 μM solution of AA (n = 6). In differential pulse voltammetric measurements, the NE-modified glassy carbon electrode can separate the AA and uric acid (UA) signals. Ascorbic acid oxidizes at more negative potential than UA. Also, the simultaneous determination of UA and AA is achieved at the NE-modified electrode

Design of a candidate vibrational signal for mating disruption against the glassy-winged sharpshooter, Homalodisca Vitripennis

Science.gov (United States)

The glassy-winged sharpshooter (GWSS), Homalodisca vitripennis, is an important pest of grapevines due to its ability to transmit Xylella fastidiosa, the causal agent of Pierce’s disease. GWSS mating communication is based on vibrational signals; therefore, vibrational mating disruption could be an ...

In situ nanocalorimetry of thin glassy organic films

Science.gov (United States)

León-Gutierrez, E.; Garcia, G.; Lopeandía, A. F.; Fraxedas, J.; Clavaguera-Mora, M. T.; Rodríguez-Viejo, J.

2008-11-01

In this work, we describe the design and first experimental results of a new setup that combines evaporation of liquids in ultrahigh vacuum conditions with in situ high sensitivity thermal characterization of thin films. Organic compounds are deposited from the vapor directly onto a liquid nitrogen cooled substrate, permitting the preparation and characterization of glassy films. The substrate consists of a microfabricated, membrane-based nanocalorimeter that permits in situ measurements of heat capacity under ultrafast heating rates (up to 105 K/s) in the temperature range of 100-300 K. Three glass forming liquids—toluene, methanol, and acetic acid—are characterized. The spikes in heat capacity related to the glass-transition temperature, the fictive temperature and, in some cases, the onset temperature of crystallization are determined for several heating rates.

Fabrication of β-cyclodextrin-coated poly (diallyldimethylammonium chloride)-functionalized graphene composite film modified glassy carbon-rotating disk electrode and its application for simultaneous electrochemical determination colorants of sunset yellow and tartrazine.

Science.gov (United States)

Ye, Xiaoliang; Du, Yongling; Lu, Daban; Wang, Chunming

2013-05-24

We proposed a green and facile approach for the synthesis of β-cyclodextrin-coated poly(diallyldimethylammonium chloride)-functionalized graphene composite film (β-CD-PDDA-Gr) by using L-ascorbic acid (L-AA) as the reducing agent at room temperature. The β-CD-PDDA-Gr composite film modified glassy carbon-rotating disk electrode (GC-RDE) was then developed for the sensitive simultaneous determination of two synthetic food colorants: sunset yellow (SY) and tartrazine (TT). By cyclic voltammetry (CV), the peak currents of SY and TT increased obviously on the developed electrochemical sensor. The kinetic parameters, such as diffusion coefficient D and standard heterogeneous rate constant kb, were estimated by linear sweep voltammetry (LSV). Under the optimal conditions, the differential pulse voltammetry (DPV) signals of SY and TT on the β-CD-PDDA-Gr modified GC-RDE were significantly enhanced. The enhanced anodic peak currents represented the excellent analytical performance of simultaneous detection of SY and TT in the range of 5.0×10(-8) to 2.0×10(-5) mol L(-1), with a low limit of detection (LOD) of 1.25×10(-8) mol L(-1) for SY and 1.43×10(-8) mol L(-1) for TT (SN(-1)=3). This proposed method displayed outstanding selectivity, good stability and acceptable repeatability and reproducibility, and also has been used to simultaneously determine SY and TT in some commercial soft drinks with satisfactory results. The obtained results were compared to HPLC of analysis for those two colorants and no significant differences were found. By the treatment of the experimental data, the electrochemical reaction mechanisms of SY and TT both involved a one-electron-one-proton-transfer process. Copyright © 2013 Elsevier B.V. All rights reserved.

Development of tantalum oxynitride thin films produced by PVD: Study of structural stability

Energy Technology Data Exchange (ETDEWEB)

Cristea, D. [Centro de Física, Universidade do Minho, Campus de Gualtar, 4710-057 Braga (Portugal); Department of Materials Science, Transylvania University, 500036 Brasov (Romania); Crisan, A. [Department of Materials Science, Transylvania University, 500036 Brasov (Romania); Barradas, N.P.; Alves, E. [Instituto Superior Técnico, Universidade Técnica de Lisboa Estrada Nacional 10, ao km 139,7 2695-066, Bobadela LRS (Portugal); Moura, C.; Vaz, F. [Centro de Física, Universidade do Minho, Campus de Gualtar, 4710-057 Braga (Portugal); Cunha, L., E-mail: lcunha@fisica.uminho.pt [Centro de Física, Universidade do Minho, Campus de Gualtar, 4710-057 Braga (Portugal)

2013-11-15

The purpose of this work is to study the evolution of the structure and of the thermal stability of a group of tantalum oxynitride thin films, prepared by magnetron sputtering, under the influence of vacuum annealing, up to a temperature of 800 °C. When varying the partial pressure of the reactive gases (P{sub O{sub 2+N{sub 2}}}), during the deposition process, the films change from a structure with a combination of poorly developed crystallites of the tetragonal β-Ta and of the face centred cubic (fcc) Ta(O,N) phases, for the films deposited with low P{sub O2+N2}, to a quasi-amorphous structure, for the films deposited with highest pressures. For intermediate pressures, the films reveal the presence of the fcc-Ta(O,N) structure. This structure corresponds to O atoms substituting some of the N atoms on the fcc-TaN structure and/or N atoms substituting O atoms of the fcc-γ-TaO structure. When subjected to the thermal annealing at 700 °C or higher, the film produced with lowest partial pressure revealed a remarkable structural change. New diffraction peaks appear and can only be attributed to a sub-stoichiometric hexagonal tantalum nitride structure. The film did not reveal any signs of delamination or cracks after all annealing temperatures. The two films produced with highest partial pressure proved to be the most stable. Structurally, they maintain the amorphous structure after all the annealing treatments and, in addition, no cracks or delamination were detected.

Joining of SiCf/SiC composites for thermonuclear fusion reactors

International Nuclear Information System (INIS)

Ferraris, M.; Badini, C.; Montorsi, M.; Appendino, P.; Scholz, H.W.

1994-01-01

Due to their favourable radiological behaviour, SiC f /SiC composites are promising structural materials for future use in fusion reactors. A problem to cope with is the joining of the ceramic composite material (CMC) to itself for more complex structures. Maintenance concepts for a reactor made of SiC f /SiC will demand a method of joining. The joining agents should comply with the low-activation approach of the base material. With the acceptable elements Si and Mg, sandwich structures of composite/metal/composite were prepared in Ar atmosphere at temperatures just above the melting points of the metals. Another promising route is the use of joining agents of boro-silicate glasses: their composition can be tailored to obtain softening temperatures of interest for fusion applications. The glassy joint can be easily ceramised to improve thermomechanical properties. The joining interfaces were investigated by SEM-EDS, XRD and mechanical tests. ((orig.))

De-chlorination and solidification of radioactive LiCl waste salt by using SiO{sub 2}-Al{sub 2}O{sub 3}-P{sub 2}O{sub 5} (SAP) inorganic composite including B{sub 2}O{sub 3} component

Energy Technology Data Exchange (ETDEWEB)

Lee, Ki Rak; Park, Hwan-Seo; Cho, In-Hak; Choi, Jung-Hoon; Eun, Hee-Chul; Lee, Tae-Kyo; Han, Seung Youb; Ahn, Do-Hee [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

2017-09-15

SAP (SiO{sub 2}-Al{sub 2}O{sub 3}-P{sub 2}O{sub 5}) composite has been recently studied in KAERI to deal with the immobilization of radioactive salt waste, one of the most problematic wastes in the pyro-chemical process. Highly unstable salt waste was successfully converted into stable compounds by the dechlorination process with SAPs, and then a durable waste form with a high waste loading was produced when adding glassy materials to dechlorination product. In the present study, U-SAP composite which is SAP bearing glassy component (Boron) was synthesized to remove the adding and mixing steps of glassy materials for a monolithic wasteform. With U-SAPs prepared by a sol-gel process, a series of wasteforms were fabricated to identify a proper reaction condition. Physical and chemical properties of dechlorination products and U-SAP wasteforms were characterized by XRD, DSC, SEM, TGA and PCT-A. A U-SAP wasteform showed suitable properties as a radioactive wasteform such as dense surface morphology, high waste loading, and high durability at the optimized U-SAP/salt ratio 2.

Fine kinetics of natural physical ageing in glassy As10Se90

International Nuclear Information System (INIS)

Balitska, V.; Golovchak, R.; Kozdras, A.; Shpotyuk, O.

2014-01-01

Sigmoid behavior of natural physical ageing in glassy As 10 Se 90 reveals multi-step-wise growing kinetics of enthalpy losses. Phenomenological description of this kinetics can be adequately developed in terms of first-order relaxation processes, tending atomic structure from initial towards more thermodynamically equilibrium state. This kinetics is shown to obey characteristic stretched exponential behavior originated from a number of growing steps, attributed to the interconnected processes of chalcogen chain alignment and cooperative shrinkage of glass network

The Effects of Cooling Rate on the Microstructure and Mechanical Properties of Ti{sub 4}0Zr{sub 1}0Cu{sub 3}6Pd{sub 1}4 Metallic Glass Matrix Composites

Energy Technology Data Exchange (ETDEWEB)

Park, Seon Yong; Lim, Ka Ram; Na, Young Sang; Kim, Seong Eon [Korea Institute of Materials Science, Changwon (Korea, Republic of); Choi, Youn Suk [Pusan National University, Busan (Korea, Republic of)

2016-11-15

In this paper, we demonstrate that the microstructure and mechanical properties in the Ti{sub 4}0Zr{sub 1}0Cu{sub 3}6Pd{sub 1}4 alloy can be tailored by controlling the cooling rate during solidification. A lower cooling rate increases the volume fraction of crystalline phase such as B2 but decreases the free volume of the glassy matrix. The increase of the B2 volume fraction can dramatically enhance the toughness of the composites, since the B2 phase is relatively ductile compared to the glassy matrix and seems to have good interface stability with the matrix. From the experimental results, it was found that there is a transition point in the plasticity of the composites depending on the cooling rate. Here, we explain how the toughness of the composites varies in accordance with the cooling rate in the Ti{sub 4}0Zr{sub 1}0Cu{sub 3}6Pd{sub 1}4 alloy system.

Gold nanoparticle/multi-walled carbon nanotube modified glassy carbon electrode as a sensitive voltammetric sensor for the determination of diclofenac sodium

International Nuclear Information System (INIS)

Afkhami, Abbas; Bahiraei, Atousa; Madrakian, Tayyebeh

2016-01-01

A simple and highly sensitive sensor for the determination of diclofenac sodium based on gold nanoparticle/multi-walled carbon nanotube modified glassy carbon electrode is reported. Scanning electron microscopy along with energy dispersive X-ray spectroscopy, electrochemical impedance spectroscopy, cyclic voltammetry and square wave voltammetry was used to characterize the nanostructure and performance of the sensor and the results were compared with those obtained at the multi-walled carbon nanotube modified glassy carbon electrode and bare glassy carbon electrode. Under the optimized experimental conditions diclofenac sodium gave linear response over the range of 0.03–200 μmol L −1 . The lower detection limits were found to be 0.02 μmol L −1 . The effect of common interferences on the current response of DS was investigated. The practical application of the modified electrode was demonstrated by measuring the concentration of diclofenac sodium in urine and pharmaceutical samples. This revealed that the gold nanoparticle/multiwalled carbon nanotube modified glassy carbon electrode shows excellent analytical performance for the determination of diclofenac sodium in terms of a very low detection limit, high sensitivity, very good accuracy, repeatability and reproducibility. - Highlights: • GCE was modified with multiwalled carbon nanotube and gold nanoparticles. • AuNP/MWCNT/GCE was used for the determination of diclofenac sodium. • Modified electrode was characterized by SEM, EDS and EIS. • The proposed method showed excellent analytical figures of merit. • This sensor was used for the determination of diclofenac sodium in real samples.

Gold nanoparticle/multi-walled carbon nanotube modified glassy carbon electrode as a sensitive voltammetric sensor for the determination of diclofenac sodium

Energy Technology Data Exchange (ETDEWEB)

Afkhami, Abbas, E-mail: afkhami@basu.ac.ir; Bahiraei, Atousa; Madrakian, Tayyebeh

2016-02-01

A simple and highly sensitive sensor for the determination of diclofenac sodium based on gold nanoparticle/multi-walled carbon nanotube modified glassy carbon electrode is reported. Scanning electron microscopy along with energy dispersive X-ray spectroscopy, electrochemical impedance spectroscopy, cyclic voltammetry and square wave voltammetry was used to characterize the nanostructure and performance of the sensor and the results were compared with those obtained at the multi-walled carbon nanotube modified glassy carbon electrode and bare glassy carbon electrode. Under the optimized experimental conditions diclofenac sodium gave linear response over the range of 0.03–200 μmol L{sup −1}. The lower detection limits were found to be 0.02 μmol L{sup −1}. The effect of common interferences on the current response of DS was investigated. The practical application of the modified electrode was demonstrated by measuring the concentration of diclofenac sodium in urine and pharmaceutical samples. This revealed that the gold nanoparticle/multiwalled carbon nanotube modified glassy carbon electrode shows excellent analytical performance for the determination of diclofenac sodium in terms of a very low detection limit, high sensitivity, very good accuracy, repeatability and reproducibility. - Highlights: • GCE was modified with multiwalled carbon nanotube and gold nanoparticles. • AuNP/MWCNT/GCE was used for the determination of diclofenac sodium. • Modified electrode was characterized by SEM, EDS and EIS. • The proposed method showed excellent analytical figures of merit. • This sensor was used for the determination of diclofenac sodium in real samples.

Encoding Gaussian Curvature in Glassy and Elastomeric Liquid Crystal Solids (Postprint)

Science.gov (United States)

2016-05-04

attention to director fields of the form n = cosψ(x2) ê1 + sinψ(x2) ê2, whose alignment angle field varies only with respect to one of the...λ−2 − λ2ν)/L2 < 0. (Online version in colour .) For a fixed two-dimensional metric, the problem of identifying equilibrium configurations that...length of 10 mm. (b) Positive (left) and negative (right) Gaussian curvature in 15µm thick glassy LC solid film at 175◦C. (Online version in colour .) (b

FTIR and Mössbauer spectroscopic study of sodium–aluminum–iron phosphate glassy materials for high level waste immobilization

Energy Technology Data Exchange (ETDEWEB)

Stefanovsky, S.V., E-mail: serge.stefanovsky@yandex.ru [Frumkin Institute of Physical Chemistry and Electrochemistry of the Russian Academy of Sciences, Laboratory of Radioecology and Radiation Problems, Moscow (Russian Federation); Stefanovsky, O.I. [Frumkin Institute of Physical Chemistry and Electrochemistry of the Russian Academy of Sciences, Laboratory of Radioecology and Radiation Problems, Moscow (Russian Federation); Remizov, M.B.; Belanova, E.A.; Kozlov, P.V. [FSUE PA Mayak, Central Plant Laboratory, Ozersk, Chelyabinsk Reg. (Russian Federation); Glazkova, Ya.S.; Sobolev, A.V.; Presniakov, I.A. [Lomonosov Moscow State University, Department of Radiochemistry (Russian Federation); Kalmykov, S.N. [Frumkin Institute of Physical Chemistry and Electrochemistry of the Russian Academy of Sciences, Laboratory of Radioecology and Radiation Problems, Moscow (Russian Federation); Lomonosov Moscow State University, Department of Radiochemistry (Russian Federation); Vernadsky Institute of Geochemistry and Analytical Chemistry of the Russian Academy of Sciences, Laboratory of Radiochemistry, Moscow (Russian Federation); Myasoedov, B.F. [Frumkin Institute of Physical Chemistry and Electrochemistry of the Russian Academy of Sciences, Laboratory of Radioecology and Radiation Problems, Moscow (Russian Federation); Vernadsky Institute of Geochemistry and Analytical Chemistry of the Russian Academy of Sciences, Laboratory of Radiochemistry, Moscow (Russian Federation)

2015-11-15

Complex sodium-aluminum-iron phosphate glassy materials with various Al{sub 2}O{sub 3} to Fe{sub 2}O{sub 3} ratio containing high level waste (HLW) surrogate were characterized by X-ray diffraction and scanning electron microscopy and studied in details by Fourier transform infrared (FTIR) spectroscopy. The samples with high Al{sub 2}O{sub 3} content and not containing Fe{sub 2}O{sub 3} were predominantly amorphous but subjected to devitrification under annealing. Addition of B{sub 2}O{sub 3} and partial Fe{sub 2}O{sub 3} substitution for Al{sub 2}O{sub 3} in the materials increases their resistance to devitrification whereas further substitution and NiO incorporation significantly increase the tendency to devitrification. FTIR spectra demonstrate changes in the structure of glassy materials caused by both structural variations in the anionic motif and occurrence of crystalline phases in the materials. According to Mössbauer spectroscopy data, iron in the glassy samples is present as octahedrally coordinated Fe{sup 3+} ions while in the partly devitrified samples iron is partitioned among vitreous and crystalline phases entering the vitreous phase mainly as Fe{sup 3+}O{sub 6} units and crystalline phases as major Fe{sup 3+} and minor Fe{sup 2+} ions in a magnetically ordered state and participating in a “fast” electronic exchange.

Layer-by-layer construction of graphene/cobalt phthalocyanine composite film on activated GCE for application as a nitrite sensor

International Nuclear Information System (INIS)

Cui, Lili; Pu, Tao; Liu, Ying; He, Xingquan

2013-01-01

Graphical abstract: A novel nitrite sensor was prepared by using LBL technique which for the first time used the activated positively charged glassy carbon electrode (A-GCE) as the substrate. The nitrite sensor shows super stability for consecutive CV testing and rather low detection limit. -- Abstract: In this paper, a novel graphene/cobalt phthalocyanine composite film was prepared by layer-by-layer (LBL) technique which for the first time used the activated positively charged glassy carbon electrode (A-GCE) as the substrate. The surface morphology of graphene/cobalt phthalocyanine composite film was characterized by scanning electron microscopy (SEM) and atomic force microscope (AFM). It is found that graphene/cobalt phthalocyanine composite film modified GCE exhibits good catalytic activity toward the oxidation of nitrite. The oxidation current barely decreases in consecutive CV test. Furthermore, the modified GCE shows long-term stability after 70 days. The super good stability can be attributed to the immobilization and dispersion of electroactive cobalt phthalocyanine by graphene, and using A-GCE as substrate which can enhance the interaction force between GCE and electroactive cobalt phthalocyanine. The nitrite sensor shows rather low detection limit of 0.084 μM at a signal-to-noise ratio = 3 (S/N = 3)

Electrochemical immunoassay for the carcinoembryonic antigen based on the use of a glassy carbon electrode modified with an octahedral Cu2O-gold nanocomposite and staphylococcal protein for signal amplification.

Science.gov (United States)

Qin, Zhen; Xu, Wei; Chen, Shuai; Chen, Jun; Qiu, Jing Fu; Li, Chao Rui

2018-04-24

The authors describe an electrochemical immunoassay for ultrasensitive direct determination of the carcinoembryonic antigen (CEA). A nanocomposite consisting of octahedral Cu2O nanocrystals covered with gold nanoparticles was utilized to modify a glassy carbon electrode which gives a strongly enhanced chronoamperometric signal for H 2 O 2 which is used as an electrochemical probe. The morphology and elemental composition of the the nanocomposite was studied by field emission scanning electron microscopy and energy dispersive X-ray spectroscopy. In addition, staphylococcal protein A was placed on the electrode for efficient capture of antibody to further enhance the sensitivity of the assay. Under optimal conditions and at a typical working voltage of -0.4 V (vs. Ag/AgCl), the response covers the 2 pg·mL -1 to 20 ng·mL -1 CEA concentration range with a 200 fg·mL -1 lower detection limit. The method was successfully applied to the determination of CEA in (spiked) human serum. Graphical abstract Schematic of the fabrication of an electrochemical immunosensor for ultrasensitive detection the carcinoembryonic antigen. The sensor is based on the use of a glassy carbon electrode modified with an octahedral Cu 2 O-gold nanocomposite and staphylococcal protein A for signal amplification.

Intermixing of InGaAs/GaAs quantum wells and quantum dots using sputter-deposited silicon oxynitride capping layers

International Nuclear Information System (INIS)

McKerracher, Ian; Fu Lan; Hoe Tan, Hark; Jagadish, Chennupati

2012-01-01

Various approaches can be used to selectively control the amount of intermixing in III-V quantum well and quantum dot structures. Impurity-free vacancy disordering is one technique that is favored for its simplicity, however this mechanism is sensitive to many experimental parameters. In this study, a series of silicon oxynitride capping layers have been used in the intermixing of InGaAs/GaAs quantum well and quantum dot structures. These thin films were deposited by sputter deposition in order to minimize the incorporation of hydrogen, which has been reported to influence impurity-free vacancy disordering. The degree of intermixing was probed by photoluminescence spectroscopy and this is discussed with respect to the properties of the SiO x N y films. This work was also designed to monitor any additional intermixing that might be attributed to the sputtering process. In addition, the high-temperature stress is known to affect the group-III vacancy concentration, which is central to the intermixing process. This stress was directly measured and the experimental values are compared with an elastic-deformation model.

Perovskite oxynitride LaTiO{sub x}N{sub y} thin films: Dielectric characterization in low and high frequencies

Energy Technology Data Exchange (ETDEWEB)

Lu, Y.; Ziani, A. [Institut d' Electronique et de Telecommunications de Rennes (IETR) UMR-CNRS 6164, groupe ' Antennes et Hyperfrequences' , University of Rennes 1, UEB, IUT Saint Brieuc, 18 rue Henri Wallon, 22004 Saint Brieuc cedex (France); Le Paven-Thivet, C., E-mail: claire.lepaven@univ-rennes1.fr [Institut d' Electronique et de Telecommunications de Rennes (IETR) UMR-CNRS 6164, groupe ' Antennes et Hyperfrequences' , University of Rennes 1, UEB, IUT Saint Brieuc, 18 rue Henri Wallon, 22004 Saint Brieuc cedex (France); Benzerga, R.; Le Gendre, L. [Institut d' Electronique et de Telecommunications de Rennes (IETR) UMR-CNRS 6164, groupe ' Antennes et Hyperfrequences' , University of Rennes 1, UEB, IUT Saint Brieuc, 18 rue Henri Wallon, 22004 Saint Brieuc cedex (France); Fasquelle, D. [Laboratoire d' Etude des Materiaux et des Composants pour l' Electronique (LEMCEL) UPRES-EA 2601, University of Littoral-Cote d' Opale, 50 rue Ferdinand Buisson, F-62228 Calais cedex (France); Kassem, H. [Laboratoire de l' Integration du Materiau au Systeme(IMS) UMR-CNRS 5218, groupe Materiaux, University of Bordeaux 1, 16 avenue Pey-Berland, 33607 Pessac (France); and others

2011-11-01

Lanthanum titanium oxynitride (LaTiO{sub x}N{sub y}) thin films are studied with respect to their dielectric properties in low and high frequencies. Thin films are deposited by radio frequency magnetron sputtering on different substrates. Effects of nitrogen content and crystalline quality on dielectric properties are investigated. In low-frequency range, textured LaTiO{sub x}N{sub y} thin films deposited on conductive single crystal Nb-STO show a dielectric constant {epsilon} Prime Almost-Equal-To 140 with low losses tan{delta} = 0.012 at 100 kHz. For the LaTiO{sub x}N{sub y} polycrystalline films deposited on conductive silicon substrates with platinum (Pt/Ti/SiO{sub 2}/Si), the tunability reached up to 57% for a weak electric field of 50 kV/cm. In high-frequency range, epitaxial LaTiO{sub x}N{sub y} films deposited on MgO substrate present a high dielectric constant with low losses ({epsilon} Prime Almost-Equal-To 170, tan{delta} = 0.011, 12 GHz).

Cytochrome C Dynamics at Gold and Glassy Carbon Surfaces Monitored by in Situ Scanning Tunnel Microscopy

DEFF Research Database (Denmark)

Andersen, Jens Enevold Thaulov; Møller, Per; Pedersen, Marianne Vind

1995-01-01

We have investigated the absorption of cytochrome c on gold and glassy carbon substrates by in situ scanning tunnel microscopy under potentiostatic control of both substrate and tip. Low ionic strength and potential ranges where no Faradaic current flows were used. Cyt c aggregates into flat...

Carbon composite micro- and nano-tubes-based electrodes for detection of nucleic acids

Directory of Open Access Journals (Sweden)

Huska Dalibor

2011-01-01

Full Text Available Abstract The first aim of this study was to fabricate vertically aligned multiwalled carbon nanotubes (MWCNTs. MWCNTs were successfully prepared by using plasma enhanced chemical vapour deposition. Further, three carbon composite electrodes with different content of carbon particles with various shapes and sizes were prepared and tested on measuring of nucleic acids. The dependences of adenine peak height on the concentration of nucleic acid sample were measured. Carbon composite electrode prepared from a mixture of glassy and spherical carbon powder and MWCNTs had the highest sensitivity to nucleic acids. Other interesting result is the fact that we were able to distinguish signals for all bases using this electrode.

Crystallization processes in Ni-Ti-B glassy alloys of near-ternary-eutectic composition

International Nuclear Information System (INIS)

Merk, N.; Morris, D.G.; Stadelmann, P.

1987-01-01

The crystallization kinetics and mechanisms of three Ni-Ti-B glasses have been examined with a view to elucidating the roles of chemical composition and quenched structure on behaviour. Alloys of composition near a ternary-eutectic point have been chosen because they represent a real and complex situation where several crystalline phases may form simultaneously. Crystallization processes are analysed in terms of nucleation and growth stages. Different nucleation mechanisms seem to be best explained in terms of the short range ordered structure of the quenched glass. Analysis of crystal glass interface energies indicates that it is not this energy term which controls the nucleation of crystals on annealing. Crystal growth may involve a eutectic mechanism or a single-phase mechanism controlled by interface or matrix-diffusion kinetics. Crystallization is fastest when eutectic nucleation and growth occurs. Formation of the eutectic colony requires the initial formation of the phase of complex structure followed by the phase of simpler structure

Electrochemical behavior of cysteine at a CuGeO3 nanowires modified glassy carbon electrode

International Nuclear Information System (INIS)

Dong Yongping; Pei Lizhai; Chu Xiangfeng; Zhang Wangbing; Zhang Qianfeng

2010-01-01

A CuGeO 3 nanowire modified glassy carbon electrode was fabricated and characterized by scanning electron microscopy. The results of electrochemical impedance spectroscopy reveal that electron transfer through nanowire film is facile compared with that of bare glassy carbon electrode. The modified electrode exhibited a novel electrocatalytic behavior to the electrochemical reactions of L-cysteine in neutral solution, which was not reported previously. Two pairs of semi-reversible electrochemical peaks were observed and assigned to the processes of oxidation/reduction and adsorption/desorption of cysteine at the modified electrode, respectively. The electrochemical response of cysteine is poor in alkaline condition and is enhanced greatly in acidic solution, suggesting that hydrogen ions participate in the electrochemical oxidation process of cysteine. The intensities of two anodic peaks varied linearly with the concentration of cysteine in the range of 1 x 10 -6 to 1 x 10 -3 mol L -1 , which make it possible to sensitive detection of cysteine with the CuGeO 3 nanowire modified electrode. Furthermore, the modified electrode exhibited good reproducibility and stability.

