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Sample records for situ xas study

  1. Design of an electrochemical cell for in situ XAS studies

    Energy Technology Data Exchange (ETDEWEB)

    Watanabe, N. [Instituto de Quimica, Universidade Estadual de Campinas (UNICAMP), Box 6154, CEP 13083-970, Campinas, SP (Brazil); Morais, J. [Instituto de Fisica, Universidade Federal do Rio Grande do Sul (UFRGS), Avenida Bento Goncalves, 9500, Bairro Agronomia, CP 15051, CEP 91501-970, Porto Alegre, RS (Brazil); Alves, M.C.M. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul (UFRGS), Avenida Bento Goncalves, 9500, Bairro Agronomia, CP 15003, CEP 91501-970, Porto Alegre, RS (Brazil)], E-mail: maria@iq.ufrgs.br

    2007-05-15

    In situ X-ray absorption spectroscopy (XAS) studies have been carried out on the electrochemical insertion of Co metal particles in polypyrrole. This has become possible due to the development of an electrochemical cell to allow XAS studies in fluorescence geometry under steady-state conditions. The experimental set-up allows the in situ monitoring of the structural and electronic changes of the selected atom in a matrix. The project of the electrochemical cell is presented with the results obtained at different stages of the electrochemical process. XANES and EXAFS results showed that the initial stage of the cobalt insertion in polypyrrole took place in an ionic form, like [-[(C{sub 4}H{sub 2}N){sub 3}CH{sub 3}(CH{sub 2}){sub 11}OSO{sub 3}{sup -}]{sub 6}Co{sup 2+}] with posterior reduction to a metallic form. The quantitative analysis of the first shell shows that, at -0.60 V, the cobalt atoms are surrounded by 6 ({+-}0.5) atoms located at 2.12 ({+-}0.05) A with a large Debye-Waller factor ({sigma}{sup 2}) value of 0.0368 ({+-}0.0074). At -0.80 V, two distances of R = 1.99 ({+-}0.01) and R = 2.50 ({+-}0.01) A show the coexistence of cobalt in the oxidized and reduced (Co{sup 0}) forms. The Co-Co distance corresponds to that of bulk cobalt. At -1.20 V, the obtained values of N = 12 ({+-}0.5) and R = 2.56 ({+-}0.01) A and a Debye-Waller factor of 0.0176 ({+-}0.0004) suggest the formation of metallic cobalt in a quite disordered form.

  2. A PEM fuel cell for in situ XAS studies

    International Nuclear Information System (INIS)

    Wiltshire, Richard J.K.; King, Colin R.; Rose, Abigail; Wells, Peter P.; Hogarth, Martin P.; Thompsett, David; Russell, Andrea E.

    2005-01-01

    A miniature proton exchange membrane (PEM) fuel cell has been designed to enable in situ XAS investigations of the anode catalyst using fluorescence detection. The development of the cell is described, in particular the modifications required for elevated temperature operation and humidification of the feed gasses. The impact of the operating conditions is observed as an increase in the catalyst utilisation, which is evident in the EXAFS collected at the Pt L III and Ru K edges for a PtRu/C catalyst. The Pt component of the catalyst was found to be readily reduced by hydrogen in the fuel, while the Ru was only fully reduced under conditions of good gas flow and electrochemical contact. Under such conditions no evidence of O neighbours were found at the Ru edge. The results are interpreted in relation to the lack of surface sensitivity of the EXAFS method and indicate that the equilibrium coverage of O species on the Ru surface sites is too low to be observed using EXAFS

  3. Structural and chemical reactivity modifications of a cobalt perovskite induced by Sr-substitution. An in situ XAS study

    International Nuclear Information System (INIS)

    Hueso, Jose L.; Holgado, Juan P.; Pereñíguez, Rosa; Gonzalez-DelaCruz, V.M.; Caballero, Alfonso

    2015-01-01

    LaCoO 3 and La 0.5 Sr 0.5 CoO 3−δ perovskites have been studied by in situ Co K-edge XAS. Although the partial substitution of La(III) by Sr(II) species induces an important increase in the catalytic oxidation activity and modifies the electronic state of the perovskite, no changes could be detected in the oxidation state of cobalt atoms. So, maintaining the electroneutrality of the perovskite requires the generation of oxygen vacancies in the network. The presence of these vacancies explains that the substituted perovskite is now much more reducible than the original LaCoO 3 perovskite. As detected by in situ XAS, after a consecutive reduction and oxidation treatment, the original crystalline structure of the LaCoO 3 perovskite is maintained, although in a more disordered state, which is not the case for the Sr doped perovskite. So, the La 0.5 Sr 0.5 CoO 3−δ perovskite submitted to the same hydrogen reduction treatment produces metallic cobalt, while as determined by in situ XAS spectroscopy the subsequent oxidation treatment yields a Co(III) oxide phase with spinel structure. Surprisingly, no Co(II) species are detected in this new spinel phase. - Highlights: • A Sr-substituted lanthanum cobalt perovskite has been prepared by spray pyrolysis. • It has been established that Co(III) cations are present in both perovskites. • LaCoO 3 is a less reducible phase than the substituted La 0.5 Sr 0.5 CoO 3−δ . • After reoxidation of reduced La 0.5 Sr 0.5 CoO 3−δ , a 100% Co(III) spinel is obtained

  4. A combined in situ XAS-XRPD-Raman study of Fischer-Tropsch synthesis over a carbon supported Co catalyst

    DEFF Research Database (Denmark)

    Tsakoumis, Nikolaos E.; Dehghan, Roya; Johnsen, Rune

    2013-01-01

    A cobalt based Fischer-Tropsch synthesis (FTS) catalyst, supported on a carbon nanofibers/carbon felt composite (Co/CNF/CF) was studied in situ at realistic conditions. The catalyst was monitored by Xray absorption spectroscopy (XAS), high-resolution X-ray powder diffraction (HR-XRPD) and Raman...... spectroscopy, while changes in the gas phase were observed by mass spectrometry (MS). Transmission electron microscopy (TEM) was also applied to characterise the catalyst. The catalyst has a bimodal particle size distribution and exhibits a high deactivation rate. During the in situ study the catalyst appears...... to reduce further at the induction period of FTS, while crystallite growth is been detected in the same period. At steady state FTS the amount of metallic Co is constant. A change in the volumetric flow towards higher conversions did not affect the degree of reduction or the crystallite size of the catalyst...

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

    NARCIS (Netherlands)

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

    2012-01-01

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

  6. In situ, Cr K-edge XAS study on the Phillips catalyst : activation and ethylene polymerization

    NARCIS (Netherlands)

    Groppo, E.; Prestipino, C.; Cesano, F.; Bonino, F.; Bordiga, S.; Lamberti, C.; Thuene, P.C.; Niemantsverdriet, J.W.; Zecchina, A.

    2005-01-01

    In this in situ EXAFS and XANES study on the Phillips ethylene-polymerization Cr/SiO2 catalyst, two polymerization routes are investigated and compared. The first mimics that adopted in industrial plants, where ethylene is dosed directly on the oxidized catalyst, while in the second the oxidized

  7. The Silicon Environment in Silica Polymorphs, Aluminosilicate Crystals and Melts: An In Situ High Temperature XAS Study

    International Nuclear Information System (INIS)

    Cormier, L.; Neuville, D. R.; Roux, J.; Ligny, D. de; Henderson, G. S.; Flank, A.-M.; Lagarde, P.

    2007-01-01

    High temperature X-ray absorption spectroscopy at the Si K-edge has been used to obtain in situ information on SiO2 phase transitions upon heating. Important modifications are observed for the XANES spectra of the high temperature polymorphs, in relation to disordering of the SiO4 tetrahedra beyond the short-range correlations. This paper also presents the XANES spectra of anorthite (CaAl2Si2O8) from room temperature up to the melt (1900 K). This study shows the possibilities for determining the Si environment in crystals and glasses up to the liquid state using in situ XANES measurements

  8. XAS studies on selenite reduction by pyrite

    International Nuclear Information System (INIS)

    Kang Mingliang; Liu Chunli; Chen Fanrong; Charlet, Laurnet

    2012-01-01

    The interaction of aqueous Se (IV) with pyrite were systematically investigated in light of thermodynamic calculations and X-ray Absorption Spectroscopy (XAS). The results from the speciation study reveal that the reduction product is Se (O) when natural pyrite reacts with Se (N) at pH≤5.65, while small amount of FeSeO 3 or iron selenides may be formed at pH 6.1. At pH≥6.94, due to the precipitation of Fe (Ⅲ) -oxyhydroxide, the formation of the thermodynamically most stable species, FeSe 2 , is inhibited. However, when the reactive nanopyrite-greigite was used for reaction, the thermodynamically most stable species, FeSe 2 , was found for the first time as the predominant product in the present study, suggesting that 79 Se can be immobilized in its most insoluble form, FeSe 2 , in Fe (Ⅱ) -sulfide containing environment. This study confirms that pyrite can significantly attenuate the mobility of Se by reductive precipitation, and that the reaction process does not produce protons under acidic or neutral condition when Se (O) is formed. (authors)

  9. In situ XAS study of the Mn(III)(salen)Br catalyzed synthesis of cyclic organic carbonates from epoxides and CO2

    DEFF Research Database (Denmark)

    Jutz, Fabian; Grunwaldt, Jan-Dierk; Baiker, Alfons

    2009-01-01

    In situ X-ray absorption spectroscopy at the Mn K- and Br K-edge was employed to study the cycloaddition of carbon dioxide to propylene oxide and styrene oxide, catalyzed by Mn(III) salen bromide complexes. Three homogeneous complexes with varying salen ligand structure and one complex immobilized...... coordination of the bromine neighbors to the Mn central atom was also evidenced by EXAFS spectra, e.g. loss of Br backscattering in the Mn K-EXAFS spectra and the Mn-backscattering in the Br K-edge spectra. In the catalytic studies it was observed that propylene oxide usually reacted much faster than styrene...

  10. An XAS experimental approach to study low Pt content electrocatalysts operating in PEM fuel cells.

    Science.gov (United States)

    Principi, Emiliano; Witkowska, Agnieszka; Dsoke, Sonia; Marassi, Roberto; Di Cicco, Andrea

    2009-11-21

    We present an X-ray absorption spectroscopy (XAS) study of a low Pt content catalyst layer (Pt loading 0.1 mg cm(-2)) operating at the cathode of a proton exchange membrane fuel cell (PEMFC). This catalyst is based on the use of a mesoporous inorganic matrix as a support for the catalyst Pt nanoparticles. Due to the high Pt dilution, in situ measurements of its structural properties by XAS are challenging and suitable experimental strategies must be devised for this purpose. In particular, we show that accurate XAS in situ fluorescence measurements can be obtained using an optimized fuel cell, suitable protocols for alignment of a focused X-ray beam and an appropriate filter for the background signal of the other atomic species contained in the electrodes. Details, advantages and limitations of the XAS technique for in situ measurements are discussed. Analysis of the near-edge XAS and EXAFS (extended X-ray absorption fine structure) data, corroborated by a HRTEM (high-resolution transmission electron microscopy) study, shows that the Pt particles have a local structure compatible with that of bulk Pt (fcc) and coordination numbers match those expected for particles with typical sizes in the 1.5-2.0 nm range. Substantial changes in the oxidation state and in local atomic arrangement of the Pt particles are found for different applied potentials. The catalyst support, containing W atoms, exhibits a partial reduction upon PEMFC activation, thus mimicking the catalyst behavior. This indicates a possible role of the mesoporous matrix in favouring the oxygen reduction reaction (ORR) and stimulates further research on active catalyst supports.

  11. Growth of block copolymer stabilized metal nanoparticles probed simultaneously by in situ XAS and UV-Vis spectroscopy.

    Science.gov (United States)

    Nayak, C; Bhattacharyya, D; Jha, S N; Sahoo, N K

    2016-01-01

    The growth of Au and Pt nanoparticles from their respective chloride precursors using block copolymer-based reducers has been studied by simultaneous in situ measurement of XAS and UV-Vis spectroscopy at the energy-dispersive EXAFS beamline (BL-08) at INDUS-2 SRS at RRCAT, Indore, India. While the XANES spectra of the precursor give real-time information on the reduction process, the EXAFS spectra reveal the structure of the clusters formed at the intermediate stages of growth. The growth kinetics of both types of nanoparticles are found to be almost similar and are found to follow three stages, though the first stage of nucleation takes place earlier in the case of Au than in the case of Pt nanoparticles due to the difference in the reduction potential of the respective precursors. The first two stages of the growth of Au and Pt nanoparticles as obtained by in situ XAS measurements could be corroborated by simultaneous in situ measurement of UV-Vis spectroscopy also.

  12. NMR and XAS Study of Fe-Mo Double Perovskites

    International Nuclear Information System (INIS)

    Zajac, D.A.; Kapusta, C.; Borowiec, M.; Sikora, M.; Marquina, C.; Blasco, J.; Ibarra, M.R.

    2005-01-01

    The results of NMR and XAS measurements of the A 2 FeMoO 6 double perovskites (DP) (A 2 =Sr 2 , SrBa, Ba 2 , Ca 2 ) at the Fe and Mo K edges are reported and the information on the individual site electronic and magnetic properties is analysed. The compounds studied belong to the family of materials exhibiting a high field '' colossal '' magnetoresistance as well as a low field '' giant '' magnetoresistance. Magnetoresistive properties of the compounds arise from their half-metallicity, i.e. only one spin direction being populated in the conduction band, which consists of overlapping spin down 3d Fe, 2p O and 4d Mo electron bands. Within the model, a spin-down electron undergoes a fast hopping through unoccupied oxygen 2p orbitals between Fe 3+ (3d 5 - spin up) and Mo 6+ (4d 0 ) ionic cores. This mechanism implicates an anti-parallel coupling of the Fe and Mo spins and leads to non-integer magnetic moments and a metallic character below TC. The interaction, in analogy with the '' double exchange '' (DE) in manganites, is called '' double exchange-like '' interaction. The superexchange interaction (SE) is also expected to be present, resulting also in an anti-parallel coupling of 3d Fe 3+ and 4d Mo 5+ spins through occupied oxygen 2p orbitals. The insulating character of SE is connected with an increase of the tilt angle of the Fe-O-Mo bond, which is related to a change of the structural tolerance factor f and results in structural distortions. The molybdenum NMR measurements revealed the existence of a non-integer magnetic moment at Mo and Fe, which can be attributed to the DE-like interaction. However, experiments using Moessbauer spectroscopy have shown the existence of two Fe ionisation states - with integer (SE) and non integer (DE) magnetic moments. The 95 Mo and 97 Mo NMR measurements on A 2 FeMoO 6 (A 2 =Sr 2 , SrBa, Ba 2 , Ca 2 ) presented in this work show different values of the Mo hyperfine field and the corresponding magnetic moment. This is attributed

  13. Real-Time Observation of Platinum Redispersion on Ceria-Based Oxide by In-situ Turbo-XAS in Fluorescence Mode

    International Nuclear Information System (INIS)

    Nagai, Yasutaka; Dohmae, Kazuhiko; Tanabe, Toshitaka; Shinjoh, Hirofumi; Takagi, Nobuyuki; Ikeda, Yasuo; Guilera, Gemma; Pascarelli, Sakura; Newton, Mark; Matsumoto, Shin'ichi

    2007-01-01

    A real-time observation of the redispersion behavior of sintered Pt on ceria-based oxide was made possible by in-situ time-resolved Turbo-XAS in fluorescence mode. 2 wt% Pt/Ce-Zr-Y mixed oxide samples were prepared, and then treated under an aging condition. The average Pt particle size measured by CO absorption method after aging was 7 nm. Redispersion treatments of the previously aged catalyst were carried out at 600 deg. C within an in-situ XAS cell in a cyclical flow of reducing/oxidizing gases. Pt L3-edge XANES spectra were collected every 1.1 second under in-situ conditions. From a change in the XANES spectra, we observed that the Pt particle size of the aged catalyst decreased from 7 to 5 nm after 60 seconds and then to 3 nm after 1000 seconds

  14. XAS study of brownmillerites and Ruddlesden-Popper manganites

    International Nuclear Information System (INIS)

    Szczerba, W.; Oates, C.J.; Sikora, M.; Borowiec, M.; Kapusta, C.; Spalek, L.; Allix, M.; Rosseinsky, M.R.; Ruiz-Bustos, R.; Battle, P.D.

    2005-01-01

    X-Ray Absorption Spectroscopy study of selected compounds of the Ruddlesden-Popper and the browmillerite families is presented. Experiments were carried out at the beamline A1 in HASYLAB/DESY, Hamburg. The n = 1 and n = 2 compounds of the Ruddlesden Popper series, Sr 2 Mn 0.5 Ru 0.5 O 4 and Sr 3 MnRuO 7 as well as oxygen nonstoichiometric and gallium doped brownmillerite compounds, Ca 2.5 Sr 0.5 Ga 1+x Mn 2-x O 8- δ have been studied. Polycrystalline powder samples were measured at room temperature in transmission mode

  15. Local environment of zirconium in nuclear gels studied by XAS

    International Nuclear Information System (INIS)

    Pelegrin, E.; Ildefonse, Ph.; Calas, G.; Ricol, St.; Flank, A.M.

    1997-01-01

    During lixiviation experiments, nuclear gels are formed and heavy metals are retained. In order to understand this retardation mechanisms, we performed an analysis of the local environment of Zr in parent glasses and derived alteration gels both at the Zr-L II,III , and Zr-K edges. Calibration of the method was conducted through the analysis of model compounds with known coordination number (CN): catapleite Na 2 ZrSi 3 O 9 ,2H 2 O (CN=6), baddeleyite ZrO 2 (CN=7) and zircon SiZrO 4 (CN=8). Nuclear glasses (R7T7, and a simplified nuclear glass V 1) and gels obtained at 90 deg C, with leaching times from 7 to 12 months and with solution renewal. were also investigated (GR7T7R and GV1). Zr-L II,III XANES spectra evidenced that zirconium is 6-fold coordinated in R7T7 and V1 nuclear glasses. For GR7T7R and GV1 gels, Zr local environment is significantly changed, and a mixture of CN (6 and 7J has been evidenced. Quantitative structural results were derived from EXAFS analysis at Zr-K edge. In parent glasses, derived Zr-O distance is 2.10±0.01 10 -10 m, and is in the range Zr-O distances for octahedral coordination in model compounds. In both gels studied, Zr-O distances increase significantly up to 2.15 ±0.01 10 -10 m. This distance is close to that known in baddeleyite (2,158 10 -10 m). A better understanding of the Zr retention mechanism has to be made by studying the second neighbors contributions. (authors)

  16. XAS study of TiO2-based nanomaterials

    Science.gov (United States)

    Schneider, K.; Zajac, D.; Sikora, M.; Kapusta, Cz.; Michalow-Mauke, K.; Graule, Th.; Rekas, M.

    2015-07-01

    X-Ray Absorption Spectroscopy studies of the W (0-1 at% W) and Mo-doped TiO2 (0-1 at% Mo) nanoparticle specimens at the K edges of titanium and molybdenum as well as at the L2 L3 edges of tungsten are presented. The materials were prepared with Flame Spray Synthesis process by oxidation of metal-organic precursors. The Ti:K edge spectra in the XANES range show pre-edge and post-edge features characteristic for anatase. A decrease of the amplitude of the EXAFS function with doping is observed and attributed to a softening of the crystal lattice. The Mo EXAFS functions show a considerable decrease of the second-neighbour-shell peak with increasing Mo content, which is attributed to an increased number of cation vacancies. For tungsten a less pronounced effect is observed. The Mo and W XANES spectra do not show noticeable changes with doping level, which indicates their unchanged oxidation states.

  17. Theoretical study on the electronic and optical properties of bulk and surface (001) InxGa1-xAs

    Science.gov (United States)

    Liu, XueFei; Ding, Zhao; Luo, ZiJiang; Zhou, Xun; Wei, JieMin; Wang, Yi; Guo, Xiang; Lang, QiZhi

    2018-05-01

    The optical properties of surface and bulk InxGa1-xAs materials are compared systematically first time in this paper. The band structures, density of states and optical properties including dielectric function, reflectivity, absorption coefficient, loss function and refractive index of bulk and surface InxGa1-xAs materials are investigated by first-principles based on plane-wave pseudo-potentials method within the LDA approximation. The results agree well with the available theoretical and experimental studies and indicate that the electronic and optical properties of bulk and surface InxGa1-xAs materials are much different, and the results show that the considered optical properties of the both materials vary with increasing indium composition in an opposite way. The calculations show that the optical properties of surface In0.75Ga0.25As material are unexpected to be far from the other two indium compositions of surface InxGa1-xAs materials while the optical properties of bulk InxGa1-xAs materials vary with increasing indium composition in an expected regular way.

  18. Electronic state of cerium-based catalysts studied by spectroscopic methods (XPS, XAS)

    International Nuclear Information System (INIS)

    Le Normand, F.; Bernhardt, P.; Hilaire, L.; Kili, K.; Maire, G.; Krill, G.

    1987-01-01

    X-ray Photoelectron Spectroscopy (XPS) of the 3d core level of cerium and X-ray Absorption Spectroscopy (XAS) of the L III absorption edge of cerium have been used to study Pd/CeO 2 , Pd-Ce/γAl 2 O 3 and Ce/γAl 2 O 3 catalysts. The oxidation state of cerium was found to decrease with decreasing amounts of cerium on the surface. It was quite close to III for very low contents of cerium (2-3%). For higher cerium contents the oxidation state was nearer to IV but differences between the two methods were found, owing to the fact that XAS is a volume sensitive probe. The oxidation state of cerium was also lower for Pd-Ce/γAl 2 O 3 than for Ce/γAl 2 O 3 , suggesting the formation of Ce III OCl, chlorine coming from the precursor salt of palladium. 15 refs.; 5 figs.; 1 table

  19. XAS study of V2O5/Al2O3 catalysts doped with rare earth oxides

    International Nuclear Information System (INIS)

    Centeno, M.A.; Malet, P.; Capitan, M.J.; Benitez, J.J.; Carrizosa, I.; Odriozola, J.A.