Novel catalysts for upgrading coal-derived liquids. Final technical progress report

Energy Technology Data Exchange (ETDEWEB)

Thompson, L.T.; Savage, P.E.; Briggs, D.E.

1995-03-31

Research described in this report was aimed at synthesizing and evaluating supported Mo oxynitrides and oxycarbides for the selective removal of nitrogen, sulfur and oxygen from model and authentic coal-derived liquids. The Al{sub 2}O{sub 3}-supported oxynitrides and oxycarbides were synthesized via the temperature programmed reaction of supported molybdenum oxides or hydrogen bronzes with NH{sub 3} or an equimolar mixture of CH{sub 4} and H{sub 2}. Phase constituents and composition were determined by X-ray diffraction, CHN analysis, and neutron activation analysis. Oxygen chemisorption was used to probe the surface structure of the catalysts. The reaction rate data was collected using specially designed micro-batch reactors. The Al{sub 2}O{sub 3}-supported Mo oxynitrides and oxycarbides were competitively active for quinoline hydrodenitrogenation (HDN), benzothiophene hydrodesulfurization (HDS) and benzofuran hydrodeoxygenation (HDO). In fact, the HDN and HDO specific reaction rates for several of the oxynitrides and oxycarbides were higher than those of a commercial Ni-Mo/Al{sub 2}O{sub 3} hydrotreatment catalyst. Furthermore, the product distributions indicated that the oxynitrides and oxycarbides were more hydrogen efficient than the sulfide catalysts. For HDN and HDS the catalytic activity was a strong inverse function of the Mo loading. In contrast, the benzofuran hydrodeoxygenation (HDO) activities did not appear to be affected by the Mo loading but were affected by the heating rate employed during nitridation or carburization. This observation suggested that HDN and HDS occurred on the same active sites while HDO was catalyzed by a different type of site.

Thermal Stability and Flammability of Styrene-Butadiene Rubber-Based (SBR Ceramifiable Composites

Directory of Open Access Journals (Sweden)

Rafał Anyszka

2016-07-01

Full Text Available Ceramifiable styrene-butadiene (SBR-based composites containing low-softening-point-temperature glassy frit promoting ceramification, precipitated silica, one of four thermally stable refractory fillers (halloysite, calcined kaolin, mica or wollastonite and a sulfur-based curing system were prepared. Kinetics of vulcanization and basic mechanical properties were analyzed and added as Supplementary Materials. Combustibility of the composites was measured by means of cone calorimetry. Their thermal properties were analyzed by means of thermogravimetry and specific heat capacity determination. Activation energy of thermal decomposition was calculated using the Flynn-Wall-Ozawa method. Finally, compression strength of the composites after ceramification was measured and their micromorphology was studied by scanning electron microscopy. The addition of a ceramification-facilitating system resulted in the lowering of combustibility and significant improvement of the thermal stability of the composites. Moreover, the compression strength of the mineral structure formed after ceramification is considerably high. The most promising refractory fillers for SBR-based ceramifiable composites are mica and halloysite.

A study on enhancement of Np extraction by TBP through the electrochemical adjustment of Np valance by using a glassy carbon fiber column electrode system

International Nuclear Information System (INIS)

Kim, K. W.; Song, K. C.; Lee, I. H.; Choi, I. K.; Yoo, J. H.

1999-01-01

The Np valance state in nitric acid and the effect of nitrous acid on the Np valance composition were studied through ways of absorbance by spectrophotometer, extraction by TBP, and electrochemistry. Enhancement of Np extraction to 30 vol.% TBP was carried out through adjustment of Np valance state by using a glassy carbon fiber column electrode system. The Np solution used in this work consisted of only Np(V) and Np(VI) without Np(IV). The composition of Np(V) in the range of 0.5M ∼ 5.5 M nitric acid was 32% ∼ 19%. The electrolytic oxidation of Np(V) coexisting with Np(VI) in the solution enhanced Np extraction by 30 vol.% TBP about five times more than the one without the electrolytic oxidation. The facts were confirmed that the nitrous acid of less than about 10 -5 M acted as a catalyst to accelerate the chemical oxidation reaction of Np(V) to Np(VI) and the nitrous acid of more than 10 -3 M reduced Np(VI) to Np(V) reversely

Glassy and Metastable Crystalline BaTi2O5 by Containerless Processing

Science.gov (United States)

Yoda, Shinichi; Kentei Yu, Yu; Kumar, Vijaya; Kameko, Masashi

Many efforts have been devoted to forming bulk glass from the melt of ferroelectric crystalline materials without adding any network-forming oxides such as SiO2 due to the potential for producing transparent glass ceramics with high dielectric constant and enhanced piezoelectric, pyroelectric and electro-optic use. The containerless processing is an attractive synthesis tech-nique as it can prevent melt contamination, minimize heterogeneous nucleation, and allow melt to achieve deep undercooling for forming metastable and glassy materials. We have fabricated a new ferroelectric materiel BaTi2 O5 [1] as bulk glass from melt by us-ing containerless processing and studied the phase relationship between microstructure and ferroelectric properties of BaTi2 O5 [2]. The structures of glassy and metastable crystalline BaTi2 O5 fabricated by the containerless pro-cessing were comprehensively investigated by combined X-ray and neutron diffractions, XANES analyses and computer simulations [3]. The 3-dimensional atomic structure of glassy BaTi2 O5 (g-BaTi2 O5 ), simulated by Reverse Monte Carlo (RMC) modelling on diffraction data, shows that extremely distorted TiO5 polyhedra interconnected with both corner-and edge-shared oxy-gen, formed a higher packing density structure than that of conventional silicate glass linked with only corner-sharing of SiO4 polyhedra. In addition, XANES measurement reveales that five-coordinated TiO5 polyhedra were formable in the crystallized metastable a-and b-BaTi2 O5 phases. The structure of metastable b-BaTi2 O5 was solved by ab initio calculation, and refined by Rietveld refinement as group Pnma with unit lattices a = 10.23784 ˚, b = 3.92715 ˚, c A A = 10.92757 A ˚. Our results show that the glass-forming ability enhanced by containerless pro-cessing, not by `strong glass former', fabricated new bulk oxide glasses with peculiar structures and properties. The intermediate-range structure of g-BaTi2 O5 and the crystalline structure of

Electrochemical evaluation and determination of antiretroviral drug fosamprenavir using boron-doped diamond and glassy carbon electrodes.

Science.gov (United States)

Gumustas, Mehmet; Ozkan, Sibel A

2010-05-01

Fosamprenavir is a pro-drug of the antiretroviral protease inhibitor amprenavir and is oxidizable at solid electrodes. The anodic oxidation behavior of fosamprenavir was investigated using cyclic and linear sweep voltammetry at boron-doped diamond and glassy carbon electrodes. In cyclic voltammetry, depending on pH values, fosamprenavir showed one sharp irreversible oxidation peak or wave depending on the working electrode. The mechanism of the oxidation process was discussed. The voltammetric study of some model compounds allowed elucidation of the possible oxidation mechanism of fosamprenavir. The aim of this study was to determine fosamprenavir levels in pharmaceutical formulations and biological samples by means of electrochemical methods. Using the sharp oxidation response, two voltammetric methods were described for the determination of fosamprenavir by differential pulse and square-wave voltammetry at the boron-doped diamond and glassy carbon electrodes. These two voltammetric techniques are 0.1 M H(2)SO(4) and phosphate buffer at pH 2.0 which allow quantitation over a 4 x 10(-6) to 8 x 10(-5) M range using boron-doped diamond and a 1 x 10(-5) to 1 x 10(-4) M range using glassy carbon electrodes, respectively, in supporting electrolyte. All necessary validation parameters were investigated and calculated. These methods were successfully applied for the analysis of fosamprenavir pharmaceutical dosage forms, human serum and urine samples. The standard addition method was used in biological media using boron-doped diamond electrode. No electroactive interferences from the tablet excipients or endogenous substances from biological material were found. The results were statistically compared with those obtained through an established HPLC-UV technique; no significant differences were found between the voltammetric and HPLC methods.

Adsorptive stripping differential pulse voltammetric determination of venlafaxine and desvenlafaxine employing Nafion-carbon nanotube composite glassy carbon electrode

Energy Technology Data Exchange (ETDEWEB)

Sanghavi, Bankim J. [Department of Chemistry, University of Mumbai, Vidyanagari, Santacruz (East), Mumbai 400 098, Maharashtra (India); Srivastava, Ashwini K., E-mail: aksrivastava@chem.mu.ac.i [Department of Chemistry, University of Mumbai, Vidyanagari, Santacruz (East), Mumbai 400 098, Maharashtra (India)

2011-04-15

A Nafion-carbon nanotube-modified glassy carbon electrode (NAF-CNT-GCE) was developed for the determination of venlafaxine (VF) and desvenlafaxine (DVF). The electrochemical behavior of both these molecules was investigated employing cyclic voltammetry (CV), chronocoulometry (CC), electrochemical impedance spectroscopy (EIS) and adsorptive stripping differential pulse voltammetry (AdSDPV). The surface morphology of the electrodes has been studied by means of scanning electron microscopy (SEM). These studies revealed that the oxidation of VF and DVF is facilitated at NAF-CNT-GCE. After optimization of analytical conditions employing this electrode at pH 7.0 in Britton-Robinson buffer (0.05 M) for VF and pH 5.0 in acetate buffer (0.1 M) for DVF, the peak currents for both the molecules were found to vary linearly with their concentrations in the range of 3.81 x 10{sup -8}-6.22 x 10{sup -5} M for VF and 5.33 x 10{sup -8}-3.58 x 10{sup -5} M for DVF. The detection limits (S/N = 3) of 1.24 x 10{sup -8} and 2.11 x 10{sup -8} M were obtained for VF and DVF, respectively, using AdSDPV. The prepared modified electrode showed several advantages, such as simple preparation method, high sensitivity, very low detection limits and excellent reproducibility. The proposed method was employed for the determination of VF and DVF in pharmaceutical formulations, urine and blood serum samples.

Compositional dependence of physical properties in Se-Sb-In glassy system

Energy Technology Data Exchange (ETDEWEB)

Sharma, Shaveta, E-mail: shaveta.sharma1987@yahoo.com; Sharma, Rita; Kumar, Praveen; Chander, Ravi; Thangaraj, R.; Mian, M. [Semiconductors Laboratory, Department of Physics, GND University, Amritsar (India)

2015-08-28

The growing interest in the investigation of the properties of chalcogenide glasses stems from their potential application as phase change recording media and photoconductive elements in solid state devices.In the present work, the different theoretical parameters viz. coordination number, constraints, number of lone pair electrons, bond energy, heat of atomization, mean bond energy and glass transition temperature for Se{sub 75-x}Sb{sub 25}In{sub x} (x= 0, 1, 3, 5, 7, 9, 11) chalcogenide system have been calculated and their composition variation has been discussed. It has been found that average heat of atomization increases with In content. The glass transition temperature and mean bond energy increases with In. An attempt has been made to explain the varying trend of various parameters with increasing In content.

Partially and fully de-alloyed glassy ribbons based on Au: Application in methanol electro-oxidation studies

Energy Technology Data Exchange (ETDEWEB)

Paschalidou, Eirini Maria, E-mail: epaschal@unito.it [Dipartimento di Chimica e Centro Interdipartimentale NIS (Nanostructured Surfaces and Interfaces), Università di Torino, Via Pietro Giuria 7, 10125, Torino (Italy); Scaglione, Federico [Dipartimento di Chimica e Centro Interdipartimentale NIS (Nanostructured Surfaces and Interfaces), Università di Torino, Via Pietro Giuria 7, 10125, Torino (Italy); Gebert, Annett; Oswald, Steffen [Leibniz Institut für Festkörper- und Werkstoffforschung IFW, Helmholtzstraße 20, 01069, Dresden (Germany); Rizzi, Paola; Battezzati, Livio [Dipartimento di Chimica e Centro Interdipartimentale NIS (Nanostructured Surfaces and Interfaces), Università di Torino, Via Pietro Giuria 7, 10125, Torino (Italy)

2016-05-15

In this work, electrochemical de-alloying of an amorphous alloy, Au{sub 40}Cu{sub 28}Ag{sub 7}Pd{sub 5}Si{sub 20}, cast in ribbon form by melt spinning, has been performed, obtaining self standing nanoporous materials suitable for use as electrodes for electrocatalytic applications. The de-alloying encompasses removal of less noble elements and the crystallization of Au, resulting in interconnected ligaments whose size and morphology are described as a function of time. Depending on de-alloying time, the crystals may contain residual amounts of Cu, Ag and Pd, as shown by Auger Electron Spectroscopy (AES), Energy Dispersive Spectroscopy (EDS) and Cyclic Voltammetry (CV) in a basic solution. Current density peaks in the 0.16–0.28 V range (vs Ag/AgCl) indicate that the porous ribbons are active for the electro-oxidation of methanol. The partially de-alloyed samples, which still partially contain the amorphous phase because of the shorter etching times, have finer ligaments and display peaks at lower potential. However, the current density decreases rapidly during repeated potential scans. This is attributed to the obstruction of Au sites, mainly by the Cu oxides formed during the scans. The fully de-alloyed ribbons display current peaks at about 0.20 V and remain active for hundreds of scans at more than 60% of the initial current density. They can be fully re-activated to achieve the same performance levels after a brief immersion in nitric acid. The good activity is due to trapped Ag and Pd atoms in combination with ligament morphology. - Graphical abstract: Fine ligaments and pores made by de-alloying a glassy ribbon of a Au-based alloy, homogeneously produced across the thickness (25 μm) for studying methanol's electro-oxidation behavior. - Highlights: • Size and composition of nanoporous layers tailored in de-alloying Au-based glassy ribbons. • From amorphous precursor fine crystals occur in ligaments with residual Pd and Ag. • Fully de

Non-Gaussian nature of glassy dynamics by cage to cage motion

International Nuclear Information System (INIS)

Vorselaars, Bart; Lyulin, Alexey V.; Michels, M. A. J.; Karatasos, K.

2007-01-01

A model based on a single Brownian particle moving in a periodic effective field is used to understand the non-Gaussian dynamics in glassy systems of cage escape and subsequent recaging, often thought to be caused by a heterogeneous glass structure. The results are compared to molecular-dynamics simulations of systems with varying complexity: quasi-two-dimensional colloidlike particles, atactic polystyrene, and a dendritic glass. The model nicely describes generic features of all three topologically different systems, in particular around the maximum of the non-Gaussian parameter. This maximum is a measure for the average distance between cages

Electrocatalytic behahiour of cobalt tetraamino-phthalocyanine in the presence of a composite of reduced graphene nanosheets and of multi-walled carbon nanotubes

International Nuclear Information System (INIS)

Nyoni, Stephen; Nyokong, Tebello

2014-01-01

Graphical abstract: A composite of multi-walled carbon nanotubes, reduced graphene nanosheets and cobalt tetraamino phthalocyanine was used for electrode modification, resulting in a rough surface as judged by scanning electrochemical microscopy. - Highlights: • Conjugates of multi-walled carbon nanotubes and reduced graphene nanosheets were used to modify glassy carbon electrode. • The electrode was further modified with cobalt tetraamino phthalocyanine. • The modified electrode was employed for the detection of paraquat. • A mechanism for paraquat detection using the composite electrodes is proposed. - Abstract: A composite of multi-walled carbon nanotubes (MWCNT) with reduced graphene nanosheets (rGNS-2) was developed in order to minimize the restacking of the latter. The composite was used to modify a glassy carbon electrode (GCE). GCE was further modified with cobalt tetraamino phthalocyanine (CoTAPc). The modified electrode is represented as rGNS-2-MWCNT-CoTAPc-GCE. X-ray photoelectron spectroscopy, transmission electron microscopy, scanning electrochemical microscopy and Raman spectroscopy were used to explore into surface functionalities, morphology and topography of the nanocomposite. The rGNS-2-MWCNT-CoTAPc-GCE had a low limit of detection of 3.32 × 10 −8 M towards the detection of paraguat as a test analyte. A mechanism for paraquat detection using an rGNS-2-MWCNT-CoTAPc-GCE is also proposed in this work

In-Vivo Characterization of Glassy Carbon Micro-Electrode Arrays for Neural Applications and Histological Analysis of the Brain Tissue

Science.gov (United States)

Vomero, Maria

The aim of this work is to fabricate and characterize glassy carbon Microelectrode Arrays (MEAs) for sensing and stimulating neural activity, and conduct histological analysis of the brain tissue after the implant to determine long-term performance. Neural applications often require robust electrical and electrochemical response over a long period of time, and for those applications we propose to replace the commonly used noble metals like platinum, gold and iridium with glassy carbon. We submit that such material has the potential to improve the performances of traditional neural prostheses, thanks to better charge transfer capabilities and higher electrochemical stability. Great interest and attention is given in this work, in particular, to the investigation of tissue response after several weeks of implants in rodents' brain motor cortex and the associated materials degradation. As part of this work, a new set of devices for Electrocorticography (ECoG) has been designed and fabricated to improve durability and quality of the previous generation of devices, designed and manufactured by the same research group in 2014. In-vivo long-term impedance measurements and brain activity recordings were performed to test the functionality of the neural devices. In-vitro electrical characterization of the carbon electrodes, as well as the study of the adhesion mechanisms between glassy carbon and different substrates is also part of the research described in this book.

Physical properties of Zr50Cu40-xAl10Pdx bulk glassy alloys

International Nuclear Information System (INIS)

Wencka, M.; Jagodic, M.; Gradisek, A.; Kocjan, A.; Jaglicic, Z.; McGuiness, P.J.; Apih, T.; Yokoyama, Y.; Dolinsek, J.

2010-01-01

It was shown recently (Yokoyama et al. ) that the addition of a small amount of Pd to the Zr 50 Cu 40 Al 10 bulk glassy alloy (BGA) has a beneficial effect on fatigue-strength enhancement, where the composition Zr 50 Cu 37 Al 10 Pd 3 behaved in a resonant-like way by showing the highest fatigue limit of 1050 MPa and the minimum Vickers hardness. We performed a study of the magnetic properties, the specific heat, the electrical resistivity and the hydrogen-diffusion constant for a series of compositions Zr 50 Cu 40-x Al 10 Pd x (x = 0-7 at.%), in order to determine their physical properties and to check for the influence of the Pd content on these properties. The Zr 50 Cu 40-x Al 10 Pd x BGAs are nonmagnetic, conducting alloys, where the Pauli spin susceptibility of the conduction electrons is the only source of paramagnetism. The low-temperature specific heat indicates an enhancement of the conduction-electron effective mass m* below 5 K, suggesting that the Zr 50 Cu 40-x Al 10 Pd x BGAs are not free-electron-like compounds. The electrical resistivities of the Zr 50 Cu 40-x Al 10 Pd x BGAs amount to about 200 μΩ cm and show a small, negative temperature coefficient (NTC) with an increase from 300 to 2 K of 4%. The hydrogen self-diffusion constant D in hydrogen-loaded samples shows classical over-barrier-hopping temperature dependence and is of comparable magnitude to the related icosahedral and amorphous Zr 69.5 Cu 12 Ni 11 Al 7.5 hydrogen-storage alloys. No correlation between the investigated physical parameters and the Pd content of the samples could be observed.

Voltammetric behavior of sedative drug midazolam at glassy carbon electrode in solubilized systems

OpenAIRE

Jain, Rajeev; Yadav, Rajeev Kumar

2012-01-01

Redox behavior of midazolam was studied at a glassy carbon electrode in various buffer systems, supporting electrolytes and pH using differential pulse, square-wave and cyclic voltammetry. Based on its reduction behavior, a direct differential pulse voltammetric method has been developed and validated for the determination of midazolam in parenteral dosage. Three well-defined peaks were observed in 0.1% SLS, BrittonâRobinson (BR) buffer of pH 2.5. The effect of surfactants like sodium lauryl ...

Voltammetric behavior of sedative drug midazolam at glassy carbon electrode in solubilized systems

OpenAIRE

Jain, Rajeev; Yadav, Rajeev Kumar

2011-01-01

Redox behavior of midazolam was studied at a glassy carbon electrode in various buffer systems, supporting electrolytes and pH using differential pulse, square-wave and cyclic voltammetry. Based on its reduction behavior, a direct differential pulse voltammetric method has been developed and validated for the determination of midazolam in parenteral dosage. Three well-defined peaks were observed in 0.1% SLS, Britton–Robinson (BR) buffer of pH 2.5. The effect of surfactants like sodium lauryl ...

Photoluminescence, energy transfer and tunable color of Ce(3+), Tb(3+) and Eu(2+) activated oxynitride phosphors with high brightness.

Science.gov (United States)

Lü, Wei; Huo, Jiansheng; Feng, Yang; Zhao, Shuang; You, Hongpeng

2016-06-21

New tuneable light-emitting Ca3Al8Si4O17N4:Ce(3+)/Tb(3+)/Eu(2+) oxynitride phosphors with high brightness have been prepared. When doped with trivalent cerium or divalent europium they present blue luminescence under UV excitation. The energy transfer from Ce(3+) to Tb(3+) and Ce(3+) to Eu(2+) ions is deduced from the spectral overlap between Ce(3+) emission and Tb(3+)/Eu(2+) excitation spectra. The energy-transfer efficiencies and corresponding mechanisms are discussed in detail, and the mechanisms of energy transfer from the Ce(3+) to Tb(3+) and Ce(3+) to Eu(2+) ions are demonstrated to be a dipole-quadrupole and dipole-dipole mechanism, respectively, by the Inokuti-Hirayama model. The International Commission on Illumination value of color tuneable emission as well as luminescence quantum yield (23.8-80.6%) can be tuned by controlling the content of Ce(3+), Tb(3+) and Eu(2+). All results suggest that they are suitable for UV light-emitting diode excitation.

EXPERIMENTAL ANALYSIS OF BIOLOGICAL PARAMETERS AND VECTOR ABILITY OF GLASSY-WINGED SHARPSHOOTERS FROM ALLOPATRIC POPULATIONS IN CALIFORNIA

Science.gov (United States)

The glassy-winged sharpshooter (GWSS), Homalodisca vitripennis (Germar), is native to the southeastern United States and northeastern Mexico. It was detected in southern California in the late 1980s and in the San Joaquin Valley in 1999, where it transmits the bacterium Xylella fastidiosa to grapev...

Structural and surface changes in glassy carbon due to strontium implantation and heat treatment

Science.gov (United States)

Odutemowo, O. S.; Malherbe, J. B.; Prinsloo, L. C.; Njoroge, E. G.; Erasmus, R.; Wendler, E.; Undisz, A.; Rettenmayr, M.

2018-01-01

There are still questions around the microstructure of glassy carbon (GC), like the observation of the micropores. These were proposed to explain the low density of GC. This paper explains the effect of ion bombardment (200 keV Sr+, 1 × 1016 Sr+/cm2 at RT) on the microstructure of GC. TEM and AFM show that micropores in pristine GC are destroyed leading to densification of GC from 1.42 g/cm3 to 2.03 g/cm3. The amorphisation of glassy carbon was also not complete with graphitic strands embedded within the GC. These were relatively few, as Raman analysis showed that the Sr implantation resulted in a typical amorphous Raman spectrum. Annealing of the sample at 900 °C only resulted in a slight recovery of the GC structure. AFM and SEM analysis showed that the surface of the sample became rougher after Sr implantation. The roughness increased after the sample was annealed at 600 °C due to segregation of Sr towards the surface of the GC. SEM measurements of a sample with both implanted and un-implanted edges after annealing at 900 °C, showed that the high temperature heat treatment did not affect the surface topography of un-irradiated GC.

In Situ Determination of Bisphenol A in Beverage Using a Molybdenum Selenide/Reduced Graphene Oxide Nanoparticle Composite Modified Glassy Carbon Electrode

Directory of Open Access Journals (Sweden)

Rongguang Shi

2018-05-01

Full Text Available Due to the endocrine disturbing effects of bisphenol A (BPA on organisms, rapid detection has become one of the most important techniques for monitoring its levels in the aqueous solutions associated with plastics and human beings. In this paper, a glassy carbon electrode (GCE modified with molybdenum selenide/reduced graphene oxide (MoSe2/rGO was fabricated for in situ determination of bisphenol A in several beverages. The surface area of the electrode dramatically increases due to the existence of ultra-thin nanosheets in a flower-like structure of MoSe2. Adding phosphotungstic acid in the electrolyte can significantly enhance the repeatability (RSD = 0.4% and reproducibility (RSD = 2.2% of the electrode. Under the optimized condition (pH = 6.5, the linear range of BPA was from 0.1 μM–100 μM and the detection limit was 0.015 μM (S/N = 3. When using the as-prepared electrode for analyzing BPA in beverage samples without any pretreatments, the recoveries ranged from 98–107%, and the concentrations were from below the detection limit to 1.7 μM, indicating its potential prospect for routine analysis of BPA.

In Situ Determination of Bisphenol A in Beverage Using a Molybdenum Selenide/Reduced Graphene Oxide Nanoparticle Composite Modified Glassy Carbon Electrode.

Science.gov (United States)

Shi, Rongguang; Liang, Jing; Zhao, Zongshan; Liu, Yi; Liu, Aifeng

2018-05-22

Due to the endocrine disturbing effects of bisphenol A (BPA) on organisms, rapid detection has become one of the most important techniques for monitoring its levels in the aqueous solutions associated with plastics and human beings. In this paper, a glassy carbon electrode (GCE) modified with molybdenum selenide/reduced graphene oxide (MoSe₂/rGO) was fabricated for in situ determination of bisphenol A in several beverages. The surface area of the electrode dramatically increases due to the existence of ultra-thin nanosheets in a flower-like structure of MoSe₂. Adding phosphotungstic acid in the electrolyte can significantly enhance the repeatability (RSD = 0.4%) and reproducibility (RSD = 2.2%) of the electrode. Under the optimized condition (pH = 6.5), the linear range of BPA was from 0.1 μM⁻100 μM and the detection limit was 0.015 μM (S/ N = 3). When using the as-prepared electrode for analyzing BPA in beverage samples without any pretreatments, the recoveries ranged from 98⁻107%, and the concentrations were from below the detection limit to 1.7 μM, indicating its potential prospect for routine analysis of BPA.

Crystal structure study of dielectric oxynitride perovskites La{sub 1−x}Sr{sub x}TiO{sub 2+x}N{sub 1−x} (x=0, 0.2)

Energy Technology Data Exchange (ETDEWEB)

Habu, Daiki; Masubuchi, Yuji [Faculty of Engineering, Hokkaido University, N13W8, Kita-ku, Sapporo 060-8628 (Japan); Torii, Shuki [Institute of Materials Structure Science, High Energy Accelerator Organization, 203-1, Shirakata, Tokai-Mura, Naka-gun, Ibaraki 319-1106 (Japan); Kamiyama, Takashi [Institute of Materials Structure Science, High Energy Accelerator Organization, 203-1, Shirakata, Tokai-Mura, Naka-gun, Ibaraki 319-1106 (Japan); School of High Energy Accelerator Science, Sokendai (The Graduate University for Advanced Studies), Tokai 319-1106 (Japan); Kikkawa, Shinichi, E-mail: kikkawa@eng.hokudai.ac.jp [Faculty of Engineering, Hokkaido University, N13W8, Kita-ku, Sapporo 060-8628 (Japan)

2016-05-15

As is the case with SrTaO{sub 2}N, both cis-ordering of nitride anions and octahedral titling are also preferable in La{sub 1−x}Sr{sub x}TiO{sub 2+x}N{sub 1−x} (x=0, 0.2) oxynitride perovskites. A larger dielectric constant of ε{sub r}≈5.0×10{sup 3} was estimated for the pure oxynitride with x=0.2, compared with ε{sub r}≈750 for the product with x=0, by extrapolating the ε{sub r} values obtained from powders mixed with paraffin at various mixing ratios. The crystal structure of x=0.2 with larger tolerance factor than x=0 increased the octahedral tilting, which contributes to the increased dielectric constant. The increased dielectric constant supports the exchange mechanism for the dielectric property between two kinds of –Ti–N– helical coils (clockwise and anticlockwise) derived from the above cis-ordering of nitride anions. - Graphical abstract: Very large dielectric constant values were estimated for La{sub 1−x}Sr{sub x}TiO{sub 2+x}N{sub 1−x}; ε{sub r}≈5.0×10{sup 3} in x=0.2 and ε{sub r}≈750 in x=0. - Highlights: • Cis-configuration of nitride anions was confirmed in La{sub 1−x}Sr{sub x}TiO{sub 2+x}N{sub 1−x} (x=0, 0.2). • Dielectric constant values were estimated to be 750 for x=0 and 5.0×10{sup 3} for x=0.2, respectively. • The large dielectric property is to the exchange mechanism between clockwise and anticlockwise –Ti–N– coil motifs.

Influence of the Sr and Mg Alloying Additions on the Bonding Between Matrix and Reinforcing Particles in the AlSi7Mg/SiC-Cg Hybrid Composite

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Dolata A. J.

2016-06-01

Full Text Available The aim of the work was to perform adequate selection of the phase composition of the composite designated for permanent - mould casting air compressor pistons. The hybrid composites based on AlSi7Mg matrix alloy reinforced with mixture of silicon carbide (SiC and glassy carbon (Cg particles were fabricated by the stir casting method. It has been shown that the proper selection of chemical composition of matrix alloy and its modification by used magnesium and strontium additions gives possibility to obtain both the advantageous casting properties of composite suspensions as well as good bonding between particles reinforcements and matrix.

A consequence of local equilibration and heterogeneity in glassy materials

International Nuclear Information System (INIS)

Berthier, Ludovic

2003-01-01

The existence of a generalized fluctuation-dissipation theorem observed in simulations and experiments performed in various glassy materials is related to the concepts of local equilibration and heterogeneity in space. Assuming the existence of a dynamic coherence length scale up to which the system is locally equilibrated, we extend previous generalizations of the FDT relating static to dynamic quantities to the physically relevant domain where asymptotic limits of large times and sizes are not reached. The formulation relies on a simple scaling argument and thus does not have the character of a theorem. Extensive numerical simulations support this proposition. Our results quite generally apply to systems with slow dynamics, independently of the space dimensionality, the chosen dynamics or the presence of disorder

Molecular imprinted polypyrrole modified glassy carbon electrode for the determination of tobramycin

International Nuclear Information System (INIS)

Gupta, Vinod Kumar; Yola, Mehmet Lütfi; Özaltın, Nuran; Atar, Necip; Üstündağ, Zafer; Uzun, Lokman

2013-01-01

Graphical abstract: Atomic force microscopic images of (A) bare GCE and (B) TOB imprinted PPy/GCE surface. - Highlights: • Glassy carbon electrode based on molecularly imprinted polypyrrole was prepared. • The developed surfaces were characterized by AFM, FTIR, EIS and CV. • The developed nanosensor was applied to egg and milk samples. - Abstract: Over the past two decades, molecular imprinted polymers have attracted a broad interest from scientists in sensor development. In the preparation of molecular imprinted polymers the desired molecule (template) induces the creation of specific recognition sites in the polymer. In this study, the glassy carbon electrode (GCE) based on molecularly imprinted polypyrrole (PPy) was fabricated for the determination of tobramycin (TOB). The developed electrode was prepared by incorporation of a template molecule (TOB) during the electropolymerization of pyrrole on GCE in aqueous solution using cyclic voltammetry (CV) method. The performance of the imprinted and non-imprinted electrodes was evaluated by square wave voltammetry (SWV). The effect of pH, monomer and template concentrations, electropolymerization cycles on the performance of the imprinted and non-imprinted electrodes was investigated and optimized. The non-modified and TOB-imprinted surfaces were characterized by using atomic force microscopy (AFM), Fourier transform infrared spectroscopy (FTIR), electrochemical impedance spectroscopy (EIS) and CV. The linearity range of TOB was 5.0 × 10 −10 –1.0 × 10 −8 M with the detection limit of 1.4 × 10 −10 M. The developed nanosensor was applied successfully for the determination of TOB in egg and milk

Voltammetric Determination of Acetaminophen in the Presence of Codeine and Ascorbic Acid at Layer-by-Layer MWCNT/Hydroquinone Sulfonic Acid-Overoxidized Polypyrrole Modified Glassy Carbon Electrode

OpenAIRE

Shahrokhian, Saeed; Saberi, Reyhaneh-Sadat

2011-01-01

A very sensitive electrochemical sensor constructed of a glassy carbon electrode modified with a layer-by-layer MWCNT/doped-overoxidized polypyrrole (oppy/MWCNT /GCE) was used for the determination of acetaminophen (AC) in the presence of codeine and ascorbic acid (AA). In comparison to the bare glassy carbon electrode, a considerable shift in the peak potential together with an increase in the peak current was observed for AC on the surface of oppy/MWCNT/GCE, which can be related to the enla...

SeZnSb alloy and its nano tubes, graphene composites properties

Directory of Open Access Journals (Sweden)

Abhay Kumar Singh

2013-04-01

Full Text Available Composite can alter the individual element physical property, could be useful to define the specific use of the material. Therefore, work demonstrates the synthesis of a new composition Se96-Zn2-Sb2 and its composites with 0.05% multi-walled carbon nano tubes and 0.05% bilayer graphene, in the glassy form. The diffused amorphous structure of the multi walled carbon nano tubes and bilayer gaphene in the Se96-Zn2-Sb2 alloy have been analyzed by using the Raman, X-ray photoluminescence spectroscopy, Furrier transmission infrared spectra, photoluminescence, UV/visible absorption spectroscopic measurements. The diffused prime Raman bands (G and D have been appeared for the multi walled carbon nano tubes and graphene composites, while the X-ray photoluminescence core energy levels peak shifts have been observed for the composite materials. Subsequently the photoluminescence property at room temperature and a drastic enhancement (upto 80% in infrared transmission percentage has been obtained for the bilayer graphene composite, along with optical energy band gaps for these materials have been evaluated 1.37, 1.39 and 1.41 eV.

Impedance aspect of charge storage at graphite and glassy carbon electrodes in potassium hexacyanoferrate (II redox active electrolyte

Directory of Open Access Journals (Sweden)

Katja Magdić

2016-04-01

Full Text Available Different types of charge storage mechanisms at unmodified graphite vs. glassy carbon electrodes in acid sulphate supporting solution containing potassium hexacyanoferrate (II redox active electrolyte, have been revealed by electrochemical impedance spectroscopy and supported by cyclic voltammetry experiments. Reversible charge transfer of Fe(CN63-/4- redox reaction detected by assessment of CVs of glassy carbon electrode, is in impedance spectra indicated by presence of bulk diffusion impedance and constant double-layer/pseudocapacitive electrode impedance compared to that measured in the pure supporting electrolyte. Some surface retention of redox species detected by assessment of CVs of graphite electrode is in impedance spectra indicated by diffusion impedance coupled in this case by diminishing of double-layer/pseudo­capacitive impedance compared to that measured in the pure supporting electrolyte. This phenomenon is ascribed to contribution of additional pseudocapacitive impedance generated by redox reaction of species confined at the electrode surface.

Electrochemical deposition of gold nanoparticles on carbon nanotube coated glassy carbon electrode for the improved sensing of tinidazole

International Nuclear Information System (INIS)

Shahrokhian, Saeed; Rastgar, Shokoufeh

2012-01-01

The electrochemical reduction of tinidazole (TNZ) is studied on gold-nanoparticle/carbon-nanotubes (AuNP/CNT) modified glassy carbon electrodes using the linear sweep voltammetry. An electrochemical procedure was used for the deposition of gold nanoparticles onto the carbon nanotube film pre-cast on a glassy carbon electrode surface. The resulting nanoparticles were characterized by scanning electron microscopy and cyclic voltammetry. The effect of the electrodeposition conditions, e.g., salt concentration and deposition time on the response of the electrode was studied. Also, the effect of experimental parameters, e.g., potential and time of accumulation, pH of the buffered solutions and the potential sweep rate on the response is examined. Under the optimal conditions, the modified electrode showed a wide linear response toward the concentration of TNZ in the range of 0.1–50 μM with a detection limit of 10 nM. The prepared electrode was successfully applied for the determination of TNZ in pharmaceutical and clinical samples.

A 3D Microfluidic Chip for Electrochemical Detection of Hydrolysed Nucleic Bases by a Modified Glassy Carbon Electrode

Directory of Open Access Journals (Sweden)

Jana Vlachova

2015-01-01

Full Text Available Modification of carbon materials, especially graphene-based materials, has wide applications in electrochemical detection such as electrochemical lab-on-chip devices. A glassy carbon electrode (GCE modified with chemically alternated graphene oxide was used as a working electrode (glassy carbon modified by graphene oxide with sulphur containing compounds and Nafion for detection of nucleobases in hydrolysed samples (HCl pH = 2.9, 100 °C, 1 h, neutralization by NaOH. It was found out that modification, especially with trithiocyanuric acid, increased the sensitivity of detection in comparison with pure GCE. All processes were finally implemented in a microfluidic chip formed with a 3D printer by fused deposition modelling technology. As a material for chip fabrication, acrylonitrile butadiene styrene was chosen because of its mechanical and chemical stability. The chip contained the one chamber for the hydrolysis of the nucleic acid and another for the electrochemical detection by the modified GCE. This chamber was fabricated to allow for replacement of the GCE.

A 3D microfluidic chip for electrochemical detection of hydrolysed nucleic bases by a modified glassy carbon electrode.

Science.gov (United States)

Vlachova, Jana; Tmejova, Katerina; Kopel, Pavel; Korabik, Maria; Zitka, Jan; Hynek, David; Kynicky, Jindrich; Adam, Vojtech; Kizek, Rene

2015-01-22

Modification of carbon materials, especially graphene-based materials, has wide applications in electrochemical detection such as electrochemical lab-on-chip devices. A glassy carbon electrode (GCE) modified with chemically alternated graphene oxide was used as a working electrode (glassy carbon modified by graphene oxide with sulphur containing compounds and Nafion) for detection of nucleobases in hydrolysed samples (HCl pH = 2.9, 100 °C, 1 h, neutralization by NaOH). It was found out that modification, especially with trithiocyanuric acid, increased the sensitivity of detection in comparison with pure GCE. All processes were finally implemented in a microfluidic chip formed with a 3D printer by fused deposition modelling technology. As a material for chip fabrication, acrylonitrile butadiene styrene was chosen because of its mechanical and chemical stability. The chip contained the one chamber for the hydrolysis of the nucleic acid and another for the electrochemical detection by the modified GCE. This chamber was fabricated to allow for replacement of the GCE.

MIPs-graphene nanoplatelets-MWCNTs modified glassy carbon electrode for the determination of cardiac troponin I.

Science.gov (United States)

Ma, Ya; Shen, Xiao-Lei; Wang, Hai-Shui; Tao, Jia; Huang, Jian-Zhi; Zeng, Qiang; Wang, Li-Shi

2017-03-01

An electrochemical sensor with high selectivity in addition to sensitivity was developed for the determination of cardiac troponin I (cTnI), based on the modification of cTnI imprinted polymer film on a glassy carbon electrode (GCE). The sensor was fabricated by layer-by-layer assembled graphene nanoplatelets (GS), multiwalled carbon nanotubes (MWCNTs), chitosan (CS), glutaraldehyde (GA) composites, which can increase the electronic transfer rate and the active surface area to capture a larger number of antigenic proteins. MWCNTs/GS based imprinted polymers (MIPs/MWCNTs/GS) were synthesized by means of methacrylic acid (MAA) as the monomer, ethylene glycol dimethacrylate (EGDMA) as the cross linker α,α'-azobisisobutyronitrile (AIBN) as the initiator and cTnI as the template. In comparison with conventional methods, the proposed electrochemical sensor is highly sensitive for cTnI, providing a better linear response range from 0.005 to 60 ng cm -3 and a lower limit of detection (LOD) of 0.0008 ng cm -3 under optimal experimental conditions. In addition, the electrochemical sensor exhibited good specificity, acceptable reproducibility and stability. Moreover, satisfactory results were obtained in real human serum samples, indicating that the developed method has the potential to find application in clinical detection of cTnI as an alternative approach. Copyright © 2016 Elsevier Inc. All rights reserved.

Kinetic studies of oxidation of {gamma}-AlON-TiN composites

Energy Technology Data Exchange (ETDEWEB)

Zhang Zuotai; Wang Xidong; Li Wenchao

2005-01-25

The present article deals with the investigation of the oxidation kinetics of {gamma}-aluminum oxynitride-Titanium Nitride composites (AlON-TiN) in the temperature range of 1100-1300 deg. C by thermogravimetry. Oxidation experiments with AlON-TiN composite plates have been carried out in air both in isothermal and nonisothermal modes. The results showed that the rate of oxidation was negligible below 1000 deg. C, and showed an increase with increasing temperature at higher temperature. Both isothermal studies as well as experiments with ramped temperature clearly indicated that the mechanism of the reaction changes around 1400 deg. C. In the nonisothermal mode, the oxidation curve showed an increased reaction rate in this temperature range. Oxidation of AlON-TiN composite results in {alpha}-Al{sub 2}O{sub 3} and TiO{sub 2} at a low temperature and Al{sub 2}TiO{sub 5} at higher temperature. The buildup of the product layer leads to diffusion controlled kinetics. In the nonisothermal experiments, the phase transformation from Al{sub 2}O{sub 3} and TiO{sub 2}, to a Al{sub 2}TiO{sub 5} product layer at higher temperature would lead to crack formation, thereby leading to direct chemical reaction. From the experiments for the isothermal oxidation of AlON-TiN composite plates, the overall reactions are separated into three stages: chemistry reaction-controlling stage; chemical reaction- and diffusion-mixed-controlled stage; diffusion-controlled stage. The apparent activation energy for the experiments were calculated to be 10.109, 2.19 and 5.614 kJ mol{sup -1}, respectively, in the above three stages.

A wrinkling-based method for investigating glassy polymer film relaxation as a function of film thickness and temperature.

Science.gov (United States)

Chung, Jun Young; Douglas, Jack F; Stafford, Christopher M

2017-10-21

We investigate the relaxation dynamics of thin polymer films at temperatures below the bulk glass transition T g by first compressing polystyrene films supported on a polydimethylsiloxane substrate to create wrinkling patterns and then observing the slow relaxation of the wrinkled films back to their final equilibrium flat state by small angle light scattering. As with recent relaxation measurements on thin glassy films reported by Fakhraai and co-workers, we find the relaxation time of our wrinkled films to be strongly dependent on film thickness below an onset thickness on the order of 100 nm. By varying the temperature between room temperature and T g (≈100 °C), we find that the relaxation time follows an Arrhenius-type temperature dependence to a good approximation at all film thicknesses investigated, where both the activation energy and the relaxation time pre-factor depend appreciably on film thickness. The wrinkling relaxation curves tend to cross at a common temperature somewhat below T g , indicating an entropy-enthalpy compensation relation between the activation free energy parameters. This compensation effect has also been observed recently in simulated supported polymer films in the high temperature Arrhenius relaxation regime rather than the glassy state. In addition, we find that the film stress relaxation function, as well as the height of the wrinkle ridges, follows a stretched exponential time dependence and the short-time effective Young's modulus derived from our modeling decreases sigmoidally with increasing temperature-both characteristic features of glassy materials. The relatively facile nature of the wrinkling-based measurements in comparison to other film relaxation measurements makes our method attractive for practical materials development, as well as fundamental studies of glass formation.

Bioactive glass/hydroxyapatite composites: mechanical properties and biological evaluation.

Science.gov (United States)

Bellucci, Devis; Sola, Antonella; Anesi, Alexandre; Salvatori, Roberta; Chiarini, Luigi; Cannillo, Valeria

2015-06-01

Bioactive glass/hydroxyapatite composites for bone tissue repair and regeneration have been produced and discussed. The use of a recently developed glass, namely BG_Ca/Mix, with its low tendency to crystallize, allowed one to sinter the samples at a relatively low temperature thus avoiding several adverse effects usually reported in the literature, such as extensive crystallization of the glassy phase, hydroxyapatite (HA) decomposition and reaction between HA and glass. The mechanical properties of the composites with 80wt.% BG_Ca/Mix and 20wt.% HA are sensibly higher than those of Bioglass® 45S5 reference samples due to the presence of HA (mechanically stronger than the 45S5 glass) and to the thermal behaviour of the BG_Ca/Mix, which is able to favour the sintering process of the composites. Biocompatibility tests, performed with murine fibroblasts BALB/3T3 and osteocites MLO-Y4 throughout a multi-parametrical approach, allow one to look with optimism to the produced composites, since both the samples themselves and their extracts do not induce negative effects in cell viability and do not cause inhibition in cell growth. Copyright © 2015 Elsevier B.V. All rights reserved.

Photogeneration of singlet oxygen by the phenothiazine derivatives covalently bound to the surface-modified glassy carbon

Energy Technology Data Exchange (ETDEWEB)

Blacha-Grzechnik, Agata, E-mail: agata.blacha@polsl.pl [Faculty of Chemistry, Silesian University of Technology, Strzody 9, 44-100 Gliwice (Poland); Piwowar, Katarzyna; Krukiewicz, Katarzyna [Faculty of Chemistry, Silesian University of Technology, Strzody 9, 44-100 Gliwice (Poland); Koscielniak, Piotr; Szuber, Jacek [Institute of Electronics, Silesian University of Technology, Akademicka 16, 44-100 Gliwice (Poland); Zak, Jerzy K. [Faculty of Chemistry, Silesian University of Technology, Strzody 9, 44-100 Gliwice (Poland)

2016-05-15

Highlights: • The selected group of four NH{sub 2}-derivatives of phenothiazine was grafted to Glassy Carbon (GC) surface. • The grafted phenothiazines are able to generate {sup 1}O{sub 2} when activated by the radiation. • Such modified solid surfaces may find their application in the wastewater treatment. - Abstract: The selected group of four amine-derivatives of phenothiazine was covalently grafted to the glassy carbon surface in the four-step procedure consisting of the electrochemical reduction of the diazonium salt followed by the electrochemical and chemical post-modification steps. The proposed strategy involves the bonding of linker molecule to which the photosensitizer is attached. The synthesized organic layers were characterized by means of cyclic voltammetry, XPS and Raman Spectroscopy. It was shown that the phenothiazines immobilized via proposed strategy retain their photochemical properties and are able to generate {sup 1}O{sub 2} when activated by the laser radiation. The effectiveness of in situ singlet oxygen generation by those new solid photoactive materials was determined by means of UVVis spectroscopy. The reported, covalently modified solid surfaces may find their application as the singlet oxygen photogenerators in the fine chemicals’ synthesis or in the wastewater treatment.

Electrocatalytic Determination of Isoniazid by a Glassy Carbon Electrode Modified with Poly (Eriochrome Black T

Directory of Open Access Journals (Sweden)

Karim Asadpour-Zeynali

2017-06-01

Full Text Available In this work poly eriochrome black T (EBT was electrochemically synthesized on the glassy carbon electrode as electrode modifier. On the modified electrode, voltammetric behavior of isoniazid (INH was investigated. The poly (EBT-modified glassy carbon electrode has excellent electrocatalytic ability for the electrooxidation of isoniazid. This fact was appeared as a reduced overpotential of INH oxidation in a wide operational pH range from 2 to 13. It has been found that the catalytic peak current depends on the concentration of INH and solution pH. The number of electrons involved in the rate determining step was found 1. The diffusion coefficient of isoniazid was also estimated using chronoamperometry technique. The experimental results showed that the mediated oxidation peak current of isoniazid is linearly dependent on the concentration of isoniazid in the ranges of 8.0 × 10-6 – 1.18 × 10-3 M and 2.90 × 10-5 M – 1.67× 10-3 M with differential pulse voltammetry (DPV and amperometry methods, respectively. The detection limits (S/N = 3 were found to be 6.0 μM and 16.4 μM by DPV and amperometry methods, respectively. This developed method was applied to the determination of isoniazid in tablet samples with satisfactory results.

Age and petrogenetic constraints on the Lower Glassy Ignimbrite of the Mount Somers Volcanic Group, New Zealand

DEFF Research Database (Denmark)

van der Meer, Quinten; Waight, Tod Earle; Whitehouse, Martin

2017-01-01

The Mount Somers Volcanic Group (MSVG) forms a large (~18000 km2) calc-alkaline volcanic complex on New Zealand’s Eastern Province. U-Pb SIMS spot ages on zircon from the lower glassy ignimbrite in Rakaia Gorge reveal a bimodal distribution of 99.0 ± 0.5 and 96.3 ± 0.5 Ma (2σ). These ages...

Glassy carbon electrode modified with multi-walled carbon nanotubes sensor for the quantification of antihistamine drug pheniramine in solubilized systems

Directory of Open Access Journals (Sweden)

Rajeev Jain

2012-02-01

Full Text Available A sensitive electroanalytical method for quantification of pheniramine in pharmaceutical formulation has been investigated on the basis of the enhanced electrochemical response at glassy carbon electrode modified with multi-walled carbon nanotubes in the presence of sodium lauryl sulfate. The experimental results suggest that the pheniramine in anionic surfactant solution exhibits electrocatalytic effect resulting in a marked enhancement of the peak current response. Peak current response is linearly dependent on the concentration of pheniramine in the range 200–1500 μg/mL with correlation coefficient 0.9987. The limit of detection is 58.31 μg/mL. The modified electrode shows good sensitivity and repeatability. Keywords: Pheniramine, Sodium lauryl sulfate (SLS, Glassy carbon electrode modified with multi-walled carbon nanotubes (GCE-MWCNTs, Solubilized systems, Voltammetric quantification

Fine kinetics of natural physical ageing in glassy As{sub 10}Se{sub 90}

Energy Technology Data Exchange (ETDEWEB)

Balitska, V. [Institute of Materials, Scientific Research Company “Carat”, 202 Stryjska Str., 79031 Lviv (Ukraine); Lviv State University of Vital Activity Safety, 35, Kleparivska Str., Lviv 79007 (Ukraine); Golovchak, R. [Department of Physics and Astronomy, Austin Peay State University, Clarksville, TN 37044 (United States); Kozdras, A. [Faculty of Physics of Opole Technical University, 75, Ozimska Str., Opole 45370 (Poland); Shpotyuk, O., E-mail: shpotyuk@novas.lviv.ua [Institute of Materials, Scientific Research Company “Carat”, 202 Stryjska Str., 79031 Lviv (Ukraine); Institute of Physics, Jan Dlugosz University, Al. Armii Krajowej 13/15, Czestochowa 42201 (Poland)

2014-02-01

Sigmoid behavior of natural physical ageing in glassy As{sub 10}Se{sub 90} reveals multi-step-wise growing kinetics of enthalpy losses. Phenomenological description of this kinetics can be adequately developed in terms of first-order relaxation processes, tending atomic structure from initial towards more thermodynamically equilibrium state. This kinetics is shown to obey characteristic stretched exponential behavior originated from a number of growing steps, attributed to the interconnected processes of chalcogen chain alignment and cooperative shrinkage of glass network.

Fabrication and properties of carbon network reinforced composite fuel

International Nuclear Information System (INIS)

Umer, Malik Adeel; Mistarihi, Qusai Mahmoud; Kim, Joon Hui; Hong, Soon Hyung; Ryu, Ho Jin

2014-01-01

Zirconium dioxide composites reinforced with 3D glassy carbon foam was fabricated using Spark Plasma Sintering (SPS) with a heating rate of 100degC/min and a uniaxial pressure of 50 MPa at 1500degC, 1600degC, and 1700degC, respectively. The effect of carbon foam on the thermal properties of the ZrO 2 composites was investigated. In addition, the effect of the sintering temperature on the densification of the composites was also investigated and the optimized sintering temperature was identified. The microstructures of 3D carbon foam reinforced ZrO 2 composites showed that the 3D shape of carbon foam was retained after the sintering process, and the ZrO 2 was homogeneously distributed within the 3D carbon foam. At the interfaces between the 3D carbon foam and ZrO 2 , neither a chemical reaction nor a new phase formation was detected by Scanning Electron Microscopy (SEM) and X-ray Diffractometry (XRD). The thermal diffusivity of carbon foam reinforced ZrO 2 composites measured at 1100degC was increased by 47% and reached to 0.66 mm 2 s -1 and the thermal conductivity was increased by 50% and reached to 2.428 W/m-K. (author)

Direct 4D printing via active composite materials

Science.gov (United States)

Ding, Zhen; Yuan, Chao; Peng, Xirui; Wang, Tiejun; Qi, H. Jerry; Dunn, Martin L.

2017-01-01

We describe an approach to print composite polymers in high-resolution three-dimensional (3D) architectures that can be rapidly transformed to a new permanent configuration directly by heating. The permanent shape of a component results from the programmed time evolution of the printed shape upon heating via the design of the architecture and process parameters of a composite consisting of a glassy shape memory polymer and an elastomer that is programmed with a built-in compressive strain during photopolymerization. Upon heating, the shape memory polymer softens, releases the constraint on the strained elastomer, and allows the object to transform into a new permanent shape, which can then be reprogrammed into multiple subsequent shapes. Our key advance, the markedly simplified creation of high-resolution complex 3D reprogrammable structures, promises to enable myriad applications across domains, including medical technology, aerospace, and consumer products, and even suggests a new paradigm in product design, where components are simultaneously designed to inhabit multiple configurations during service. PMID:28439560

Direct 4D printing via active composite materials.

Science.gov (United States)

Ding, Zhen; Yuan, Chao; Peng, Xirui; Wang, Tiejun; Qi, H Jerry; Dunn, Martin L

2017-04-01

We describe an approach to print composite polymers in high-resolution three-dimensional (3D) architectures that can be rapidly transformed to a new permanent configuration directly by heating. The permanent shape of a component results from the programmed time evolution of the printed shape upon heating via the design of the architecture and process parameters of a composite consisting of a glassy shape memory polymer and an elastomer that is programmed with a built-in compressive strain during photopolymerization. Upon heating, the shape memory polymer softens, releases the constraint on the strained elastomer, and allows the object to transform into a new permanent shape, which can then be reprogrammed into multiple subsequent shapes. Our key advance, the markedly simplified creation of high-resolution complex 3D reprogrammable structures, promises to enable myriad applications across domains, including medical technology, aerospace, and consumer products, and even suggests a new paradigm in product design, where components are simultaneously designed to inhabit multiple configurations during service.