    1995-01-01

    This paper reports on XAS studies of well dispersed V 2 O 5 /Al 2 O 3 and V 2 O 5 /Sm 2 O 3 /Al 2 O 3 samples. XAS spectra at V-K and Sm-L III edges show that the rare earth oxide favours the formation of regular tetrahedral units, [VO 4 ], over the surface of the support. Positions of the preedge peak at the V-K edge, and intensities of the white line at the Sm-L III edge also suggest modifications in the electronic density around V and Sm atoms when they are simultaneously supported over Al 2 O 3 . ((orig.))

  20. In situ investigation of wet chemical processes for chalcopyrite solar cells by L-edge XAS under ambient conditions

    Energy Technology Data Exchange (ETDEWEB)

    Greil, Stefanie M. [Helmholtz-Zentrum Berlin fuer Materialien und Energie, Albert-Einstein-Strasse 15, 12489 Berlin (Germany); Lauermann, Iver, E-mail: Iver.lauermann@helmholtz-berlin.d [Helmholtz-Zentrum Berlin fuer Materialien und Energie, Albert-Einstein-Strasse 15, 12489 Berlin (Germany); Ennaoui, Ahmed; Kropp, Timo; Lange, Kathrin M.; Weber, Matthieu [Helmholtz-Zentrum Berlin fuer Materialien und Energie, Albert-Einstein-Strasse 15, 12489 Berlin (Germany); Aziz, Emad F., E-mail: Emad.Aziz@helmholtz-berlin.d [Helmholtz-Zentrum Berlin fuer Materialien und Energie, Albert-Einstein-Strasse 15, 12489 Berlin (Germany)

    2010-02-15

    Two instrumental setups for in situ soft X-ray absorption spectroscopy in liquid systems are demonstrated in this work. One for investigating chemical reactions in solutions and a new one for the solid component of a liquid / (as in both / absorber) solid interface. We used these setups for investigating two production processes for chalcopyrite solar cells under ambient conditions, probing the L-edge of Zn and Cu. The first one is a flow cell with a silicon nitride membrane to study the chemical bath deposition process for Cd-free buffer layers. Examining the electronic structure of involved Zn complexes allows to determine the exact reaction mechanism taking place during this process. The second setup is a rotating disk for investigating the bath/absorber interface upon the etching process of superficial binary copper compounds of the absorber as a function of time. The time resolution of the chemical reaction demonstrated in this study ranges from the second to minute time scale.

  1. In situ investigation of wet chemical processes for chalcopyrite solar cells by L-edge XAS under ambient conditions

    International Nuclear Information System (INIS)

    Greil, Stefanie M.; Lauermann, Iver; Ennaoui, Ahmed; Kropp, Timo; Lange, Kathrin M.; Weber, Matthieu; Aziz, Emad F.

    2010-01-01

    Two instrumental setups for in situ soft X-ray absorption spectroscopy in liquid systems are demonstrated in this work. One for investigating chemical reactions in solutions and a new one for the solid component of a liquid / (as in both / absorber) solid interface. We used these setups for investigating two production processes for chalcopyrite solar cells under ambient conditions, probing the L-edge of Zn and Cu. The first one is a flow cell with a silicon nitride membrane to study the chemical bath deposition process for Cd-free buffer layers. Examining the electronic structure of involved Zn complexes allows to determine the exact reaction mechanism taking place during this process. The second setup is a rotating disk for investigating the bath/absorber interface upon the etching process of superficial binary copper compounds of the absorber as a function of time. The time resolution of the chemical reaction demonstrated in this study ranges from the second to minute time scale.

  2. In situ investigation of wet chemical processes for chalcopyrite solar cells by L-edge XAS under ambient conditions

    Science.gov (United States)

    Greil, Stefanie M.; Lauermann, Iver; Ennaoui, Ahmed; Kropp, Timo; Lange, Kathrin M.; Weber, Matthieu; Aziz, Emad F.

    2010-02-01

    Two instrumental setups for in situ soft X-ray absorption spectroscopy in liquid systems are demonstrated in this work. One for investigating chemical reactions in solutions and a new one for the solid component of a liquid / (as in both / absorber) solid interface. We used these setups for investigating two production processes for chalcopyrite solar cells under ambient conditions, probing the L-edge of Zn and Cu. The first one is a flow cell with a silicon nitride membrane to study the chemical bath deposition process for Cd-free buffer layers. Examining the electronic structure of involved Zn complexes allows to determine the exact reaction mechanism taking place during this process. The second setup is a rotating disk for investigating the bath/absorber interface upon the etching process of superficial binary copper compounds of the absorber as a function of time. The time resolution of the chemical reaction demonstrated in this study ranges from the second to minute time scale.

  3. Interaction of selenite with reduced Fe and/or S species: An XRD and XAS study.

    Science.gov (United States)

    Finck, Nicolas; Dardenne, Kathy

    2016-05-01

    In this study, we investigated the interaction between selenite and either Fe((II))aq or S((-II))aq in solution, and the results were used to investigate the interaction between Se((IV))aq and FeS in suspension. The reaction products were characterized by a combination of methods (SEM, XRD and XAS) and the reaction mechanisms were identified. In a first experiment, Se((IV))aq was reduced to Se((0)) by interaction with Fe((II))aq which was oxidized to Fe((III)), but the reaction was only partial. Subsequently, some Fe((III)) produced akaganeite (β-FeOOH) and the release of proton during that reaction decreased the pH. The pH decrease changed the Se speciation in solution which hindered further Se((IV)) reduction by Fe((II))aq. In a second experiment, Se((IV))aq was quantitatively reduced to Se((0)) by S((-II))aq and the reaction was fast. Two sulfide species were needed to reduce one Se((IV)), and the observed pH increase was due to a proton consumption. For both experiments, experimental results are consistent with expectations based on the oxidation reduction potential of the various species. Upon interaction with FeS, Se((IV))aq was reduced to Se((0)) and minute amounts of pyrite were detected, a consequence of partial mackinawite oxidation at surface sulfur sites. These results are of prime importance with respect to safe deep disposal of nuclear waste which contains the long-lived radionuclide (79)Se. This study shows that after release of (79)Se((IV)) upon nuclear waste matrix corrosion, selenite can be reduced in the near field to low soluble Se((0)) by interaction with Fe((II))aq and/or S((-II))aq species. Because the solubility of Se((0)) species is significantly lower than that of Se((IV)), selenium will become much less (bio)available and its migration out of deep HLW repositories may be drastically hindered. Copyright © 2016. Published by Elsevier B.V.

  4. UMo nuclear fuels behaviour under heavy ion irradiation: a μ-XAS study

    International Nuclear Information System (INIS)

    Palancher, H.; Martin, P.; Dubois, S.; Valot, C.; Sabathier, C.; Palancher, H.; Nassif, V.; Proux, O.; Hazemann, J.L.; Wieschalla, N.; Petry, W.; Jarousse, C.

    2007-01-01

    Full text of publication follows. A worldwide program encourages the use of low enriched uranium (LEU, 235 U 235 U concentration up to 93 wt. %). Due to the decrease in 235 U enrichment for the conversion to LEU, the total density of uranium atoms in the fuel must be increased accordingly. To preserve the neutron flux, metallic uranium alloys could be the best fuel material. The fuel, which consists of UMo alloy spherical particles surrounded by an Al matrix (cf. Figure 1-A), is rolled between two aluminium claddings. Post-irradiation examinations of U-7 wt%Mo demonstrated its strong potentialities as fuel but they also pointed out its interaction with aluminium (cf. Figure 1-B). In certain cases this interaction can cause a break-away swelling of the plate. The aim of this project is the understanding of: - the phenomena driving the growth of the interaction layer. - the influence on interaction layer composition of limited adjunction of elements (silicon...) to the Al matrix. To overcome the difficulties inherent to the in-pile irradiated samples, an out-of-pile methodology (collaboration between CEA, FRM II and CERCA) has been developed based on heavy ion irradiation. This methodology enables to simulate the fission fragment damages using a 80 MeV iodine beam at the Maier Leibnitz laboratory (Garching, Germany). After irradiation, samples are characterised at micrometer scale by microscopy (SEM coupled with EDX) and X-Ray techniques (XRD and XAS). The irradiation (final dose: 2 x 10 17 at/cm 2 ) of undoped U-7 wt%Mo fuel plates leads to the formation of an interaction layer surrounding each fuel particles (cf. Figure 1-C). μ-XRD analysis performed at the ESRF (ID18f) showed only the presence of UAl 3 phase in the interaction layer. Same results have been obtained on in-pile irradiated fuel by Sears et al using neutron diffraction confirming the interest of the developed methodology. However the behaviour of the Mo atoms in the interaction layer could not be

  5. XAS Investigations of PEM Fuel Cells

    Science.gov (United States)

    Roth, Christina; Ramaker, David E.

    Polymer-electrolyte membrane (PEM) fuel cells are still far from an area-wide market launch due in part to long-term stability, reliability and cost issues. A more detailed knowledge of the underlying reaction mechanisms is expected to further their application, as it would allow for the design of tailor-made catalysts. However, this will only be possible by complementing traditional in situ studies on single-crystals in electrochemical cells with more sophisticated metal/electrolyte interfacial studies by novel spectroscopic methodologies, which can provide complementary insights into the behaviour of commercial catalysts under real fuel cell operating conditions. This review will focus on the advances of Xray absorption spectroscopy (XAS) in applied fuel cell research utilizing several examples. XAS enables both the nanoparticle morphology and the adsorbate coverage and binding site to be investigated with just one technique. The latter is possible when complementing the conventional extended X-ray absorption fine structure (EXAFS) analysis with the more novel Δμ XANES approach.

  6. Biological X-ray absorption spectroscopy (BioXAS): a valuable tool for the study of trace elements in the life sciences.

    Science.gov (United States)

    Strange, Richard W; Feiters, Martin C

    2008-10-01

    Using X-ray absorption spectroscopy (XAS) the binding modes (type and number of ligands, distances and geometry) and oxidation states of metals and other trace elements in crystalline as well as non-crystalline samples can be revealed. The method may be applied to biological systems as a 'stand-alone' technique, but it is particularly powerful when used alongside other X-ray and spectroscopic techniques and computational approaches. In this review, we highlight how biological XAS is being used in concert with crystallography, spectroscopy and computational chemistry to study metalloproteins in crystals, and report recent applications on relatively rare trace elements utilised by living organisms and metals involved in neurodegenerative diseases.

  7. A solid-state NMR and DFT study of compositional modulations in AlxGa1-xAs

    NARCIS (Netherlands)

    Knijn, Paulus J.; Bentum, P. Jan M. van; Eck, Ernst R.H. van; Fang, Changming; Grimminck, Dennis L.A.G.; Groot, Robert A. de; Havenith, Remco W.A.; Marsman, Martijn; Meerts, W. Leo; Wijs, Gilles A. de; Kentgens, Arno P.M.

    2010-01-01

    We have conducted 75As and 69Ga Nuclear Magnetic Resonance (NMR) experiments to investigate order/disorder in AlxGa1-xAs lift-off films with x ~ 0.297 and 0.489. We were able to identify all possible As(AlnGa4-n) sites with n = 0–4 coordinations in 75As NMR spectra using spin-echo experiments at

  8. A flexible gas flow reaction cell for in situ x-ray absorption spectroscopy studies

    Energy Technology Data Exchange (ETDEWEB)

    Kroner, Anna B., E-mail: anna.kroner@diamond.ac.uk; Gilbert, Martin; Duller, Graham; Cahill, Leo; Leicester, Peter; Woolliscroft, Richard; Shotton, Elizabeth J. [Diamond Light Source Ltd., Diamond House, Harwell Science and Innovation Campus, Chilton, Oxfordshire, OX110DE (United Kingdom); Mohammed, Khaled M. H. [UK Catalysis Hub, Research Complex at Harwell, Rutherford Appleton Laboratory, Chilton, Oxfordshire, OX110FA (United Kingdom); School of Chemistry, University of Southampton, Southampton, SO17 1BJ (United Kingdom)

    2016-07-27

    A capillary-based sample environment with hot air blower and integrated gas system was developed at Diamond to conduct X-ray absorption spectroscopy (XAS) studies of materials under time-resolved, in situ conditions. The use of a hot air blower, operating in the temperature range of 298-1173 K, allows introduction of other techniques e.g. X-ray diffraction (XRD), Raman spectroscopy for combined techniques studies. The flexibility to use either quartz or Kapton capillaries allows users to perform XAS measurement at energies as low as 5600 eV. To demonstrate performance, time-resolved, in situ XAS results of Rh catalysts during the process of activation (Rh K-edge, Ce L{sub 3}-edge and Cr K-edge) and the study of mixed oxide membrane (La{sub 0.6}Sr{sub 0.4}Co{sub 0.2}Fe{sub 0.8}O{sub 3−δ}) under various partial oxygen pressure conditions are described.

  9. Formation of nanostructures in Eu3+ doped glass-ceramics: an XAS study.

    Science.gov (United States)

    Pellicer-Porres, J; Segura, A; Martínez-Criado, G; Rodríguez-Mendoza, U R; Lavín, V

    2013-01-16

    We describe the results of x-ray absorption experiments carried out to deduce structural and chemical information in Eu(3+) doped, transparent, oxyfluoride glass and nanostructured glass-ceramic samples. The spectra were measured at the Pb and Eu-L(III) edges. The Eu environment in the glass samples is observed to be similar to that of EuF(3). Complementary x-ray diffraction experiments show that thermal annealing creates β-PbF(2) type nanocrystals. X-ray absorption indicates that Eu ions act as seeds in the nanocrystal formation. There is evidence of interstitial fluorine atoms around Eu ions as well as Eu dimers. X-ray absorption at the Pb-L(III) edge shows that after the thermal treatment most lead atoms form a PbO amorphous phase and that only 10% of the lead atoms remain available to form β-PbF(2) type nanocrystals. Both x-ray diffraction and absorption point to a high Eu content in the nanocrystals. Our study suggests new approaches to the oxyfluoride glass-ceramic synthesis in order to further improve their properties.

  10. Silver Accumulation in the Green Microalga Coccomyxa actinabiotis: Toxicity, in Situ Speciation, and Localization Investigated Using Synchrotron XAS, XRD, and TEM.

    Science.gov (United States)

    Leonardo, Thomas; Farhi, Emmanuel; Pouget, Stéphanie; Motellier, Sylvie; Boisson, Anne-Marie; Banerjee, Dipanjan; Rébeillé, Fabrice; den Auwer, Christophe; Rivasseau, Corinne

    2016-01-05

    Microalgae are good candidates for toxic metal remediation biotechnologies. This study explores the cellular processes implemented by the green microalga Coccomyxa actinabiotis to take up and cope with silver over the concentration range of 10(-7) to 10(-2) M Ag(+). Understanding these processes enables us to assess the potential of this microalga for applications for bioremediation. Silver in situ speciation and localization were investigated using X-ray absorption spectroscopy, X-ray diffraction, and transmission electron microscopy. Silver toxicity was evaluated by monitoring microalgal growth and photochemical parameters. Different accumulation mechanisms were brought out depending on silver concentration. At low micromolar concentration, microalgae fixed all silver initially present in solution, trapping it inside the cells into the cytosol, mainly as unreduced Ag(I) bound with molecules containing sulfur. Silver was efficiently detoxified. When concentration increased, silver spread throughout the cell and particularly entered the chloroplast, where it damaged the photosystem. Most silver was reduced to Ag(0) and aggregated to form crystalline silver nanoparticles of face-centered cubic structure with a mean size of 10 nm. An additional minor interaction of silver with molecules containing sulfur indicated the concomitant existence of the mechanism observed at low concentration or nanoparticle capping. Nanoparticles were observed in chloroplasts, in mitochondria, on the plasma membrane, on cytosolic membrane structures, and in vacuoles. Above 10(-4) M Ag(+), damages were irreversible, and photosynthesis and growth were definitely inhibited. However, high silver amounts remained confined inside microalgae, showing their potential for the bioremediation of contaminated water.

  11. XAS study of the local environment of impurities in doped TiO{sub 2} thin films

    Energy Technology Data Exchange (ETDEWEB)

    Rodriguez Torres, C.E. [Departamento de Fisica e IFLP (CONICET), Facultad de Ciencias Exactas, Universidad Nacional de La Plata (Argentina)]. E-mail: torres@fisica.unlp.edu.ar; Cabrera, A.F. [Departamento de Fisica e IFLP (CONICET), Facultad de Ciencias Exactas, Universidad Nacional de La Plata (Argentina); Errico, L.A. [Departamento de Fisica e IFLP (CONICET), Facultad de Ciencias Exactas, Universidad Nacional de La Plata (Argentina); Duhalde, S. [Lab. de Ablacion Laser, FI-UBA (Argentina); Renteria, M. [Departamento de Fisica e IFLP (CONICET), Facultad de Ciencias Exactas, Universidad Nacional de La Plata (Argentina); Golmar, F. [Lab. de Ablacion Laser, FI-UBA (Argentina); Sanchez, F.H. [Departamento de Fisica e IFLP (CONICET), Facultad de Ciencias Exactas, Universidad Nacional de La Plata (Argentina)

    2007-09-01

    In this work, we present an X-ray absorption spectroscopy (XAS) characterization of the local environment of the impurity in room temperature ferromagnetic (RTF) anatase TiO{sub 2} thin films doped with Co, Ni, Cu, or Zn, deposited on LaAlO{sub 3} substrate by pulsed laser deposition (PLD). It was found that there is a considerable amount of impurity atoms substituting Ti in TiO{sub 2} anatase, although the presence of metal transition monoxide clusters can not be discarded. From our results, we infer that the observed RT ferromagnetism of the samples could be assigned to the metal transition atoms replacing Ti in TiO{sub 2} anatase.

  12. Electrical conductivity studies in (Ag3AsS3)x(As2S3)1-x superionic glasses and composites

    Science.gov (United States)

    Studenyak, I. P.; Neimet, Yu. Yu.; Kranjčec, M.; Solomon, A. M.; Orliukas, A. F.; Kežionis, A.; Kazakevičius, E.; Šalkus, T.

    2014-01-01

    Compositional, frequency, and temperature studies of impedance and electrical conductivity in (Ag3AsS3)x(As2S3)1-x superionic glasses and composites were performed. Frequency range from 10 Hz to 3 × 109 Hz and temperature interval 300-400 K were used for the measurements. Compositional dependences of electrical conductivity and activation energy are analyzed; the most substantial changes are observed with the transition from (Ag3AsS3)0.4(As2S3)0.6 glass to (Ag3AsS3)0.5(As2S3)0.5 composite. With increase of Ag3AsS3 content, the investigated materials are found to have crystalline inclusions and show the two-phase composite nature. Addition of Ag3AsS3 leads to the increase of electrical conductivity whereas the activation energy decreases.

  13. Genesis of Co/SiO2 catalysts : XAS study at the cobalt L-III,L- II absorption edges

    NARCIS (Netherlands)

    Bazin, D.; Kovacs, I.; Guczi, L.; Parent, P.; Laffon, C.; De Groot, F.; Ducreux, O.; Lynch, J.

    2000-01-01

    Silica-supported cobalt catalysts have been investigated by soft X-ray absorption techniques. Soft X-ray absorption spectra were collected at the Co LII,III edge during in situ reduction of calcined samples in a stream of hydrogen in the temperature range between 300 and 650°C. Using reference

  14. Composition-driven Cu-speciation and reducibility in Cu-CHA zeolite catalysts: a multivariate XAS/FTIR approach to complexity† †Electronic supplementary information (ESI) available: Sample description and synthesis details, experimental setup for in situ XAS and FTIR spectroscopy, details on the MCR-ALS method, details on DFT-assisted XANES simulations, details on the determination of N pure by PCA, MCR-ALS results for downsized and upsized component spaces, additional information to support the assignment of theoretical XANES curves, details on EXAFS analysis, details on IR spectral deconvolution. See DOI: 10.1039/c7sc02266b Click here for additional data file.

    Science.gov (United States)

    Martini, A.; Lomachenko, K. A.; Pankin, I. A.; Negri, C.; Berlier, G.; Beato, P.; Falsig, H.; Bordiga, S.; Lamberti, C.

    2017-01-01

    The small pore Cu-CHA zeolite is attracting increasing attention as a versatile platform to design novel single-site catalysts for deNOx applications and for the direct conversion of methane to methanol. Understanding at the atomic scale how the catalyst composition influences the Cu-species formed during thermal activation is a key step to unveil the relevant composition–activity relationships. Herein, we explore by in situ XAS the impact of Cu-CHA catalyst composition on temperature-dependent Cu-speciation and reducibility. Advanced multivariate analysis of in situ XANES in combination with DFT-assisted simulation of XANES spectra and multi-component EXAFS fits as well as in situ FTIR spectroscopy of adsorbed N2 allow us to obtain unprecedented quantitative structural information on the complex dynamics during the speciation of Cu-sites inside the framework of the CHA zeolite. PMID:29147509

  15. The structure of ZrO2 phases and deviltrification processes in a Ca-Zr-Si-O-based glass ceramic: a combined a-XRD and XAS study

    International Nuclear Information System (INIS)

    Meneghini, C.; Mobilio, S.

    2004-01-01

    The structure of Zr atomic environment in a CaO-ZrO 2 -Si 2 glass ceramic as a function of thermal treatments has been studied, combining X-ray absorption spectroscopy (XAS), X-ray diffraction (XRD) and anomalous XRD (a-XRD) techniques. The analysis of XRD patterns demonstrates that the devitrification process proceeds through the partial segregation of Zr-depleted phases (wollastonite-like) and Zr-rich phases (Zr oxides). The XAS and a-XRD measurements at the Zr K-edge have been exploited in order to obtain a closer insight into the atomic structure around the Zr atoms. In the as-quenched glass the Zr atom is sixfold coordinated to O atoms in an amorphous environment rich in Ca and Si. Thermal treatment firstly (T=1273-1323 K) causes partial segragation of Zr in the form of an oxide with a tetragonal zirconia (t-ZrO 2 ) crystalline structure. Raising the temperature (T=1373 K) causes the formation of ZrO 2 crystallites in the monoclinic crystallographic phase (baddeleyite, m-ZrO 2 ). Analysis of the XAS data shows that a considerable amount of Zr remains in an amorphous calcium silicate phase. (orig.)

  16. Combined XRD and XAS

    International Nuclear Information System (INIS)

    Ehrlich, S.N.; Hanson, J.C.; Lopez Camara, A.; Barrio, L.; Estrella, M.; Zhou, G.; Si, R.; Khalid, S.; Wang, Q.