Electrocatalytic reduction of nitrite on tetraruthenated metalloporphyrins/Nafion glassy carbon modified electrode

Energy Technology Data Exchange (ETDEWEB)

Calfuman, Karla [Facultad de Ciencias, Departamento de Quimica, Universidad de Chile, Las Palmeras 3425, Casilla 653, Nunoa, Santiago (Chile); Aguirre, Maria Jesus [Facultad de Quimica y Biologia, Departamento de Quimica de los Materiales, Universidad de Santiago de Chile, Santiago (Chile); Canete-Rosales, Paulina; Bollo, Soledad [Facultad de Ciencias Quimicas y Farmaceuticas, Departamento de Quimica Farmacologica y Toxicologica, Universidad de Chile, Santiago (Chile); Llusar, Rosa [Departamento de Quimica Fisica y Analitica, Universidad de Jaume I, Castellon (Spain); Isaacs, Mauricio, E-mail: misaacs@uchile.cl [Facultad de Ciencias, Departamento de Quimica, Universidad de Chile, Las Palmeras 3425, Casilla 653, Nunoa, Santiago (Chile)

2011-10-01

Highlights: > Preparation and characterization of modified electrodes with M(II) Tetraruthenated porphyrins onto a Nafion film. > The electrodes were characterized by SEM, TEM, AFM and SECM techniques. > The modified electrodes are active in the electrochemical reduction of nitrite at -660 mV vs Ag/AgCl. > GC/Nf/CoTRP modified electrode is more electrochemically active than their Ni and Zn analogues. - Abstract: This paper describes the electrochemical reduction of nitrite ion in neutral aqueous solution mediated by tetraruthenated metalloporphyrins (Co(II), Ni(II) and Zn(II)) electrostatically assembled onto a Nafion film previously adsorbed on glassy carbon or ITO electrodes. Scanning electron microscope (SEM-EDX) and transmission electron microscopy (TEM) results have shown that on ITO electrodes the macrocycles forms multiple layers with a disordered stacking orientation over the Nafion film occupying hydrophobic and hydrophilic sites in the polyelectrolyte. Atomic force microscopy (AFM) results demonstrated that the Nafion film is 35 nm thick and tetraruthenated metalloporphyrins layers 190 nm thick presenting a thin but compacted morphology. Scanning electrochemical microscopy (SECM) images shows that the Co(II) tetraruthenated porphyrins/Nf/GC modified electrode is more electrochemically active than their Ni and Zn analogues. These modified electrodes are able to reduce nitrite at -660 mV showing enhanced reduction current and a decrease in the required overpotential compared to bare glassy carbon electrode. Controlled potential electrolysis experiments verify the production of ammonia, hydrazine and hydroxylamine at potentials where reduction of solvent is plausible demonstrating some selectivity toward the nitrite ion. Rotating disc electrode voltammetry shows that the factor that governs the kinetics of nitrite reduction is the charge propagation in the film.

Raman spectra of zinc phthalocyanine monolayers absorbed on glassy carbon and gold electrodes by application of a confocal Raman microspectrometer

NARCIS (Netherlands)

Palys-Staron, B.J.; Palys, B.J.; Puppels, G.J.; Puppels, G.J.; van den Ham, D.M.W.; van den Ham, D.M.W.; Feil, D.; Feil, D.

1992-01-01

Raman spectra of zinc phthalocyanine monolayers, adsorbed on gold and on glassy carbon surfaces (electrodes), are presented. These spectra have been recorded with the electrodes inside and outside an electrochemical cell filled with an aqueous electrolyte. A confocal Raman microspectrometer was

Alkali-ions diffusion, mullite formation, and crystals dissolution during sintering of porcelain bodies: Microstructural approach

DEFF Research Database (Denmark)

Leonelli, C.; Kamseu, E.; Boccaccini, Dino

2009-01-01

The effect of alkali-silicate glassy matrix as replacement for feldspar in soft and hard porcelain compositions was studied. SEM and X-ray diffraction analysis were used to evidence phase evolution. For each composition, the influence of soaking time was evaluated. The difference in chemical...... to hard porcelain. Replacing the feldspar by alkali-silicate glassy matrices with similar chemical composition, the amount of secondary mullite and mechanical properties increased in both soft and hard compositions....

Thermal conductivity of glass copper-composite

International Nuclear Information System (INIS)

Kinoshita, Makoto; Terai, Ryohei; Haidai, Haruki

1980-01-01

Glass-metal composites are to be one of the answers for promoting thermal conduction in the glassy solids containing high-level radioactive wastes. In order to investigate the effect of metal addition on thermal conductivity of glasses, glass-copper composites were selected, and the conductivities of the composites were measured and discussed in regards to copper content and microstructure. Fully densified composites were successfully prepared by pressure sintering of the powder mixtures of glass and copper at temperatures above the yield points of the constituent glasses if the copper content was not so much. The conductivity was measured by means of a comparative method, in which the thermal gradient of the specimen was compared with that of quartz glass as standard under thermally steady state. Measurements were carried out at around 50 0 C. The thermal conductivity increased with increasing content of copper depending on the kind of copper powder used. The conductivities of the composites of the same copper content differed considerably each another. Fine copper powder was effective on increasing conductivity, and the conductivity became about threefold of that of glass by mixing the fine copper powder about 10 vol%. For the composites containing the fine copper powder less than 5 vol%, the conductivity obeyed so-called logarithmic rule, one of the mixture rules of conductivity, whereas for composites containing more than 5 vol%, the conductivity remarkably increased apart from the rule. This fact suggests that copper becomes continuous in the composite when the copper content increased beyond 5 vol%. For the composites containing coarse copper powder, the conductivity was increased not significantly, and obeyed an equation derived from the model in which conductive material dispersed in less conductive one. (author)

Activation of glassy carbon electrodes by photocatalytic pretreatment

Energy Technology Data Exchange (ETDEWEB)

Dumanli, Onur [Department of Chemistry, Faculty of Science and Art, Ondokuz Mayis University, Kurupelit, 55139 Samsun (Turkey); Onar, A. Nur [Department of Chemistry, Faculty of Science and Art, Ondokuz Mayis University, Kurupelit, 55139 Samsun (Turkey)], E-mail: nonar@omu.edu.tr

2009-11-01

This paper describes a simple and rapid photocatalytic pretreatment procedure that removes contaminants from glassy carbon (GC) surfaces. The effectiveness of TiO{sub 2} mediated photocatalytic pretreatment procedure was compared to commonly used alumina polishing procedure. Cyclic voltammetric and chronocoulometric measurements were carried out to assess the changes in electrode reactivity by using four redox systems. Electrochemical measurements obtained on photocatalytically treated GC electrodes showed a more active surface relative to polished GC. In cyclic voltammograms of epinephrine, Fe(CN){sub 6}{sup 3-/4-} and ferrocene redox systems, higher oxidation and reduction currents were observed. The heterogeneous electron transfer rate constants (k{sup o}) were calculated for Fe(CN){sub 6}{sup 3-/4-} and ferrocene which were greater for photocatalytic pretreatment. Chronocoulometry was performed in order to find the amount of adsorbed methylene blue onto the electrode and was calculated as 0.34 pmol cm{sup -2} for photocatalytically pretreated GC. The proposed photocatalytic GC electrode cleansing and activating pretreatment procedure was more effective than classical alumina polishing.

Simulations of tensile failure in glassy polymers: effect of cross-link density

International Nuclear Information System (INIS)

Panico, M; Narayanan, S; Brinson, L C

2010-01-01

Molecular dynamics simulations are adopted to investigate the failure mechanisms of glassy polymers, particularly with respect to increasing density of cross-links. In our simulations thermosetting polymers, which are cross-linked, exhibit an embrittlement compared with uncross-linked thermoplastics in a similar fashion to several experimental investigations (Levita et al 1991 J. Mater. Sci. 26 2348; Sambasivam et al 1997 J. Appl. Polym. Sci. 65 1001; Iijima et al 1992 Eur. Polym. J. 28 573). We perform a detailed analysis of this phenomenon and propose an interpretation based on the predominance of chain scission process over disentanglement in thermosetting polymers. We also elucidate the brittle fracture response of the thermosetting polymers

Fracture and subcritical crack-growth behavior of Y-Si-Al-O-N glasses and Si3N4 ceramics

International Nuclear Information System (INIS)

Bhatnagar, A.; Hoffman, M.J.; Dauskardt, R.H.

2000-01-01

Fracture and environmentally assisted subcritical crack-growth processes are examined in bulk Y-Si-Al-O-N oxynitride glasses with compositions typical of the grain boundary phase of silicon nitride ceramics. Both long-crack (in compact tension specimens) as well as short-crack behavior (using indentation techniques) were investigated to establish a reliable fracture toughness and to elucidate the anomalous densification behavior of the oxynitride glass. Environmentally assisted subcritical crack-growth processes were studied in inert, moist, and wet environments under both cyclic and static loading conditions. Behavior is discussed in terms of the interaction of the environment with the crack tip. Likely mechanisms for environmentally assisted crack growth are discussed and related to the subcritical crack-growth behavior of silicon nitride ceramics

Laser irradiation and thermal treatment inducing selective crystallization in Sb2O3-Sb2S3 glassy films

Science.gov (United States)

Avila, L. F.; Pradel, A.; Ribeiro, S. J. L.; Messaddeq, Y.; Nalin, M.

2015-02-01

The influence of both thermal treatment and laser irradiation on the structural and optical properties of films in the Sb2O3-Sb2S3 system was investigated. The films were prepared by RF-sputtering using glass compositions as raw materials. Irreversible photodarkening effect was observed after exposure the films to a 458 nm solid state laser. It is shown, for the first time, the use of holographic technique to measure "in situ", simultaneously and independently, the phase and amplitude modulations in glassy films. The films were also photo-crystallized and analysed "in situ" using a laser coupled to a micro-Raman equipment. Results showed that Sb2S3 crystalline phase was obtained after irradiation. The effect of thermal annealing on the structure of the films was carried out. Different from the result obtained by irradiation, thermal annealing induces the crystallization of the Sb2O3 phase. Photo and thermal induced effects on films were studied using UV-Vis and Raman spectroscopy, atomic force microscopy (AFM), thermal analysis (DSC), X-ray diffraction, scanning electron microscopy (MEV) and energy-dispersive X-ray spectroscopy (EDX).

Anodic Stripping Voltammetric Detection of Arsenic(III) at Platinum-Iron(III) Nanoparticle Modified Carbon Nanotube on Glassy Carbon Electrode

International Nuclear Information System (INIS)

Shin, Seung Hyun; Hong, Hun Gi

2010-01-01

The electrochemical detection of As(III) was investigated on a platinum-iron(III) nanoparticles modified multiwalled carbon nanotube on glassy carbon electrode(nanoPt-Fe(III)/MWCNT/GCE) in 0.1 M H 2 SO 4 . The nanoPt-Fe(III)/ MWCNT/GCE was prepared via continuous potential cycling in the range from .0.8 to 0.7 V (vs. Ag/AgCl), in 0.1 M KCl solution containing 0.9 mM K 2 PtCl 6 and 0.6 mM FeCl 3 . The Pt nanoparticles and iron oxide were co-electrodeposited into the MWCNT-Nafion composite film on GCE. The resulting electrode was examined by cyclic voltammetry (CV), scanning electron microscopy (SEM), and anodic stripping voltammetry (ASV). For the detection of As(III), the nanoPt-Fe(III)/MWCNT/GCE showed low detection limit of 10 nM (0.75 ppb) and high sensitivity of 4.76 μAμM -1 , while the World Health Organization's guideline value of arsenic for drinking water is 10 ppb. It is worth to note that the electrode presents no interference from copper ion, which is the most serious interfering species in arsenic detection

Etched ion tracks in silicon oxide and silicon oxynitride as charge injection or extraction channels for novel electronic structures

International Nuclear Information System (INIS)

Fink, D.; Petrov, A.V.; Hoppe, K.; Fahrner, W.R.; Papaleo, R.M.; Berdinsky, A.S.; Chandra, A.; Chemseddine, A.; Zrineh, A.; Biswas, A.; Faupel, F.; Chadderton, L.T.

2004-01-01

The impact of swift heavy ions onto silicon oxide and silicon oxynitride on silicon creates etchable tracks in these insulators. After their etching and filling-up with highly resistive matter, these nanometric pores can be used as charge extraction or injection paths towards the conducting channel in the underlying silicon. In this way, a novel family of electronic structures has been realized. The basic characteristics of these 'TEMPOS' (=tunable electronic material with pores in oxide on silicon) structures are summarized. Their functionality is determined by the type of insulator, the etch track diameters and lengths, their areal densities, the type of conducting matter embedded therein, and of course by the underlying semiconductor and the contact geometry. Depending on the TEMPOS preparation recipe and working point, the structures may resemble gatable resistors, condensors, diodes, transistors, photocells, or sensors, and they are therefore rather universally applicable in electronics. TEMPOS structures are often sensitive to temperature, light, humidity and organic gases. Also light-emitting TEMPOS structures have been produced. About 37 TEMPOS-based circuits such as thermosensors, photosensors, humidity and alcohol sensors, amplifiers, frequency multipliers, amplitude modulators, oscillators, flip-flops and many others have already been designed and successfully tested. Sometimes TEMPOS-based circuits are more compact than conventional electronics

Novel high-strength Fe-based composite materials with large plasticity

Energy Technology Data Exchange (ETDEWEB)

Werniewicz, Katarzna; Kuehn, Uta; Mattern, Norbert; Eckert, Juergen; Siegel, Uwe; Bartusch, Birgit; Schultz, Ludwig [IFW Dresden, P.O. Box 270116, D-01171 Dresden (Germany); Kulik, Tadeusz [Warsaw University of Technology, Faculty of Materials Science and Engineering (Poland)

2007-07-01

Among glass-forming alloy systems reported so far, Fe-based bulk metallic glasses play a special role. Compared to other amorphous alloys e.g. Zr-, Ti-based, such glasses show superior mechanical strength. However, due to the general brittleness their wider application as structural materials is strongly restricted. The alternative approach to overcome this defect is to design BMG composites. In this work we present a series of new Fe-Cr-Mo-Ga-(Si,C) composite materials derived from an Fe-Cr-Mo-Ga-C-P-B glassy alloy, with the aim to improve the ductility of this high-strength material. The effect of the composition and the phase formation on the resulting mechanical properties was investigated. It has been found that the formation of a complex microstructure, which essentially consists of soft Ga-rich dendrites embedded in a hard Cr- and Mo-rich matrix, leads to a material with excellent compressive mechanical properties. While the obtained values of true strength are comparable with data reported for Fe-Cr-Mo-Ga-C-P-B BMG, the values of true strain are greatly improved for investigated composites.

Phase formation, structural and microstructural characterization of novel oxynitride-perovskites synthesized by thermal ammonolysis of (Ca,Ba)MoO4 and (Ca,Ba)MoO3

International Nuclear Information System (INIS)

Logvinovich, D.; Aguirre, M.H.; Hejtmanek, J.; Aguiar, R.; Ebbinghaus, S.G.; Reller, A.; Weidenkaff, A.

2008-01-01

Reactions of AMoO 4 and AMoO 3 (A=Ca 2+ , Ba 2+ ) with ammonia were investigated at 873 K 3 and to study their crystal structure. CaMo(O,N) 3 and BaMo(O,N) 3 were prepared by thermal ammonolysis of the corresponding CaMoO 3 and BaMoO 3 precursors at T=898 and 998 K, respectively. The structural parameters of the oxynitrides were obtained from Rietveld refinements of X-ray and neutron powder diffraction data. CaMo(O,N) 3 crystallizes in the GdFeO 3 distorted perovskite structure with orthorhombic space group Pbnm and a=5.5029(1) A, b=5.5546(1) A, c=7.8248(1) A as determined by X-ray powder diffraction. Its O/N content refined from the neutron diffraction data corresponds to the composition CaMoO 1.7(1) N 1.3(1) . BaMo(O,N) 3 crystallizes in the cubic perovskite structure with space group Pm3-bar m and a=4.0657(1) A as determined by X-ray powder diffraction. Transmission electron microscopy reveals a complex microstructure for both CaMoO 3 and CaMoO 1.7(1) N 1.3(1) represented by twin domains of different orientation. - Graphical abstract: Reactions of AMoO 4 and AMoO 3 (A=Ca 2+ , Ba 2+ ) oxides with ammonia have been studied at T=873-1123 K. Orthorhombic CaMoO 1.7(1) N 1.3(1) (Pbnm) and cubic BaMo(O,N) 3 (Pm3-bar m) were prepared by thermal ammonolysis of the corresponding CaMoO 3 and BaMoO 3 precursors at T=898 and 998 K, respectively. Display Omitted

A novel highly selective and sensitive detection of serotonin based on Ag/polypyrrole/Cu2O nanocomposite modified glassy carbon electrode.

Science.gov (United States)

Selvarajan, S; Suganthi, A; Rajarajan, M

2018-06-01

A silver/polypyrrole/copper oxide (Ag/PPy/Cu 2 O) ternary nanocomposite was prepared by sonochemical and oxidative polymerization simple way, in which Cu 2 O was decorated with Ag nanoparticles, and covered by polyprrole (PPy) layer. The as prepared materials was characterized by UV-vis-spectroscopy (UV-vis), FT-IR, X-ray diffraction (XRD), thermo-gravimetric analysis (TGA), scanning electron microscopy (SEM) with EDX, high resolution transmission electron microscopy (HR-TEM) and X-ray photoelectron spectroscopy (XPS). Sensing of serotonin (5HT) was evaluated electrocatalyst using polypyrrole/glassy carbon electrode (PPy/GCE), polypyrrole/copper oxide/glassy carbon electrode (PPy/Cu 2 O/GCE) and silver/polypyrrole/copper oxide/glassy carbon electrode (Ag/PPy/Cu 2 O/GCE). The Ag/PPy/Cu 2 O/GCE was electrochemically treated in 0.1MPBS solution through cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The peak current response increases linearly with 5-HT concentration from 0.01 to 250 µmol L -1 and the detection limit was found to be 0.0124 μmol L -1 . It exhibits high electrocatalytic activity, satisfactory repeatability, stability, fast response and good selectivity against potentially interfering species, which suggests its potential in the development of sensitive, selective, easy-operation and low-cost serotonin sensor for practical routine analyses. The proposed method is potential to expand the possible applied range of the nanocomposite material for detection of various concerned electro active substances. Copyright © 2018 Elsevier B.V. All rights reserved.

Local atomic and electronic structure in glassy metallic alloys. Final report, March 1, 1979-May 31, 1982

International Nuclear Information System (INIS)

Messmer, R.P.; Wong, J.

1982-01-01

The research results reported, represent the first coordinated experimental-theoretical effort to arrive at important local atomic and electronic structure information in glassy alloys. During the three years covered by the contract, significant experimental and theoretical developments have taken place both in the general technical community and at General Electric which have had an important impact on the approach to this problem. This is particularly true in the theoretical area where two important advances, the development of a general Xα-LCAO approach, and the development of a general and accurate effective potential approach for density functional methods, have allowed us to construct a new computational capability which combines these two advances. Two subsections briefly review the experimental and theoretical technical developments, respectively. These developments have changed initial perspectives regarding research on local atomic and electronic structure in glassy metallic alloys. Section II presents a synopsis of our accomplishments during the contract period and Section III contains a more detailed discussion of some of these accomplishments, namely those portions of the work which have been published or submitted for publication at the time of writing this final report

Electrochemical Determination of Caffeine Content in Ethiopian Coffee Samples Using Lignin Modified Glassy Carbon Electrode

Directory of Open Access Journals (Sweden)

Meareg Amare

2017-01-01

Full Text Available Lignin film was deposited at the surface of glassy carbon electrode potentiostatically. In contrast to the unmodified glassy carbon electrode, an oxidative peak with an improved current and overpotential for caffeine at modified electrode showed catalytic activity of the modifier towards oxidation of caffeine. Linear dependence of peak current on caffeine concentration in the range 6×10-6 to 100×10-6 mol L−1 with determination coefficient and method detection limit (LoD = 3 s/slope of 0.99925 and 8.37×10-7 mol L−1, respectively, supplemented by recovery results of 93.79–102.17% validated the developed method. An attempt was made to determine the caffeine content of aqueous coffee extracts of Ethiopian coffees grown in four coffee cultivating localities (Wonbera, Wolega, Finoteselam, and Zegie and hence to evaluate the correlation between users preference and caffeine content. In agreement with reported works, caffeine contents (w/w% of 0.164 in Wonbera coffee; 0.134 in Wolega coffee; 0.097 in Finoteselam coffee; and 0.089 in Zegie coffee were detected confirming the applicability of the developed method for determination of caffeine in a complex matrix environment. The result indicated that users’ highest preference for Wonbera and least preference for Zegie cultivated coffees are in agreement with the caffeine content.

Electrochemical Determination of Caffeine Content in Ethiopian Coffee Samples Using Lignin Modified Glassy Carbon Electrode.

Science.gov (United States)

Amare, Meareg; Aklog, Senait

2017-01-01

Lignin film was deposited at the surface of glassy carbon electrode potentiostatically. In contrast to the unmodified glassy carbon electrode, an oxidative peak with an improved current and overpotential for caffeine at modified electrode showed catalytic activity of the modifier towards oxidation of caffeine. Linear dependence of peak current on caffeine concentration in the range 6 × 10 -6 to 100 × 10 -6  mol L -1 with determination coefficient and method detection limit (LoD = 3 s/slope) of 0.99925 and 8.37 × 10 -7  mol L -1 , respectively, supplemented by recovery results of 93.79-102.17% validated the developed method. An attempt was made to determine the caffeine content of aqueous coffee extracts of Ethiopian coffees grown in four coffee cultivating localities (Wonbera, Wolega, Finoteselam, and Zegie) and hence to evaluate the correlation between users preference and caffeine content. In agreement with reported works, caffeine contents (w/w%) of 0.164 in Wonbera coffee; 0.134 in Wolega coffee; 0.097 in Finoteselam coffee; and 0.089 in Zegie coffee were detected confirming the applicability of the developed method for determination of caffeine in a complex matrix environment. The result indicated that users' highest preference for Wonbera and least preference for Zegie cultivated coffees are in agreement with the caffeine content.

Gas barrier properties of titanium oxynitride films deposited on polyethylene terephthalate substrates by reactive magnetron sputtering

Energy Technology Data Exchange (ETDEWEB)

Lin, M.-C. [Department of Materials Science and Engineering, National ChungHsin University, 250, Kuo-Kung Road, 40227 Taichung, Taiwan (China); Chang, L.-S. [Department of Materials Science and Engineering, National ChungHsin University, 250, Kuo-Kung Road, 40227 Taichung, Taiwan (China)], E-mail: lschang@dragon.nchu.edu.tw; Lin, H.C. [Department of Materials Science and Engineering, National Taiwan University, 1, Roosevelt Road, Sec. 4, 106 Taipei, Taiwan (China)

2008-03-30

Titanium oxynitride (TiN{sub x}O{sub y}) films were deposited on polyethylene terephthalate (PET) substrates by means of a reactive radio frequency (RF) magnetron sputtering system in which the power density and substrate bias were the varied parameters. Experimental results show that the deposited TiN{sub x}O{sub y} films exhibited an amorphous or a columnar structure with fine crystalline dependent on power density. The deposition rate increases significantly in conjunction as the power density increases from 2 W/cm{sup 2} to 7 W/cm{sup 2}. The maximum deposition rate occurs, as the substrate bias is -40 V at a certain power densities chosen in this study. The film's roughness slightly decreases with increasing substrate bias. The TiN{sub x}O{sub y} films deposited at power densities above 4 W/cm{sup 2} show a steady Ti:N:O ratio of about 1:1:0.8. The water vapor and oxygen transmission rates of the TiN{sub x}O{sub y} films reach values as low as 0.98 g/m{sup 2}-day-atm and 0.60 cm{sup 3}/m{sup 2}-day-atm which are about 6 and 47 times lower than those of the uncoated PET substrate, respectively. These transmission rates are comparable to those of DLC, carbon-based and Al{sub 2}O{sub 3} barrier films. Therefore, TiN{sub x}O{sub y} films are potential candidates to be used as a gas permeation barrier for PET substrate.

Novel tunable green-red-emitting oxynitride phosphors co-activated with Ce3+, Tb3+, and Eu3+: photoluminescence and energy transfer.

Science.gov (United States)

Huo, Jiansheng; Dong, Langping; Lü, Wei; Shao, Baiqi; You, Hongpeng

2017-07-14

A series of novel Ce 3+ , Tb 3+ and Eu 3+ ion doped Y 4 SiAlO 8 N-based oxynitride phosphors were synthesized by the solid-state method and characterized by X-ray powder diffraction, scanning electron microscopy, photoluminescence, lifetimes and thermo-luminescence. The excitation of the Ce 3+ /Tb 3+ co-doped and Ce 3+ /Tb 3+ /Eu 3+ tri-doped phosphor with near-UV radiation results in strong linear Tb 3+ green and Eu 3+ red emission. The occurrence of Ce 3+ -Tb 3+ and Ce 3+ -Tb 3+ -Eu 3+ energy transfer processes is responsible for the bright green or red luminescence. The Tb 3+ ion acting as an energy transfer bridge can alleviate MMCT quenching between the Ce 3+ -Eu 3+ ion pairs. The lifetime measurements demonstrated that the energy-transfer mechanisms of Ce 3+ → Tb 3+ and Tb 3+ → Eu 3+ are dipole-quadrupole and quadrupole-quadrupole interactions, respectively. The temperature dependent luminescence measurements showed that as-prepared green/red phosphors have good thermal stability against temperature quenching. The obtained results indicate that these phosphors might serve as promising candidates for n-UV LEDs.

Raman, photoluminescence and EPR spectroscopic characterization of europium(III) oxide–lead dioxide–tellurite glassy network

Energy Technology Data Exchange (ETDEWEB)

Dehelean, A. [National Research and Development Institute for Isotopic and Molecular Technologies, Cluj-Napoca (Romania); Rada, S. [Technical University of Cluj-Napoca (Romania); Popa, A.; Suciu, R.C. [National Research and Development Institute for Isotopic and Molecular Technologies, Cluj-Napoca (Romania); Culea, E., E-mail: eugen.culea@phys.utcluj.ro [Technical University of Cluj-Napoca (Romania)

2016-09-15

Raman, photoluminescence and EPR spectroscopies were used to characterize some xEu{sub 2}O{sub 3}·(100−x)[4TeO{sub 2}·PbO{sub 2}] glasses with x=0–50 mol% obtained by melt quenching technique. Raman spectra of these glasses were interpreted in terms of vibration modes of deformed Te–O–Te linkages due to the intercalation of [PbO{sub n}] and [EuO{sub n}] entities produced by addition of Eu{sub 2}O{sub 3} to the host lead–tellurite glass. Photoluminescence spectra of xEu{sub 2}O{sub 3}·(100−x)[4TeO{sub 2}·PbO{sub 2}] glasses reveal the presence of Pb{sup 2+}, Eu{sup 2+} and Eu{sup 3+} ions. EPR data confirm the presence of Eu{sup 2+} ions in the europium–lead–tellurite glassy network and offer information about the compositional evolution of the Eu{sup 2+} ions local environment and Eu{sup 3+}↔Eu{sup 2+} redox process. PL and EPR data show that the decrease of the Eu{sup 2+} ions luminescence intensity for the x≥40 mol% Eu{sub 2}O{sub 3} region is not due to the clusterization of europium ions but is due the decrease of the amount of Eu{sup 2+} ions as result of changes in the Eu{sup 3+}→Eu{sup 2+} redox equilibrium.