    2011-01-01

    X-ray diffraction (XRD) and X-ray absorption fine structure (XAFS) are complementary techniques for investigating the structure of materials. XRD probes long range order and XAFS probes short range order. We have combined the two techniques at one synchrotron beamline, X18A at the NSLS, allowing samples to be studied in a single experiment. This beamline will allow for coordinated measurements of local and long range structural changes in chemical transformations and phase transitions using both techniques.

  17. The Reduction of Cr(VI) to Cr(III) by Natural Fe-Bearing Minerals: A Synchrotron XAS Study

    Science.gov (United States)

    Xu, H.; Guo, X.; Ding, M.; Migdissov, A. A.; Boukhalfa, H.; Sun, C.; Roback, R. C.; Reimus, P. W.; Katzman, D.

    2017-12-01

    Cr(VI) in the form of CrO42- is a pollutant species in groundwater and soils that can pose health and environmental problems. Cr(VI) associated with use as a corrosion inhibitor at a power plant from 1956-1972 is present in a deep groundwater aquifer at Los Alamos National Laboratory. A potential remediation strategy for the Cr contamination is reduction of Cr(VI) to Cr(III) via the acceptance of electrons from naturally occurring or induced Fe(II) occurring in Fe-bearing minerals. In this work, using synchrotron-based X-ray techniques, we investigated the Cr reduction behavior by Fe-bearing minerals from outcrop and core samples representative of the contaminated portion of the aquifer. Samples were exposed to solutions with a range of known Cr (VI) concentrations. XANES and EXAFS spectra showed that all the Cr(VI) had been reduced to Cr(III), and micro XRF mapping revealed close correlation of Cr and Fe distribution, implying that Fe(II) in minerals reduced Cr(VI) in the solution. Similar behavior was observed from in-situ XANES measurements on Cr reduction and adsorption by mineral separates from the rock samples in Cr(VI)-bearing solutions. In addition, to obtain reference parameters for interpreting the data of natural samples, we collected Cr and Fe EXAFS spectra of Cr(III)-Fe(III) hydroxide solid solutions, which show progressive changes in the local structure around Cr and Fe over the whole series.

  18. Influence of interstitial solutions (H, N) on cerium electronic state in Ce-Fe intermetallic compounds: X-ray Absorption Spectroscopy (XAS) study

    International Nuclear Information System (INIS)

    Chaboy, J.; Marcelli, A.; Bozukov, L.

    1995-03-01

    It is presented an x-ray absorption spectroscopy (XAS) investigation performed at the L-edges of the rare-earth and at the K-edge of iron in the R-Fe intermetallic compounds (La, Ce) 2 Fe 14 BH χ and Ce 2 Fe 17 (H,N) χ , to elucidate the role of the interstitial doping into the electronic and magnetic properties of these systems. Comparison with x-ray circular magnetic dichroism (XCMD) experiments has been carried out to clarify the localization of 4f magnetic moment at the Ce sites upon hydriding. Both XAS and XCMD results evidence the interplay between the structural and magnetic changes, that are associated to the modification of the hybridization between the Fe(3d) and Ce(5d) bands

  19. The Effect of Electrical Polarization on Electronic Structure in LSM Electrodes: An Operando XAS, RIXS and XES Study

    DEFF Research Database (Denmark)

    Traulsen, Marie Lund; Carvalho, H.W.P.; Zielke, Philipp

    2017-01-01

    in the Mn K edge energy towards lower energies. The shift is assigned to a decrease in the average Mn oxidation state, which based on Kβ XES changes from 3.4 at open circuit voltage to 3.2 at −800 mV applied potential. Furthermore, RIXS rendered pronounced changes in the population of the Mn 3d orbitals...... (RIXS) at the Mn K-edge. The study of polarization induced changes in the electronic properties and structure has been carried out at 500°C in 10–20% O2 with electrical polarization applied in the range from −850 mV to 800 mV. Cathodic polarizations in the range −600 mV to −850 mV induced a shift......, due to filling of the Mn d-orbitals during the cathodic polarization. Overall, the study experimentally links the electrical polarization of LSM electrodes to the structural and electronic properties of Mn - these properties are expected to be of major importance for the electrocatalytic performance...

  20. Comparative study of the hydrostatic pressure and temperature effects on the impurity-related optical properties in single and double GaAs-Ga{sub 1-x}Al{sub x}As quantum wells

    Energy Technology Data Exchange (ETDEWEB)

    Odhiambo Oyoko, H. [Department of Physics, Westville Campus, University of KwaZulu-Natal, Private Bag X 54001, Durban 4000 (South Africa); Porras-Montenegro, N. [Departamento de Fisica, Universidad del Valle, AA 25360, Cali (Colombia); Lopez, S.Y. [Facultad de Educacion, Universidad de Antioquia, AA 1226, Medellin (Colombia); Duque, C.A. [Instituto de Fisica, Universidad de Antioquia, AA 1226, Medellin (Colombia)

    2007-07-01

    Using a variational technique within the effective mass approximation we have carried out a comparative study of the effect of hydrostatic pressure and temperature on the shallow-impurity related optical absorption spectra in GaAs-Ga{sub 1-x}Al{sub x}As single and double quantum wells. The results show a pressure dependent read-shift and a temperature dependent blue-shift in the optical absorption spectra. (copyright 2007 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  1. Solution XAS Analysis for Exploring the Active Species in Homogeneous Vanadium Complex Catalysis

    Science.gov (United States)

    Nomura, Kotohiro; Mitsudome, Takato; Tsutsumi, Ken; Yamazoe, Seiji

    2018-06-01

    Selected examples in V K-edge X-ray Absorption Near Edge Structure (XANES) analysis of a series of vanadium complexes containing imido ligands (possessing metal-nitrogen double bond) in toluene solution have been introduced, and their pre-edge and the edge were affected by their structures and nature of ligands. Selected results in exploring the oxidation states of the active species in ethylene dimerization/polymerization using homogeneous vanadium catalysts [consisting of (imido)vanadium(V) complexes and Al cocatalysts] by X-ray absorption spectroscopy (XAS) analyses have been introduced. It has been demonstrated that the method should provide more clear information concerning the active species in situ, especially by combination with the other methods (NMR and ESR spectra, X-ray crystallographic analysis, and reaction chemistry), and should be powerful tool for study of catalysis mechanism as well as for the structural analysis in solution.

  2. XAS and XMCD investigation of Mn12 monolayers on gold.

    Science.gov (United States)

    Mannini, Matteo; Sainctavit, Philippe; Sessoli, Roberta; Cartier dit Moulin, Christophe; Pineider, Francesco; Arrio, Marie-Anne; Cornia, Andrea; Gatteschi, Dante

    2008-01-01

    The deposition of Mn(12) single molecule magnets on gold surfaces was studied for the first time using combined X-ray absorption spectroscopy (XAS) and X-ray magnetic circular dichroism (XMCD) methods at low temperature. The ability of the proposed approach to probe the electronic structure and magnetism of Mn(12) complexes without significant sample damage was successfully checked on bulk samples. Detailed information on the oxidation state and magnetic polarization of manganese ions in the adsorbates was obtained from XAS and XMCD spectra, respectively. Partial reduction of metal ions to Mn(II) was clearly observed upon deposition on Au(111) of two different Mn(12) derivatives bearing 16-acetylthio-hexadecanoate and 4-(methylthio)benzoate ligands. The average oxidation state, as well as the relative proportions of Mn(II), Mn(III) and Mn(IV) species, are strongly influenced by the deposition protocol. Furthermore, the local magnetic polarizations are significantly decreased as compared with bulk Mn(12) samples. The results highlight an utmost redox instability of Mn(12) complexes at gold surfaces, presumably accompanied by structural rearrangements, which cannot be easily revealed by standard surface analysis based on X-ray photoelectron spectroscopy and scanning tunnelling microscopy.

  3. Synchrotron radiation based analytical techniques (XAS and XRF)

    International Nuclear Information System (INIS)

    Jha, Shambhu Nath

    2014-01-01

    A brief description of the principles of X-ray absorption spectroscopy (XAS) and X-ray fluorescence (XRF) techniques is given in this article with emphasis on the advantages of using synchrotron radiation-based instrumentation/beamline. XAS technique is described in more detail to emphasize the strength of the technique as a local structural probe. (author)

  4. Coherent dynamics of interwell excitons in GaAs/AlxGa1-xAs superlattices

    DEFF Research Database (Denmark)

    Mizeikis, V.; Birkedal, Dan; Langbein, Wolfgang Werner

    1997-01-01

    Coherent exciton dynamics in a GaAs/AlxGa1-xAs narrow-miniband superlattice is studied by spectrally resolved transient four-wave mixing. Coherent optical properties of the investigated structure are found to be strongly affected by the existence of two different heavy-hole excitonic states. One...

  5. In-situ burning: NIST studies

    International Nuclear Information System (INIS)

    Evans, D.D.

    1992-01-01

    In-situ burning of spilled oil has distinct advantages over other countermeasures. It offers the potential to convert rapidly large quantities of oil into its primary combustion products, carbon dioxide and water, with a small percentage of other unburned and residue byproducts. Because the oil is converted to gaseous products of combustion by burning, the need for physical collection, storage, and transport of recovered fluids is reduced to the few percent of the original spill volume that remains as residue after burning. Burning oil spills produces a visible smoke plume containing smoke particulate and other products of combustion which may persist for many kilometers from the burn. This fact gives rise to public health concerns, related to the chemical content of the smoke plume and the downwind deposition of particulate, which need to be answered. In 1985, a joint Minerals Management Service (MMS) and Environment Canada (EC) in-situ burning research program was begun at the National Institute of Standards and Technology (NIST). This research program was designed to study the burning of large crude oil spills on water and how this burning would affect air quality by quantifying the products of combustion and developing methods to predict the downwind smoke particulate deposition. To understand the important features of in-situ burning, it is necessary to perform both laboratory and mesoscale experiments. Finally, actual burns of spilled oil at sea will be necessary to evaluate the method at the anticipated scale of actual response operations. In this research program there is a continuing interaction between findings from measurements on small fire experiments performed in the controlled laboratory environments of NIST and the Fire Research Institute (FRI) in Japan, and large fire experiments at facilities like the USCG Fire Safety and Test Detachment in Mobile, Alabama where outdoor liquid fuel burns in large pans are possible

  6. Na, Mg, Ni and Cs distribution and speciation after long-term alteration of a simulated nuclear waste glass: A micro-XAS/XRF/XRD and wet chemical study

    Science.gov (United States)

    Curti, Enzo; Dähn, Rainer; Farges, François; Vespa, Marika

    2009-04-01

    Microscopic distribution and speciation of Na, Mg, Ni and Cs in a simulated (inactive) nuclear waste glass were studied using micro X-ray fluorescence (μ-XRF) and micro X-ray absorption spectroscopy (μ-XAS), after aqueous leaching during 12 years at 90 °C. Na and Mg are major constituents of the glass that can be used to determine the progress of the glass corrosion process and the nature of secondary alteration phases. Ni and Cs represent dose determining long-lived radionuclides ( 59Ni, 135Cs) in vitrified nuclear waste. The Na-Mg μ-XRF maps revealed that the core regions of the glass fragments are apparently unaltered and compositionally homogeneous, whereas rims and interstitial spaces are enriched with Mg-rich smectite formed during the leaching process. The micro X-ray absorption near edge structure (μ-XANES) spectra collected at the Mg K-edge in the altered zones show three sharp resonances typical for crystalline Mg-silicates. These resonances are distinctive of Mg occupying undistorted octahedral positions. In contrast, the μ-XANES spectra collected in the core zones of the glass fragments lack this resonance pattern and are identical to the spectra measured on the pristine (unleached) MW glass. Micro extended X-ray absorption fine structure (μ-EXAFS) and μ-XANES analyses at the Ni K-edge revealed three distinct Ni(II) species: (a) Ni uniformly distributed in the glass matrix, (b) micro-inclusions with high Ni concentrations and (c) Ni associated to the Mg-clay. The comparison with reference spectra of unleached MW and other Ni-bearing silicate glasses indicated that species (a) represents the original coordinative environment of Ni in the glass. The μ-EXAFS analyses revealed that species (b) is structural Ni in trevorite (NiFe 2O 4), which probably formed through unmixing processes during the cooling of the glass melt. The μ-EXAFS of species (c) could be successfully modeled assuming specific adsorption or incorporation of Ni into the lattice of

  7. High pressure flow reactor for in situ X-ray absorption spectroscopy of catalysts in gas-liquid mixtures—A case study on gas and liquid phase activation of a Co-Mo/Al2O3 hydrodesulfurization catalyst

    NARCIS (Netherlands)

    van Haandel, L.; Hensen, E.J.M.; Weber, Th.

    2017-01-01

    An in situ characterization of heterogeneous catalysts under industrial operating conditions may involve high pressure and reactants in both the gas and the liquid phase. In this paper, we describe an in situ XAS flow reactor, which is suitable to operate under such conditions (pmax 20 bar, Tmax 350

  8. Structure and spectroscopic study of aqueous Fe(III)-As(V) complexes using UV-Vis, XAS and DFT-TDDFT.

    Science.gov (United States)

    Chai, Liyuan; Yang, Jinqin; Zhang, Ning; Wu, Pin-Jiun; Li, Qingzhu; Wang, Qingwei; Liu, Hui; Yi, Haibo

    2017-09-01

    Aqueous complexes between ferric (Fe(III)) and arsenate (As(V)) are indispensable for understanding the mobility of arsenic (As) in Fe(III)-As(V)-rich systems. In this study, aqueous Fe(III)-As(V) complexes, FeH 2 AsO 4 2+ and FeHAsO 4 + , were postulated based on the qualitative analysis of UV-Vis spectra in both Fe(III)-As(V)-HClO 4 and Fe(III)-As(V)-H 2 SO 4 systems. Subsequently, monodentate structures were evidenced by Fe K-edge EXAFS and modeled as [FeH 2 AsO 4 (H 2 O) 5 ] 2+ and [FeHAsO 4 (H 2 O) 5 ] + by DFT. The feature band at ∼280 nm was verified as electron excitation chiefly from Fe-As-bridged O atoms to d-orbital of Fe in [FeH 2 AsO 4 (H 2 O) 5 ] 2+ and [FeHAsO 4 (H 2 O) 5 ] + . The structural and spectral information of Fe(III)-As(V) complexes will enable future speciation analysis in Fe(III)-As(V)-rich system. Copyright © 2017. Published by Elsevier Ltd.

  9. Co-ordination properties of diglycol-amide (DGA) to trivalent curium and lanthanides studied by XAS, XRD and XPS methods

    International Nuclear Information System (INIS)

    Yaita, T.; Hirata, M.; Narita, H.; Tachimori, S.; Yamamoto, H.; Edelstein, N.M.; Bucher, J.J.; Shuh, D.K.; Rao, L.

    2001-01-01

    Co-ordination properties of diglycol-amide (DGA) to trivalent curium and to the trivalent lanthanides were studied by the EXAFS, the XRD and the XPS methods. The structural determinations by both the crystal XRD and the solution EXAFS methods showed that the DGA co-ordinated to the trivalent lanthanide ion in a tridentate fashion: co-ordination of three oxygen atoms of each ligand to the metal ion. The bond distances of Er-O (carbonyl) and Er-O (ether) in the Er-DGA complex were 2.35 Angstrom, and 2.46 Angstrom, respectively, while the atom distances of Cm-O (carbonyl) and Cm-O (ether) in the Cm-DGA complex were 2.42 Angstrom and 3.94 Angstrom, respectively from the EXAFS data for the Cm-DGA complex. Accordingly, the DGA would behave only as a semi-tridentate in the co-ordination to trivalent curium in solution. We determined the valence band structures of the Er-DGA complex by the XPS in order to clarify the bond properties of the complex, and assigned the XPS spectrum by using the DV-DS molecular orbital calculation method. (authors)

  10. XAS Studies of Arsenic in the Environment

    International Nuclear Information System (INIS)

    Charnock, J. M.; Polya, D. A.; Gault, A. G.; Morgan, A. J.

    2007-01-01

    Arsenic is present in low concentrations in much of the Earth's crust and changes in its speciation are vital to understanding its transport and toxicity in the environment. We have used X-ray absorption spectroscopy to investigate the coordination sites of arsenic in a wide variety of samples, including soil and earthworm tissues from arsenic-contaminated land, and human hair and nail samples from people exposed to arsenic in Cambodia. Our results confirm the effectiveness of using X-ray absorption near edge structure (XANES) and X-ray absorption fine structure (EXAFS) spectroscopy to determine speciation changes in environmental samples

  11. X-ray absorption spectroscopy study of the LixFePO4 cathode during cycling using a novel electrochemical in situ reaction cell

    International Nuclear Information System (INIS)

    Deb, A.; Bergmann, U.; Cairns, E.L.; California Univ., Berkeley, CA; Cramer, S.P.; California Univ., Davis, CA

    2004-01-01

    The extraction and insertion of lithium in LiFePO 4 has been investigated in practical Li-ion intercalation electrodes for Li-ion batteries using Fe K-edge X-ray absorption spectroscopy (XAS). A versatile electrochemical in situ reaction cell was utilized, specifically designed for long-term X-ray experiments on battery electrodes during the lithium-extraction/insertion process in electrode materials for Li-ion batteries. The electrode contained about 7.7 mg of LiFePO 4 on a 20 μm-thick Al foil. In order to determine the charge compensation mechanism and structural perturbations occurring in the system during cycling, in situ X-ray absorption fine-structure spectroscopy (XAFS) measurements were conducted on the cell at a moderate rate using typical Li-ion battery operating voltages (3.0-4.1 V versus Li/Li + ).XAS studies of the LiFePO 4 electrode measured at the initial state (LiFePO 4 ) showed iron to be in the Fe(II) state corresponding to the initial state (0.0 mAh) of the battery, whereas in the delithiated state (FePO 4 ) iron was found to be in the FE(III) state corresponding to the final charged state (3 m Ah) of the battery. The X-ray absorption near-edge structure (XANES) region of the XAS spectra revealed a high-spin configuration for the two states [Fe(II), d 6 and Fe(III), d 5 ]. The XAFS data analysis confirmed that the olivine structure of the LeFePO 4 and FePO 4 is retained by the electrodes, which is in agreement with the X-ray diffraction observations on these compounds. The XAFS data that were collected continuously during cycling revealed details about the response of the cathode to Li insertion and extraction. These measurements on the LiFePO 4 cathode show that the material retains good structural short-range order leading to superior cycling

  12. Electronic structures of GaAs/AlxGa1-xAs quantum double rings

    Directory of Open Access Journals (Sweden)

    Li Shu-Shen

    2006-01-01

    Full Text Available AbstractIn the framework of effective mass envelope function theory, the electronic structures of GaAs/AlxGa1-xAs quantum double rings (QDRs are studied. Our model can be used to calculate the electronic structures of quantum wells, wires, dots, and the single ring. In calculations, the effects due to the different effective masses of electrons and holes in GaAs and AlxGa1-xAs and the valence band mixing are considered. The energy levels of electrons and holes are calculated for different shapes of QDRs. The calculated results are useful in designing and fabricating the interrelated photoelectric devices. The single electron states presented here are useful for the study of the electron correlations and the effects of magnetic fields in QDRs.

  13. Comparison between XAS, AWAXS and DAFS applied to nanometer scale supported metallic clusters. Pt.2; bimetallic clusters

    International Nuclear Information System (INIS)

    Bazin, D.; Sayers, D.

    1993-01-01

    The structural information obtained using three techniques related to synchrotron radiation are compared. XAS (X-ray Absorption Spectroscopy), AWAXS (Anomalous Wide Angle X-ray Scattering) and DAFS (Diffraction Anomalous Fine Structure) are applied to the study of nanometer scale bimetallic clusters. (author)

  14. In-situ Multimodal Imaging and Spectroscopy of Mg Electrodeposition at Electrode-Electrolyte Interfaces

    Science.gov (United States)

    Wu, Yimin A.; Yin, Zuwei; Farmand, Maryam; Yu, Young-Sang; Shapiro, David A.; Liao, Hong-Gang; Liang, Wen-I.; Chu, Ying-Hao; Zheng, Haimei

    2017-02-01

    We report the study of Mg cathodic electrochemical deposition on Ti and Au electrode using a multimodal approach by examining the sample area in-situ using liquid cell transmission electron microscopy (TEM), scanning transmission X-ray microscopy (STXM) and X-ray absorption spectroscopy (XAS). Magnesium Aluminum Chloride Complex was synthesized and utilized as electrolyte, where non-reversible features during in situ charging-discharging cycles were observed. During charging, a uniform Mg film was deposited on the electrode, which is consistent with the intrinsic non-dendritic nature of Mg deposition in Mg ion batteries. The Mg thin film was not dissolvable during the following discharge process. We found that such Mg thin film is hexacoordinated Mg compounds by in-situ STXM and XAS. This study provides insights on the non-reversibility issue and failure mechanism of Mg ion batteries. Also, our method provides a novel generic method to understand the in situ battery chemistry without any further sample processing, which can preserve the original nature of battery materials or electrodeposited materials. This multimodal in situ imaging and spectroscopy provides many opportunities to attack complex problems that span orders of magnitude in length and time scale, which can be applied to a broad range of the energy storage systems.

  15. Pseudocapacitance of MnO{sub 2} originates from reversible insertion/desertion of thiocyanate anions studied using in situ X-ray absorption spectroscopy in ionic liquid electrolyte

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Ming-Tsung; Tsai, Wen-Ta; Chang, Jeng-Kuei [Department of Materials Science and Engineering, National Cheng Kung University, 1 University Road, Tainan (China); Deng, Ming-Jay; Cheng, Hui-Fang; Sun, I-Wen [Department of Chemistry, National Cheng Kung University, 1 University Road, Tainan (China)

    2010-02-01

    Charge storage mechanisms of electrodeposited MnO{sub 2} in various aprotic ionic liquids (ILs) are studied using in situ X-ray absorption spectroscopy (XAS). The analytical results show that a unique thiocyanate (SCN{sup -}) anion can reversibly insert/desert into/from the tunnels between the [MnO{sub 6}] octahedral subunits depending on the applied potential. This process charge compensates the Mn{sup 3+}/Mn{sup 4+} redox transition upon charging-discharging and thus contributes to an ideal pseudocapacitive behavior of the MnO{sub 2} electrode. The present work would open up a route for developing a novel oxide-based supercapacitor, with high cell-voltage, high thermal stability, and high safety, incorporating IL electrolytes. (author)

  16. Mineralogical characterization of arsenic, iron, and nickel in uranium mine tailings using XAS and EMPA

    International Nuclear Information System (INIS)

    Essilfie-Dughan, J.; Hendry, M.J.; Warner, J.; Kotzer, T.

    2010-01-01

    In northern Saskatchewan, Canada, high-grade uranium ores and the resulting tailings can contain high levels of arsenic (As), iron (Fe), and nickel (Ni). An environmental concern in the uranium mining industry is the long-term stabilization of these elements of concern (EOCs) within tailings management facilities thereby mitigating their transfer to the surrounding groundwater. Characterization of these As-, Fe- and Ni-bearing minerals and complexes must be carried out to evaluate their solubility and long-term stability within the tailings mass. Synchrotron-based bulk x-ray absorption spectroscopy (XAS) has been used to study the speciation of these EOCs in mine tailing samples obtained from the Deilmann Tailings Management Facility (DTMF) at Key Lake, Saskatchewan. Electron microprobe analysis (EMPA) and synchrotron-based micro-focussing x-ray fluorescence mapping and absorption spectroscopy (μXRF; μXAS ) have also been employed to study spatial distribution and speciation at the micron scale. Comparisons of K-edge absorption spectra of tailings samples and reference compounds indicate the dominant oxidation states of As, Fe, and Ni in the mine tailings samples are +5, +3, and +2, respectively, largely reflecting their deposition in an oxidized environment and complexation within stable oxic phases. Backscattered electron (BSE) images of the tailings from the electron microprobe indicate the presence of gypsum/lime nodules surrounded by metallic rims mainly consisting of As, Fe, and Ni. μXRF elemental mapping confirms these EPMA results. μXAS collected within the metal-bearing rims indicates As and Fe is present mainly in the +5 and +3 oxidation state, respectively. (author)

  17. The relationship between Al and Si in biogenic silica as determined by PIXE and XAS

    International Nuclear Information System (INIS)

    Beck, L.; Gehlen, M.; Flank, A.-M.; Bennekom, A.J. van; Beusekom, J.E.E. van

    2002-01-01

    Biogenic silica, one of the major constituents of marine sediments, is a potentially powerful paleoceanographic tool, revealing information on past productivity. Interpreting the sedimentary records of the biogenic silica requires, however, an understanding of its preservation. Dissolution of biogenic silica is controlled by the presence of trace elements such as Al. The work in this paper focuses on the association of Al and Si in biogenic silica. The composition and the atomic structure of cultured and natural diatoms were determined by using PIXE and XAS techniques. This study provides the first evidence for a structural association of Al and Si in biogenic silica

  18. The adsorption of methanol and water on SAPO-34: in situ and ex situ X-ray diffraction studies

    DEFF Research Database (Denmark)

    Wragg, David S.; Johnsen, Rune; Norby, Poul

    2010-01-01

    The adsorption of methanol on SAPO-34 has been studied using a combination of in situ synchrotron powder X-ray diffraction to follow the process and ex situ high resolution powder diffraction to determine the structure. The unit cell volume of SAPO-34 is found to expand by 0.5% during methanol ad...

  19. In situ study on the formation of FeTe

    DEFF Research Database (Denmark)

    Grivel, Jean-Claude; Wulff, Anders Christian; Yue, Zhao

    2011-01-01

    The formation of the FeTe compound from a mixture of Fe and Te powders was studied in situ by means of high-energy synchrotron X-ray diffraction. FeTe does not form directly from the starting elements; instead, FeTe2 forms as an intermediate product. During a 2 °C/min heating ramp, Te first reacts...

  20. Structural investigations of LiFePO4 electrodes and in situ studies by Fe X-ray absorption spectroscopy

    International Nuclear Information System (INIS)

    Deb, Aniruddha; Bergmann, Uwe; Cramer, S.P.; Cairns, Elton J.

    2005-01-01

    Fe K-edge X-ray absorption near edge spectroscopy (XANES) and extended X-ray absorption fine structure (EXAFS) have been performed on electrodes containing LiFePO 4 to determine the local atomic and electronic structure and their stability with electrochemical cycling. A versatile electrochemical in situ cell has been constructed for long-term soft and hard X-ray experiments for the structural investigation on battery electrodes during the lithium-insertion/extraction processes. The device is used here for an X-ray absorption spectroscopic study of lithium insertion/extraction in a LiFePO 4 electrode, where the electrode contained about 7.7 mg of LiFePO 4 on a 20 μm thick Al-foil. Fe K-edge X-ray absorption near edge spectroscopy (XANES) and extended X-ray absorption fine structure (EXAFS) have been performed on this electrode to determine the local atomic and electronic structure and their stability with electrochemical cycling. The initial state (LiFePO 4 ) showed iron to be in the Fe 2+ state corresponding to the initial state (0.0 mAh) of the cell, whereas in the delithiated state (FePO 4 ) iron was found to be in the Fe 3+ state corresponding to the final charged state (3 mAh). XANES region of the XAS spectra revealed a high spin configuration for the two states (Fe (II), d 6 and Fe (III), d 5 ). The results confirm that the olivine structure of the LiFePO 4 and FePO 4 is retained by the electrodes in agreement with the XRD observations reported previously. These results confirm that LiFePO 4 cathode material retains good structural short-range order leading to superior cycling capability

  1. In situ stress determination research study

    International Nuclear Information System (INIS)

    Austin, W.G.; Thompson, P.M.

    1994-01-01

    The objectives of this study are to evaluate and implement rock stress determination instruments and techniques developed by Atomic Energy of Canada Limited (AECL) at its Underground Research Laboratory (URL) for use in jointed rock and to continue the development of analytical and interpretation methods for stress determination results including effects of scale, structure and anisotropy. Testing and evaluation of the instruments and methods developed at URL need to be done in a similar rock type prior to underground access at the Yucca Mountain Site Characterization Project

  2. Acoustic phonon dephasing in shallow GaAs/Ga 1- xAl xAs single quantum wells

    Science.gov (United States)

    Cassabois, G.; Meccherini, S.; Roussignol, Ph.; Bogani, F.; Gurioli, M.; Colocci, M.; Planel, R.; Thierry-Mieg, V.

    1998-07-01

    The intermediate dimensionality regime is studied on a set of shallow GaAs/Ga 1- xAl xAs single quantum wells. Such heterostructures exhibit 2D strong excitonic electroabsorption together with near 3D fast transport properties. We report dephasing time measurements ( T2) of the heavy-hole exciton and we show that the acoustic phonon contribution decreases with x to a value in good agreement with theoretical predictions for GaAs bulk.

  3. 2D-PES/XAS method for atomic-layer-resolved magnetic structure analysis

    International Nuclear Information System (INIS)

    Matsui, F.; Daimon, H.; Matsushita, T.; Guo, F.Z.

    2008-01-01

    Photoelectron and Auger electron angular distributions from a localized core level provide information on atomic configurations. Forward-focusing peaks indicate the directions of atoms surrounding the excited atom. X-ray absorption fine structure and X-ray magnetic circular dichroism measurements by Auger electron yield detection on the other hand are excellent methods for studying of the electronic and magnetic structures of surfaces, adsorbates, and thin films. However, all the information from atoms within the electron mean-free-path region is averaged into the obtained spectra. Here, we introduce a new method of X-ray absorption spectroscopy (XAS) combined with measurements of Auger electron angular distribution using a display-type analyzer. Taking advantage of the forward-focusing peak as an excellent element- and site-selective probe, 2D-XAS enables direct access to the individual electronic and magnetic structures of each atomic layer. This method was applied to studying the electronic and magnetic structures of Ni thin film at atomic level. (author)

  4. SOFC anode reduction studied by in situ TEM

    DEFF Research Database (Denmark)

    Simonsen, Søren Bredmose; Wagner, Jakob Birkedal; Hansen, Thomas Willum

    The Solid Oxide Fuel Cell (SOFC) is a promising part of future energy approaches due to a relatively high energy conversion efficiency and low environmental pollution. SOFCs are typically composed of ceramic materials which are highly complex at the nanoscale. TEM is routinely applied ex situ...... for studying these nanoscale structures, but only few SOFC studies have applied in situ TEM to observe the ceramic nanostructures in a reactive gas environment at elevated temperatures. The present contribution focuses on the reduction of an SOFC anode which is a necessary process to form the catalytically...... active Ni surface before operating the fuel cells. The reduction process was followed in the TEM while exposing a NiO/YSZ (YSZ = Y2O3-stabilized ZrO2) model anode to H2 at T = 250-1000⁰C. Pure NiO was used in reference experiments. Previous studies have shown that the reduction of pure Ni...

  5. Recent progress in the use of in situ X-ray methods for the study of heterogeneous catalysts in packed-bed capillary reactors

    NARCIS (Netherlands)

    Jacques, S.D.M.; Leynaud, O.; Strusevich, D.; Stukas, P.; Barnes, P.; Sankar, G.; Sheehy, M.; O’Brien, M.G.; Iglesias-Juez, A.; Beale, A.M.

    2009-01-01

    Synchrotron-based X-ray techniques, such as Diffraction and Absorption Spectroscopy (XAS), can be readily employed to study catalysts in action, thereby offering great potential for revealing the mechanism and behaviour of catalytic solids both during preparation and reaction. The continued

  6. High Throughput In Situ XAFS Screening of Catalysts

    International Nuclear Information System (INIS)

    Tsapatsaris, Nikolaos; Beesley, Angela M.; Weiher, Norbert; Tatton, Helen; Schroeder, Sven L. M.; Dent, Andy J.; Mosselmans, Frederick J. W.; Tromp, Moniek; Russu, Sergio; Evans, John; Harvey, Ian; Hayama, Shu

    2007-01-01

    We outline and demonstrate the feasibility of high-throughput (HT) in situ XAFS for synchrotron radiation studies. An XAS data acquisition and control system for the analysis of dynamic materials libraries under control of temperature and gaseous environments has been developed. The system is compatible with the 96-well industry standard and coupled to multi-stream quadrupole mass spectrometry (QMS) analysis of reactor effluents. An automated analytical workflow generates data quickly compared to traditional individual spectrum acquisition and analyses them in quasi-real time using an HT data analysis tool based on IFFEFIT. The system was used for the automated characterization of a library of 91 catalyst precursors containing ternary combinations of Cu, Pt, and Au on γ-Al2O3, and for the in situ characterization of Au catalysts supported on Al2O3 and TiO2

  7. In-situ spectroelectrochemical studies of radionuclide- contaminated surface films on metals and the mechanism of their formation and dissolution. 1997 annual progress report

    International Nuclear Information System (INIS)

    Balasubramanian, M.; Mansour, A.N.; Melendres, C.A.; Mini, S.; Papapanayiotou, D.

    1997-01-01

    'The incorporation of radioactive contaminants into corrosion product scales on metals is being investigated using in-situ spectroscopic and electrochemical techniques. To facilitate the study, stable isotopes are used initially, while the corrosion films are simulated by electrodeposition of the appropriate oxide (hydroxide) onto a graphite substrate. Synchrotron x-ray absorption spectroscopy (XAS) is used to determine the structure and composition of the host oxide film, as well as the local structure of the impurity ion. Results on the incorporation of Sr and Ce into surface films of Ni(OH) 2 and NiOOH are reported. Cathodically deposited Ni(OH) 2 was found to be mainly in the α form while anodically prepared NiOOH consists of Ni +2 and Ni +4 phases. Sr in the films consists mainly of Sr 2+ which appears to be coordinated to oxygen atoms and is likely to exist as small domains of co-precipitated material. Ce in Ni(OH) 2 exists mainly as Ce +3 and as a Ce +4 species when co-deposited with NiOOH. The structure of the Ce +4 phase appears similar to a Ce(OH) 4 standard. However, x-ray diffraction and laser Raman measurements indicate that the latter chemical formulation is probably incorrect and that the material is more likely to be a disordered hydrous cerium oxide. Ce chemisorbed on Ni(OH) 2 and NiOOH films is predominantly in the +3 valency state. Iron oxide films prepared by anodic deposition from borate buffer solution containing Fe +2 , has been found by XAS to consist mainly of α FeOOH. The latter has been found by others to be the constituent of the corrosion film on iron; this lends credence to the present simulation approach. Future work will involve studies on the incorporation of radioactive Sr, Ce, and Cs, as well as U, into nickel and iron oxide films. Investigations on the structure and composition of chromium oxide films, the effect of temperature on the energetics and mechanism of incorporation of heavy metal ions, as well as the subsequent

  8. A new in situ model to study erosive enamel wear, a clinical pilot study.

    NARCIS (Netherlands)

    Ruben, J.L.; Truin, G.J.; Bronkhorst, E.M.; Huysmans, M.C.D.N.J.M.

    2017-01-01

    OBJECTIVES: To develop an in situ model for erosive wear research which allows for more clinically relevant exposure parameters than other in situ models and to show tooth site-specific erosive wear effect of an acid challenge of orange juice on enamel. METHODS: This pilot study included 6

  9. IFMIF - Design Study for in Situ Creep Fatigue Tests

    International Nuclear Information System (INIS)

    Gordeev, S.; Heinzel, V.; Simakov, St.; Stratmanns, E.; Vladimirov, P.; Moeslang, A.

    2006-01-01

    While the high flux volume (20-50 dpa/fpy) of the International Fusion Materials Irradiation Facility (IFMIF) is dedicated to the irradiation of ∼ 1100 qualified specimens that will be post irradiation examined after disassembling in dedicated Hot Cells, various in situ experiments are foreseen in the medium flux volume (1-20 dpa/fpy). Of specific importance for structural lifetime assessments of fusion power reactors are instrumented in situ creep-fatigue experiments, as they can simulate realistically a superposition of thermal fatigue or creep fatigue and irradiation with fusion relevant neutrons. Based on former experience with in situ fatigue tests under high energy light ion irradiation, a design study has been performed to evaluate the feasibility of in situ creep fatigue tests in the IFMIF medium flux position. The vertically arranged test module for such experiments consists basically of a frame similar to a universal testing machine, but equipped with three pulling rods, driven by independent step motors, instrumentation systems and specimen cooling systems. Therefore, three creep fatigue specimens may be tested at one time in this apparatus. Each specimen is a hollow tube with coolant flow in the specimen interior to maintain individual specimen temperatures. The recently established IFMIF global 3D geometry model was used together the latest McDeLicious code for the neutral and charged particle transport calculations. These comprehensive neutronics calculations have been performed with a fine special resolution of 0.25 cm 3 , showing among others that the specimens will be irradiated with a homogeneous damage rate of up to 13(∼ 9%) dpa/fpy and a fusion relevant damage to helium ratio of 10-12 appm He/dpa. In addition, damage and gas production rates as well as the heat deposition in structural parts of the test module have been calculated. Despite of the vertical gradients in the nuclear heating, CFD code calculations with STAR-CD revealed very

  10. Behavior of fission gases in nuclear fuel: XAS characterization of Kr in UO{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Martin, P.M., E-mail: Philippe-m.martin@cea.fr [CEA, DEN, Cadarache DEC/SESC, F-13108 St-Paul-Lez-Durance Cedex (France); Vathonne, E.; Carlot, G.; Delorme, R.; Sabathier, C.; Freyss, M.; Garcia, P.; Bertolus, M. [CEA, DEN, Cadarache DEC/SESC, F-13108 St-Paul-Lez-Durance Cedex (France); Glatzel, P. [European Synchrotron Radiation Facility, 6 Rue Jules Horowitz, 38043 Grenoble (France); Proux, O. [OSUG, Observatoire des Sciences de l’Univers de Grenoble, CNRS and Université Joseph Fourier, BP 53, 38041 Grenoble Cedex 9 (France)

    2015-11-15

    X-ray Absorption Spectroscopy (XAS) was used to study the behavior of krypton as a function of its concentration in UO{sub 2} samples implanted with Kr ions. For a 0.5 at.% krypton local concentration, by combining XAS results and DFT + U calculations, we show that without any thermal treatment Kr atoms are mainly incorporated in the UO{sub 2} lattice as single atoms inside a neutral bound Schottky defect with O vacancies aligned along the (100) direction (BSD1). A thermal treatment at 1273 K induces the precipitation of dense Kr nano-aggregates, most probably solid at room temperature. In addition, 26 ± 2% of the Kr atoms remain inside BSD1 showing that Kr-BSD1 complex is stable up to this temperature. Consequently, the (in-)solubility of krypton in UO{sub 2} has to be re-evaluated. For high Kr concentration (8 at.%), XAS signals show that Kr atoms have precipitated in nanometer-sized aggregates with internal densities ranging between 4.15(7) g cm{sup −3} and 3.98(5) g cm{sup −3} even after annealing at 873 K. By neglecting the effect due to the UO{sub 2} matrix, the corresponding krypton pressures at 300 K were equal to 2.6(3) GPa and 2.0(2) GPa, respectively. After annealing at 1673 K, regardless of the initial Kr concentration, a bi-modal distribution is observed with solid nano-aggregates even at room temperature and larger cavities only partially filled with Kr. These results are very close to those observed in UO{sub 2} fuel irradiated in reactor. In this study we show that a rare gas can be used as a probe to investigate the defect creation and their stability in UO{sub 2}.

  11. Analysis of the suitability of Al{sub x}Ga{sub 1-x}As as active material in III-V multiple-junction solar cells; Analyse zur Eignung von Al{sub x}Ga{sub 1-x}As als aktives Material in III-V Mehrfachsolarzellen

    Energy Technology Data Exchange (ETDEWEB)

    Heckelmann, Stefan

    2017-05-01

    In the past, Al{sub x}Ga{sub 1-x}As single and multiple-junction solar cells have been manufactured and tested. Although the ternary Al{sub x}Ga{sub 1-x}As is one of the most studied semiconductor systems, the results have often lagged behind expectations. In the thesis presented here, for the first time, the deep understanding of the Al{sub x}Ga{sub 1-x}As material system resulting from material analysis was linked with its application in solar cells. As has been shown, many cell results can only be explained if the peculiarities of the material, in particular the formation of DX centers and the transition from direct to indirect semiconductor, are also included. From this purposeful consideration of the material in terms of its usefulness in the semiconductor device and the technological significance of individual properties, not only high-quality solar cells based on Al{sub x}Ga{sub 1-x}As were produced but also new insights into the material properties of (Al{sub y}Ga{sub 1-y}){sub 1-z}In{sub z}As and the information gain from photoluminescence measurements can be significantly increased. [German] In der Vergangenheit wurden bereits Einfach- und Mehrfachsolarzellen aus Al{sub x}Ga{sub 1-x}As hergestellt und untersucht. Obwohl das ternaere Al{sub x}Ga{sub 1-x}As eines der meist untersuchten Halbleitersysteme ist, blieben die Ergebnisse oft hinter den Erwartungen zurueck. In der hier vorgestellten Dissertation wurde zum ersten Mal das aus der Materialanalytik heraus entstandene, tiefe Verstaendnis ueber das AlxGa1-xAs Materialsystem mit seiner Anwendung in Solarzellen verknuepft. Wie sich gezeigt hat, werden viele Zellergebnisse erst erklaerbar, wenn auch die Besonderheiten des Materials, insbesondere die Bildung von DX-Zentren und der Uebergang vom direkten zum indirekten Halbleiter, mit einbezogen werden. Aus dieser zielgerichteten Betrachtung des Materials im Hinblick auf seinen Nutzen im Halbleiterbauelement und der technologischen Bedeutung einzelner

  12. Electrochemical studies, in-situ and ex-situ characterizations of different manganese compounds electrodeposited in aerated solutions

    International Nuclear Information System (INIS)

    Peulon, S.; Lacroix, A.; Chausse, A.; Larabi-Gruet, N.

    2007-01-01

    This work deals with the electrodeposition of manganese compounds. A systematic study of the synthesis experimental conditions has been carried out, and the obtained depositions have been characterized by different ex-situ analyses methods (XRD, FTIR, SEM). The in-situ measurements of mass increase with a quartz microbalance during the syntheses have allowed to estimate the growth mechanisms which are in agreement with the ex-situ characterizations. The cation has an important role in the nature of the electrodeposited compounds. In presence of sodium, a mixed lamellar compound Mn(III)/Mn(IV), the birnessite, is deposited, whereas in presence of potassium, bixbyite is formed (Mn 2 O 3 ), these two compounds having a main role in the environment. The substrate can also influence the nature of the formed intermediary compounds. Little studied compounds such as feitkneichtite (β-MnOOH) and groutite (α-MnOOH) have been revealed. (O.M.)

  13. Case study of the gradient features of in situ concrete

    Directory of Open Access Journals (Sweden)

    Pengkun Hou

    2014-01-01

    Full Text Available The recognition of gradient features of the properties of in situ concrete is important for the interpretation/prediction of service life. In this work, the gradient features: water absorption, porosity, mineralogy, morphology and micromechanical properties were studied on two in situ road concretes (15 and 5 years old, respectively by weighing, MIP, XRD, IR, SEM/EDS and micro-indentation techniques. Results showed that a coarsening trend of the pores of the concrete leads to a gradual increase of liquid transport property from inside to outside. Although the carbonation of the exposed surface results in a compact microstructure of the paste, its combined action with calcium-leaching leads to a comparable porosity of different concrete layers. Moreover, the combining factors result in three morphological features, i.e. a porous and granular exposed-layer, a fibrous and porous subexposed-layer and a compact inner-layer. Micro-indentation test results showed that a hard layer that moves inward with aging exists due to the alterations of the mineralogy, the pore and the gel structure.

  14. A Novel Penetration System for in situ Astrobiological Studies

    Directory of Open Access Journals (Sweden)

    Yang Gao

    2005-12-01

    Full Text Available Due to ultraviolet flux in the surface layers of most solar bodies, future astrobiological research is increasingly seeking to conduct subsurface penetration and drilling to detect chemical signature for extant or extinct life. To address this issue, we present a micro-penetrator concept (mass < 10 kg that is suited for extraterrestrial planetary deployment and in situ investigation of chemical and physical properties. The instrumentation in this concept is a bio-inspired drill to access material beneath sterile surface layer for biomarker detection. The proposed drill represents a novel concept of two-valve-reciprocating motion, inspired by the working mechanism of wood wasp ovipositors. It is lightweight (0.5 kg, driven at low power (3 W, and able to drill deep (1-2 m. Tests have shown that the reciprocating drill is feasible and has potential of improving drill efficiency without using any external force. The overall penetration system provides a small, light and energy efficient solution to in situ astrobiological studies, which is crucial for space engineering. Such a micro-penetrator can be used for exploration of terrestrial-type planets or other small bodies of the solar system with the minimum of modifications.