Electrocatalysis of oxygen reduction on nitrogen-containing multi-walled carbon nanotube modified glassy carbon electrodes

International Nuclear Information System (INIS)

Vikkisk, Merilin; Kruusenberg, Ivar; Joost, Urmas; Shulga, Eugene; Tammeveski, Kaido

2013-01-01

Highlights: ► Pyrolysis in the presence of urea was used for nitrogen doping of carbon nanotubes. ► N-doped carbon nanotubes were used as catalysts for the oxygen reduction reaction. ► N-doped carbon material showed a high catalytic activity for ORR in alkaline media. ► N-containing CNT material is an attractive cathode catalyst for alkaline membrane fuel cells. - Abstract: The electrochemical reduction of oxygen was studied on nitrogen-doped multi-walled carbon nanotube (NCNT) modified glassy carbon (GC) electrodes employing the rotating disk electrode (RDE) method. Nitrogen doping was achieved by simple pyrolysis of the carbon nanotube material in the presence of urea. The surface morphology and composition of the NCNT samples were investigated by scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The SEM images revealed a rather uniform distribution of NCNTs on the GC electrode substrate. The XPS analysis showed a successful doping of carbon nanotubes with nitrogen species. The RDE results revealed that in alkaline solution the N-doped nanotube materials showed a remarkable electrocatalytic activity towards oxygen reduction. At low overpotentials the reduction of oxygen followed a two-electron pathway on undoped carbon nanotube modified GC electrodes, whereas on NCNT/GC electrodes a four-electron pathway of O 2 reduction predominated. The results obtained are significant for the development of nitrogen-doped carbon-based cathodes for alkaline membrane fuel cells.

Hydrogen peroxide biosensor based on hemoglobin immobilized at graphene, flower-like zinc oxide, and gold nanoparticles nanocomposite modified glassy carbon electrode.

Science.gov (United States)

Xie, Lingling; Xu, Yuandong; Cao, Xiaoyu

2013-07-01

In this work, a highly sensitive hydrogen peroxide (H2O2) biosensor based on immobilization of hemoglobin (Hb) at Au nanoparticles (AuNPs)/flower-like zinc oxide/graphene (AuNPs/ZnO/Gr) composite modified glassy carbon electrode (GCE) was constructed, where ZnO and Au nanoparticles were modified through layer-by-layer onto Gr/GCE. Flower-like ZnO nanoparticles could be easily prepared by adding ethanol to the precursor solution having higher concentration of hydroxide ions. The Hb/AuNPs/ZnO/Gr composite film showed a pair of well-defined, quasi-reversible redox peaks with a formal potential (E(0)) of -0.367 V, characteristic features of heme redox couple of Hb. The electron transfer rate constant (k(s)) of immobilized Hb was 1.3 s(-1). The developed biosensor showed a very fast response (<2 s) toward H2O2 with good sensitivity, wide linear range, and low detection limit of 0.8 μM. The fabricated biosensor showed interesting features, including high selectivity, acceptable stability, good reproducibility, and repeatability along with excellent conductivity, facile electron mobility of Gr, and good biocompatibility of ZnO and AuNPs. The fabrication method of this biosensor was simple and effective for determination of H2O2 in real samples with quick response, good sensitivity, high selectivity, and acceptable recovery. Copyright © 2013 Elsevier B.V. All rights reserved.

Effect of compositional dependence on physical and optical parameters of Te{sub 17}Se{sub 83−x}Bi{sub x} glassy system

Energy Technology Data Exchange (ETDEWEB)

Sharma, Pankaj, E-mail: pks_phy@yahoo.co.in [Department of Physics and Materials Science, Jaypee University of Information Technology, Waknaghat, Solan, HP 173234 (India); El-Bana, M.S.; Fouad, S.S. [Nano-Science and Semiconductor Laboratories, Department of Physics, Faculty of Education, Ain Shams University, Cairo (Egypt); Sharma, Vineet [Department of Physics and Materials Science, Jaypee University of Information Technology, Waknaghat, Solan, HP 173234 (India)

2016-05-15

In the present paper we have studied the effect of Bi addition on the physical and optical properties of thermally evaporated Te{sub 17}Se{sub 83−x}Bi{sub x} thin films. With Bi addition the density, mean coordination number, mechanical constraints, glass transition temperature increases. The other parameters theoretical energy gap, lone pair electron, deviation from stoichiometry decreases. Transmission spectra have been taken in the spectral range 400 nm–2500 nm using ultraviolet–visible–near infrared spectrophotometer. The fundamental absorption edge shifts towards longer wavelength with Bi incorporation. Optical energy gap and linear refractive index have been determined using transmission spectra. A good correlation has been drawn between the optical and theoretical parameters. Using linear optical parameters, the nonlinear optical susceptibility and nonlinear refractive index have been estimated. - Highlights: • Physical and optical parameters have been analyzed for Te{sub 17}Se{sub 83−x}Bi{sub x} glassy alloys. • The addition of Bi leads to decrease of average heat of atomization and cohesive energy. • The optical band gap decreases with increasing Bi content. • The third order susceptibility and nonlinear refractive index show an increase with increase in the Bi content.

Lowered operation voltage in Pt/SBi2Ta2O9/HfO2/Si ferroelectric-gate field-effect transistors by oxynitriding Si

International Nuclear Information System (INIS)

Horiuchi, Takeshi; Takahashi, Mitsue; Li, Qiu-Hong; Wang, Shouyu; Sakai, Shigeki

2010-01-01

Oxynitrided Si (SiON) surfaces show smaller subthreshold swings than do directly nitrided Si (SiN) surfaces when used in ferroelectric-gate field-effect transistors (FeFETs) having the following stacked-gate structure: Pt/SrBi 2 Ta 2 O 9 (SBT)/HfO 2 /Si. SiON/Si substrates for FeFETs were prepared by rapid thermal oxidation (RTO) in O 2 at 1000 °C and subsequent rapid thermal nitridation (RTN) in NH 3 at various temperatures in the range 950–1150 °C. The electrical properties of the Pt/SBT/HfO 2 /SiON/Si FeFET were compared with those of reference FETs, i.e. Pt/SBT/HfO 2 gate stacks formed on Si substrates subjected to various treatments: SiN x /Si formed by RTN, SiO 2 /Si formed by RTO and untreated Si. The Pt/SBT/HfO 2 /SiON/Si FeFET had a larger memory window than all the other reference FeFETs, particularly at low operation voltages when the RTN temperature was 1050 °C

Fabrication of β-cyclodextrin-coated poly (diallyldimethylammonium chloride)-functionalized graphene composite film modified glassy carbon-rotating disk electrode and its application for simultaneous electrochemical determination colorants of sunset yellow and tartrazine

International Nuclear Information System (INIS)

Ye, Xiaoliang; Du, Yongling; Lu, Daban; Wang, Chunming

2013-01-01

Graphical abstract: -- Highlights: •A green and facile approach for synthesis of β-CD-PDDA-Gr at room temperature. •We present the β-CD-PDDA-Gr modified GC-RDE for simultaneous detection of SY and TT. •SY and TT's electrooxidations are both the one-electron-one-proton-transfer process. •Diffusion coefficients and standard rate constants of SY and TT were discussed. -- Abstract: We proposed a green and facile approach for the synthesis of β-cyclodextrin-coated poly(diallyldimethylammonium chloride)-functionalized graphene composite film (β-CD-PDDA-Gr) by using L-ascorbic acid (L-AA) as the reducing agent at room temperature. The β-CD-PDDA-Gr composite film modified glassy carbon-rotating disk electrode (GC-RDE) was then developed for the sensitive simultaneous determination of two synthetic food colorants: sunset yellow (SY) and tartrazine (TT). By cyclic voltammetry (CV), the peak currents of SY and TT increased obviously on the developed electrochemical sensor. The kinetic parameters, such as diffusion coefficient D and standard heterogeneous rate constant k b , were estimated by linear sweep voltammetry (LSV). Under the optimal conditions, the differential pulse voltammetry (DPV) signals of SY and TT on the β-CD-PDDA-Gr modified GC-RDE were significantly enhanced. The enhanced anodic peak currents represented the excellent analytical performance of simultaneous detection of SY and TT in the range of 5.0 × 10 −8 to 2.0 × 10 −5 mol L −1 , with a low limit of detection (LOD) of 1.25 × 10 −8 mol L −1 for SY and 1.43 × 10 −8 mol L −1 for TT (S N −1 = 3). This proposed method displayed outstanding selectivity, good stability and acceptable repeatability and reproducibility, and also has been used to simultaneously determine SY and TT in some commercial soft drinks with satisfactory results. The obtained results were compared to HPLC of analysis for those two colorants and no significant differences were found. By the treatment of the

Fabrication of β-cyclodextrin-coated poly (diallyldimethylammonium chloride)-functionalized graphene composite film modified glassy carbon-rotating disk electrode and its application for simultaneous electrochemical determination colorants of sunset yellow and tartrazine

Energy Technology Data Exchange (ETDEWEB)

Ye, Xiaoliang; Du, Yongling; Lu, Daban; Wang, Chunming, E-mail: wangcm@lzu.edu.cn

2013-05-24

Graphical abstract: -- Highlights: •A green and facile approach for synthesis of β-CD-PDDA-Gr at room temperature. •We present the β-CD-PDDA-Gr modified GC-RDE for simultaneous detection of SY and TT. •SY and TT's electrooxidations are both the one-electron-one-proton-transfer process. •Diffusion coefficients and standard rate constants of SY and TT were discussed. -- Abstract: We proposed a green and facile approach for the synthesis of β-cyclodextrin-coated poly(diallyldimethylammonium chloride)-functionalized graphene composite film (β-CD-PDDA-Gr) by using L-ascorbic acid (L-AA) as the reducing agent at room temperature. The β-CD-PDDA-Gr composite film modified glassy carbon-rotating disk electrode (GC-RDE) was then developed for the sensitive simultaneous determination of two synthetic food colorants: sunset yellow (SY) and tartrazine (TT). By cyclic voltammetry (CV), the peak currents of SY and TT increased obviously on the developed electrochemical sensor. The kinetic parameters, such as diffusion coefficient D and standard heterogeneous rate constant k{sub b}, were estimated by linear sweep voltammetry (LSV). Under the optimal conditions, the differential pulse voltammetry (DPV) signals of SY and TT on the β-CD-PDDA-Gr modified GC-RDE were significantly enhanced. The enhanced anodic peak currents represented the excellent analytical performance of simultaneous detection of SY and TT in the range of 5.0 × 10{sup −8} to 2.0 × 10{sup −5} mol L{sup −1}, with a low limit of detection (LOD) of 1.25 × 10{sup −8} mol L{sup −1} for SY and 1.43 × 10{sup −8} mol L{sup −1} for TT (S N{sup −1} = 3). This proposed method displayed outstanding selectivity, good stability and acceptable repeatability and reproducibility, and also has been used to simultaneously determine SY and TT in some commercial soft drinks with satisfactory results. The obtained results were compared to HPLC of analysis for those two colorants and no significant

Study of optical properties of vacuum evaporated carbon nanotube containing Se80Te16Cu4 thin films

Science.gov (United States)

Upadhyay, A. N.; Tiwari, R. S.; Singh, Kedar

2016-08-01

Thin films of Se80Te16Cu4 glassy alloy and 3 wt.% of carbon nanotubes (CNTs) containing Se80Te16Cu4 glassy composite were deposited on clean glass substrate by thermal evaporation technique. The scanning electron microscope and energy dispersive x-ray analysis were performed to investigate the surface morphology and elemental composition of as synthesised samples. The reflectance and transmittance spectra of as-deposited thin films were recorded (200-1100 nm) by using UV/VIS/NIR spectrophotometer. The optical band gap and optical constants such as absorption coefficient (α), refractive index (n) and extinction coefficient (k) of Se80Te16Cu4 and 3 wt.% CNTs-Se80Te16Cu4 glassy composite thin films were calculated. It is observed that optical properties alter due to CNTs incorporation in Se80Te16Cu4 glassy alloy. Effect on optical properties due to CNTs incorporation can be explained in terms of concentration of unsaturated bonds/defects in the localised states.

Composite Coatings with Ceramic Matrix Including Nanomaterials as Solid Lubricants for Oil-Less Automotive Applications

Directory of Open Access Journals (Sweden)

Posmyk A.

2016-06-01

Full Text Available The paper presents the theoretical basis of manufacturing and chosen applications of composite coatings with ceramic matrix containing nanomaterials as a solid lubricant (AHC+NL. From a theoretical point of view, in order to reduce the friction coefficient of sliding contacts, two materials are required, i.e. one with a high hardness and the other with low shear strength. In case of composite coatings AHC+NL the matrix is a very hard and wear resistant anodic oxide coating (AHC whereas the solid lubricant used is the nanomaterial (NL featuring a low shear strength such as glassy carbon nanotubes (GC. Friction coefficient of cast iron GJL-350 sliding against the coating itself is much higher (0.18-0.22 than when it slides against a composite coating (0.08-0.14. It is possible to reduce the friction due to the presence of carbon nanotubes, or metal nanowires.

Electrochemical parameters of ethamsylate at multi-walled carbon nanotube modified glassy carbon electrodes.

Science.gov (United States)

Wang, Sheng-Fu; Xu, Qiao

2007-05-01

In this paper, some electrochemical parameters of ethamsylate at a multi-walled carbon nanotube modified glassy carbon electrode, such as the charge number, exchange current density, standard heterogeneous rate constant and diffusion coefficient, were measured by cyclic voltammetry, chronoamperometry and chronocoulometry. The modified electrode exhibits good promotion of the electrochemical reaction of ethamsylate and increases the standard heterogeneous rate constant of ethamsylate greatly. The differential pulse voltammetry responses of ethamsylate were linearly dependent on its concentrations in a range from 2.0 x 10(-6) to 6.0 x 10(-5) mol L(-1), with a detection limit of 4.0 x 10(-7) mol L(-1).

Electronic Transport Behaviors due to Charge Density Waves in Ni-Nb-Zr-H Glassy Alloys

Science.gov (United States)

Fukuhara, Mikio; Umemori, Yoshimasa

2013-11-01

The amorphous Ni-Nb-Zr-H glassy alloy containing subnanometer-sized icosahedral Zr5 Nb5Ni3 clusters exhibited four types of electronic phenomena: a metal/insulator transition, an electric current-induced voltage oscillation (Coulomb oscillation), giant capacitor behavior and an electron avalanche with superior resistivity. These findings could be excluded by charge density waves that the low-dimensional component of clusters, in which the atoms are lined up in chains along the [130] direction, plays important roles in various electron transport phenomena.

Electrocatalytic performance of Pu(IV)/Pu(III) redox reaction at graphene modified glassy carbon electrode

International Nuclear Information System (INIS)

Gupta, Ruma; Gamare, J.S.; Kamat, J.V.; Aggarwal, S.K.

2014-01-01

In this paper we explore the analytical perspectives of graphene modified electrode utilising commercially available graphene, which is well characterised, completely free from surfactants and has not been purposely oxidised or treated. We compare and critically contrast the electro-analytical performance of graphene modified glassy carbon electrodes (Gr/GC) with that of unmodified GC electrode towards Pu(IV)/Pu(III) redox reaction, monitoring of which has considerable importance in a plethora of areas where electrochemistry is conveniently and beneficially utilised for determination of nuclear fuels

Influence of surface morphology on methanol oxidation at a glassy carbon-supported Pt catalyst

Directory of Open Access Journals (Sweden)

S. STEVANOVIC

2008-08-01

Full Text Available Platinum supported on glassy carbon (GC was used as a model system for studying the influence of the surface morphology of a Pt catalyst on methanol oxidation in alkaline and acidic solutions. Platinum was deposited by the potential step method on GC samples from H2SO4 + H2PtCl6 solution under the same conditions with loadings from 10 to 80 mg cm-2. AFM and STM images of the GC/Pt electrodes showed that the Pt was deposited in the form of 3D agglomerates composed of spherical particles. Longer deposition times resulted in increased growth of Pt forms and a decrease in the specific area of the Pt. The real surface area of Pt increased with loading but the changes were almost negligible at higher loadings. Nevertheless, both the specific and mass activity of platinum supported on glassy carbon for methanol oxidation in acidic and in alkaline solutions exhibit a volcanic dependence with respect to the platinum loading. The increase in the activity can be explained by the increasing the particle size with the loading and thus an increase in the contiguous Pt sites available for adsorption and decomposition of methanol. However, the decrease in the activity of the catalyst with further increase of loading and particle size after reaching the maximum is related to the decrease of active sites available for methanol adsorption and their accessibility as a result of more close proximity and pronounced coalescence of the Pt particles.

Hollow fiber membranes and methods for forming same

Science.gov (United States)

Bhandari, Dhaval Ajit; McCloskey, Patrick Joseph; Howson, Paul Edward; Narang, Kristi Jean; Koros, William

2016-03-22

The invention provides improved hollow fiber membranes having at least two layers, and methods for forming the same. The methods include co-extruding a first composition, a second composition, and a third composition to form a dual layer hollow fiber membrane. The first composition includes a glassy polymer; the second composition includes a polysiloxane; and the third composition includes a bore fluid. The dual layer hollow fiber membranes include a first layer and a second layer, the first layer being a porous layer which includes the glassy polymer of the first composition, and the second layer being a polysiloxane layer which includes the polysiloxane of the second composition.

X-ray photoelectron spectroscopy and Auger electron spectroscopy studies on the passivation behavior of plasma-nitrided low alloy steel in nitric acid

Energy Technology Data Exchange (ETDEWEB)

Chyou, S.D.; Shih, H.C. (Dept. of Materials Science and Engineering, National Tsing Hua Univ., Hsinchu (Taiwan))

1991-12-14

Nitrided SAE 4140 steel has been passivated by concentrated nitric acid. The resulting film was characterized using a combination of surface-analytical techniques, such as X-ray photoelectron spectroscopy (XPS) to evaluate the chemical composition of the passive film. Auger electron spectroscopy (AES) combined with ion etching was used to determine the composition depth profiles of nitrided surface. It was found that preferential dissolution of iron leads to enhanced nitrogen and chromium concentrations within the oxynitrided layer. A dense protective oxynitrided layer was found to be formed on the nitrided surface when the concentration of nitric acid was as high as 8 M. The results of X-ray diffraction, XPS and AES analyses conclude that the protective nitride layer is composed of (Fe,Cr){sub 4}N, (Fe,Cr){sub 2-3}N and CrN in the inner layer, Fe{sub 2}O{sub 3}, Cr{sub 2}O{sub 3} and remnant nitrides in the middle layer and nitrides accompanying Cr(OH){sub 3}.H{sub 2}O and {gamma}'-FeOOH in the outermost layer. (orig.).

Size dependence of photocatalytic oxidation reactions of Rh nanoparticles dispersed on (Ga1-xZnx)(N1-xOx) support

NARCIS (Netherlands)

Zhang, Y.; Ligthart, D.A.J.M.; Liu, P.; Gao, L.; Verhoeven, M.W.G.M.; Hensen, E.J.M.

2014-01-01

Mixed Ga–Zn oxynitrides were synthesized using coprecipitation, wet-precipitation, and solid-solution methods. The oxynitrides were used as supports for Rh nanoparticle catalysts in photocatalytic water splitting, CO oxidation, and H2 oxidation. Mixed Ga–Zn oxynitrides produced by wet precipitation

Voltammetric Determination of Salbutamol Based on Electrochemical Oxidation at Platinum and Glassy Carbon Electrodes

OpenAIRE

YILMAZ, Niyazi; ÖZKAN, Sibel A.; USLU, Bengi

2014-01-01

The oxidative behavior of salbutamol was studied as a function of pH at platinum and activated glassy carbon electrodes. Between pH 1.9 and 12.0, the drug was characterized by a single oxidation step at both electrodes. The process was found to be dependent on the nature and the pH of the supporting elctrolyte. The procedure yielded a linear concentration range of 1 \\times 10-4 to 1 \\times 10-3 M and 2 \\times 10-5 to 1 \\times 10-3 M in 0.2 M sulphuric acid and a phosphate buffer of pH 6, at p...

Polymorphic ethyl alcohol as a model system for the quantitative study of glassy behaviour

Energy Technology Data Exchange (ETDEWEB)

Fischer, H E; Schober, H; Gonzalez, M A [Institut Max von Laue - Paul Langevin (ILL), 38 - Grenoble (France); Bermejo, F J; Fayos, R; Dawidowski, J [Consejo Superior de Investigaciones Cientificas, Madrid (Spain); Ramos, M A; Vieira, S [Universidad Autonoma de Madrid (Spain)

1997-04-01

The nearly universal transport and dynamical properties of amorphous materials or glasses are investigated. Reasonably successful phenomenological models have been developed to account for these properties as well as the behaviour near the glass-transition, but quantitative microscopic models have had limited success. One hindrance to these investigations has been the lack of a material which exhibits glass-like properties in more than one phase at a given temperature. This report presents results of neutron-scattering experiments for one such material ordinary ethyl alcohol, which promises to be a model system for future investigations of glassy behaviour. (author). 8 refs.

Phonon activity and intermediate glassy phase of YVO3

International Nuclear Information System (INIS)

Massa, Nestor E.; Piamonteze, Cinthia; Tolentino, Helio C.N.; Alonso, Jose Antonio; Martinez-Lope, Maria Jesus; Casais, Maria Teresa

2004-01-01

We show that in YVO 3 additional hard phonons gradually become zone center infrared active below ∼210 K, verifying that a lattice phase transition takes place at about that temperature. Their gradual increment in intensity between ∼210 and ∼77 K is associated with a 'glassy' behavior found in the temperature-dependent V K edge pseudoradial distribution. This translates into an increase in the Debye-Waller factors ascribed to the appearance of V local structural disorder below ∼150 K. Conflicts between various ordering mechanisms in YVO 3 bring up similarities of the intermediate phase to known results in dielectric incommensurate systems, suggesting the formation of commensurate domains below 116 K, the onset temperature of G-type antiferromagnetism. We propose that ∼210 and ∼77 K be understood as the temperatures where the commensurate-incommensurate and incommensurate-commensurate 'lock-in' phase transitions take place. We found support for this interpretation in the inverted λ shapes of the measured heat capacity and in the overall temperature dependence of the hard phonons

New Scenario of Dynamical Heterogeneity in Supercooled Liquid and Glassy States of 2D Monatomic System.

Science.gov (United States)

Van Hoang, Vo; Teboul, Victor; Odagaki, Takashi

2015-12-24

Via analysis of spatiotemporal arrangements of atoms based on their dynamics in supercooled liquid and glassy states of a 2D monatomic system with a double-well Lennard-Jones-Gauss (LJG) interaction potential, we find a new scenario of dynamical heterogeneity. Atoms with the same or very close mobility have a tendency to aggregate into clusters. The number of atoms with high mobility (and size of their clusters) increases with decreasing temperature passing over a maximum before decreasing down to zero. Position of the peak moves toward a lower temperature if mobility of atoms in clusters is lower together with an enhancement of height of the peak. In contrast, the number of atoms with very low mobility or solidlike atoms (and size of their clusters) has a tendency to increase with decreasing temperature and then it suddenly increases in the vicinity of the glass transition temperature leading to the formation of a glassy state. A sudden increase in the number of strongly correlated solidlike atoms in the vicinity of a glass transition temperature (Tg) may be an origin of a drastical increase in viscosity of the glass-forming systems approaching the glass transition. In fact, we find that the diffusion coefficient decays exponentially with a fraction of solidlike atoms exhibiting a sudden decrease in the vicinity of the glass transition region.

Impact of crystallization on the structure and chemical durability of borosilicate glass

International Nuclear Information System (INIS)

Nicoleau, Elodie

2016-01-01

This work describes a new approach to help understand the chemical durability of partially crystallized nuclear waste conditioning matrices. Among the studies carried out on nuclear waste deep geological disposal, long term behavior studies have so far been conducted on homogeneous glassy matrices. However, as the crystalline phases may generate modifications in the chemical composition and properties of such matrices, the description and a better understanding of their effects on the chemical durability of waste packages are of primary importance. A protocol to study the durability of heterogeneous model matrices of nuclear interest containing different types of crystalline phases was developed. It is based on a detailed description of the morphology, microstructure and structure of the glassy matrix and crystalline phases, and on the study of various alteration regimes. Three crystal phases that may form when higher concentrations of waste are immobilized in Uranium Oxide type conditioning glasses were studied: alkali and alkaline earth molybdates, rare earth silicates and ruthenium oxide. The results highlight the roles of the composition and the structure of the surrounding glassy matrix as the parameters piloting the alteration kinetics of the partially crystallized glassy matrices. This behavior is identical whatever the nature of the crystalline phases, as long as these phases do not lead to a composition gradient and do not percolate within the glassy matrix. Given these results, a methodology to study partially crystallized matrices with no composition gradient is then suggested. Its key development lies firstly in the evaluation of the behavior of partially crystallized matrices through the experimental study of the residual glassy matrix in various alteration regimes. This methodology may be adapted to the case of new glass formulations with more complex compositions (e.g. highly waste-loaded glass), which may contain crystals formed during cooling

Sensitive determination of buformin using poly-aminobenzoic acid modified glassy carbon electrode

Directory of Open Access Journals (Sweden)

Gui-Ying Jin

2012-12-01

Full Text Available Glassy carbon electrode, which is used to electrochemically determine the content of buformin, is modified with an electropolymerized film of p-aminobenzoic acid in pH 7.0 acetate buffer solution (ABS. The polymer showed an excellent electrocatalytic activity for the reduction of buformin. In pH 7.0 ABS, the cathodic peak current increased linearly over three concentration intervals of buformin, and the detection limit (S/N=3 was 2.0×10−9 g/mL. The method was successfully applied to directly determine buformin in tablets with standard addition recoveries of 95.8–102.5%. The proposed method is simple, cheap and highly efficient. Keywords: Chemically modified electrode, Aminobenzoic acid, Buformin

Voltammetric Determination of Flunixin on Molecularly Imprinted Polypyrrole Modified Glassy Carbon Electrode

Directory of Open Access Journals (Sweden)

Abd-Elgawad Radi

2016-01-01

Full Text Available A novel electrochemical sensing approach, based on electropolymerization of a molecularly imprinted polypyrrole (MIPpy film onto a glassy carbon electrode (GCE surface, was developed for the detection of flunixin (FXN. The sensing conditions and the performance of the constructed sensor were assessed by cyclic, differential pulse and (DPV square wave voltammetry (SWV. The sensor exhibited high sensitivity, with linear responses in the range of 5.0 to 50.0 µM with detection limits of 1.5 and 1.0 µM for DPV and SWV, respectively. In addition, the sensor showed high selectivity towards FXN in comparison to other interferents. The sensor was successfully utilized for the direct determination of FXN in buffalo raw milk samples.

Composite materials comprising two jonal functions and methods for making the same

Science.gov (United States)

Fareed, Ali Syed; Garnier, John Edward; Schiroky, Gerhard Hans; Kennedy, Christopher Robin; Sonuparlak, Birol

2001-01-01

The present invention generally relates to mechanisms for preventing undesirable oxidation (i.e., oxidation protection mechanisms) in composite bodies. The oxidation protection mechanisms include getterer materials which are added to the composite body which gather or scavenge undesirable oxidants which may enter the composite body. The getterer materials may be placed into at least a portion of the composite body such that any undesirable oxidant approaching, for example, a fiber reinforcement, would be scavenged by (e.g., reacted with) the getterer. The getterer materials) may form at least one compound which acts as a passivation layer, and/or is able to move by bulk transport (e.g., by viscous flow as a glassy material) to a crack, and sealing the crack, thereby further enhancing the oxidation protection of the composite body. One or more ceramic filler materials which serve as reinforcements may have a plurality of super-imposed coatings thereon, at least one of which coatings may function as or contain an oxidation protection mechanism. Specifically, a coating comprising boron nitride which has been engineered or modified to contain some silicon exhibits improved corrosion resistance, specifically to oxygen and moisture. The coated materials may be useful as reinforcing materials in high performance composites to provide improved mechanical properties such as fracture toughness. The present invention also relates to improved composites which incorporate these materials, and to their methods of manufacture.

Electrochemical tyrosine sensor based on a glassy carbon electrode modified with a nanohybrid made from graphene oxide and multiwalled carbon nanotubes

International Nuclear Information System (INIS)

Li, J.; Kuang, D.; Feng, Y.; Zhang, F.; Xu, Z.; Liu, M.; Wang, D.

2013-01-01

We report on a glassy carbon electrode that was modified with a composite made from graphene oxide (GO) and multiwalled carbon nanotubes (MWCNT) that enables highly sensitive determination of L-tyrosine. The sensor was characterized by transmission electron microscopy and electrochemical impedance spectroscopy, and its electrochemical properties by cyclic voltammetry, chronocoulometry and differential pulse voltammetry. The GO/MWCNT hybrid exhibits strong catalytic activity toward the oxidation of L-tyrosine, with a well defined oxidation peak at 761 mV. The respective current serves as the analytical information and is proportional to the L-tyrosine concentration in two ranges of different slope (0.05 to 1.0 μM and 1.0 to 650.0 μM), with limits of detection and quantification as low as 4.4 nM and 14.7 nM, respectively. The method was successfully applied to the analysis of L-tyrosine in human body fluids. The excellent reproducibility, stability, sensitivity and selectivity are believed to be due to the combination of the electrocatalytic properties of both GO and MWCNT. They are making this hybrid electrode a potentially useful electrochemical sensing platform for bioanalysis. (author)

Electrochemical tyrosine sensor based on a glassy carbon electrode modified with a nanohybrid made from graphene oxide and multiwalled carbon nanotubes

Energy Technology Data Exchange (ETDEWEB)

Li, J.; Kuang, D.; Feng, Y.; Zhang, F.; Xu, Z.; Liu, M.; Wang, D., E-mail: junhua325@yahoo.com.cn [Key Laboratory of Functional Organometallic Materials of Hunan Province College, Department of Chemistry and Material Science, Hengyang Normal University, Hunan, Hengyang, 421008 (China)

2013-01-15

We report on a glassy carbon electrode that was modified with a composite made from graphene oxide (GO) and multiwalled carbon nanotubes (MWCNT) that enables highly sensitive determination of L-tyrosine. The sensor was characterized by transmission electron microscopy and electrochemical impedance spectroscopy, and its electrochemical properties by cyclic voltammetry, chronocoulometry and differential pulse voltammetry. The GO/MWCNT hybrid exhibits strong catalytic activity toward the oxidation of L-tyrosine, with a well defined oxidation peak at 761 mV. The respective current serves as the analytical information and is proportional to the L-tyrosine concentration in two ranges of different slope (0.05 to 1.0 {mu}M and 1.0 to 650.0 {mu}M), with limits of detection and quantification as low as 4.4 nM and 14.7 nM, respectively. The method was successfully applied to the analysis of L-tyrosine in human body fluids. The excellent reproducibility, stability, sensitivity and selectivity are believed to be due to the combination of the electrocatalytic properties of both GO and MWCNT. They are making this hybrid electrode a potentially useful electrochemical sensing platform for bioanalysis. (author)

Simple flow injection for determination of sulfite by amperometric detection using glassy carbon electrode modified with carbon nanotubes-PDDA-gold nanoparticles.

Science.gov (United States)

Amatatongchai, Maliwan; Sroysee, Wongduan; Chairam, Sanoe; Nacapricha, Duangjai

2015-02-01

A new approach is presented for sensitive and selective measurement of sulfite (SO3(2-)) in beverages based on a simple flow injection system with amperometric detection. In this work, the sulfite sensor was a glassy carbon electrode modified with multiwall carbon nanotubes-poly(diallyldimethylammonium chloride)-gold nanoparticles composites (CNTs-PDDA-AuNPs/GC). Electrochemical oxidation of sulfite with this electrode was first studied in 0.1M phosphate buffer (pH 7.0) using cyclic voltammetry. The results indicated that the CNTs-PDDA-AuNPs/GC electrode possesses electrocatalytic activity for the oxidation of sulfite with high sensitivity and selectivity. Sulfite was quantified using amperometric measurement with the new sensor at +0.4V vs Ag/AgCl in conjunction with flow injection. The linear working range for the quantitation of sulfite was 2-200 mg L(-1) (r(2)=0.998) with a detection limit of 0.03 mg L(-1) (3σ of blank) and an estimated precision of 1.5%.The proposed method was successfully applied to the determination of sulfite in fruit juices and wines with a sample throughput of 23 samples per hour. Copyright © 2014 Elsevier B.V. All rights reserved.

Al-oxynitride interfacial layer investigations for Pr{sub X}O{sub Y} on SiC and Si

Energy Technology Data Exchange (ETDEWEB)

Henkel, K; Karavaev, K; Torche, M; Schwiertz, C; Burkov, Y; Schmeisser, D [Brandenburgische Technische Universitaet Cottbus, Angewandte Physik-Sensorik, K-Wachsmann-Allee 17, 03046 Cottbus (Germany)], E-mail: henkel@tu-cottbus.de

2008-01-15

We investigate the dielectric properties of Praseodymium based oxides Pr{sub X}O{sub Y} by preparing MIS (metal insulator semiconductor) structures consisting of Pr{sub X}O{sub Y} as a high-k insulating layer and silicon (Si) or silicon carbide (SiC) as semiconductor substrates. The use of a buffer layer between Pr{sub X}O{sub Y} and the semiconductor is necessary as we found deleterious reactions between these materials such as silicate and graphite formation. Possessing a higher permittivity value ({epsilon}{sub r}) than silicon dioxide (SiO{sub 2}) and good lattice matching in conjunction with similar thermal expansion coefficient to SiC, we focus on aluminum oxynitride (AlON) as a suitable buffer layer for this high-k/wide-bandgap system. In our spectroscopic investigations we found a decrease or indeed prevention of silicon diffusion into the oxide and an increased Pr{sub 2}O{sub 3} fraction after deposition. In electrical characterizations of Pr{sub X}O{sub Y}/AlON stacks we found considerable improvements in the leakage current by several orders on both substrates, especially on silicon where we obtain values down to 10{sup -7}A/cm{sup 2} at a CET (capacitance equivalent thickness) of 4nm. We observed interface state densities in the range of 5 x 10{sup 11}-1 x 10{sup 12}/eVcm{sup 2} and 1-5 x 10{sup 12}/eVcm{sup 2} on Si and SiC, respectively.

Structure, phases, and mechanical response of Ti-alloy bioactive glass composite coatings

Energy Technology Data Exchange (ETDEWEB)

Nelson, G.M.; Nychka, J.A. [Department of Chemical and Materials Engineering, University of Alberta, 7th Floor, Electrical and Computer Engineering Research Facility, Edmonton, Alberta T6G 2V4 (Canada); McDonald, A.G., E-mail: andre2@ualberta.ca [Department of Mechanical Engineering, University of Alberta, 4-9 Mechanical Engineering Building, Edmonton, Alberta T6G 2G8 (Canada)

2014-03-01

Porous titanium alloy-bioactive glass composite coatings were manufactured via the flame spray deposition process. The porous coatings, targeted for orthodontic and bone-fixation applications, were made from bioactive glass (45S5) powder blended with either commercially pure titanium (Cp-Ti) or Ti-6Al-4V alloy powder. Two sets of spray conditions, two metallic particle size distributions, and two glass particle size distributions were used for this study. Negative control coatings consisting of pure Ti-6Al-4V alloy or Cp-Ti were sprayed under both conditions. The as-sprayed coatings were characterized through quantitative optical cross-sectional metallography, X-ray diffraction (XRD), and ASTM Standard C633 tensile adhesion testing. Determination of the porosity and glassy phase distribution was achieved by using image analysis in accordance with ASTM Standard E2109. Theoretical thermodynamic and heat transfer modeling was conducted to explain experimental observations. Thermodynamic modeling was performed to estimate the flame temperature and chemical environment for each spray condition and a lumped capacitance heat transfer model was developed to estimate the temperatures attained by each particle. These models were used to establish trends among the choice of alloy, spray condition, and particle size distribution. The deposition parameters, alloy composition, and alteration of the feedstock powder size distribution had a significant effect on the coating microstructure, porosity, phases present, mechanical response, and theoretical particle temperatures that were attained. The most promising coatings were the Ti-6Al-4V-based composite coatings, which had bond strength of 20 ± 2 MPa (n = 5) and received reinforcement and strengthening from the inclusion of a glassy phase. It was shown that the use of the Ti-6Al-4V-bioactive glass composite coatings may be a superior choice due to the possible osteoproductivity from the bioactive glass, the potential ability to

Glass composite waste forms for iodine confined in bismuth-embedded SBA-15

Science.gov (United States)

Yang, Jae Hwan; Park, Hwan Seo; Ahn, Do-Hee; Yim, Man-Sung

2016-11-01

The aim of this study was to stabilize bismuth-embedded SBA-15 that captured iodine gas by fabrication of monolithic waste forms. The iodine containing waste was mixed with Bi2O3 (a stabilizing additive) and low-temperature sintering glass followed by pelletizing and the sintering process to produce glass composite materials. Iodine volatility during the sintering process was significantly affected by the ratio of Bi2O3 and the glass composition. It was confirmed that BiI3, the main iodine phase within bismuth-embedded SBA-15, was effectively transformed to the mixed phases of Bi5O7I and BiOI. The initial leaching rates of iodine from the glass composite waste forms ranged 10-3-10-2 g/m2 day, showing the stability of the iodine phases encapsulated by the glassy networks. It was also observed that common groundwater anions (e.g., chloride, carbonate, sulfite, and fluoride) elevated the iodine leaching rate by anion exchange reactions. The present results suggest that the glass composite waste form of bismuth-embedded SBA-15 could be a candidate material for stable storage of 129I.

Electrochemical determination of mesotrione at organoclay modified glassy carbon electrodes.

Science.gov (United States)

Kamga Wagheu, Josephine; Forano, Claude; Besse-Hoggan, Pascale; Tonle, Ignas K; Ngameni, Emmanuel; Mousty, Christine

2013-01-15

A natural Cameroonian smectite-type clay (SaNa) was exchanged with cationic surfactants, namely cetyltrimethylammonium (CTA) and didodecyldimethyl ammonium (DDA) modifying its physico-chemical properties. The resulting organoclays that have higher adsorption capacity for mesotrione than the pristine SaNa clay, have been used as modifiers of glassy carbon electrode for the electrochemical detection of this herbicide by square wave voltammetry. The stripping performances of SaNa, SaCTA and SaDDA modified electrodes were therefore evaluated and the experimental parameters were optimized. SaDDA gives the best results in deoxygenated acetate buffer solution (pH 6.0) after 2 min accumulation under open circuit conditions. Under optimal conditions, the reduction current is proportional to mesotrione concentration in the range from 0.25 to 2.5 μM with a detection limit of 0.26 μM. The fabricated electrode was also applied for the commercial formulation CALLISTO, used in European maize market. Copyright © 2012 Elsevier B.V. All rights reserved.

Mechanical Properties for Reliability Analysis of Structures in Glassy Carbon

CERN Document Server

Garion, Cédric

2014-01-01

Despite its good physical properties, the glassy carbon material is not widely used, especially for structural applications. Nevertheless, its transparency to particles and temperature resistance are interesting properties for the applications to vacuum chambers and components in high energy physics. For example, it has been proposed for fast shutter valve in particle accelerator [1] [2]. The mechanical properties have to be carefully determined to assess the reliability of structures in such a material. In this paper, mechanical tests have been carried out to determine the elastic parameters, the strength and toughness on commercial grades. A statistical approach, based on the Weibull’s distribution, is used to characterize the material both in tension and compression. The results are compared to the literature and the difference of properties for these two loading cases is shown. Based on a Finite Element analysis, a statistical approach is applied to define the reliability of a structural component in gl...

Formation, thermal stability and mechanical properties of bulk glassy alloys with a diameter of 20 mm in Zr-(Ti,Nb)-Al-Ni-Cu system

International Nuclear Information System (INIS)

Inoue, A.; Zhang, Q.S.; Zhang, W.; Yubuta, K.; Son, K.S.; Wang, X.M.

2009-01-01

Bulk glassy alloy rods with a diameter of 20 mm were produced for Zr 61 Ti 2 Nb 2 Al 7.5 Ni 10 Cu 17.5 and Zr 60 Ti 2 Nb 2 Al 7.5 Ni 10 Cu 18.5 by a tilt casting method. The replacement of Zr by a small amount of Ti and Nb caused a distinct increase in the maximum diameter from 16 mm for Zr 65 Al 7.5 Ni 10 Cu 17.5 to 20 mm, accompanying the decrease in liquidus temperature and the increase in reduced glass transition temperature. The primary precipitation phase from supercooled liquid also shows a distinct change, i.e., from coexistent Zr 2 Cu, Zr 2 Ni and Zr 6 NiAl 2 phases for the 65%Zr alloy to an icosahedral phase for the 61%Zr and 60%Zr alloys. These results allow us to presume that the enhancement of the glass-forming ability is due to an increase in the stability of supercooled liquid against crystallization caused by the development of icosahedral short-range ordered atomic configurations. The 60%Zr specimens taken from the central and near-surface regions in the transverse cross section at the site which is 15 mm away from the bottom surface of the cast glassy rod with a diameter of 20 mm exhibit good mechanical properties under a compressive deformation mode, i.e., Young's modulus of 81 GPa, large elastic strain of 0.02, high yield strength of 1610 MPa and distinct plastic strain of 0.012. Besides, a number of shear bands are observed along the maximum shear stress plane on the peripheral surface near the final fracture site. The finding of producing the large scale Zr-based bulk glassy alloys exhibiting reliable mechanical properties is encouraging for future advancement of bulk glassy alloys as a new type of functional material. (author)

Study of crystallization kinetics and structural relaxation behavior in phase separated Ag{sub 33}Ge{sub 17}Se{sub 50} glassy alloys

Energy Technology Data Exchange (ETDEWEB)

Kumar, Praveen, E-mail: prafiziks@gmail.com [Semiconductors Laboratory, Department of Physics, GND University, Amritsar 143005 (India); Nanotechnology Research Centre, DAV Institute of Engineering and Technology, Kabir Nagar, Jalandhar 144008 (India); Yannopoulos, S.N. [Foundation for Research and Technology Hellas, Institute of Chemical Engineering and High Temperature Chemical Processes (FORTH/ICE-HT), P.O. Box 1414, GR-26 504, Rio-Patras (Greece); Sathiaraj, T.S. [Department of Physics, University of Botswana, Gaborone (Botswana); Thangaraj, R., E-mail: rthangaraj@rediffmail.com [Semiconductors Laboratory, Department of Physics, GND University, Amritsar 143005 (India)

2012-07-16

We report on the crystallization processes and structure (crystal phases) of Ag{sub 33}Ge{sub 17}Se{sub 50} glassy alloy using differential scanning calorimetry and x-ray diffraction techniques, respectively. The devitrification that gives rise to the first exothermic peak results in the crystallization of Ag{sub 2}Se and Ag{sub 8}GeSe{sub 6} phases, while the growth of GeSe{sub 2} accompanied by the transformation of Ag{sub 8}GeSe{sub 6} to Ag{sub 2}Se phase occurs during the second crystallization process. Different theoretical models are used to elucidate various kinetic parameters for the crystallization transformation process in this phase separated system. With annealing below the glass transition temperature, an inverse behavior between the variation of the optical gap and the band tailing parameter is observed for the thermally evaporated films. These results are explained as the mixing of different clusters/species in the amorphous state and/or changes caused by structural relaxation of the glassy network for the thermally evaporated films. - Highlights: Black-Right-Pointing-Pointer Phase separation in Ag{sub 33}Ge{sub 17}Se{sub 50} glassy alloy bordering two glass forming regions. Black-Right-Pointing-Pointer Transformation of Ag{sub 8}GeSe{sub 6} {yields} Ag{sub 2}Se along with crystallization GeSe{sub 2} phase. Black-Right-Pointing-Pointer Elucidation of various kinetic parameters for the crystalline transformation. Black-Right-Pointing-Pointer Structural relaxation in thermally evaporated films by optical spectroscopy.

Alizarin red S functionalized mesoporous silica modified glassy carbon electrode for electrochemical determination of anthracene

International Nuclear Information System (INIS)

Liu, Shan; Wei, Maochao; Zheng, Xiangli; Xu, Shuai; Xia, Fangquan; Zhou, Changli

2015-01-01

Highlights: • Alizarin red S-SBA15 composite was prepared and characterized. • A novel sensing platform was constructed for anthracene determination. • The proposed sensor exhibited high sensitivity and low detection limit for detecting anthracene. • This method can be applied to the practical detection of anthracene in waste water. - Abstract: In the paper, a novel and sensitive electrochemical sensor based on modification of electroactive alizarin red S functionalized mesoporous silica material SBA15 onto glassy carbon electrode (ARS-SBA15/GCE) was developed. Alizarin red S, called electrochemical probe that can selectively recognize polycyclic aromatic hydrocarbons (PAHs), as tools for the detection of tricyclic aromatic hydrocarbon anthracene. The morphology and interface property of ARS modified SBA15 (ARS-SBA15) were examined by transmission electron microscopy (TEM) and fourier transform infrared spectroscopy (FTIR). Taking advantage of the π-π stacking force between alizarin red S and anthracene, the ARS-SBA15/GCE sensor could detect anthracene quantitatively in a wide range of 1.0 pM–10.0 nM and a low detection limit of 0.5 pM (S/N = 3). Other PAHs, such as naphthalene, phenanthrene, pyrene, and benzo[a]pyrene show little interference on the detection. Consequently, a simple and sensitive electrochemical method was proposed for the determination of anthracene, which can be used to determine anthracene in waste water samples. The electrochemical method provides a general tool that complements the commonly used spectroscopic methods and immune method for the detection of PAHs

Fabrication of calix[4]pyrrole nanofilms at the glassy carbon surface and their characterization by spectroscopic, optic and electrochemical methods

International Nuclear Information System (INIS)

Taner, Bilge; Ozcan, Emine; Ustuendag, Zafer; Keskin, Selda; Solak, Ali Osman; Eksi, Haslet

2010-01-01

meso-Octamethylcalix[4]pyrrole (CP) and meso-heptaethylcalix[4]pyrrole-meso-4-aminophenyl (4APCP) modified glassy carbon (GC) electrodes were prepared by the electrochemical oxidation in acetonitrile solution. Binding of the calix[4]pyrroles with the glassy carbon surface was investigated that it is through the etheric linkage revealed from the reflection-absorption infrared spectroscopy (RAIRS). Surface films of CP and 4APCP were investigated by cyclic voltammetry (CV), ellipsometry, X-ray photoelectron spectroscopy, RAIRS and the contact angle measurements. The thicknesses of the films were determined by ellipsometry which confirmed that the film was multilayer and homogeneous over the surface. Ellipsometric measurements also provided that the CP and 4APCP film thicknesses were 2.49 nm and 4.58 nm for 6 CV cycle modification, corresponding to 66 μF/cm 2 and 106 μF/cm 2 capacitances obtained by CV. The wetting behavior was examined by contact angle measurements and found that the hydrophobicity of the GC-4APCP surface was higher than that of GC-CP, probably due to the aromatic meso substituent present in the former.

Voltammetric behavior of sedative drug midazolam at glassy carbon electrode in solubilized systems.

Science.gov (United States)

Jain, Rajeev; Yadav, Rajeev Kumar

2012-04-01

Redox behavior of midazolam was studied at a glassy carbon electrode in various buffer systems, supporting electrolytes and pH using differential pulse, square-wave and cyclic voltammetry. Based on its reduction behavior, a direct differential pulse voltammetric method has been developed and validated for the determination of midazolam in parenteral dosage. Three well-defined peaks were observed in 0.1% SLS, Britton-Robinson (BR) buffer of pH 2.5. The effect of surfactants like sodium lauryl sulfate (SLS), cetyl trimethyl ammonium bromide (CTAB) and Tween 20 was studied. Among these surfactants SLS showed significant enhancement in reduction peak. The cathodic peak currents were directly proportional to the concentration of midazolam with correlation coefficient of 0.99.

Thermal shock behavior of nano-sized SiC particulate reinforced AlON composites

Energy Technology Data Exchange (ETDEWEB)

Zhao, X.J. [Department of Materials Science and Engineering, School of Materials and Metallurgy, Northeastern University, Shenyang, Liaoning 110004 (China); Department of Mechanical and Industrial Engineering, Ryerson University, Toronto, Ontario M5B 2K3 (Canada); Ru, H.Q., E-mail: ruhq@smm.neu.edu.cn [Department of Materials Science and Engineering, School of Materials and Metallurgy, Northeastern University, Shenyang, Liaoning 110004 (China); Chen, D.L., E-mail: dchen@ryerson.ca [Department of Mechanical and Industrial Engineering, Ryerson University, Toronto, Ontario M5B 2K3 (Canada); Zhang, N.; Liang, B. [Key Laboratory of Advanced Materials Manufacturing Technology of Liaoning Province, Shenyang University, Shenyang, Liaoning 110044 (China)

2012-03-25

Highlights: Black-Right-Pointing-Pointer Addition of nano-SiC particles enhances residual strength and critical temperature. Black-Right-Pointing-Pointer Young's modulus decreases with increasing quenching temperature. Black-Right-Pointing-Pointer Linear relationship between residual strength and thermal shock times is obtained. Black-Right-Pointing-Pointer Rougher fracture surfaces in the SiC-AlON composites are observed. - Abstract: Aluminum oxynitride (AlON) has been considered as a potential ceramic material for high-performance structural and advanced refractory applications. Thermal shock resistance is a major concern and an important performance index of high-temperature ceramics. While silicon carbide (SiC) particles have been proven to improve mechanical properties of AlON ceramic, the high-temperature thermal shock behavior was unknown. The aim of this investigation was to identify the thermal shock resistance and underlying mechanisms of AlON ceramic and 8 wt% SiC-AlON composites over a temperature range between 175 Degree-Sign C and 275 Degree-Sign C. The residual strength and Young's modulus after thermal shock decreased with increasing quenching temperature and thermal shock times due to large temperature gradients and thermal stresses caused by abrupt water-quenching. A linear relationship between the residual strength and thermal shock times was observed in both pure AlON and SiC-AlON composites. The addition of nano-sized SiC particles increased both residual strength and critical temperature from 200 Degree-Sign C in the monolithic AlON to 225 Degree-Sign C in the SiC-AlON composites due to the toughening effect, the lower coefficient of thermal expansion and higher thermal conductivity of SiC. The enhancement of the thermal shock resistance in the SiC-AlON composites was directly related to the change of fracture mode from intergranular cracking along with cleavage-type fracture in the AlON to a rougher fracture surface with ridge

Layer by layer assembly of glucose oxidase and thiourea onto glassy carbon electrode: Fabrication of glucose biosensor

Energy Technology Data Exchange (ETDEWEB)

Salimi, Abdollah, E-mail: absalimi@yahoo.com [Department of Chemistry, University of Kurdistsn, P.O. Box 416, Sanandaj (Iran, Islamic Republic of); Research Center for Nanotechnology, University of Kurdistan, P.O. Box 416, Sanandaj (Iran, Islamic Republic of); Noorbakhsh, Abdollah [Department of Chemistry, University of Kurdistsn, P.O. Box 416, Sanandaj (Iran, Islamic Republic of); Department of Nanotechnology Engenering, Faculty of Advanced Science and Technology, University of Isfahan, 81746-73441 (Iran, Islamic Republic of)

2011-07-01

Highlights: > Although various enzymes immobilization have been approve for the construction of glucose biosensor, a layer by layer (LBL) technique has attracted more attention due to simplicity of the procedure, wide choice of materials that can be used, controllability of film thickness and unique mechanical properties. > In this paper, we described a novel and simple strategy for developing an amperometric glucose biosensor based on layer-by-layer self assembly of glucose oxidase on the glassy carbon electrode modified by thiourea. > Thiourea has two amino groups that the one can be immobilized on the activated glassy carbon electrode and the other can be used for the coupling of glucose oxidase enzyme. > The biosensor exhibited good performance for electrocatalytic oxidation of glucose, such as high sensitivity, low detection limit, short response time and wide concentration range. > Finally, the new method is strongly recommended for immobilization of many other enzymes or proteins containing carbaldehyde or carboxylic groups for fabricating third generation biosensors and bioelectronics devices. - Abstract: For the first time a novel, simple and facile approach is described to construct highly stable glucose oxidase (GOx) multilayer onto glassy carbon (GC) electrode using thiourea (TU) as a covalent attachment cross-linker. The layer by layer (LBL) attachment process was confirmed by cyclic voltammetry, electrochemical impedance spectroscopy and Fourier transform infrared reflection spectroscopy (FT-IR-RS) techniques. Immobilized GOx shows excellent electrocatalytic activity toward glucose oxidation using ferrocenemethanol as artificial electron transfer mediator and biosensor response was directly correlated to the number of bilayers. The surface coverage of active GOx per bilayer, heterogeneous electron transfer rate constant (k{sub s}) and Michaelis-Menten constant (K{sub M}), of immobilized GOx were 1.50 x 10{sup -12} mol cm{sup -2}, 9.2 {+-} 0.5 s{sup -1

Layer by layer assembly of glucose oxidase and thiourea onto glassy carbon electrode: Fabrication of glucose biosensor

International Nuclear Information System (INIS)

Salimi, Abdollah; Noorbakhsh, Abdollah

2011-01-01

Highlights: → Although various enzymes immobilization have been approve for the construction of glucose biosensor, a layer by layer (LBL) technique has attracted more attention due to simplicity of the procedure, wide choice of materials that can be used, controllability of film thickness and unique mechanical properties. → In this paper, we described a novel and simple strategy for developing an amperometric glucose biosensor based on layer-by-layer self assembly of glucose oxidase on the glassy carbon electrode modified by thiourea. → Thiourea has two amino groups that the one can be immobilized on the activated glassy carbon electrode and the other can be used for the coupling of glucose oxidase enzyme. → The biosensor exhibited good performance for electrocatalytic oxidation of glucose, such as high sensitivity, low detection limit, short response time and wide concentration range. → Finally, the new method is strongly recommended for immobilization of many other enzymes or proteins containing carbaldehyde or carboxylic groups for fabricating third generation biosensors and bioelectronics devices. - Abstract: For the first time a novel, simple and facile approach is described to construct highly stable glucose oxidase (GOx) multilayer onto glassy carbon (GC) electrode using thiourea (TU) as a covalent attachment cross-linker. The layer by layer (LBL) attachment process was confirmed by cyclic voltammetry, electrochemical impedance spectroscopy and Fourier transform infrared reflection spectroscopy (FT-IR-RS) techniques. Immobilized GOx shows excellent electrocatalytic activity toward glucose oxidation using ferrocenemethanol as artificial electron transfer mediator and biosensor response was directly correlated to the number of bilayers. The surface coverage of active GOx per bilayer, heterogeneous electron transfer rate constant (k s ) and Michaelis-Menten constant (K M ), of immobilized GOx were 1.50 x 10 -12 mol cm -2 , 9.2 ± 0.5 s -1 and 3.42(±0

Probing Properties of Glassy Water and Other Liquids with Site Selective Spectroscopies

Energy Technology Data Exchange (ETDEWEB)

Dang, Nhan Chuong [Iowa State Univ., Ames, IA (United States)

2005-01-01

The standard non-photochemical hole burning (NPHB) mechanism, which involves phonon-assisted tunneling in the electronically excited state, was originally proposed to explain the light-induced frequency change of chemically stable molecules in glassy solids at liquid helium temperatures by this research group more than two decades ago. The NPHB mechanism was then further elucidated and the concept of intrinsic to glass configurational relaxation processes as pre-mediating step to the hole burning process was introduced. The latter provided the theoretical basis for NPHB to evolve into a powerful tool probing the dynamics and nature of amorphous media, which aside from ''simple'' inorganic glasses may include also ''complex'' biological systems such as living cells and cancerous/normal tissues. Presented in this dissertation are the experimental and theoretical results of hole burning properties of aluminum phthalocyanine tetrasulphonate (APT) in several different matrices: (1) hyperquenched glassy water (HGW); (2) cubic ice (I_c); and (3) water confined into poly(2-hydroxyethylmethacrylate) (poly-HEMA). In addition, results of photochemical hole burning (PHB) studies obtained for phthalocyanine tetrasulphonate (P_cT) in HGW and free base phthalocyanine (P_c) in ortho-dichlorobenzene (DCB) glass are reported. The goal of this dissertation was to provide further evidence supporting the NPHB mechanism and to provide more insight that leads to a better understanding of the kinetic events (dynamics) in glasses, and various dynamical processes of different fluorescent chromorphores in various amorphous solids and the liquid that exist above the glass transition temperature (T_g). The following issues are addressed in detail: (1) time evolution of hole being burned under different conditions and in different hole burning systems; (2) temperature dependent hole profile; and (3) the structure

Mode coupling theory for nonequilibrium glassy dynamics of thermal self-propelled particles.