  15. A Novel Penetration System for in situ Astrobiological Studies

    Directory of Open Access Journals (Sweden)

    Yang Gao

    2008-11-01

    Full Text Available Due to ultraviolet flux in the surface layers of most solar bodies, future astrobiological research is increasingly seeking to conduct subsurface penetration and drilling to detect chemical signature for extant or extinct life. To address this issue, we present a micro-penetrator concept (mass < 10 kg that is suited for extraterrestrial planetary deployment and in situ investigation of chemical and physical properties. The instrumentation in this concept is a bio-inspired drill to access material beneath sterile surface layer for biomarker detection. The proposed drill represents a novel concept of two-valve-reciprocating motion, inspired by the working mechanism of wood wasp ovipositors. It is lightweight (0.5 kg, driven at low power (3 W, and able to drill deep (1-2 m. Tests have shown that the reciprocating drill is feasible and has potential of improving drill efficiency without using any external force. The overall penetration system provides a small, light and energy efficient solution to in situ astrobiological studies, which is crucial for space engineering. Such a micro-penetrator can be used for exploration of terrestrial-type planets or other small bodies of the solar system with the minimum of modifications.

  16. K- and L-edge X-ray Absorption Spectroscopy (XAS) and Resonant Inelastic X-ray Scattering (RIXS) Determination of Differential Orbital Covalency (DOC) of Transition Metal Sites.

    Science.gov (United States)

    Baker, Michael L; Mara, Michael W; Yan, James J; Hodgson, Keith O; Hedman, Britt; Solomon, Edward I

    2017-08-15

    Continual advancements in the development of synchrotron radiation sources have resulted in X-ray based spectroscopic techniques capable of probing the electronic and structural properties of numerous systems. This review gives an overview of the application of metal K-edge and L-edge X-ray absorption spectroscopy (XAS), as well as K resonant inelastic X-ray scattering (RIXS), to the study of electronic structure in transition metal sites with emphasis on experimentally quantifying 3d orbital covalency. The specific sensitivities of K-edge XAS, L-edge XAS, and RIXS are discussed emphasizing the complementary nature of the methods. L-edge XAS and RIXS are sensitive to mixing between 3d orbitals and ligand valence orbitals, and to the differential orbital covalency (DOC), that is, the difference in the covalencies for different symmetry sets of the d orbitals. Both L-edge XAS and RIXS are highly sensitive to and enable separation of and donor bonding and back bonding contributions to bonding. Applying ligand field multiplet simulations, including charge transfer via valence bond configuration interactions, DOC can be obtained for direct comparison with density functional theory calculations and to understand chemical trends. The application of RIXS as a probe of frontier molecular orbitals in a heme enzyme demonstrates the potential of this method for the study of metal sites in highly covalent coordination sites in bioinorganic chemistry.

  17. In situ ellipsometric study of surface immobilization of flagellar filaments

    Energy Technology Data Exchange (ETDEWEB)

    Kurunczi, S., E-mail: kurunczi@mfa.kfki.hu [Department of Photonics, Research Institute for Technical Physics and Materials Science, H-1121, Konkoly Thege Miklos ut 29-33, Budapest (Hungary); Nemeth, A.; Huelber, T. [Department of Photonics, Research Institute for Technical Physics and Materials Science, H-1121, Konkoly Thege Miklos ut 29-33, Budapest (Hungary); Kozma, P. [Department of Photonics, Research Institute for Technical Physics and Materials Science, H-1121, Konkoly Thege Miklos ut 29-33, Budapest (Hungary); Department of Nanotechnology, Research Institute of Chemical and Process Engineering, Faculty of Information Technology, University of Pannonia, Egyetem u. 10, Veszprem, H-8200 (Hungary); Petrik, P. [Department of Photonics, Research Institute for Technical Physics and Materials Science, H-1121, Konkoly Thege Miklos ut 29-33, Budapest (Hungary); Jankovics, H. [Department of Nanotechnology, Research Institute of Chemical and Process Engineering, Faculty of Information Technology, University of Pannonia, Egyetem u. 10, Veszprem, H-8200 (Hungary); Sebestyen, A. [Department of Photonics, Research Institute for Technical Physics and Materials Science, H-1121, Konkoly Thege Miklos ut 29-33, Budapest (Hungary); Department of Nanotechnology, Research Institute of Chemical and Process Engineering, Faculty of Information Technology, University of Pannonia, Egyetem u. 10, Veszprem, H-8200 (Hungary); Vonderviszt, F. [Department of Photonics, Research Institute for Technical Physics and Materials Science, H-1121, Konkoly Thege Miklos ut 29-33, Budapest (Hungary); Department of Nanotechnology, Research Institute of Chemical and Process Engineering, Faculty of Information Technology, University of Pannonia, Egyetem u. 10, Veszprem, H-8200 (Hungary); Institute of Enzymology, Karolina ut 29-33, Budapest, H-1113 (Hungary); and others

    2010-10-15

    Protein filaments composed of thousands of subunits are promising candidates as sensing elements in biosensors. In this work in situ spectroscopic ellipsometry is applied to monitor the surface immobilization of flagellar filaments. This study is the first step towards the development of layers of filamentous receptors for sensor applications. Surface activation is performed using silanization and a subsequent glutaraldehyde crosslinking. Structure of the flagellar filament layers immobilized on activated and non-activated Si wafer substrates is determined using a two-layer effective medium model that accounted for the vertical density distribution of flagellar filaments with lengths of 300-1500 nm bound to the surface. The formation of the first interface layer can be explained by the multipoint covalent attachment of the filaments, while the second layer is mainly composed of tail pinned filaments floating upwards with the free parts. As confirmed by atomic force microscopy, covalent immobilization resulted in an increased surface density compared to absorption.

  18. In situ Raman spectroscopy studies of bulk and surface metal

    NARCIS (Netherlands)

    Weckhuysen, B.M.; Wachs, I.E.; Jehng, J.M.; Deo, G.; Guliants, V.V.; Benziger, J.B.

    1996-01-01

    Bulk V-P-O and model supported vanadia catalysts were investigated with in situ Raman spectroscopy during n-butane oxidation to maleic anhydride in order to determine the fundamental molecular structure-reactivity/selectivity insights that can be obtained from such experiments. The in situ Raman

  19. Spin excitation and band-narrowing in Al{sub x}Ga{sub 1-x}As heterostructures

    Energy Technology Data Exchange (ETDEWEB)

    Miah, M. Idrish, E-mail: m.miah@griffith.edu.au [Department of Physics, University of Chittagong, Chittagong 4331 (Bangladesh)

    2010-11-01

    We studied the spin excitation in dependences of the applied electric field and lattice temperature (LT) via the measurements of the circularly polarized photoluminescence (CPPL) in Al{sub x}Ga{sub 1-x}As heterostructures (HSs). The intensity of CPPL was found to strongly depend on the electric field applied to the HSs. The CPPL was also found to enhance with decreasing LT. It was demonstrated that the observed LT dependence might be due to the LT-dependent band-gap shift of the HS materials.

  20. Predicted electronic and structural properties of B{sub x}In{sub 1-x}As

    Energy Technology Data Exchange (ETDEWEB)

    Tayebi, N. [Laboratory of Applied Materials, University of Sidi Bel Abbes, 31 rue de Madagascar, Sidi Bel Abbes (Algeria); Benkabou, K., E-mail: kbenkabou@yahoo.fr [Laboratory of Applied Materials, University of Sidi Bel Abbes, 31 rue de Madagascar, Sidi Bel Abbes (Algeria); Aoumeur-Benkabou, F.Z. [Laboratory of Applied Materials, University of Sidi Bel Abbes, 31 rue de Madagascar, Sidi Bel Abbes (Algeria)

    2012-07-15

    Structural and electronic properties of the B{sub x}In{sub 1-x}As ternary alloy are studied using the tight binding method. The optical band gap bowing is calculated for the first time in the full range of Boron composition x. It is found to be strong. A small deviation from virtual crystal approximation is found for the bond length. New results on elastic constants are reported. The obtained results are in good agreement with the available data in the literature.

  1. Comparative study of in-situ filter test methods

    International Nuclear Information System (INIS)

    Marshall, M.; Stevens, D.C.

    1981-01-01

    Available methods of testing high efficiency particulate aerosol (HEPA) filters in-situ have been reviewed. In order to understand the relationship between the results produced by different methods a selection has been compared. Various pieces of equipment for generating and detecting aerosols have been tested and their suitability assessed. Condensation-nuclei, DOP (di-octyl phthalate) and sodium-flame in-situ filter test methods have been studied, using the 500 cfm (9000 m 3 /h) filter test rig at Harwell and in the field. Both the sodium-flame and DOP methods measure the penetration through leaks and filter material. However the measured penetration through filtered leaks depends on the aerosol size distribution and the detection method. Condensation-nuclei test methods can only be used to measure unfiltered leaks since condensation nuclei have a very low penetration through filtered leaks. A combination of methods would enable filtered and unfiltered leaks to be measured. A condensation-nucleus counter using n-butyl alcohol as the working fluid has the advantage of being able to detect any particle up to 1 μm in diameter, including DOP, and so could be used for this purpose. A single-particle counter has not been satisfactory because of interference from particles leaking into systems under extract, particularly downstream of filters, and because the concentration of the input aerosol has to be severely limited. The sodium-flame method requires a skilled operator and may cause safety and corrosion problems. The DOP method using a total light scattering detector has so far been the most satisfactory. It is fairly easy to use, measures reasonably low values of penetration and gives rapid results. DOP has had no adverse effect on HEPA filters over a long series of tests

  2. In-Situ Optical Studies of Oxidation/Reduction Kinetics on SOFC Cermet Anodes

    Science.gov (United States)

    2010-12-28

    DATES COVERED (From - To) 1/29/10-9/30/10 4. TITLE AND SUBTITLE In situ optical studies of oxidation/reduction kinetics on SOFC cermet anodes 5a...0572 In-situ Optical Studies of Oxidation/Reduction Kinetics on SOFC Cermet Anodes Department of Chemistry and Biochemistry Montana State University...of Research In-situ Optical Studies of Oxidation/Reduction Kinetics on SOFC Cermet Anodes Principal Investigator Robert Walker Organization

  3. Summary of feasibility studies on in situ disposal as a decommissioning option for nuclear facilities

    International Nuclear Information System (INIS)

    Helbrecht, R.A.

    2002-01-01

    A scoping study was conducted over the period 1998-2000 to consider the feasibility of in situ disposal as a decommissioning option for AECL's Nuclear Power Demonstration Reactor located at Rolphton, Ontario. The results of a detailed assessment are summarized and the study concludes that in situ disposal appears feasible. Additional work required to confirm the results is also identified. A second in situ component, contaminated Winnipeg River sediments at AECL's Whiteshell Laboratory located in Manitoba, was also evaluated. That study concluded that in situ abandonment would have no adverse impact on aquatic life, humans and the environment. A summary of the study is presented as an appendix to the report. (author)

  4. Electrochemical studies, in-situ and ex-situ characterizations of different manganese compounds electrodeposited in aerated solutions; Etudes electrochimiques, suivis in-situ et caracterisations ex-situ de divers composes de manganese electrodeposes dans des solutions aerees

    Energy Technology Data Exchange (ETDEWEB)

    Peulon, S.; Lacroix, A.; Chausse, A. [Univ. d' Evry-val-d' Essonne, Laboratoire Analyse et Modelisation pour la Biologie et l' Environnement (LAMBE CNRS UMR 8587), 91 - Evry (France); Larabi-Gruet, N. [CEA Saclay, Dept. de Physico-Chimie (DEN/DPC/SECR/L3MR), 91 - Gif sur Yvette (France)

    2007-07-01

    This work deals with the electrodeposition of manganese compounds. A systematic study of the synthesis experimental conditions has been carried out, and the obtained depositions have been characterized by different ex-situ analyses methods (XRD, FTIR, SEM). The in-situ measurements of mass increase with a quartz microbalance during the syntheses have allowed to estimate the growth mechanisms which are in agreement with the ex-situ characterizations. The cation has an important role in the nature of the electrodeposited compounds. In presence of sodium, a mixed lamellar compound Mn(III)/Mn(IV), the birnessite, is deposited, whereas in presence of potassium, bixbyite is formed (Mn{sub 2}O{sub 3}), these two compounds having a main role in the environment. The substrate can also influence the nature of the formed intermediary compounds. Little studied compounds such as feitkneichtite ({beta}-MnOOH) and groutite ({alpha}-MnOOH) have been revealed. (O.M.)

  5. In situ XAS study of Li{sub x}Ni{sub 0.7}Fe{sub 0.15}Co{sub 0.15}O{sub 2} cathode material

    Energy Technology Data Exchange (ETDEWEB)

    Mansour, A.N. [Naval Surface Warfare Center, West Bethesda, MD (United States); Croguennec, L.; Prado, G.; Delmas, C. [Inst. de Chimie de la Matiere Condensee de Bordeaus-CNRS and Ecole Nationale Superieure de Chimie et Physique de Bordeaux, Pesssac Cedex (France)

    2001-03-01

    We have examined the oxidation states and local atomic structures of Ni, Fe, and Co in Li{sub x}Ni{sub 0.7}Fe{sub 0.15}Co{sub 0.15}O{sub 2} as a function of Li content during the first charge in a Li//Li{sub x}Ni{sub 0.7}Fe{sub 0.15}Co{sub 0.}1{sub 5O2} nonaqueous cell. We show that the composition of the material in the pristine state is more accurately described by Li{sub 0.95}Ni(II){sub 0.09}Ni(III){sub 0.66}Fe(III){sub 0.15}Co(III){sub 0.15}O{sub 2}. Half Ni(II) resides in Li-vacant sites. Both Fe and Co substitute for Ni within the NiO{sub 2} slabs with no significant amounts of Fe or Co that can be attributed to Li-vacant sites. The local structure parameters are consistent with oxidation states observed on the basis of the XANES data. The Ni {kappa}-edge energy continuously shifts to a higher energy with decrease in Li content due to oxidation of Ni( II) to Ni( III) and Ni( III) to Ni( IV). After the complete oxidation of Ni( III) to Ni( IV), the Fe KAPPA(-edge energy begins to increase with further decrease in Li content indicating the oxidation of Fe( III) to Fe( IV). The Co )KAPPA-edge energy at half-height, on the other hand, is unchanged during the whole range of Li de-intercalation indicating that no significant change in the oxidation state of Co occurs upon the complete removal of Li. (au)

  6. Stability of mineral fibres in contact with human cell cultures. An in situ μXANES, μXRD and XRF iron mapping study.

    Science.gov (United States)

    Pollastri, Simone; Gualtieri, Alessandro F; Vigliaturo, Ruggero; Ignatyev, Konstantin; Strafella, Elisabetta; Pugnaloni, Armanda; Croce, Alessandro

    2016-12-01

    Relevant mineral fibres of social and economic importance (chrysotile UICC, crocidolite UICC and a fibrous erionite from Jersey, Nevada, USA) were put in contact with cultured diploid human non-tumorigenic bronchial epithelial (Beas2B) and pleural transformed mesothelial (MeT5A) cells to test their cytotoxicity. Slides of each sample at different contact times up to 96 h were studied in situ using synchrotron XRF, μ-XRD and μ-XAS (I18 beamline, Diamond Light Source, UK) and TEM investigations. XRF maps of samples treated for 96 h evidenced that iron is still present within the chrysotile and crocidolite fibres and retained at the surface of the erionite fibres, indicating its null to minor mobilization in contact with cell media; this picture was confirmed by the results of XANES pre-edge analyses. μ-XRD and TEM data indicate greater morphological and crystallinity modifications occurring in chrysotile, whereas crocidolite and erionite show to be resistant in the biological environment. The contact of chrysotile with the cell cultures seems to lead to earlier amorphization, interpreted as the first dissolution step of these fibres. The formation of such silica-rich fibre skeleton may prompt the production of HO in synergy with surface iron species and could indicate that chrysotile may be much more reactive and cytotoxic in vitro in the (very) short term whereas the activity of crocidolite and erionite would be much more sluggish but persistent in the long term. Copyright © 2016 Elsevier Ltd. All rights reserved.

  7. Exhaust catalysis studies using in-situ positron emission

    International Nuclear Information System (INIS)

    Vonkeman, K.A.

    1990-01-01

    In this thesis the kinetics of noble metal catalysts with a formulation related to that of commercial automotive exhaust catalysts, have been examined. The application of a new radioisotope tracer technique in studies of catalyst kinetics is described. Reactant and product molecules were pulsed over a catalyst under conditions such, that the reaction rates were kinetically controlled. Labelling of the reacting molecules enables the in-situ measurement of transient phenomena in a reactor as a function of time and position, if a tomograph is used as detection system. Integral reactor profiles are measured, by which concentration gradients occurring in the reactor can be studied. The large amount of data obtained during each experiment were used to quantify the kinetics. To this end, a refined mathematical model of the kinetics based on the elementary steps of adsorption, desorption and surface reaction was used to simulate the experiments. The experimental conditions in this study were representative for the cold start of a car, when the catalyst is heating up. By applying small catalyst particles and high linear velocities the influence of transport phenomena was excluded so that the experiments were carried out in the kinetically controlled regime. Reaction kinetics of carbon monoxide oxidation by oxygen and nitrogen oxide were studied. Experimental data obtained with surface science techniques were very useful in constructing the kinetic model. By simulating the experiments, the relevant kinetic parameters could be quantified and information on the elementary reaction steps was obtained. Since carbon dioxide adsorbs strongly to the catalyst carrier; 10% carbon dioxide was added to the gas phase (in actual automotive exhaust gas the concentration of carbon dioxide is 10 - 15%). This enabled the determination of the transients due to the interaction of gas components with the catalytically active compounds of the catalyst. (author). 446 refs.; 57 figs.; 21 tabs

  8. In situ studies of NO reduction by H

    NARCIS (Netherlands)

    Roobol, S. B.; Onderwaater, W. G.; van Spronsen, M. A.; Carla, F; Balmes, O; Navarro-Paredes, V; Vendelbo, S.B.; Kooyman, P.J.; Elkjær, C. F.; Helveg, S; Felici, R; Frenken, J. W.M.; Groot, I.M.N.

    2017-01-01

    In situ surface X-ray diffraction and transmission electron microscopy at 1 bar show massive material transport of platinum during high-temperature NO reduction with H2. A Pt(110) single-crystal surface shows a wide variety of surface reconstructions and extensive faceting of the

  9. In Situ Study of Noncatalytic Metal Oxide Nanowire Growth

    DEFF Research Database (Denmark)

    Rackauskas, Simas; Jiang, Hua; Wagner, Jakob Birkedal

    2014-01-01

    a catalyst is still widely disputed and unclear. Here, we show that the nanowire growth during metal oxidation is limited by a nucleation of a new layer. On the basis of in situ transmission electron microscope investigations we found that the growth occurs layer by layer at the lowest specific surface...

  10. In situ coral reef oxygen metabolism: an eddy correlation study.

    Directory of Open Access Journals (Sweden)

    Matthew H Long

    Full Text Available Quantitative studies of coral reefs are challenged by the three-dimensional hard structure of reefs and the high spatial variability and temporal dynamics of their metabolism. We used the non-invasive eddy correlation technique to examine respiration and photosynthesis rates, through O2 fluxes, from reef crests and reef slopes in the Florida Keys, USA. We assessed how the photosynthesis and respiration of different reef habitats is controlled by light and hydrodynamics. Numerous fluxes (over a 0.25 h period were as high as 4500 mmol O2 m(-2 d(-1, which can only be explained by efficient light utilization by the phototrophic community and the complex canopy structure of the reef, having a many-fold larger surface area than its horizontal projection. Over diel cycles, the reef crest was net autotrophic, whereas on the reef slope oxygen production and respiration were balanced. The autotrophic nature of the shallow reef crests implies that the export of organics is an important source of primary production for the larger area. Net oxygen production on the reef crest was proportional to the light intensity, up to 1750 µmol photons m(-2 s(-1 and decreased thereafter as respiration was stimulated by high current velocities coincident with peak light levels. Nighttime respiration rates were also stimulated by the current velocity, through enhanced ventilation of the porous framework of the reef. Respiration rates were the highest directly after sunset, and then decreased during the night suggesting that highly labile photosynthates produced during the day fueled early-night respiration. The reef framework was also important to the acquisition of nutrients as the ambient nitrogen stock in the water had sufficient capacity to support these high production rates across the entire reef width. These direct measurements of complex reefs systems yielded high metabolic rates and dynamics that can only be determined through in situ, high temporal resolution

  11. Sulfur X-Ray Absorption Spectroscopy of Living Mammalian Cells: An Enabling Tool for Sulfur Metabolomics. in Situ Observation of Uptake of Taurine Into MDCK Cells

    Energy Technology Data Exchange (ETDEWEB)

    Gnida, M.; Sneeden, E.Yu; Whitin, J.C.; Prince, R.C.; Pickering, I.J.; Korbas, M.; George, G.N.

    2009-06-01

    Sulfur is essential for life, with important roles in biological structure and function. However, because of a lack of suitable biophysical techniques, in situ information about sulfur biochemistry is generally difficult to obtain. Here, we present an in situ sulfur X-ray absorption spectroscopy (S-XAS) study of living cell cultures of the mammalian renal epithelial MDCK cell line. A great deal of information is retrieved from a characteristic sulfonate feature in the X-ray absorption spectrum of the cell cultures, which can be related to the amino acid taurine. We followed the time and dose dependence of uptake of taurine into MDCK cell monolayers. The corresponding uptake curves showed a typical saturation behavior with considerable levels of taurine accumulation inside the cells (as much as 40% of total cellular sulfur). We also investigated the polarity of uptake of taurine into MDCK cells, and our results confirmed that uptake in situ is predominantly a function of the basolateral cell surface.

  12. Beam-induced redox transformation of arsenic during As K-edge XAS measurements: availability of reducing or oxidizing agents and As speciation.