Science.gov (United States)

Feng, Mengkai; Hou, Zhonghuai

2017-06-28

We present a mode coupling theory study for the relaxation and glassy dynamics of a system of strongly interacting self-propelled particles, wherein the self-propulsion force is described by Ornstein-Uhlenbeck colored noise and thermal noises are included. Our starting point is an effective Smoluchowski equation governing the distribution function of particle positions, from which we derive a memory function equation for the time dependence of density fluctuations in nonequilibrium steady states. With the basic assumption of the absence of macroscopic currents and standard mode coupling approximation, we can obtain expressions for the irreducible memory function and other relevant dynamic terms, wherein the nonequilibrium character of the active system is manifested through an averaged diffusion coefficient D[combining macron] and a nontrivial structural function S 2 (q) with q being the magnitude of wave vector q. D[combining macron] and S 2 (q) enter the frequency term and the vertex term for the memory function, and thus influence both the short time and the long time dynamics of the system. With these equations obtained, we study the glassy dynamics of this thermal self-propelled particle system by investigating the Debye-Waller factor f q and relaxation time τ α as functions of the persistence time τ p of self-propulsion, the single particle effective temperature T eff as well as the number density ρ. Consequently, we find the critical density ρ c for given τ p shifts to larger values with increasing magnitude of propulsion force or effective temperature, in good accordance with previously reported simulation work. In addition, the theory facilitates us to study the critical effective temperature T for fixed ρ as well as its dependence on τ p . We find that T increases with τ p and in the limit τ p → 0, it approaches the value for a simple passive Brownian system as expected. Our theory also well recovers the results for passive systems and can be

Leaching behaviour of a glassy slag and derived glass-ceramics from arc-plasma vitrification of hospital wastes

OpenAIRE

Romero, Maximina; Hernández, M. S.; Rincón López, Jesús María

2009-01-01

The arc-plasma vitrification of a hospital wastes containing metals and inorganic oxides yields to a leach-resistant glassy or vitreous slag, which can be environmentally safe for landfill disposal or could be transformed in glass-ceramic tiles with physical and mechanical properties similar to those showed by marketable products for building applications. Standard methods have been used for testing the leachability of elements from this new type of tiles. The water resistance was evaluated b...

Permeability and Selectivity of PPO/Graphene Composites as Mixed Matrix Membranes for CO2 Capture and Gas Separation

Directory of Open Access Journals (Sweden)

Riccardo Rea

2018-01-01

Full Text Available We fabricated novel composite (mixed matrix membranes based on a permeable glassy polymer, Poly(2,6-dimethyl-1,4-phenylene oxide (PPO, and variable loadings of few-layer graphene, to test their potential in gas separation and CO2 capture applications. The permeability, selectivity and diffusivity of different gases as a function of graphene loading, from 0.3 to 15 wt %, was measured at 35 and 65 °C. Samples with small loadings of graphene show a higher permeability and He/CO2 selectivity than pure PPO, due to a favorable effect of the nanofillers on the polymer morphology. Higher amounts of graphene lower the permeability of the polymer, due to the prevailing effect of increased tortuosity of the gas molecules in the membrane. Graphene also allows dramatically reducing the increase of permeability with temperature, acting as a “stabilizer” for the polymer matrix. Such effect reduces the temperature-induced loss of size-selectivity for He/N2 and CO2/N2, and enhances the temperature-induced increase of selectivity for He/CO2. The study confirms that, as observed in the case of other graphene-based mixed matrix glassy membranes, the optimal concentration of graphene in the polymer is below 1 wt %. Below such threshold, the morphology of the nanoscopic filler added in solution affects positively the glassy chains packing, enhancing permeability and selectivity, and improving the selectivity of the membrane at increasing temperatures. These results suggest that small additions of graphene to polymers can enhance their permselectivity and stabilize their properties.

Effect of additive gases and injection methods on chemical dry etching of silicon nitride, silicon oxynitride, and silicon oxide layers in F2 remote plasmas

International Nuclear Information System (INIS)

Yun, Y. B.; Park, S. M.; Kim, D. J.; Lee, N.-E.; Kim, K. S.; Bae, G. H.

2007-01-01

The authors investigated the effects of various additive gases and different injection methods on the chemical dry etching of silicon nitride, silicon oxynitride, and silicon oxide layers in F 2 remote plasmas. N 2 and N 2 +O 2 gases in the F 2 /Ar/N 2 and F 2 /Ar/N 2 /O 2 remote plasmas effectively increased the etch rate of the layers. The addition of direct-injected NO gas increased the etch rates most significantly. NO radicals generated by the addition of N 2 and N 2 +O 2 or direct-injected NO molecules contributed to the effective removal of nitrogen and oxygen in the silicon nitride and oxide layers, by forming N 2 O and NO 2 by-products, respectively, and thereby enhancing SiF 4 formation. As a result of the effective removal of the oxygen, nitrogen, and silicon atoms in the layers, the chemical dry etch rates were enhanced significantly. The process regime for the etch rate enhancement of the layers was extended at elevated temperature

Electrochemical Determination of Glycoalkaloids Using a Carbon Nanotubes-Phenylboronic Acid Modified Glassy Carbon Electrode

Directory of Open Access Journals (Sweden)

Huiying Wang

2013-11-01

Full Text Available A versatile strategy for electrochemical determination of glycoalkaloids (GAs was developed by using a carbon nanotubes-phenylboronic acid (CNTs-PBA modified glassy carbon electrode. PBA reacts with α-solanine and α-chaconine to form a cyclic ester, which could be utilized to detect GAs. This method allowed GA detection from 1 μM to 28 μM and the detection limit was 0.3 μM. Affinity interaction of GAs and immobilized PBA caused an essential change of the peak current. The CNT-PBA modified electrodes were sensitive for detection of GAs, and the peak current values were in quite good agreement with those measured by the sensors.

Electrochemical determination of serotonin in urine samples based on metal oxide nanoparticles/MWCNT on modified glassy carbon electrode

Directory of Open Access Journals (Sweden)

Omolola E. Fayemi

2017-04-01

Full Text Available The electrochemical response of serotonin on the modified electrode based on multiwalled-carbon-nanotube (MWCNT doped respectively with nickel, zinc and iron oxide nanoparticles coating on glassy carbon electrode (GCE at physiological pH 7 was determined using cyclic voltammetry (CV and square wave voltammetry (SWV. The modified GCE/MWCNT-metal oxide electrodes exhibited excellent electrocatalytic activity towards the detection of serotonin at large peak current and lower oxidation potentials compared to other electrodes investigated. The dynamic range for the serotonin determination was between 5.98 × 10−3 μM to 62.8 μM with detection limits 118, 129 and 166 nM for GCE/MWCNT-NiO, GCE/MWCNT-ZnO and GCE/MWCNT-Fe3O4 sensors respectively. GCE-MWCNT-NiO was the best electrode in terms of serotonin current response, electrode stability, resistance to fouling and limit of detection towards the analyte. The developed sensors were found to be electrochemically stable, reusable, economically effective due to their extremely low operational cost, and have demonstrated good limit of detection, sensitivity and selectivity towards serotonin determination in urine samples. Keywords: Metal oxides nanoparticles, Multiwalled carbon nanotubes, Glassy carbon electrode, Serotonin, Cyclic voltammetry, Square wave voltammetry

Molecularly imprinted poly(4-amino-5-hydroxy-2,7-naphthalenedisulfonic acid) modified glassy carbon electrode as an electrochemical theophylline sensor.

Science.gov (United States)

Aswini, K K; Vinu Mohan, A M; Biju, V M

2016-08-01

Theophylline is an inexpensive drug employed in asthma and chronic obstructive pulmonary disorder medications and is toxic at higher concentration. The development of a molecularly imprinted polymer based theophylline electrochemical sensor on glassy carbon electrode by the electropolymerization of 4-amino-5-hydroxy-2,7-naphthalenedisulfonic acid is being discussed in this work. The MIP modification enhances the theophylline recognition ability and the electron transfer kinetics of the bare electrode. The parameters, controlling the performance of the imprinted polymer based sensor, like number of electropolymerization cycles, composition of the pre-polymerization mixture, pH and immersion time were investigated and optimized. The interaction energy and the most stable conformation of the template-monomer complex in the pre-polymerization mixture were determined computationally using ab initio calculations based on density functional theory. The amperometric measurements showed that the developed sensor has a method detection limit of 0.32μM for the dynamic range of 0.4 to 17μM, at optimized conditions. The transducer possesses appreciable selectivity in the presence of structurally similar interferents such as theobromine, caffeine and doxofylline. The developed sensor showed remarkable stability and reproducibility and was also successfully employed in theophylline detection from commercially available tablets. Copyright © 2016 Elsevier B.V. All rights reserved.

Glassy carbon electrodes modified with a film of nanodiamond-graphite/chitosan: Application to the highly sensitive electrochemical determination of Azathioprine

International Nuclear Information System (INIS)

Shahrokhian, Saeed; Ghalkhani, Masoumeh

2010-01-01

A novel modified glassy carbon electrode with a film of nanodiamond-graphite/chitosan is constructed and used for the sensitive voltammetric determination of azathioprine (Aza). The surface morphology and thickness of the film modifier are characterized using atomic force microscopy. The electrochemical response characteristics of the electrode toward Aza are investigated by means of cyclic voltammetry. The modified electrode showed an efficient catalytic role for the electrochemical reduction of Aza, leading to a remarkable decrease in reduction overpotential and enhancement of the kinetics of the electrode reaction with a significant increase of peak current. The effects of experimental variables, such as the deposited amount of modifier suspension, the pH of the supporting electrolyte, the accumulation potential and time were investigated. Under optimal conditions, the modified electrode showed a wide linear response to the concentration of Aza in the range of 0.2-100 μM with a detection limit of 65 nM. The prepared modified electrode showed several advantages: simple preparation method, high stability and uniformity in the composite film, high sensitivity, excellent catalytic activity in physiological conditions and good reproducibility. The modified electrode can be successfully applied to the accurate determination of trace amounts of Aza in pharmaceutical and clinical preparations.

Inter-granular glassy phases in the low-CaO-doped HIPed Si{sub 3}N{sub 4} ceramics. A review

Energy Technology Data Exchange (ETDEWEB)

Gu, Hui [State Key Lab of High Performance Ceramics and Superfine Microstructures, Shanghai Inst. of Ceramics, Chinese Academy of Sciences, SH (China); Tanaka, Isao [Dept. of Materials Science and Engineering, Kyoto Univ. (Japan); Cannon, Rowland M. [Materials Science Div., Lawrence Berkeley National Lab., CA (United States); Pan, Xiaoqing [Dept. of Materials Science and Engineering, Michigan Univ., Ann Arbor (United States); Ruehle, Manfred [Max Planck Inst. for Metals Research, Stuttgart (Germany)

2010-01-15

This review outlines the essence of a progressive study on the glassy inter-granular film (IGF) in a model ceramic system, the low-CaO-doped HIPed high-purity Si{sub 3}N{sub 4}. This was initiated from the finding of a systematic variation of equilibrium IGF thickness following the dopant chemistry, manifesting its fundamental important to ceramic processing. By employing analytical transmission electron microscopy to measure the local chemistry in IGF, however, significant discrepancy was found between trends of local IGF chemistry and thickness. A stable IGF composition was revealed in this system, while a bi-level distribution of Ca segregation establishes a correspondence between the IGF structure and the surface crystallography. The detection of similar levels of nitrogen in IGF through the whole series further supports the presence of a rather stable IGF chemistry. After the saturation of dopants in the stable IGF, extra CaO was found to re-distribute in pockets by enrichment at tips, leading to a liquid phase separation with the Ca-rich phase wetting the entrance zone contacting IGF. The perspective for establishing a comprehensive correlation between the inter-granular phases and the bi-modal microstructure induced by faster growth of basal facets is briefly discussed to pave the way for future work. (orig.)

Glassy carbon electrodes modified with a film of nanodiamond-graphite/chitosan: Application to the highly sensitive electrochemical determination of Azathioprine

Energy Technology Data Exchange (ETDEWEB)

Shahrokhian, Saeed, E-mail: shahrokhian@sharif.ed [Department of Chemistry, Sharif University of Technology, Tehran 11155-9516 (Iran, Islamic Republic of); Institute for Nanoscience and Technology, Sharif University of Technology, Tehran (Iran, Islamic Republic of); Ghalkhani, Masoumeh [Department of Chemistry, Sharif University of Technology, Tehran 11155-9516 (Iran, Islamic Republic of)

2010-04-15

A novel modified glassy carbon electrode with a film of nanodiamond-graphite/chitosan is constructed and used for the sensitive voltammetric determination of azathioprine (Aza). The surface morphology and thickness of the film modifier are characterized using atomic force microscopy. The electrochemical response characteristics of the electrode toward Aza are investigated by means of cyclic voltammetry. The modified electrode showed an efficient catalytic role for the electrochemical reduction of Aza, leading to a remarkable decrease in reduction overpotential and enhancement of the kinetics of the electrode reaction with a significant increase of peak current. The effects of experimental variables, such as the deposited amount of modifier suspension, the pH of the supporting electrolyte, the accumulation potential and time were investigated. Under optimal conditions, the modified electrode showed a wide linear response to the concentration of Aza in the range of 0.2-100 muM with a detection limit of 65 nM. The prepared modified electrode showed several advantages: simple preparation method, high stability and uniformity in the composite film, high sensitivity, excellent catalytic activity in physiological conditions and good reproducibility. The modified electrode can be successfully applied to the accurate determination of trace amounts of Aza in pharmaceutical and clinical preparations.

Perspectives of the Si3N4-TiN ceramic composite as a biomaterial and manufacturing of complex-shaped implantable devices by electrical discharge machining (EDM).

Science.gov (United States)

Bucciotti, Francesco; Mazzocchi, Mauro; Bellosi, Alida

2010-01-01

In this work we investigated the suitability of electroconductive silicon nitride/titanium nitride composite for biomedical implantable devices with particular attention on the processing route that allows the net-shaping of complex components by electrical discharge machining (EDM). The composite, constituted mainly of a beta-Si3N4, dispersed TiN grains and a glassy grain boundary phase, exhibited a low density and high hardness, strength and toughness. Bulk, surface characteristics and properties of the Si3N4-TiN composite were analyzed. After the EDM process, the microstructure of the machined surface was examined. The obtained results showed that the Si3N4-TiN ceramic composite together with the EDM manufacturing process might potentially play a key role in implantable load-bearing prosthesis applications.

Treatment of radioactive waste salt by using synthetic silica-based phosphate composite for de-chlorination and solidification

Science.gov (United States)

Cho, In-Hak; Park, Hwan-Seo; Lee, Ki-Rak; Choi, Jung-Hun; Kim, In-Tae; Hur, Jin Mok; Lee, Young-Seak

2017-09-01

In the radioactive waste management, waste salts as metal chloride generated from a pyrochemical process to recover uranium and transuranic elements are one of problematic wastes due to their intrinsic properties such as high volatility and low compatibility with conventional glasses. This study reports a method to stabilize and solidify LiCl waste via de-chlorination using a synthetic composite, U-SAP (SiO2-Al2O3-B2O3-Fe2O3-P2O5) prepared by a sol-gel process. The composite was reacted with alkali metal elements to produce some metal aluminosilicates, aluminophosphates or orthophosphate as a crystalline or amorphous compound. Different from the original SAP (SiO2-Al2O3-P2O5), the reaction product of U-SAP could be successfully fabricated as a monolithic wasteform without a glassy binder at a proper reaction/consolidation condition. From the results of the FE-SEM, FT-IR and MAS-NMR analysis, it could be inferred that the Si-rich phase and P-rich phase as a glassy grains would be distributed in tens of nm scale, where alkali metal elements would be chemically interacted with Si-rich or P-rich region in the virgin U-SAP composite and its products was vitrified into a silicate or phosphate glass after a heat-treatment at 1150 °C. The PCT-A (Product Consistency Test, ASTM-1208) revealed that the mass loss of Cs and Sr in the U-SAP wasteform had a range of 10-3∼10-1 g/m2 and the leach-resistance of the U-SAP wasteform was comparable to other conventional wasteforms. From the U-SAP method, LiCl waste salt was effectively stabilized and solidified with high waste loading and good leach-resistance.

Electrocatalytic Oxidation of Hydroxylamine at a Quinizarine Modified Glassy Carbon Electrode: Application to Differential Pulse Voltammetry Detection of Hydroxylamine

OpenAIRE

MAZLOUMARDAKANI, Mohammad; KARAMI, Payam EBRAHIMI

2014-01-01

The electrocatalytic behavior of hydroxylamine was studied on a glassy carbon electrode modified by electrodeposition of quinizarine, using cyclic voltammetry, chronoamperometry, and rotating disk voltammetry as diagnostic techniques. Cyclic voltammetry showed that the catalytic current of the system depends on the concentration of hydroxylamine. The magnitude of the peak current for quinizarine increased sharply in the presence of hydroxylamine and proportional to hydroxylamine conc...

Importance of thiol-functionalized molecules for the structure and properties of compression-molded glassy wheat gluten bioplastics.

Science.gov (United States)

Jansens, Koen J A; Lagrain, Bert; Brijs, Kristof; Goderis, Bart; Smet, Mario; Delcour, Jan A

2013-11-06

High-temperature compression molding of wheat gluten at low water levels yields a rigid plastic-like material. We performed a systematic study to determine the effect of additives with multiple thiol (SH) groups on gluten network formation during processing and investigate the impact of the resulting gluten network on the mechanical properties of the glassy end product. To this end, a fraction of the hydroxyl groups of different polyols was converted into SH functionalities by esterifying with 3-mercaptopropionic acid (MPA). The monofunctional additive MPA was evaluated as well. During low-temperature mixing SH-containing additives decreased the gluten molecular weight, whereas protein cross-linking occurred during high-temperature compression molding. The extent of both processes depended on the molecular architecture of the additives and their concentration. After molding, the material strength and failure strain increased without affecting the modulus, provided the additive concentration was low. The strength decreased again at too high concentrations for polyols with low SH functionalization. Attributing these effects solely to the interplay of plasticization and the SH-facilitated introduction of cross-links is inadequate, since an improvement in both strength and failure strain was also observed in the presence of high levels of MPA. It is hypothesized that, regardless of the molecular structure of the additive, the presence of SH-containing groups induces conformational changes which contribute to the mechanical properties of glassy gluten materials.

Modification of glassy carbon electrode with poly(hydroxynaphthol blue)/multi-walled carbon nanotubes composite and construction a new voltammetric sensor for the simultaneous determination of hydroquinone, catechol, and resorcinol

Science.gov (United States)

Daneshinejad, Hassan; Arab Chamjangali, Mansour; Goudarzi, Nasser; Hossain Amin, Amir

2018-03-01

A novel voltammetric sensor is developed based on a poly(hydroxynaphthol blue)/multi-walled carbon nanotubes-modified glassy carbon electrode for the simultaneous determination of the dihydroxybenzene isomers hydroquinone (HQ), catechol (CC), and resorcinol (RS). The preparation and basic electrochemical performance of the sensor are investigated in details. The electrochemical behavior of the dihydroxybenzene isomers at the sensor is studied by the cyclic and differential pulse voltammetric techniques. The results obtained show that this new electrochemical sensor exhibits an excellent electro-catalytic activity towards oxidation of the three isomers. The mechanism of this electro-catalytic activity is discussed. Using the optimum parameters, limit of detection obtained 0.24, 0.24, and 0.26 μmol L-1 for HQ, CC, and RS, respectively. The modified electrode is also successfully applied to the simultaneous determination of dihydroxybenzene in water samples.

Laser gas assisted texturing and formation of nitride and oxynitride compounds on alumina surface: Surface response to environmental dust

Science.gov (United States)

Yilbas, B. S.; Ali, H.; Al-Sharafi, A.; Al-Aqeeli, N.

2018-03-01

Laser gas assisted texturing of alumina surface is carried out, and formation of nitride and oxynitride compounds in the surface vicinity is examined. The laser parameters are selected to create the surface topology consisting of micro/nano pillars with minimum defect sites including micro-cracks, voids and large size cavities. Morphological and hydrophobic characteristics of the textured surface are examined using the analytical tools. The characteristics of the environmental dust and its influence on the laser textured surface are studied while mimicking the local humid air ambient. Adhesion of the dry mud on the laser textured surface is assessed through the measurement of the tangential force, which is required to remove the dry mud from the surface. It is found that laser texturing gives rise to micro/nano pillars topology and the formation of AlN and AlON compounds in the surface vicinity. This, in turn, lowers the free energy of the textured surface and enhances the hydrophobicity of the surface. The liquid solution resulted from the dissolution of alkaline and alkaline earth metals of the dust particles in water condensate forms locally scattered liquid islands at the interface of mud and textured surface. The dried liquid solution at the interface increases the dry mud adhesion on the textured surface. Some dry mud residues remain on the textured surface after the dry mud is removed by a pressurized desalinated water jet.

Glassy behavior of the Nd sublattice induced by Fe doping in NdFexGa1-xO3

International Nuclear Information System (INIS)

Bartolome, F.; Parra-Borderias, M.; Blasco, J.; Bartolome, J.

2007-01-01

The evolution of the magnetic ordering of Nd with the Fe content in NdFe x Ga 1-x O 3 is studied by low-temperature specific-heat measurements for x= =0.2. Fe doping creates a distribution of internal fields on Nd, originating a Schottky contribution to the specific heat which is present for x>0. The power law followed by the low-temperature specific heat suggests a glassy behavior for x>=0.1

Amperometric sensing of anti-HIV drug zidovudine on Ag nanofilm-multiwalled carbon nanotubes modified glassy carbon electrode

Energy Technology Data Exchange (ETDEWEB)

Rafati, Amir Abbas, E-mail: aa_rafati@basu.ac.ir; Afraz, Ahmadreza

2014-06-01

The zidovudine (ZDV) is the first drug approved for the treatment of HIV virus infection. The detection and determination of this drug are very importance in human serum because of its undesirable effects. A new ZDV sensor was fabricated on the basis of nanocomposite of silver nanofilm (Ag-NF) and multiwalled carbon nanotubes (MWCNTs) immobilized on glassy carbon electrode (GCE). The modified electrodes were characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), cyclic voltammetry (CV), and linear sweep voltammetry (LSV) techniques. Results showed that the electrodeposited silver has a nanofilm structure and further electrochemical studies showed that the prepared nanocomposite has high electrocatalytic activity and is appropriate for using in sensors. The amperometric technique under optimal conditions is used for the determination of ZDV ranging from 0.1 to 400 ppm (0.37 μM–1.5 mM) with a low detection limit of 0.04 ppm (0.15 μM) (S/N = 3) and good sensitivity. The prepared sensor possessed accurate and rapid response to ZDV and shows an average recovery of 98.6% in real samples. - Highlights: • New anti-HIV drug sensor was fabricated on the basis of nanomaterials composite. • The GCE modified by prepared hydrophilic MWCNT silver nanoparticles. • Silver nanofilm electrodeposited on MWCNT/GCE and characterized by SEM, EDX, CV and LSV • Response of electrode to ZDV was thoroughly investigated by electrochemical techniques.

Understanding the processes involved in weathering and experimental alteration of glassy materials. The case of some volcanic glasses from eastern Sicily (Italy)

International Nuclear Information System (INIS)

Liotta, Angelo

2014-01-01

The objective of this thesis is to study the effects of weathering and experimental alteration in order to understand the geochemical processes involved and the variation of mineral phases in altered natural glasses. For the first time, five samples of natural volcanic glasses having different composition were collected in eastern Sicily (Italy) in order to be artificially altered and analyzed. The study of naturally altered samples has allowed to observe the effects of weathering after a period of time corresponding to the age of the sample. Moreover, the use of samples of natural glass of volcanic origin has allowed to obtain some powder or thin plates of fresh silicate glass that have been subjected to artificial alteration in the laboratory, in order to model the geochemical processes that have occurred. Alteration experiments were conducted in pure water at 90 C; samples have been altered from 1 to 1000 days of experiment. The characterization of the samples was obtained by Raman spectroscopy, which showed the effects of the devitrification and the presence of some secondary minerals such as carbonates and anatase on the obsidian thin plates, but also phillipsite and chabazite, two varieties of zeolite usually found in the cavities of oldest basalts. Solid modifications were observed by SEM. The analysis showed the formation of several secondary minerals having a composition compatible with smectites, determined by EDS spectroscopy. All these results allow to test the geochemical modeling in the long term. Further analysis will be needed to reach a full understanding of the weathering of glassy materials. (author)

3Y-TZP/Si2N2O composite obtained by pressureless sintering

International Nuclear Information System (INIS)

Santos, Carlos Augusto Xavier

2006-01-01

Zirconia 3YTZP presents excellent properties at room temperature. These properties decrease as the temperature increases because high temperature acts negatively over the stress induced transformation toughening in the matrix. The addition of Si 3 N 4 and SiC in a Y-TZP matrix is very interesting because leads to formation of silicon oxynitride and it increases the mechanical properties like toughness and hardness. Certainly the mechanical properties increment is limited by several difficulties which have appeared during processing and heating of these materials. This paper studies the Y-TZP/Si 2 N 2 0 pressureless sintered composite, under different temperatures, showing the behavior of 20 vol %Si 3 N 4 -SiC when added in YTZP matrix and heated under no pressure system. Al 2 O 3 and Y 2 O 3 were used as sintering aids. The mixture was milled and molded by cold isostatic pressure. Samples were heated at 1500 deg, 1600 deg and 17000 deg C x 2h without pressure under atmospheric conditions using Si 3 N 4 bed-powder. Samples were characterized by XRD and density, hardness, toughness, bending strength were measured. The structure of the material was observed in SEMITEM/EPMA to verify the distribution and composition of the materials in the composite and the contact between filler surface and the matrix. The formation of SiON 2 was observed in the sintered material due to reaction between both nitride and carbide with Y - TZP matrix. Furthermore the material showed an increment of both hardness and toughness as temperature increases. The samples presented considerable resistance to oxidation below 1000 deg C. (author)

Pressure-induced positive electrical resistivity coefficient in Ni-Nb-Zr-H glassy alloy

Science.gov (United States)

Fukuhara, M.; Gangli, C.; Matsubayashi, K.; Uwatoko, Y.

2012-06-01

Measurements under hydrostatic pressure of the electrical resistivity of (Ni0.36Nb0.24Zr0.40)100-xHx (x = 9.8, 11.5, and 14) glassy alloys have been made in the range of 0-8 GPa and 0.5-300 K. The resistivity of the (Ni0.36Nb0.24Zr0.40)86H14 alloy changed its sign from negative to positive under application of 2-8 GPa in the temperature range of 300-22 K, coming from electron-phonon interaction in the cluster structure under pressure, accompanied by deformation of the clusters. In temperature region below 22 K, the resistivity showed negative thermal coefficient resistance by Debye-Waller factor contribution, and superconductivity was observed at 1.5 K.

Poly(amidosulfonic acid) modified glassy carbon electrode for determination of isoniazid in pharmaceuticals.

Science.gov (United States)

Yang, Gongjun; Wang, Cunxiao; Zhang, Rui; Wang, Chenying; Qu, Qishu; Hu, Xiaoya

2008-06-01

Amidosulfonic acid was electropolymerized by cyclic voltammetry onto the surface of glassy carbon electrode (GCE) to fabricate the chemically modified electrode, which showed high stability, good selectivity and reproducibility for determination of isoniazid. The modified electrode showed an excellent electrocatalytical effect on the oxidation of isoniazid. Under the optimum conditions, there was a good linear relationship between anodic peak current and isoniazid concentration in the range of 5.0 x 10(-8)- 1.0 x 10(-5) M, and a detection limit of 1.0 x 10(-8) M (S/N = 3) was obtained after 120 s at the accumulation potential of - 0.2 V (vs. SCE). This developed method had been applied to the direct determination of isoniazid in injection and tablet samples with satisfactory results.

Platinum nanoparticles decorated dendrite-like gold nanostructure on glassy carbon electrodes for enhancing electrocatalysis performance to glucose oxidation

Energy Technology Data Exchange (ETDEWEB)

Jia, Hongmei [Hubei Collaborative Innovation Center for Advanced Organic Chemical Materials, Ministry-of-Education Key Laboratory for the Green Preparation and Application of Functional Materials, School of Materials Science and Engineering, Hubei University, No. 368 Youyi Avenue, Wuchang, Wuhan 430062 (China); Chang, Gang, E-mail: changgang@hubu.edu.cn [Hubei Collaborative Innovation Center for Advanced Organic Chemical Materials, Ministry-of-Education Key Laboratory for the Green Preparation and Application of Functional Materials, School of Materials Science and Engineering, Hubei University, No. 368 Youyi Avenue, Wuchang, Wuhan 430062 (China); Lei, Ming [State Key Laboratory of Information Photonics and Optical Communications, Beijing University of Posts and Telecommunications, Beijing 100876 (China); He, Hanping [College of Chemistry and Chemical Engineer, Hubei University, Youyi Road 368, Wuchang, Wuhan, Hubei 430062 (China); Liu, Xiong; Shu, Honghui; Xia, Tiantian; Su, Jie [Hubei Collaborative Innovation Center for Advanced Organic Chemical Materials, Ministry-of-Education Key Laboratory for the Green Preparation and Application of Functional Materials, School of Materials Science and Engineering, Hubei University, No. 368 Youyi Avenue, Wuchang, Wuhan 430062 (China); He, Yunbin, E-mail: ybhe@hubu.edu.cn [Hubei Collaborative Innovation Center for Advanced Organic Chemical Materials, Ministry-of-Education Key Laboratory for the Green Preparation and Application of Functional Materials, School of Materials Science and Engineering, Hubei University, No. 368 Youyi Avenue, Wuchang, Wuhan 430062 (China)

2016-10-30

Highlights: • Pt/DGNs/GC composites were obtained via a clean and facile method without any templates, surfactants, or stabilizers. • Controlling chemical reduction deposition time, the amount of platinum nanoparticles on Au surface could be regulated, which further tuned electrocatalytic properties toward glucose oxidation. • The obtained Pt/DGNs/GC composites with high electrochemical active surface area (ECSA) show superior electrocatalytic activity to glucose. • The sensor based on Pt/DGNs/GC exhibited excellent sensitivity, selectivity and stability for nonenzymatic glucose detection. - Abstract: Platinum nanoparticles decorated dendrite-like gold nanostructure, bimetal composite materials on glassy carbon electrode (Pt/DGNs/GC) for enhancing electrocatalysis to glucose oxidation was designed and successfully fabricated by a facile two-step deposition method without any templates, surfactants, or stabilizers. Dendrite-like gold nanostructure was firstly deposited on the GC electrode via the potentiostatic method, and then platinum nanoparticles were decorated on the surface of gold substrate through chemical reduction deposition. X-ray diffraction (XRD), field-emission scanning electron microscope (FE-SEM), energy-dispersive X-ray spectroscopy (EDS) were applied to characterize the evolution of morphology and structure of the as-prepared Pt/DGNs/GC. Based on electrochemical measurements such as cyclic voltammetry, linear voltammetry and chronoamperometry, Pt/DGNs/GC exhibited significantly enhanced electrocatalytic performance to glucose oxidation compared those of pure dendrite-like Au nanoparticles in our previous report. Controlling chemical reduction deposition time, the amount of platinum nanoparticles on Au surface could be regulated, which further tuned electrocatalytic properties toward glucose oxidation. The dendrite-like gold surface partially covered by platinum nanoparticles dramatically enhanced the electrocatalytic performance for the

Rotating speed effect on electronic transport behaviors of Ni–Nb–Zr–H glassy alloys

International Nuclear Information System (INIS)

Fukuhara, Mikio

2012-01-01

Highlights: ► The electronic transport behaviors of (Ni 0.39 Nb 0.25 Zr 0.35 ) 100−y H y (0 ≤ y ≤ 15) glassy alloys, which produced by rotating (or quenching) speeds of 3000 and 10,000 rpm, have been studied as a function of hydrogen content. ► The resistivity for (Ni 0.39 Nb 0.25 Zr 0.35 ) 97.8 H 2.2 alloy, produced by rotating speed of 10,000 rpm, displayed 0.1 nΩ cm, which is 0.01% of silver (1.62 μΩ cm) at room temperature, between 40 and 252 K. ► Supercooling of the molten alloy induces a superior ballistic conductor and a room-temperature Coulomb oscillation. - Abstract: The electronic transport behaviors of (Ni 0.39 Nb 0.25 Zr 0.35 ) 100−y H y (0 ≤ y ≤ 15) glassy alloys, produced by rotating (or quenching) speeds of 3000 and 10,000 rpm, have been studied as a function of hydrogen content. These alloys show semiconducting, superior ballistic transport, superconducting and electric current-induced Coulomb oscillation, as hydrogen content increases. The resistivity for (Ni 0.39 Nb 0.25 Zr 0.35 ) 97.8 H 2.2 alloy, produced by rotating speed of 10,000 rpm, displayed 0.1 nΩ cm, which is 0.01% of silver (1.62 μΩ cm) at room temperature, between 40 and 252 K. The Coulomb oscillation of the 10,000 rpm-(Ni 0.39 Nb 0.25 Zr 0.35 ) 95.2 H 4.8 alloy is about 4-fold larger than that of the 3000 rpm-(Ni 0.39 Nb 0.25 Zr 0.35 ) 91.1 H 8.9 alloy. Supercooling of the molten alloy induces a superior ballistic conductor and a room-temperature Coulomb oscillation at lower and higher hydrogen contents, respectively.

Dissociative electron attachment to methylhalides in 3-methylhexane glassy matrix

International Nuclear Information System (INIS)

Harada, K.; Irie, M.; Yoshida, H.

1976-01-01

Dissociative electron attachment reaction to CH 3 I, CH 3 Cl and CH 3 F in a 3-methylhexane glassy matrix was studied by determining the yield of trapped electrons and that of methyl radicals immediately after γ irradiation at 77 K as a function of the scavenger concentration. The efficiency of conversion from the trapped electrons to the methyl radicals was also studied by photobleaching the trapped electrons. The results obtained are (1) the dissociative electron attachment occurs to CH 3 F, for which the gas phase data indicate that the reaction is endothermic by 1.2 eV, during either the γ irradiation or the photobleaching, and (2) CH 3 F is relatively less efficient in scavenging photo-liberated electrons than in scavenging the electrons during the γ irradiation, whereas CH 3 I and CH 3 Cl are efficient scavengers for both the electrons. The dependence of the yields of the trapped electrons and the methyl radicals is discussed in terms of the electron-tunnelling mechanism and the epithermal electron-scavenging mechanism. (author)

Fabrication of calix[4]pyrrole nanofilms at the glassy carbon surface and their characterization by spectroscopic, optic and electrochemical methods

Energy Technology Data Exchange (ETDEWEB)

Taner, Bilge; Ozcan, Emine [Selcuk University, Faculty of Science, Dept. of Chemistry, Konya (Turkey); Ustuendag, Zafer [Dumlupinar University, Faculty of Arts and Sciences, Dept. of Chemistry, Kuetahya (Turkey); Keskin, Selda [Middle East Technical University, Central Research Laboratory, Ankara (Turkey); Solak, Ali Osman, E-mail: osolak@science.ankara.edu.t [Ankara University, Faculty of Science, Department of Chemistry, Ankara (Turkey); Eksi, Haslet [Ankara University, Faculty of Science, Department of Chemistry, Ankara (Turkey)

2010-10-29

meso-Octamethylcalix[4]pyrrole (CP) and meso-heptaethylcalix[4]pyrrole-meso-4-aminophenyl (4APCP) modified glassy carbon (GC) electrodes were prepared by the electrochemical oxidation in acetonitrile solution. Binding of the calix[4]pyrroles with the glassy carbon surface was investigated that it is through the etheric linkage revealed from the reflection-absorption infrared spectroscopy (RAIRS). Surface films of CP and 4APCP were investigated by cyclic voltammetry (CV), ellipsometry, X-ray photoelectron spectroscopy, RAIRS and the contact angle measurements. The thicknesses of the films were determined by ellipsometry which confirmed that the film was multilayer and homogeneous over the surface. Ellipsometric measurements also provided that the CP and 4APCP film thicknesses were 2.49 nm and 4.58 nm for 6 CV cycle modification, corresponding to 66 {mu}F/cm{sup 2} and 106 {mu}F/cm{sup 2} capacitances obtained by CV. The wetting behavior was examined by contact angle measurements and found that the hydrophobicity of the GC-4APCP surface was higher than that of GC-CP, probably due to the aromatic meso substituent present in the former.

Gold nanoparticles embedded electropolymerized thin film of pyrimidine derivative on glassy carbon electrode for highly sensitive detection of l-cysteine.

Science.gov (United States)

Kannan, Ayyadurai; Sevvel, Ranganathan

2017-09-01

This paper demonstrates the fabrication of novel gold nanoparticles incorporated poly (4-amino-6-hydroxy-2-mercaptopyrimidine) (Nano-Au/Poly-AHMP) film modified glassy carbon electrode and it is employed for highly sensitive detection of l-cysteine (CYS). The modified electrode was characterized by scanning electron microscope (SEM), cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). SEM images of modified electrode revealed the homogeneous distribution of gold nanoparticles on poly (4-amino-6-hydroxy-2-mercaptopyrimidine) thin film modified glassy carbon electrode. The modified electrode was successfully utilized for highly selective and sensitive determination of l-cysteine at physiological pH7.0. The present electrochemical sensor successfully resolved the voltammetric signals of ascorbic acid (AA) and l-cysteine with peak separation of 0.510V. To the best of our knowledge, this is the first report of larger peak separation between AA and CYS. Wide linear concentration ranges (2μM-500μM), low detection limit (0.020μM), an excellent reproducibility and stability are achieved for cysteine sensing with this Nano-Au/Poly-AHMP/GCE. Copyright © 2017 Elsevier B.V. All rights reserved.

Análise da expansão por umidade e absorção de água de pisos cerâmicos comerciais em relação à composição química e à quantidade estimada de fase vítrea Analysis of moisture expansion and water absorption of commercial ceramic tiles in relation with chemical composition and estimated glassy phase content

Directory of Open Access Journals (Sweden)

R. R. Menezes

2003-04-01

Full Text Available Expansão por umidade (EPU é o aumento das dimensões do corpo cerâmico devido à adsorção de água, podendo ter grande influência na vida útil dos materiais cerâmicos. Este trabalho tem por objetivo relacionar a EPU e a absorção de água de pisos cerâmicos comerciais, com a sua composição química e a quantidade estimada de fase vítrea, calculada utilizando-se o diagrama de equilíbrio de fases do sistema SiO2.Al2O3.K2 O e a regra da alavanca. Foram estudadas amostras de vinte e três tipos de pisos cerâmicos comerciais. Foi realizada a análise química das amostras (via úmida e determinada a sua EPU e absorção de água (ensaios realizados de acordo com a norma Brasileira NBR 13818. Foi também determinada a área superficial específica de algumas amostras por adsorção de nitrogênio (BET. Os resultados obtidos mostram genericamente uma proporcionalidade inversa entre a EPU e a absorção de água, para a maioria das amostras, e a análise utilizando o diagrama de fases sugere uma relação decrescente entre a absorção de água e a quantidade estimada de fase vítrea, e uma relação crescente entre a EPU e a quantidade estimada de fase vítrea.Moisture expansion is the size increase of the ceramic body due to water adsorption and can have a great influence in the ceramic material service life. This work aims to relate the moisture expansion and water absorption of commercial ceramic tiles with their chemical composition and estimated glassy phase content, calculated from the phase equilibrium diagram of the system SiO2.Al2O3.K2 O using the lever rule. Samples of twenty three commercial ceramic tiles were studied. The chemical composition of the samples was obtained (wet route and their moisture expansion and water absorption were determined (according to the Brazilian standard NBR 13818. The specific surface area of some samples was also determined, using the nitrogen adsorption methodology (BET. The results obtained

Poly(alizarin red)/Graphene modified glassy carbon electrode for simultaneous determination of purine and pyrimidine

International Nuclear Information System (INIS)

Ba Xi; Luo Liqiang; Ding Yaping; Zhang Zhen; Chu Yuliang; Wang Bijun; Ouyang Xiaoqian

2012-01-01

Graphical abstract: DPVs of PAR/Graphene/GCE (a) and the bare GCE (c) in 0.1 M PBS containing 50.0 μM G, 50.0 μM A, 100.0 μM T and 100.0 μM C, (b) PAR/Graphene/GCE in 0.1 M PBS. Highlights: ► The sensor exhibited well-separated peaks and low detection limit. ► The sensor possesses high sensitivity and wide linear range. ► The sensor was used for simultaneous detection of G, A, T and C successfully. ► The sensor was applied in a fish sperm DNA sample with satisfactory results. ► The proposed sensor has good stability and reproducibility. - Abstract: In this work, a poly(alizarin red)/Graphene composite film modified glassy carbon electrode (PAR/Graphene/GCE) was prepared for simultaneous determination of four DNA bases (guanine, adenine, thymine and cytosine) without any pretreatment. The morphology and interface property of PAR/Graphene films were examined by scanning electron microscopy and electrochemical impedance spectroscopy. The PAR/Graphene/GCE exhibited excellent electrocatalytic activity toward purine (guanine and adenine) and pyrimidine (thymine and cytosine) in 0.1 M phosphate buffer solution (pH 7.4). Under optimum conditions, differential pulse voltammetry was used to detect the oxidation of purine and pyrimidine. The results showed that PAR/Graphene/GCE exhibited well-separated peaks, low detection limit, high sensitivity and wide linear range for simultaneous detection of purine and pyrimidine. The proposed sensor also has good stability and reproducibility. Furthermore, the modified electrode was applied for the detection of DNA bases in a fish sperm DNA sample with satisfactory results.

Anodic stripping voltammetric determination of traces of Pb(II) and Cd(II) using a glassy carbon electrode modified with bismuth nanoparticles

International Nuclear Information System (INIS)

Yang, Die; Wang, Liang; Chen, Zuliang; Megharaj, Mallavarapu; Naidu, Ravi

2014-01-01

We report on a glassy carbon electrode modified with bismuth nanoparticles (NanoBiE) for the simultaneous determination Pb 2+ and Cd 2+ by anodic stripping voltammetry. Operational parameters such as bismuth nanoparticles labelling amount, deposition potential, deposition time and stripping parameters were optimized with respect to the determination of Pb 2+ and Cd 2+ in 0.1 M acetate buffer solution (pH 4.5). The NanoBiE gives well-defined, reproducible and sharp stripping peaks. The peak current response increases linearly with the metal concentration in a range of 5.0–60.0 μg L −1 , with a detection limit of 0.8 and 0.4 μg L −1 for Pb 2+ and Cd 2+ , respectively. The morphology and composition of the modified electrode before and after voltammetric measurements were analysed by scanning electron microscopy and energy dispersive X-ray analysis. The NanoBiE was successfully applied to analysis of Pb 2+ and Cd 2+ in real water samples and the method was validated by ICP-MS technique, suggesting that the electrode can be considered as an interesting alternative to the bismuth film electrode for possible use in electrochemical studies and electro analysis. (author)

Determination of dopamine using a glassy carbon electrode modified with a graphene and carbon nanotube hybrid decorated with molybdenum disulfide flowers

International Nuclear Information System (INIS)

Mani, Veerappan; Govindasamy, Mani; Chen, Shen-Ming; Karthik, Raj; Huang, Sheng-Tung

2016-01-01

We describe a hybrid material that consists of molybdenum sulfide flowers placed on graphene nanosheets and multiwalled carbon nanotubes (GNS-CNTs/MoS_2). It was deposited on a glassy carbon electrode (GCE) which then is well suited for sensitive and selective determination of dopamine. The GNS-CNTs/MoS_2 nanocomposite was prepared by a hydrothermal method and characterized by scanning electron and transmission emission microscopies, energy-dispersive X-ray spectroscopy, cyclic voltammetry, differential pulse voltammetry and electrochemical impedance spectroscopy. Electrochemical studies show the composite to possess excellent electrochemical properties such as a large electrochemically active surface, high capacitance current, a wide potential window, high conductivity and large porosity. The electrode displays excellent electrocatalytic ability to oxidize dopamine. The modified GCE, best operated at a working potential as low as 0.15 V (vs. Ag/AgCl), responds linearly to dopamine in the 100 nM to 100 μM concentration range. The detection limit is 50 nM, and the sensitivity is 10.81 (± 0.26) μA⋅μM"−"1⋅cm"−"2. The sensor has good selectivity, appreciable stability, repeatability and reproducibility. It was applied to the determination of dopamine in (spiked) biological and pharmaceutical samples. (author)

High temperature oxidation resistance of magnetron-sputtered homogeneous CrAlON coatings on 430 steel

Energy Technology Data Exchange (ETDEWEB)

Garratt, E; Wickey, K J; Nandasiri, M I; Moore, A; AlFaify, S; Gao, X [Department of Physics, Western Michigan University, Kalamazoo, MI 49008 (United States); Smith, R J; Buchanan, T L; Priyantha, W; Kopczyk, M; Gannon, P E [Montana State University, Bozeman, MT, 59717 (United States); Kayani, A, E-mail: asghar.kayani@wmich.ed

2009-11-01

The requirements of low cost and high-temperature corrosion resistance for bipolar interconnect plates in solid oxide fuel cell stacks has directed attention to the use of metal plates with oxidation resistant coatings. We have investigated the performance of steel plates with homogenous coatings of CrAlON (oxynitrides). The coatings were deposited using RF magnetron sputtering, with Ar as a sputtering gas. Oxygen in these coatings was not intentionally added. Oxygen might have come through contaminated nitrogen gas bottle, leak in the chamber or from the partial pressure of water vapors. Nitrogen was added during the growth process to get oxynitride coating. The Cr/Al composition ratio in the coatings was varied in a combinatorial approach. The coatings were subsequently annealed in air for up to 25 hours at 800 {sup o}C. The composition of the coated plates and the rate of oxidation were characterized using Rutherford backscattering (RBS) and nuclear reaction analysis (NRA). Surface characterization was carried out using Atomic Force Microscopy (AFM) and surfaces of the coatings were found smooth on submicron scale. From our results, we conclude that Al rich coatings are more susceptible to oxidation than Cr rich coatings.

An Easily Fabricated Electrochemical Sensor Based on a Graphene-Modified Glassy Carbon Electrode for Determination of Octopamine and Tyramine

Science.gov (United States)

Zhang, Yang; Zhang, Meiqin; Wei, Qianhui; Gao, Yongjie; Guo, Lijuan; Al-Ghanim, Khalid A.; Mahboob, Shahid; Zhang, Xueji

2016-01-01

A simple electrochemical sensor has been developed for highly sensitive detection of octopamine and tyramine by electrodepositing reduced graphene oxide (ERGO) nanosheets onto the surface of a glassy carbon electrode (GCE). The electrocatalytic oxidation of octopamine and tyramine is individually investigated at the surface of the ERGO modified glassy carbon electrode (ERGO/GCE) by using cyclic voltammetry (CV) and differential pulse voltammetry (DPV). Several essential factors including the deposition cycle of reduced graphene oxide nanosheets and the pH of the running buffer were investigated in order to determine the optimum conditions. Furthermore, the sensor was applied to the quantification of octopamine and tyramine by DPV in the concentration ranges from 0.5 to 40 μM and 0.1 to 25 μM, respectively. In addition, the limits of detection of octopamine and tyramine were calculated to be 0.1 μM and 0.03 μM (S/N = 3), respectively. The sensor showed good reproducibility, selectivity and stability. Finally, the sensor successfully detected octopamine and tyramine in commercially available beer with satisfactory recovery ranges which were 98.5%–104.7% and 102.2%–103.1%, respectively. These results indicate the ERGO/GCE based sensor is suitable for the detection of octopamine and tyramine. PMID:27089341

Molecular dynamics study of dynamic and structural properties of supercooled liquid and glassy iron in the rapid-cooling processes

Energy Technology Data Exchange (ETDEWEB)

Cao, Qi-Long; Huang, Duo-Hui; Yang, Jun-Sheng; Wan, Min-Jie; Wang, Fan-Hou, E-mail: eatonch@gmail.com

2014-10-01

Molecular dynamics simulations were applied to study the dynamic and structural properties of supercooled liquid and glassy iron in the rapid-cooling processes. The mean-square displacement and the non-Gaussian parameter were used to describe the dynamic properties. The evolution of structural properties was investigated using the pair distribution functions and bond-angle distribution functions. Results for dynamic and structural relaxations indicate that the dynamic features are consistently correlated with the structure evolution, and there are three temperature regions as the temperature decreases: (1) at higher temperatures (1500 K, 1300 K, and 1100 K), the system remains in the liquid characteristics during the overall relaxation process. (2) At medial temperatures (1050 K, 900 K, and 700 K), a fast β-relaxation is followed by a much slower α-relaxation. There is a little change in the structural properties in the β-relaxation region, while major configuration rearrangements occurred in the α-relaxation range and the crystallization process was completed at the end of α-relaxation region. (3) At lower temperature (500 K), the system shows glassy characteristics during the overall relaxation process. In addition, the melting temperature, glass transition temperature and diffusion coefficients of supercooled liquid iron are also computed.

Biosensor based on a glassy carbon electrode modified with tyrosinase immobilized on multiwalled carbon nanotubes

International Nuclear Information System (INIS)

Ren, J.; Kang, T.F.; Xue, R.; Ge, C.N.; Cheng, S.Y.

2011-01-01

We describe a biosensor for phenolic compounds that is based on a glassy carbon electrode modified with tyrosinase immobilized on multiwalled carbon nanotubes (MWNTs). The MWNTs possess excellent inherent electrical conductivity which enhances the electron transfer rate and results in good electrochemical catalytic activity towards the reduction of benzoquinone produced by enzymatic reaction. The biosensor was characterized by cyclic voltammetry, and the experimental conditions were optimized. The cathodic current is linearly related to the concentration of the phenols between 0.4 μM and 10 μM, and the detection limit is 0.2 μM. The method was applied to the determination of phenol in water samples (author)

Electric resistivity and thermoelectricity of Ni-Nb-Zr and Ni-Nb-Zr-H glassy alloys

Science.gov (United States)

Fukuhara, Mikio; Inoue, Akihisa

2010-09-01

Electric resistivity ρ and thermoelectric power S of Ni 36Nb 24Zr 40 and (Ni 0.36Nb 0.24Zr 0.4) 90H 10 glassy alloys were investigated in temperature region between 1.5 and 300 K. After resistivity curves of both alloys increase gradually with decreasing temperature down to around 6 K, they dropped suddenly and then reached zero resistivity at 2.1 K, leading to superconductivity. Linear curve with negative TCR of ρ vs T2 and slight increase of S/ T in temperature region down to around 6 K clearly reveal Fermi-liquid phenomenon in electronic state for both alloys independent of hydrogen content.