    Science.gov (United States)

    Han, Young Soo; Jeong, Hoon Young; Hyun, Sung Pil; Hayes, Kim F; Chon, Chul Min

    2018-05-01

    During X-ray absorption spectroscopy (XAS) measurements of arsenic (As), beam-induced redox transformation is often observed. In this study, the As species immobilized by poorly crystallized mackinawite (FeS) was assessed for the susceptibility to beam-induced redox reactions as a function of sample properties including the redox state of FeS and the solid-phase As speciation. The beam-induced oxidation of reduced As species was found to be mediated by the atmospheric O 2 and the oxidation products of FeS [e.g. Fe(III) (oxyhydr)oxides and intermediate sulfurs]. Regardless of the redox state of FeS, both arsenic sulfide and surface-complexed As(III) readily underwent the photo-oxidation upon exposure to the atmospheric O 2 during XAS measurements. With strict O 2 exclusion, however, both As(0) and arsenic sulfide were less prone to the photo-oxidation by Fe(III) (oxyhydr)oxides than NaAsO 2 and/or surface-complexed As(III). In case of unaerated As(V)-reacted FeS samples, surface-complexed As(V) was photocatalytically reduced during XAS measurements, but arsenic sulfide did not undergo the photo-reduction.

  13. Oral microemulsions of paclitaxel: in situ and pharmacokinetic studies.

    Science.gov (United States)

    Nornoo, Adwoa O; Zheng, Haian; Lopes, Luciana B; Johnson-Restrepo, Boris; Kannan, Kurunthachalam; Reed, Rachel

    2009-02-01

    The overall goal of this study was to develop cremophor-free oral microemulsions of paclitaxel (PAC) to enhance its permeability and oral absorption. The mechanism of this enhancement, as well as characteristics of the microemulsions relevant to the increase in permeability and absorption of the low solubility, low permeability PAC was investigated. Phase diagrams were used to determine the macroscopic phase behavior of the microemulsions and to compare the efficiency of different surfactant-oil mixtures to incorporate water. The microemulsion region on the phase diagrams utilizing surfactant-myvacet oil combinations was in decreasing order: lecithin: butanol: myvacet oil (LBM, 48.5%)>centromix CPS: 1-butanol: myvacet oil (CPS, 45.15%)>capmul MCM: polysorbate 80: myvacet oil (CPM, 27.6%)>capryol 90: polysorbate 80: myvacet oil (CP-P80, 23.9%)>capmul: myvacet oil (CM, 20%). Oil-in-water (o/w) microemulsions had larger droplet sizes (687-1010 nm) than the water-in-oil (w/o) microemulsions (272-363 nm) when measured using a Zetasizer nano series particle size analyzer. Utilizing nuclear magnetic resonance spectroscopy (NMR), the self-diffusion coefficient (D) of PAC in CM, LBM and CPM containing 10% of deuterium oxide (D(2)O) was 2.24x10(-11), 1.97x10(-11) and 0.51x10(-11) m(2)/s, respectively. These values indicate the faster molecular mobility of PAC in the two w/o microemulsions (CM and LBM) than the o/w microemulsion--CPM. The in situ permeability of PAC through male CD-IGS rat intestine was 3- and 11-fold higher from LBM and CM, respectively, than that from the control clinical formulation, Taxol (CE, cremophor: ethanol) in a single pass perfusion study. PAC permeability was significantly increased in the presence of the pgp/CYP3A4 inhibitor cyclosporine A (CsA). This enhancement may be attributed to the pgp inhibitory effect of the surfactants, oil and/or the membrane perturbation effect of the surfactants. The oral disposition of PAC in CM, LBM and CPM compared

  14. In situ NMR studies of reactions on catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Haw, James F [Texas A and M Univ., College Station, TX (United States). Dept. of Chemistry

    1994-12-31

    Zeolites are useful in the synthesis of fine chemicals. The systematic understanding of organic chemistry of zeolite catalysis may contribute to: the elucidation of reaction mechanisms of existing catalytic processes; the discovery of new catalytic reactions; the application of zeolite catalysis to the synthesis of fine chemicals. This work presents species of zeolites identified by in situ NMR; reactions of organic chemicals on zeolites and proposes mechanisms as well as reactivity trends 3 refs., 7 tabs.

  15. Comparison of radiative and structural properties of 1.3 µm InxGa(1-x)As quantum-dot laser structures grown by metalorganic chemical vapor deposition and molecular-beam epitaxy: Effect on the lasing properties

    NARCIS (Netherlands)

    Passaseo, A.; Vittorio, de M.; Todaro, M.T.; Tarantini, I.; Giorgi, de M.; Cingolani, R.; Taurino, A.; Catalano, M.; Fiore, A.; Markus, A.; Chen, J.X.; Paranthoën, C.; Oesterle, U.; Ilegems, M.

    2003-01-01

    The authors have studied the radiative and structural properties of identical InxGa(1-x)As quantum dot laser structures grown by metalorg. CVD (MOCVD) and MBE. Despite the comparable emission properties found in the two devices by photoluminescence, electroluminescence, and photocurrent

  16. Study on the fabrication of Al matrix composites strengthened by combined in-situ alumina particle and in-situ alloying elements

    International Nuclear Information System (INIS)

    Huang Zanjun; Yang Bin; Cui Hua; Zhang Jishan

    2003-01-01

    A new idea to fabricate aluminum matrix composites strengthened by combined in-situ particle strengthening and in-situ alloying has been proposed. Following the concept of in-situ alloying and in-situ particle strengthening, aluminum matrix composites reinforced by Cu and α-Al 2 O 3 particulate (material I) and the same matrix reinforced by Cu, Si alloying elements and α-Al 2 O 3 particulate (material II) have been obtained. SEM observation, EDS and XRD analysis show that the alloy elements Cu and Si exist in the two materials, respectively. In-situ Al 2 O 3 particulates are generally spherical and their mean size is less than 0.5 μm. TEM observation shows that the in-situ α-Al 2 O 3 particulates have a good cohesion with the matrix. The reaction mechanism of the Al 2 O 3 particulate obtained by this method was studied. Thermodynamic considerations are given to the in-situ reactions and the distribution characteristic of in-situ the α-Al 2 O 3 particulate in the process of solidification is also discussed

  17. Effects of thermal annealing on C/FePt granular multilayers: in situ and ex situ studies

    International Nuclear Information System (INIS)

    Babonneau, D; Abadias, G; Toudert, J; Girardeau, T; Fonda, E; Micha, J S; Petroff, F

    2008-01-01

    The comprehensive study of C/FePt granular multilayers prepared by ion-beam sputtering at room temperature and subsequent annealing is reported. The as-deposited multilayers consist of carbon-encapsulated FePt nanoparticles (average size ∼3 nm) with a disordered face-centered-cubic structure. The effects of thermal annealing on the structural and magnetic properties are investigated by using dedicated ex situ and in situ techniques, including high-resolution transmission electron microscopy, extended x-ray absorption fine structure, magnetometry, and coupled grazing incidence small-angle x-ray scattering and x-ray diffraction. Our structural data show that the particle size and interparticle distance increase slightly with annealing at temperatures below 790 K by thermally activated migration of Fe and Pt atoms. We find that thermal annealing at temperatures above 870 K results in the dramatic growth of the FePt nanoparticles by coalescence and their gradual L1 0 ordering. In addition, we observe a preferential graphitization of the carbon matrix, which provides protection against oxidation for the FePt nanoparticles. Magnetization measurements indicate that progressive magnetic hardening occurs after annealing. The dependences of the blocking temperature, saturation magnetization, coercivity, and magnetocrystalline anisotropy energy on the annealing temperature are discussed on the basis of the structural data

  18. Treatability Study Report for In SITU Lead Immobilization Using Phosphate-Based Binders

    National Research Council Canada - National Science Library

    Bricka, R. M; Marwaha, Anirudha; Fabian, Gene L

    2008-01-01

    .... The treatability study described in this report was designed to develop the information necessary to support the immobilization of lead contaminants in soil by in situ treatment with phosphate-based binders...

  19. Study of the frequency of translocations and dicentrics in human spermatozoid using fluorescent in situ hybridization

    International Nuclear Information System (INIS)

    Alvarez, R.; Ponsa, I.; Tusell, L.; Genesca, A.; Miro, R.; Egozcue, J.

    1998-01-01

    Present study has intended to analyze the induction translocations and dicentrics in human sperms irradiated in vitro to the dose 4Gy by means of the use technical in situ hybridization with probes marked fluorescently

  20. Exciton dynamics in GaAs/AlxGa1-xAs quantum wells

    DEFF Research Database (Denmark)

    Litvinenko, K.; Birkedal, Dan; Lyssenko, V. G.

    1999-01-01

    The changes induced in the optical absorption spectrum of a GaAs/AlxGa1-xAs multiple quantum well due to a photoexcited carrier distribution are reexamined. We use a femtosecond pump-probe technique to excite excitons and free electron-hole pairs. We find that for densities up to 10(11) cm(-2...

  1. In Situ Raman Study of Liquid Water at High Pressure.

    Science.gov (United States)

    Romanenko, Alexandr V; Rashchenko, Sergey V; Goryainov, Sergey V; Likhacheva, Anna Yu; Korsakov, Andrey V

    2018-06-01

    A pressure shift of Raman band of liquid water (H 2 O) may be an important tool for measuring residual pressures in mineral inclusions, in situ barometry in high-pressure cells, and as an indicator of pressure-induced structural transitions in H 2 O. However, there was no consensus as to how the broad and asymmetric water Raman band should be quantitatively described, which has led to fundamental inconsistencies between reported data. In order to overcome this issue, we measured Raman spectra of H 2 O in situ up to 1.2 GPa using a diamond anvil cell, and use them to test different approaches proposed for the description of the water Raman band. We found that the most physically meaningful description of water Raman band is the decomposition into a linear background and three Gaussian components, associated with differently H-bonded H 2 O molecules. Two of these components demonstrate a pronounced anomaly in pressure shift near 0.4 GPa, supporting ideas of structural transition in H 2 O at this pressure. The most convenient approach for pressure calibration is the use of "a linear background + one Gaussian" decomposition (the pressure can be measured using the formula P (GPa) = -0.0317(3)·Δν G (cm -1 ), where Δν G represents the difference between the position of water Raman band, fitted as a single Gaussian, in measured spectrum and spectrum at ambient pressure).

  2. An in-situ X-ray absorption spectroelectrochemical study of the electroreduction of uranium ions in HCl, HNO{sub 3}, and Na{sub 2}CO{sub 3} solutions

    Energy Technology Data Exchange (ETDEWEB)

    Uehara, Akihiro; Fujii, Toshiyuki; Yamana, Hajimu [Kyoto Univ., Osaka (Japan). Div. of Nuclear Engineering Science; Okamoto, Yoshihiro [Japan Atomic Energy Agency, Ibaraki (Japan). Quantum Beam Science Directorate

    2016-04-01

    A spectroelectrochemical cell was fabricated for in-situ X-ray absorption spectroscopy (in-situ XAS). The XAS spectra of the uranium L{sub III} edge were monitored in electrolyte solutions during the electrochemical reduction. Tetravalent uranium, U{sup 4+}, in 1 mol dm{sup -3} (M) hydrochloric acid (HCl) was electrochemically prepared from hexavalent uranium, UO{sub 2}{sup 2+}, by constant current electrolysis, and the extended X-ray absorption fine structure (EXAFS) was analyzed. The concentration ratio of UO{sub 2}{sup 2+} and U{sup 4+}, which were formed via the disproportionation of pentavalent uranium, UO{sub 2}{sup +}, during the electrolysis, were calculated based on the intensity of the signal for the two axial oxygen atoms in the linear UO{sub 2}{sup 2+} unit, the U-O{sub ax}, bond that had a radial structural function. The apparent redox potential of the UO{sub 2}{sup 2+}/U{sup 4+} couple in 1 M HCl was determined based on the Nernst equation using the concentrations of UO{sub 2}{sup 2+} and U{sup 4+}. The electrode potential was shown to be close to the formal potential of the UO{sub 2}{sup 2+}/UO{sub 2}{sup +} couple as reported previously. This result indicates that the UO{sub 2}{sup +} that was formed electrochemically at the electrode disproportionated to form UO{sub 2}{sup 2+} and U{sup 4+} in the bulk solution. The in-situ XAS of UO{sub 2}{sup 2+} in 0.1 M nitric acid was also performed. The U{sup 4+} that formed was partially re-oxidized to UO{sub 2}{sup 2+} by the NO{sub 3}{sup -} present in the solution. The formation of the UO{sub 2}{sup +} carbonato complex was observed by in-situ XAS in a 1 M sodium carbonate solution during the bulk electrolysis. The edge jump of the X-ray absorption near edge structure (XANES) spectrum shifted from 17.164 to 17.163 keV, and the bond distances of U-O{sub ax} and U-O for CO{sub 3}{sup 2-} increased from 1.78 to 1.88 Aa and from 2.42 to 2.53 Aa, respectively, because of the reduction of the UO{sub 2}{sup 2

  3. In situ anodization of aluminum surfaces studied by x-ray reflectivity and electrochemical impedance spectroscopy

    International Nuclear Information System (INIS)

    Bertram, F.; Evertsson, J.; Messing, M. E.; Mikkelsen, A.; Lundgren, E.; Zhang, F.; Pan, J.; Carlà, F.; Nilsson, J.-O.

    2014-01-01

    We present results from the anodization of an aluminum single crystal [Al(111)] and an aluminum alloy [Al 6060] studied by in situ x-ray reflectivity, in situ electrochemical impedance spectroscopy and ex situ scanning electron microscopy. For both samples, a linear increase of oxide film thickness with increasing anodization voltage was found. However, the slope is much higher in the single crystal case, and the break-up of the oxide film grown on the alloy occurs at a lower anodization potential than on the single crystal. The reasons for these observations are discussed as are the measured differences observed for x-ray reflectivity and electrochemical impedance spectroscopy.

  4. Study on tertiary in-situ leachable uranium mineralization conditions in South Songliao basin

    International Nuclear Information System (INIS)

    Zhang Zhenqiang; Li Guokuan; Zhao Zonghua; Zhang Jingxun

    2001-01-01

    Tertiary in-situ leachable mineralization in Songliao Basin was analyzed in theory in the past. Since 1998, regional investigation at 1:200000 scale has been done with about 120 holes drilled. Based on drill holes recording, section compiling and sample analysis, the authors investigate into the Tertiary in-situ leachable conditions including rock character, sedimentary facies, rock chemistry, organic substances, uranium content, sandstone porosity, sandstone bodies, interlayer oxidation, and hydro-dynamic value. The study would play important role in prospecting for in-situ leachable uranium in South Songliao basin

  5. In situ study of hydrothermal MnO2 formation

    DEFF Research Database (Denmark)

    Birgisson, Steinar; Shen, Yanbin; Iversen, Bo Brummerstedt

    Our group has designed and successfully implemented an experimental setup capable of in situ measurements of solvothermal reactions. The setup uses synchrotron radiation and a time resolution in the range 1-10 seconds can be acquired [1]. The experiments can be optimized either to measure powder X......-ray diffraction (PXRD) data or total scattering (TS) data. From PXRD data properties such as what crystalline phases are present and their weight fractions, structural parameters (e.g. unit cell parameters, site occupancies, bond lengths), crystallite sizes and morphologies are extracted as a function of reaction...... time using Rietveld refinements [2]. TS data gives information about all the material in the solution; from complexes to amorphous particles to crystalline particles. Properties such as bond lengths, scale factors and particle sizes as a function of reaction time can be extracted via real space...

  6. In situ electrochemical atomic force microscope study on graphite electrodes

    Energy Technology Data Exchange (ETDEWEB)

    Hirasawa, K.A.; Sato, Tomohiro; Asahina, Hitoshi; Yamaguchi, Shoji; Mori, Shoichiro [Mitsubishi Chemical Corp., Inashiki, Ibaraki (Japan). Tsukuba Research Center

    1997-04-01

    Interest in the formation of the solid electrolyte interphase (SEI) film on graphite electrodes has increased recently in the quest to improve the performance of lithium-ion batteries. Topographic and frictional changes on the surface of a highly oriented pyrolytic graphite electrode in 1 M LiCiO{sub 4} ethylene carbonate/ethylmethyl carbonate (1:1) electrolyte were examined during charge and discharge by in situ electrochemical atomic force microscopy and friction force microscopy simultaneously in real-time. Solid electrolyte interphase film formation commenced at approximately 2 V vs. Li/Li{sup +} and stable film formation with an island-like morphology was observed below approximately 0.9 V vs. Li/Li{sup +}. Further experiments on a KS-44 graphite/polyvinylidene difluoride binder composite electrode showed similar phenomena.

  7. The effect of hydrogen absorption on the structural, electronic and magnetic properties of the C15 Friauf-Laves phase compounds CeFe2, CeRu2 and LaRu2 : an x-ray absorption spectroscopy (XAS) study

    International Nuclear Information System (INIS)

    Chaboy, J.; Garcia, J.; Marcelli, A.

    1995-08-01

    An x-ray absorption spectroscopy (XAS) investigation of the structural changes occurred upon hydriding in the Friauf-Laves phase compounds CeFe 2 , CeRu 2 and LaRu 2 compounds is presented. The analysis of the extended x-ray absorption spectroscopy (EXAFS) spectra at the L-edges of the rare-earth and at the Fe K-edge indicates that the hydrogenation process leads to the suppression of the long-range crystalline order in all the hydride derivates investigated, as well as the different influence of H 2 in both the rare earth and transition metal sublattices. The correlation between the structural and magnetic changes induced by the hydrogen in the lost matrix is discussed in terms of the modification of the electronic properties, i.e., intermediate-valence of Ce, and of the hybridization between the transition metal and rare-earth

  8. In Situ Study of Thermal Stability of Copper Oxide Nanowires at Anaerobic Environment

    Directory of Open Access Journals (Sweden)

    Lihui Zhang

    2014-01-01

    Full Text Available Many metal oxides with promising electrochemical properties were developed recently. Before those metal oxides realize the use as an anode in lithium ion batteries, their thermal stability at anaerobic environment inside batteries should be clearly understood for safety. In this study, copper oxide nanowires were investigated as an example. Several kinds of in situ experiment methods including in situ optical microscopy, in situ Raman spectrum, and in situ transmission electron microscopy were adopted to fully investigate their thermal stability at anaerobic environment. Copper oxide nanowires begin to transform as copper(I oxide at about 250°C and finish at about 400°C. The phase transformation proceeds with a homogeneous nucleation.

  9. Study of lixiviant damage of a sandstone deposit during in-situ leaching of uranium

    International Nuclear Information System (INIS)

    Liao Wensheng; Wang Limin; Jiang Yan; Jiang Guoping; Tan Yahui

    2014-01-01

    The permeability of sandstone deposit is a key factor for economical uranium recovery during in-situ leaching uranium. Low permeability sandstone uranium deposits behave low push-pull capacity, and show formation damage in leaching operations. It is important to study formation damage of permeability, therefore, and to stabilize even improve the push-pull power of drillholes during in-situ leaching. In this paper, formation damage caused by lixiviants was investigated based on a low permeability sandstone uranium deposit. The resulted showed that, under the conditions of in-situ leaching, the salinity of leaching fluid has no harm to formation permeability, on the contrary, the increment of salinity of lixiviant during in-situ leaching improve the permeability of the deposit. The alkalinity, hydrogen peroxide and productivity of the lixiviant cause no significant formation damage. But the fine particles in the lixiviant shows formation damage significantly, and the quantity of the particles should be controlled during production. (authors)

  10. Setup for in situ x-ray diffraction study of swift heavy ion irradiated materials.

    Science.gov (United States)

    Kulriya, P K; Singh, F; Tripathi, A; Ahuja, R; Kothari, A; Dutt, R N; Mishra, Y K; Kumar, Amit; Avasthi, D K

    2007-11-01

    An in situ x-ray diffraction (XRD) setup is designed and installed in the materials science beam line of the Pelletron accelerator at the Inter-University Accelerator Centre for in situ studies of phase change in swift heavy ion irradiated materials. A high vacuum chamber with suitable windows for incident and diffracted X-rays is integrated with the goniometer and the beamline. Indigenously made liquid nitrogen (LN2) temperature sample cooling unit is installed. The snapshots of growth of particles with fluence of 90 MeV Ni ions were recorded using in situ XRD experiment, illustrating the potential of this in situ facility. A thin film of C60 was used to test the sample cooling unit. It shows that the phase of the C60 film transforms from a cubic lattice (at room temperature) to a fcc lattice at around T=255 K.

  11. Setup for in situ x-ray diffraction study of swift heavy ion irradiated materials

    Science.gov (United States)

    Kulriya, P. K.; Singh, F.; Tripathi, A.; Ahuja, R.; Kothari, A.; Dutt, R. N.; Mishra, Y. K.; Kumar, Amit; Avasthi, D. K.

    2007-11-01

    An in situ x-ray diffraction (XRD) setup is designed and installed in the materials science beam line of the Pelletron accelerator at the Inter-University Accelerator Centre for in situ studies of phase change in swift heavy ion irradiated materials. A high vacuum chamber with suitable windows for incident and diffracted X-rays is integrated with the goniometer and the beamline. Indigenously made liquid nitrogen (LN2) temperature sample cooling unit is installed. The snapshots of growth of particles with fluence of 90MeV Ni ions were recorded using in situ XRD experiment, illustrating the potential of this in situ facility. A thin film of C60 was used to test the sample cooling unit. It shows that the phase of the C60 film transforms from a cubic lattice (at room temperature) to a fcc lattice at around T =255K.

  12. Solid-Phase Fe Speciation along the Vertical Redox Gradients in Floodplains using XAS and Mössbauer Spectroscopies.

    Science.gov (United States)

    Chen, Chunmei; Kukkadapu, Ravi K; Lazareva, Olesya; Sparks, Donald L

    2017-07-18

    Properties of Fe minerals are poorly understood in natural soils and sediments with variable redox conditions. In this study, we combined 57 Fe Mössbauer and Fe K-edge X-ray absorption spectroscopic (XAS) techniques to assess solid-phase Fe speciation along the vertical redox gradients of floodplains, which exhibited a succession of oxic, anoxic, and suboxic-oxic zones with increasing depth along the vertical profiles. The incised stream channel is bounded on the east by a narrow floodplain and a steep hillslope, and on the west by a broad floodplain. In the eastern floodplain, the anoxic conditions at the intermediate horizon (55-80 cm) coincided with lower Fe(III)-oxides (particularly ferrihydrite), in concurrence with a greater reduction of phyllosilicates(PS)-Fe(III) to PS-Fe(II), relative to the oxic near-surface and sandy gravel layers. In addition, the anoxic conditions in the eastern floodplain coincided with increased crystallinity of goethite, relative to the oxic layers. In the most reduced intermediate sediments at 80-120 cm of the western floodplain, no Fe(III)-oxides were detected, concurrent with the greatest PS-Fe(III) reduction (PS-Fe(II)/Fe(III) ratio ≈ 1.2 (Mössbauer) or 0.8 (XAS)). In both oxic near-surface horizon and oxic-suboxic gravel aquifers beneath the soil horizons, Fe(III)-oxides were mainly present as ferrihydrite with a much less amount of goethite, which preferentially occurred as nanogoethite or Al/Si-substituted goethite. Ferrihydrite with varying crystallinity or impurities such as organic matter, Al or Si, persisted under suboxic-oxic conditions in the floodplain. This study indicates that vertical redox gradients exert a major control on the quantity and speciation of Fe(III) oxides as well as the oxidation state of structural Fe in PS, which could significantly affect nutrient cycling and carbon (de)stabilization.

  13. Theory-driven design of high-valence metal sites for water oxidation confirmed using in situ soft X-ray absorption

    Science.gov (United States)

    Zheng, Xueli; Zhang, Bo; de Luna, Phil; Liang, Yufeng; Comin, Riccardo; Voznyy, Oleksandr; Han, Lili; García de Arquer, F. Pelayo; Liu, Min; Dinh, Cao Thang; Regier, Tom; Dynes, James J.; He, Sisi; Xin, Huolin L.; Peng, Huisheng; Prendergast, David; Du, Xiwen; Sargent, Edward H.

    2018-02-01

    The efficiency with which renewable fuels and feedstocks are synthesized from electrical sources is limited at present by the sluggish oxygen evolution reaction (OER) in pH-neutral media. We took the view that generating transition-metal sites with high valence at low applied bias should improve the activity of neutral OER catalysts. Here, using density functional theory, we find that the formation energy of desired Ni4+ sites is systematically modulated by incorporating judicious combinations of Co, Fe and non-metal P. We therefore synthesized NiCoFeP oxyhydroxides and probed their oxidation kinetics with in situ soft X-ray absorption spectroscopy (sXAS). In situ sXAS studies of neutral-pH OER catalysts indicate ready promotion of Ni4+ under low overpotential conditions. The NiCoFeP catalyst outperforms IrO2 and retains its performance following 100 h of operation. We showcase NiCoFeP in a membrane-free CO2 electroreduction system that achieves a 1.99 V cell voltage at 10 mA cm-2, reducing CO2 into CO and oxidizing H2O to O2 with a 64% electricity-to-chemical-fuel efficiency.

  14. Theory-driven design of high-valence metal sites for water oxidation confirmed using in situ soft X-ray absorption.

    Science.gov (United States)

    Zheng, Xueli; Zhang, Bo; De Luna, Phil; Liang, Yufeng; Comin, Riccardo; Voznyy, Oleksandr; Han, Lili; García de Arquer, F Pelayo; Liu, Min; Dinh, Cao Thang; Regier, Tom; Dynes, James J; He, Sisi; Xin, Huolin L; Peng, Huisheng; Prendergast, David; Du, Xiwen; Sargent, Edward H

    2018-02-01

    The efficiency with which renewable fuels and feedstocks are synthesized from electrical sources is limited at present by the sluggish oxygen evolution reaction (OER) in pH-neutral media. We took the view that generating transition-metal sites with high valence at low applied bias should improve the activity of neutral OER catalysts. Here, using density functional theory, we find that the formation energy of desired Ni 4+ sites is systematically modulated by incorporating judicious combinations of Co, Fe and non-metal P. We therefore synthesized NiCoFeP oxyhydroxides and probed their oxidation kinetics with in situ soft X-ray absorption spectroscopy (sXAS). In situ sXAS studies of neutral-pH OER catalysts indicate ready promotion of Ni 4+ under low overpotential conditions. The NiCoFeP catalyst outperforms IrO 2 and retains its performance following 100 h of operation. We showcase NiCoFeP in a membrane-free CO 2 electroreduction system that achieves a 1.99 V cell voltage at 10 mA cm -2 , reducing CO 2 into CO and oxidizing H 2 O to O 2 with a 64% electricity-to-chemical-fuel efficiency.

  15. Miniaturized Environmental Scanning Electron Microscope for In Situ Planetary Studies

    Science.gov (United States)

    Gaskin, Jessica; Abbott, Terry; Medley, Stephanie; Gregory, Don; Thaisen, Kevin; Taylor , Lawrence; Ramsey, Brian; Jerman, Gregory; Sampson, Allen; Harvey, Ralph

    2010-01-01

    The exploration of remote planetary surfaces calls for the advancement of low power, highly-miniaturized instrumentation. Instruments of this nature that are capable of multiple types of analyses will prove to be particularly useful as we prepare for human return to the moon, and as we continue to explore increasingly remote locations in our Solar System. To this end, our group has been developing a miniaturized Environmental-Scanning Electron Microscope (mESEM) capable of remote investigations of mineralogical samples through in-situ topographical and chemical analysis on a fine scale. The functioning of an SEM is well known: an electron beam is focused to nanometer-scale onto a given sample where resulting emissions such as backscattered and secondary electrons, X-rays, and visible light are registered. Raster scanning the primary electron beam across the sample then gives a fine-scale image of the surface topography (texture), crystalline structure and orientation, with accompanying elemental composition. The flexibility in the types of measurements the mESEM is capable of, makes it ideally suited for a variety of applications. The mESEM is appropriate for use on multiple planetary surfaces, and for a variety of mission goals (from science to non-destructive analysis to ISRU). We will identify potential applications and range of potential uses related to planetary exploration. Over the past few of years we have initiated fabrication and testing of a proof-of-concept assembly, consisting of a cold-field-emission electron gun and custom high-voltage power supply, electrostatic electron-beam focusing column, and scanning-imaging electronics plus backscatter detector. Current project status will be discussed. This effort is funded through the NASA Research Opportunities in Space and Earth Sciences - Planetary Instrument Definition and Development Program.

  16. Experimental study on neptunium migration under in situ geochemical conditions

    Science.gov (United States)

    Kumata, M.; Vandergraaf, T. T.

    1998-12-01

    Results are reported for migration experiments performed with Np under in situ geochemical conditions over a range of groundwater flow rates in columns of crushed rock in a specially designed facility at the 240-level of the Underground Research Laboratory (URL) near Pinawa, Manitoba, Canada. This laboratory is situated in an intrusive granitic rock formation, the Lac du Bonnet batholith. Highly altered granitic rock and groundwater were obtained from a major subhorizontal fracture zone at a depth of 250 m in the URL. The granite was wet-crushed and wet-sieved with groundwater from this fracture zone. The 180-850-μm size fraction was selected and packed in 20-cm long, 2.54-cm in diameter Teflon™-lined stainless steel columns. Approximately 30-ml vols of groundwater containing 3HHO and 237Np were injected into the columns at flow rates of 0.3, 1, and 3 ml/h, followed by elution with groundwater, obtained from the subhorizontal fracture, at the same flow rates, for a period of 95 days. Elution profiles for 3HHO were obtained, but no 237Np was detected in the eluted groundwater. After terminating the migration experiments, the columns were frozen, the column material was removed and cut into twenty 1-cm thick sections and each section was analyzed by gamma spectrometry. Profiles of 237Np were obtained for the three columns. A one-dimensional transport model was fitted to the 3HHO breakthrough curves to obtain flow parameters for this experiment. These flow parameters were in turn applied to the 237Np concentration profiles in the columns to produce sorption and dispersion coefficients for Np. The results show a strong dependence of retardation factors ( Rf) on flow rate. The decrease in the retarded velocity of the neptunium ( Vn) varied over one order of magnitude under the geochemical conditions for these experiments.

  17. In-situ synchrotron PXRD study of spinel LiMn2O4 formation

    DEFF Research Database (Denmark)

    Birgisson, Steinar; Jensen, Kirsten Marie Ørnsbjerg; Christiansen, Troels Lindahl

    structural properties for the reaction being studied. Normally the reactions are started by heating and a constant temperature is kept throughout the experiment. In this study the hydrothermal reaction previously shown to produce spinel LiMn2O4 nanoparticles is studied in-situ to learn more about the phase......O4, depending on the initial concentration if Li-ions. An impurity phase, identified as Mn3O4, is also detected in different concentrations depending on reaction time and temperature. We have developed an experimental technique for in-situ measurements of solvothermal reactions under sub...... in the in-situ measurements it gives a unique opportunity to study reaction kinetics and thermodynamic quantities of the reactions. A temperature study of the reaction has been conducted to see how the formation rate and particle growth is affected by temperature while the precursor concentration is kept...

  18. Desorption of hydrogen from magnesium hydride: in-situ electron diffraction study

    International Nuclear Information System (INIS)

    Paik, B.; Jones, I.P.; Walton, A.; Mann, V.; Book, D.; Harris, I.R.

    2009-01-01

    The dynamics of a phase change has been studied where electron beam in Transmission Electron Microscope (TEM) has been used to transform MgH 2 into magnesium. A combination of in-situ Electron Diffraction (ED) and an in-situ Electron Energy Loss Spectroscopy (EELS) study under ED mode describes the phase transformation in terms of, respectively, change in the crystal structure and Plasmon energy shift. The orientation relation [001] MgH2 //[-2110] Mg and (-110) MgH2 //(0001) Mg , obtained from the ED study, has been used to propose a model for the movements of magnesium atoms in the structural change to describe the dynamics of the process. The in-situ EELS study has been compared with the existing H-desorption model. The study aims to describe the sorption dynamics of hydrogen in MgH 2 which is a base material for a number of promising hydrogen storage systems. (author)

  19. Mechanistic studies of chemical looping desulfurization of Mn-based oxides using in situ X-ray absorption spectroscopy

    International Nuclear Information System (INIS)

    König, C.F.J.; Nachtegaal, M.; Seemann, M.; Clemens, F.; Garderen, N. van; Biollaz, S.M.A.; Schildhauer, T.J.

    2014-01-01

    Highlights: • Mn sorbents remove H 2 S from hot syngas in chemical looping desulfurization process. • State of Mn followed by in situ X-ray absorption spectroscopy and mass spectrometry. • Two-step mechanism explains the formation of SO 2 under reducing conditions. - Abstract: Cleaning of producer gas from biomass gasification is required for further processing, e.g. to avoid catalyst poisoning in subsequent conversion steps. High-temperature gas cleaning, of which sulfur removal is an important part, is a promising way to improve the overall efficiency of biomass conversion. In a high temperature “chemical looping desulfurization” process, a sorbent material, here manganese oxide, is cycled between producer gas from the gasifier to remove sulfur species, and an oxidizing atmosphere, in which the sulfur species are released as SO 2 . Alternatively, the use of such material as reactive bed material could be integrated into an allothermal dual fluidized bed gasifier. In a laboratory reactor, we subjected manganese-based materials to a periodically changing gas atmosphere, simulating a “chemical looping desulfurization” reactor. The “fuel reactor” gas contained H 2 , CO, CH 4 and H 2 S, similar as in the producer gas, and the “oxidizing reactor” contained diluted O 2 . Mass spectrometry showed that most of the H 2 S is taken up by the sample in the “fuel reactor” part, while also some unwanted SO 2 is generated in the “fuel reactor” part. Most of the sulfur is released in the oxidizing reactor. Simultaneous in situ X-ray absorption spectroscopy (XAS) of the Mn materials during different stages of the chemical looping desulfurization process showed that the initial Mn 3 O 4 is transformed in the presence of H 2 S to MnS via a MnO intermediate in the fuel reactor. Oxygen from the reduction of Mn 3 O 4 oxidizes some H 2 S to the undesired SO 2 in the fuel reactor. Upon exposure to O 2 , MnS is again oxidized to Mn 3 O 4 via MnO, releasing SO

  20. A Structural Study of Escherichia coli Cells Using an In Situ Liquid Chamber TEM Technology

    Directory of Open Access Journals (Sweden)

    Yibing Wang

    2015-01-01

    Full Text Available Studying cell microstructures and their behaviors under living conditions has been a challenging subject in microbiology. In this work, in situ liquid chamber TEM was used to study structures of Escherichia coli cells in aqueous solutions at a nanometer-scale resolution. Most of the cells remained intact under electron beam irradiation, and nanoscale structures were observed during the TEM imaging. The analysis revealed structures of pili surrounding the E. coli cells; the movements of the pili in the liquid were also observed during the in situ tests. This technology also allowed the observation of features of the nucleoid in the E. coli cells. Overall, in situ TEM can be applied as a valuable tool to study real-time microscopic structures and processes in microbial cells residing in native aqueous solutions.

  1. In Situ PDF Study of the Nucleation and Growth of Intermetallic PtPb Nanocrystals

    DEFF Research Database (Denmark)

    Saha, Dipankar; Bojesen, Espen D.; Mamakhel, Mohammad Aref Hasen

    2017-01-01

    The mechanism of Pt and PtPb nanocrystal formation under supercritical ethanol conditions has been investigated by means of in situ X-ray total scattering and pair distribution function (PDF) analysis. The metal complex structures of two different platinum precursor solutions, chloroplatinic acid...... supercritical ethanol process for obtaining phase-pure hexagonal PtPb nanocrystals. The study thus highlights the importance of in situ studies in revealing atomic-scale information about nucleation mechanisms, which can be used in design of specific synthesis pathways, and the new continuous-flow process...

  2. ''In-situ'' spectro-electrochemical studies of radionuclide-contaminated surface films on metals

    International Nuclear Information System (INIS)

    Melendres, C.A.; Mini, S.; Mansour, A.N.

    2000-01-01

    The incorporation of heavy metal ions and radioactive contaminants into hydrous oxide films has been investigated in order to provide fundamental knowledge that could lead to the technological development of cost-effective processes and techniques for the decontamination of storage tanks, piping systems, surfaces, etc., in DOE nuclear facilities. The formation of oxide/hydroxide films was simulated by electrodeposition onto a graphite substrate from solutions of the appropriate metal salt. Synchrotron X-ray Absorption Spectroscopy (XAS), supplemented by Laser Raman Spectroscopy (LRS), was used to determine the structure and composition of the host oxide film, as well as the impurity ion. Results have been obtained for the incorporation of Ce, Sr, Cr, Fe, and U into hydrous nickel oxide films. Ce and Sr oxides/hydroxides are co-precipitated with the nickel oxides in separate phase domains. Cr and Fe, on the other hand, are able to substitute into Ni lattice sites or intercalate in the interlamellar positions of the brucite structure of Ni(OH) 2 . U was found to co-deposit as a U(VI) hydroxide. The mode of incorporation of metal ions depends both on the size and charge of the metal ion. The structure of iron oxide (hydroxide) films prepared by both anodic and cathodic deposition has also been extensively studied. The structure of Fe(OH) 2 was determined to be similar to that of α-Ni(OH) 2 . Anodic deposition from solutions containing Fe 2+ results in a film with a structure similar to γ-FeOOH. From the knowledge gained from the present studies, principles and methods for decontamination have become apparent. Contaminants sorbed on oxide surfaces or co-precipitated may be removed by acid wash and selective dissolution or complexation. Ions incorporated into lattice sites and interlamellar layers will require more drastic cleaning procedures. Electropolishing and the use of an electrochemical brush are among concepts that should be considered seriously for the latter

  3. Nanoscale size effect in in situ titanium based composites with cell viability and cytocompatibility studies

    Energy Technology Data Exchange (ETDEWEB)

    Miklaszewski, Andrzej, E-mail: andrzej.miklaszewski@put.poznan.pl [Institute of Materials Science and Engineering, Poznan University of Technology, Jana Pawla II 24, 61-138 Poznan (Poland); Jurczyk, Mieczysława U. [Division Mother' s and Child' s Health, Poznan University of Medical Sciences, Polna 33, 60-535 Poznan (Poland); Kaczmarek, Mariusz [Department of Immunology, Chair of Clinical Immunology, Poznan University of Medical Sciences, Rokietnicka 5D, 60-806 Poznan (Poland); Paszel-Jaworska, Anna; Romaniuk, Aleksandra; Lipińska, Natalia [Department of Clinical Chemistry and Molecular Diagnostics, Poznan University of Medical Sciences, Przybyszewskiego 49, 60-355 Poznan (Poland); Żurawski, Jakub [Department of Immunobiochemistry, Chair of Biology and Environmental Sciences, Poznan University of Medical Sciences, Rokietnicka 8, 60-806 Poznan (Poland); Urbaniak, Paulina [Department of Cell Biology, Poznan University of Medical Sciences, Rokietnicka 5D, 60-806 Poznan (Poland); Jurczyk, Mieczyslaw [Institute of Materials Science and Engineering, Poznan University of Technology, Jana Pawla II 24, 61-138 Poznan (Poland)

    2017-04-01

    Novel in situ Metal Matrix Nanocomposite (MMNC) materials based on titanium and boron, revealed their new properties in the nanoscale range. In situ nanocomposites, obtained through mechanical alloying and traditional powder metallurgy compaction and sintering, show obvious differences to their microstructural analogue. A unique microstructure connected with good mechanical properties reliant on the processing conditions favour the nanoscale range of results of the Ti-TiB in situ MMNC example. The data summarised in this work, support and extend the knowledge boundaries of the nanoscale size effect that influence not only the mechanical properties but also the studies on the cell viability and cytocompatibility. Prepared in the same bulk, in situ MMNC, based on titanium and boron, could be considered as a possible candidate for dental implants and other medical applications. The observed relations and research conclusions are transferable to the in situ MMNC material group. Aside from all the discussed relations, the increasing share of these composites in the ever-growing material markets, heavily depends on the attractiveness and a possible wider application of these composites as well as their operational simplicity presented in this work. - Highlights: • Nano and microscale size precursor influence the final composite microstructure and properties. • Obtained from the nanoscale precursor sinters, characterise with a uniform and highly dispersed microstructure • Mechanical properties favoured Nano scale size precursor • Boron addition could be significantly reduced for moderate properties range. • A possible candidate for dental implants and other medical applications.

  4. Spontaneous dispersion of PdO onto acid sites of zeolites studied by in situ DXAFS

    CERN Document Server

    Okumura, K; Niwa, M; Yokota, S; Kato, K; Tanida, H; Uruga, T

    2003-01-01

    The generation of highly dispersed PdO over zeolite supports was studied using in situ energy-dispersive XAFS (DXAFS) technique. From the comparison with the Na-ZSM-5, it was found that the oxidation as well as the spontaneous dispersion of Pd was promoted through the interaction between PdO and acid sites of H-form zeolites. (author)

  5. Coalescence and compression in centrifuged emulsions studied with in situ optical microscopy

    NARCIS (Netherlands)

    Krebs, T.; Ershov, D.S.; Schroën, C.G.P.H.; Boom, R.M.

    2013-01-01

    We report an experimental method to investigate droplet dynamics in centrifuged emulsions and its application to study droplet compression and coalescence. The experimental setup permits in situ monitoring of an ensemble of droplets in a centrifuged monolayer of monodisperse emulsion droplets using

  6. Dynamical In Situ Study of Morphological Changes of Bentonite in ESEM

    Czech Academy of Sciences Publication Activity Database

    Navrátilová, Eva; Neděla, Vilém; Sun, H.; Mašín, D.

    2017-01-01

    Roč. 23, S1 (2017), s. 2196-2197 ISSN 1431-9276 R&D Projects: GA MŠk ED0017/01/01 Institutional support: RVO:68081731 Keywords : ESEM * morphological changes * in situ study Subject RIV: JA - Electronics ; Optoelectronics, Electrical Engineering OBOR OECD: Geology Impact factor: 1.891, year: 2016

  7. Surface phenomena revealed by in situ imaging: studies from adhesion, wear and cutting

    Science.gov (United States)

    Viswanathan, Koushik; Mahato, Anirban; Yeung, Ho; Chandrasekar, Srinivasan

    2017-03-01

    Surface deformation and flow phenomena are ubiquitous in mechanical processes. In this work we present an in situ imaging framework for studying a range of surface mechanical phenomena at high spatial resolution and across a range of time scales. The in situ framework is capable of resolving deformation and flow fields quantitatively in terms of surface displacements, velocities, strains and strain rates. Three case studies are presented demonstrating the power of this framework for studying surface deformation. In the first, the origin of stick-slip motion in adhesive polymer interfaces is investigated, revealing a intimate link between stick-slip and surface wave propagation. Second, the role of flow in mediating formation of surface defects and wear particles in metals is analyzed using a prototypical sliding process. It is shown that conventional post-mortem observation and inference can lead to erroneous conclusions with regard to formation of surface cracks and wear particles. The in situ framework is shown to unambiguously capture delamination wear in sliding. Third, material flow and surface deformation in a typical cutting process is analyzed. It is shown that a long-standing problem in the cutting of annealed metals is resolved by the imaging, with other benefits such as estimation of energy dissipation and power from the flow fields. In closure, guidelines are provided for profitably exploiting in situ observations to study large-strain deformation, flow and friction phenomena at surfaces that display a variety of time-scales.

  8. Direct Observations of Oxygen-induced Platinum Nanoparticle Ripening Studied by In Situ TEM

    DEFF Research Database (Denmark)

    Simonsen, Søren Bredmose; Chorkendorff, Ib; Dahl, Søren

    2010-01-01

    This study addresses the sintering mechanism of Pt nanoparticles dispersed on a planar, amorphous Al2O3 support as a model system for a catalyst for automotive exhaust abatement. By means of in situ transmission electron microscopy (TEM), the model catalyst was monitored during the exposure to 10...

  9. Development of equipment for in situ studies of biofilm in hot water systems

    DEFF Research Database (Denmark)

    Bagh, Lene Karen; Albrechtsen, Hans-Jørgen; Arvin, Erik

    1999-01-01

    New equipment was developed for in situ studies of biofilms in hot water tanks and hot water pipes under normal operation and pressure. Sampling ports were installed in the wall of a hot water tank and through these operating shafts were inserted with a test plug in the end. The surface of the test...

  10. In-situ TEM Studies : Heat-treatment and Corrosion

    NARCIS (Netherlands)

    Malladi, S.R.K.

    2014-01-01

    Transmission electron microscopy (TEM) has been well known as a powerful characterisation tool to understand the structure and composition of various materials down to the atomic level. Over the years, several TEM studies have been carried out to understand the compositional, structural and

  11. In-situ TEM studies of microstructure evolution under ion irradiation for nuclear engineering applications

    International Nuclear Information System (INIS)

    Kaoumi, D.

    2011-01-01

    One of the difficulties of studying processes occurring under irradiation (in a reactor environment) is the lack of kinetics information since usually samples are examined ex situ (i.e. after irradiation) so that only snapshots of the process are available. Given the dynamic nature of the phenomena, direct in situ observation is invaluable for better understanding the mechanisms, kinetics and driving forces of the processes involved. This can be done using in situ ion irradiation in a TEM at the IVEM facility at Argonne National Laboratory which, in the USA, is a unique facility. To predict the in reactor behavior of alloys, it is essential to understand the basic mechanisms of radiation damage formation (loop density, defect interactions) and accumulation (loop evolution, precipitation or dissolution of second phases etc.). In-situ Ion-irradiation in a TEM has proven a very good tool for that purpose as it allows for the direct determination of the formation and evolution of irradiation-induced damage and the spatial correlation of the defect structures with the pre-existing microstructure (including lath boundaries, network dislocations and carbides) as a function of dose, dose rate, temperature and ion type. Using this technique, different aspects of microstructure evolution under irradiation were studied, such as defect cluster formation and evolution as a function of dose in advanced Ferritic/Martensitic (F/M) steels, the irradiation stability of precipitates in Oxide Dispersion Strengthened (ODS) steels, and irradiation-induced grain-growth. Such studies will be reported in this presentation

  12. A new cryostat for 'in situ' radiation damage studies

    International Nuclear Information System (INIS)

    Hariharan, Y.; Radhakrishnan, T.S.

    1977-01-01

    Conventional cryostats to study properties of materials between 4deg K and 300deg K base their designs either on continuous flow or bath type. A new cryostat which incorporates the advantages of both these has been designed and fabricated. This essentially has three chambers isolated from each other by poor thermal links. These are enclosed in a vacuum chamber and the whole assembly is immersed in a 4 He bath. The lowermost chamber is kept in good thermal contact with the bath. The second chamber can be maintained between 4deg K and 77deg K by circulation of cold 4 He vapour. The uppermost chamber can be maintained between 77deg K and 300deg K by circulating cold nitrogen vapours. There is a through axial hole in the centre, through which the sample can be moved up and down by means of a thin walled stainless steel tube. This comes out from the top of the cryostat through a Wilson seal. Thus the specimen can be anchored in any of the three chambers. This cryostat can be used to study the radiation damages caused by α-particles the sample being kept at 4.2deg K. There is provision for isolating the sample from the radiation zone. Isothermal and isochronal annealing of the damage caused can also be studied. Provision for taking out electrical leads from both inside and outside the sample chamber are also there. (auth.)

  13. Cost studies of thermally enhanced in situ soil remediation technologies

    International Nuclear Information System (INIS)

    Bremser, J.; Booth, S.R.

    1996-05-01

    This report describes five thermally enhanced technologies that may be used to remediate contaminated soil and water resources. The standard methods of treating these contaminated areas are Soil Vapor Extraction (SVE), Excavate ampersand Treat (E ampersand T), and Pump ampersand Treat (P ampersand T). Depending on the conditions at a given site, one or more of these conventional alternatives may be employed; however, several new thermally enhanced technologies for soil decontamination are emerging. These technologies are still in demonstration programs which generally are showing great success at achieving the expected remediation results. The cost savings reported in this work assume that the technologies will ultimately perform as anticipated by their developers in a normal environmental restoration work environment. The five technologies analyzed in this report are Low Frequency Heating (LF or Ohmic, both 3 and 6 phase AC), Dynamic Underground Stripping (DUS), Radio Frequency Heating (RF), Radio Frequency Heating using Dipole Antennae (RFD), and Thermally Enhanced Vapor Extraction System (TEVES). In all of these technologies the introduction of heat to the formation raises vapor pressures accelerating contaminant evaporation rates and increases soil permeability raising diffusion rates of contaminants. The physical process enhancements resulting from temperature elevations permit a greater percentage of volatile organic compound (VOC) or semi- volatile organic compound (SVOC) contaminants to be driven out of the soils for treatment or capture in a much shorter time period. This report presents the results of cost-comparative studies between these new thermally enhanced technologies and the conventional technologies, as applied to five specific scenarios

  14. Nanoindentation studies of ex situ AlN/Al metal matrix nanocomposites

    International Nuclear Information System (INIS)

    Fale, Sandeep; Likhite, Ajay; Bhatt, Jatin

    2014-01-01

    Highlights: • Formation of in-situ phases nucleated on AlN particles strengthens the matrix. • Formation of in-situ phases increases with AlN content in nanocomposites. • Stronger in-situ phases results in increased hardness and modulus of elasticity. - Abstract: Nanocrystalline Aluminium nitride (AlN) powder is dispersed in different weight ratio in Aluminum matrix to fabricate metal matrix nanocomposite (MMNC) using ex situ melt metallurgy process. The synthesized Al–AlN nanocomposites are studied for phase analysis using high resolution scanning electron microscopy (FEG-SEM) and for hardness behavior using microindentation and nanoindentation tests. Quantitative analysis of the oxide phases is calculated from thermodynamic data and mass balance equation using elemental data obtained from energy dispersive spectroscopy (EDS) results. Role of oxide phases in association with AlN particles is investigated to understand the mechanical behavior of composites using nanoindentation tester. Load–displacement profile obtained from nanoindentation test reveals distribution of oxide phases along with AlN particle and their effect on indent penetration

  15. Auger recombination in p-type InAs and in Gasub(x)Insub(1-x)As solid solutions

    International Nuclear Information System (INIS)

    Zotova, N.V.; Yassievich, I.N.

    1977-01-01

    The probability of the Auger recombination in p-type semiconductors, which is accompanied by transition of the second hole into the zone, splitted by spin-orbital interaction, was calculated. The above process is effective when the energy of spin-orbital splitting off Δ is close to the forbidden zone energy Esub(g), which takes place in the case of InAs, GaSb and solid solutions based on these compounds. The calculation is performed for the non-degenerate hole gas at a finite difference of Esub(g) - Δ. By means of the study of radiative recombination in InAs and Gasub(x)Insub(1-x)As solid solutions with small contents of GaAs (0 17 cm -3 . It is found that the quantum yield of radiative recombination increases sharply in Gasub(x)Insub(1-x)As solid solutions with the increase of x, which is associated with the increase of the difference of Esub(g) - Δ; the radiative recombination intensity increases in correspondence with the theoretical calculation made

  16. Dispersive XAS on a High Brilliance Source: Highlights and Future Opportunities

    International Nuclear Information System (INIS)

    Pascarelli, S.; Aquilanti, G.; Guilera, G.; Mathon, O.; Newton, M. A.; Trapananti, A.; Dubrovinsky, L.; Munoz, M.; Pasquale, M.

    2007-01-01

    Energy Dispersive X-ray Absorption Spectroscopy is a now a well-established method which has been applied to a broad range of applications. Ten years from the construction of beamline ID24 at the ESRF, the first dispersive XAS spectrometer using undulator radiation on a third generation source, we report an overview of recent results in very diverse fields of research, ranging from automotive catalysts to magnetism at extreme conditions. We also illustrate how pushing the instrument to its limits has opened new opportunities, such as an enhanced sensitivity to detection of tiny atomic displacements and the potential for micro-probe redox and speciation imaging

  17. Materials testing for in situ stabilization treatability study of INEEL mixed wastes soils

    International Nuclear Information System (INIS)

    Heiser, J.; Fuhrmann, M.

    1997-09-01

    This report describes the contaminant-specific materials testing phase of the In Situ Stabilization Comprehensive Environment Response, Compensation, and Liability Act (CERCLA) Treatability Study (TS). The purpose of materials testing is to measure the effectiveness of grouting agents to stabilize Idaho National Engineering and Environmental Laboratory (INEEL) Acid Pit soils and select a grout material for use in the Cold Test Demonstration and Acid Pit Stabilization Treatability Study within the Subsurface Disposal Area (SDA) at the Radioactive Waste Management Complex (RWMC). Test results will assist the selecting a grout material for the follow-on demonstrations described in Test Plan for the Cold Test Demonstration and Acid Pit Stabilization Phases of the In Situ Stabilization Treatability Study at the Radioactive Waste Management Complex

  18. Ex-Situ and In-Situ Ellipsometric Studies of the Thermal Oxide on InP

    Science.gov (United States)

    1990-12-06

    ion---- Distribution/ Availabilit ? Codes£v l llt Codes Avail and/or Dist| Special Abstract The thermally grown InP oxide as etched by an aqueous...aqueous NH4OH/NH4F, and Law(17) has reported observations of orientational ordering of water and organic solvents on pyrex surfaces by in-situ...minutes, followed by a sequence of acetone, deionized water (d. i. water ) rinse. After being dipped in a concentrated aqueous HF solution for 15 seconds

  19. In situ NMR and modeling studies of nitroxide mediated copolymerization of styrene and n-butyl acrylate

    NARCIS (Netherlands)

    Hlalele, L.; Klumperman, L.

    2011-01-01

    The combination of in situ1H NMR and in situ31P NMR was used to study the nitroxide mediated copolymerization of styrene and n-butyl acrylate. The alkoxyamine MAMA-DEPN was employed to initiate and mediate the copolymerization. The nature of the ultimate/terminal monomer units of dormant polymer

  20. In Situ X-ray Diffraction Studies of Cathode Materials in Lithium Batteries

    International Nuclear Information System (INIS)

    Yang, X. Q.; Sun, X.; McBreen, J.; Mukerjee, S.; Gao, Yuan; Yakovleva, M. V.; Xing, X. K.; Daroux, M. L.

    1998-01-01

    There is an increasing interest in lithiated transition metal oxides because of their use as cathodes in lithium batteries. LiCoO 2 , LiNiO 2 and LiMn 2 O 4 are the three most widely used and studied materials, At present, although it is relative expensive and toxic, LiCoO 2 is the material of choice in commercial lithium ion batteries because of its ease of manufacture, better thermal stability and cycle life. However, the potential use of lithium ion batteries with larger capacity for power tools and electric vehicles in the future will demand new cathode materials with higher energy density, lower cost and better thermal stability. LiNiO 2 is isostructural with LiCoO 2 . It offers lower cost and high energy density than LiCoO 2 . However, it has much poorer thermal stability than LiCoO 2 , in the charged (delithiated) state. Co, Al, and other elements have been used to partially replace Ni in LiNiO 2 system in order to increase the thermal stability. LiMn 2 O 4 has the highest thermal stability and lowest cost and toxicity. However, the low energy density and poor cycle life at elevated temperature are the major obstacles for this material. In order to develop safer, cheaper, and better performance cathode materials, the in-depth understanding of the relationships between the thermal stability and structure, performance and structure are very important. The performance here includes energy density and cycle life of the cathode materials. X-ray diffraction (XRD) is one of the most powerful tools to study these relationships. The pioneer ex situ XRD work on cathode materials for lithium batteries was done by Ohzuku. His XRD studies on LiMn 2 O 4 , LiCoO 2 , LiNiO 2 , LiNi 0.5 Co 0.5 O 2 , and LiAl x Ni 1-x O 2 cathodes at different states of charge have provided important guidelines for the development of these new materials. However, the kinetic nature of the battery system definitely requires an in situ XRD technique to study the detail structural changes of the

  1. Demonstration testing and evaluation of in situ soil heating. Treatability study work plan (Revision 2)

    International Nuclear Information System (INIS)

    Sresty, G.C.

    1994-01-01

    A Treatability Study planned for the demonstration of the in situ electromagnetic (EM) heating process to remove organic solvents is described in this Work Plan. The treatability study will be conducted by heating subsurface vadose-zone soils in an organic plume adjacent to the Classified Burial Ground K-1070-D located at K-25 Site, Oak Ridge. The test is scheduled to start during the fourth quarter of FY94 and will be completed during the first quarter of FY95. Over the last nine years, a number of Government agencies (EPA, Army, AF, and DOE) and industries sponsored further development and testing of the in situ heating and soil decontamination process for the remediation of soils containing hazardous organic contaminants. In this process the soil is heated in situ using electrical energy. The contaminants are removed from the soil due to enhanced vaporization, steam distillation and stripping. IITRI will demonstrate the EM Process for in situ soil decontamination at K-25 Site under the proposed treatability study. Most of the contaminants of concern are volatile organics which can be removed by heating the soil to a temperature range of 85 degrees to 95 degrees C. The efficiency of the treatment will be determined by comparing the concentration of contaminants in soil samples. Samples will be obtained before and after the demonstration for a measurement of the concentration of contaminants of concern. This document is a Treatability Study Work Plan for the demonstration program. The document contains a description of the proposed treatability study, background of the EM heating process, description of the field equipment, and demonstration test design

  2. Irradiation-related amorphization and crystallization: In situ transmission electron microscope studies

    International Nuclear Information System (INIS)

    Allen, C.W.

    1994-01-01

    Interfacing an ion accelerator to a transmission electron microscope (TEM) allows the analytical functions of TEM imaging and diffraction to be employed during ion-irradiation effects studies. At present there are twelve such installations in Japan, one in France and one in the US. This paper treats several aspects of in situ studies involving electron and ion beam induced and enhanced phase transformations and presents results of several in situ experiments to illustrate the dynamics of this approach in the materials science of irradiation effects. The paper describes the ion- and electron-induced amorphization of CuTi; the ion-irradiation-enhanced transformation of TiCr 2 ; and the ion- and electron-irradiation-enhanced crystallization of CoSi 2

  3. A flow-through hydrothermal cell for in situ neutron diffraction studies of phase transformations

    International Nuclear Information System (INIS)

    O'Neill, Brian; Tenailleau, Christophe; Nogthai, Yung; Studer, Andrew; Brugger, Joel; Pring, Allan

    2006-01-01

    A flow-through hydrothermal cell for the in situ neutron diffraction study of crystallisation and phase transitions has been developed. It can be used for kinetic studies on materials that exhibit structural transformations under hydrothermal conditions. It is specifically designed for use on the medium-resolution powder diffractometer (MRPD) at ANSTO, Lucas Heights, Sydney. But it is planned to adapt the design for the Polaris beamline at ISIS and the new high-intensity powder diffractometer (Wombat) at the new Australian reactor Opal. The cell will operate in a flow-through mode over the temperature range from 25-300 deg. C and up to pressures of 100 bar. The first results of a successful transformation of pentlandite (Fe,Ni) 9 S 8 to violarite (Fe,Ni) 3 S 4 under mild conditions (pH∼4) at 120 deg. C and 3 bar using in situ neutron diffraction measurements are presented

  4. Rotating cell for in situ Raman spectroelectrochemical studies of photosensitive redox systems.

    Science.gov (United States)

    Kavan, Ladislav; Janda, Pavel; Krause, Matthias; Ziegs, Frank; Dunsch, Lothar

    2009-03-01

    A recently developed rotating spectroelectrochemical cell for in situ Raman spectroscopic studies of photoreactive compounds without marked decomposition of the sample is presented. Photochemically and thermally sensitive redox systems are difficult to be studied under stationary conditions by in situ spectroelectrochemistry using laser excitation as in Raman spectroscopy. A rotating spectroelectrochemical cell can circumvent these difficulties. It can be used for any type of a planar electrode and for all electrode materials in contact with aqueous or nonaqueous solutions as well as with ionic liquids. The innovative technical solution consists of the precession movement of the spectroelectrochemical cell using an eccentric drive. This precession movement allows a fixed electrical connection to be applied for interfacing the electrochemical cell to a potentiostat. Hence, any electrical imperfections and noise, which would be produced by sliding contacts, are removed. A further advantage of the rotating cell is a dramatic decrease of the thermal load of the electrochemical system. The size of the spectroelectrochemical cell is variable and dependent on the thickness of the cuvettes used ranging up to approximately 10 mm. The larger measuring area causes a higher sensitivity in the spectroscopic studies. The as constructed spectroelectrochemical cell is easy to handle. The performance of the cell is demonstrated for ordered fullerene C(60) layers and the spectroelectrochemical behavior of nanostructured fullerenes. Here the charge transfer at highly ordered fullerene C(60) films was studied by in situ Raman spectroelectrochemistry under appropriate laser power and accumulation time without marked photodecomposition of the sample.

  5. Coarsening of Pd nanoparticles in an oxidizing atmosphere studied by in situ TEM

    DEFF Research Database (Denmark)

    Simonsen, Søren Bredmose; Chorkendorff, Ib; Dahl, Søren

    2016-01-01

    The coarsening of supported palladium nanoparticles in an oxidizing atmosphere was studied in situ by means of transmission electron microscopy (TEM). Specifically, the Pd nanoparticles were dispersed on a planar and amorphous Al2O3 support and were observed during the exposure to 10 mbar technical...... for the Ostwald ripening process indicates that the observed change in the particle size distribution can be accounted for by wetting of the Al2O3 support by the larger Pd nanoparticles....

  6. Studying the Kinetics of Crystalline Silicon Nanoparticle Lithiation with In Situ Transmission Electron Microscopy

    KAUST Repository

    McDowell, Matthew T.

    2012-09-04

    In situ transmission electron microscopy (TEM) is used to study the electrochemical lithiation of high-capacity crystalline Si nanoparticles for use in Li-ion battery anodes. The lithiation reaction slows down as it progresses into the particle interior, and analysis suggests that this behavior is due not to diffusion limitation but instead to the influence of mechanical stress on the driving force for reaction. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. In Situ Raman Spectroscopy of Supported Chromium Oxide Catalysts: Reactivity Studies with Methanol and Butane

    NARCIS (Netherlands)

    Weckhuysen, B.M.; Wachs, I.E.

    1996-01-01

    The interactions of methanol and butane with supported chromium oxide catalysts under oxidizing and reducing conditions were studied by in situ Raman spectroscopy as a function of the specific oxide support (Al2O3, ZrO2, TiO2, SiO2, Nb2O5, 3% SiO2/TiO2, 3% TiO2/SiO2, and a physical mixture of SiO2

  8. Autoradiographic study of transcription during early germination of Zea mays embryos maintained in situ

    International Nuclear Information System (INIS)

    Deltour, Roger

    1979-01-01

    Recovery of RNA synthesis was studied by autoradiography in primary root of Zea mays embryos germinating at 16 0 C. [H 3 ] uridine was provided to embryos maintained in situ. During the first 4hrs of germination the cell radioactivity is located almost exclusively in the extranucleolar chromatin. These observations agree well with previous results obtained when [H 3 ] uridine was provided to isolated embryos [fr

  9. Studying the Kinetics of Crystalline Silicon Nanoparticle Lithiation with In Situ Transmission Electron Microscopy

    KAUST Repository

    McDowell, Matthew T.; Ryu, Ill; Lee, Seok Woo; Wang, Chongmin; Nix, William D.; Cui, Yi

    2012-01-01

    In situ transmission electron microscopy (TEM) is used to study the electrochemical lithiation of high-capacity crystalline Si nanoparticles for use in Li-ion battery anodes. The lithiation reaction slows down as it progresses into the particle interior, and analysis suggests that this behavior is due not to diffusion limitation but instead to the influence of mechanical stress on the driving force for reaction. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. In situ atomic force microscopy in the study of electrogeneration of polybithiophene on Pt electrode

    International Nuclear Information System (INIS)

    Innocenti, M.; Loglio, F.; Pigani, L.; Seeber, R.; Terzi, F.; Udisti, R.

    2005-01-01

    Electrochemical AFM technique has been used for the in situ study of the electrogeneration-deposition process of polybithiophene at varying the polymerisation conditions, such as supporting electrolyte, i.e., LiClO 4 or tetrabutylammonium hexafluorophosphate, and polymerisation procedure, i.e., either potentiostatic or potentiodynamic method. In order to better follow the evolution of the morphology of the deposit, particularly during the early stages of the polymer film growth, a suitable home-made electrochemical cell has been used

  11. Flexible metal-organic framework compounds: In situ studies for selective CO{sub 2} capture

    Energy Technology Data Exchange (ETDEWEB)

    Allen, A.J., E-mail: andrew.allen@nist.gov [Material Measurement Laboratory, National Institute of Standards and Technology (NIST), Gaithersburg, MD 20899-8520 (United States); Espinal, L.; Wong-Ng, W. [Material Measurement Laboratory, National Institute of Standards and Technology (NIST), Gaithersburg, MD 20899-8520 (United States); Queen, W.L. [NIST Center for Neutron Research, Gaithersburg, MD 20899-6102 (United States); The Molecular Foundry, Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA 94720 (United States); Brown, C.M. [NIST Center for Neutron Research, Gaithersburg, MD 20899-6102 (United States); Department of Chemical and Biomolecular Engineering, University of Delaware, Newark, DE 19716 (United States); Kline, S.R. [NIST Center for Neutron Research, Gaithersburg, MD 20899-6102 (United States); Kauffman, K.L. [National Energy Technology Laboratory (NETL), US Department of Energy, Pittsburgh, PA 15236 (United States); Culp, J.T. [National Energy Technology Laboratory (NETL), US Department of Energy, Pittsburgh, PA 15236 (United States); URS Corporation, South Park, PA 15219 (United States); Matranga, C. [National Energy Technology Laboratory (NETL), US Department of Energy, Pittsburgh, PA 15236 (United States)

    2015-10-25

    Results are presented that explore the dynamic structural changes occurring in two highly flexible nanocrystalline metal-organic framework (MOF) compounds during the adsorption and desorption of pure gases and binary mixtures. The Ni(1,2-bis(4-pyridyl)ethylene)[Ni(CN){sub 4}] and catena-bis(dibenzoylmethanato)-(4,4′-bipyridyl)nickel(II) chosen for this study are 3-D and 1-D porous coordination polymers (PCP) with a similar gate opening pressure response for CO{sub 2} isotherms at 303 K, but with differing degrees of flexibility for structural change to accommodate guest molecules. As such, they serve as a potential model system for evaluating the complex kinetics associated with dynamic structure changes occurring in response to gas adsorption in flexible MOF systems. Insights into the crystallographic changes occurring as the MOF pore structure expands and contracts in response to interactions with CO{sub 2}, N{sub 2}, and CO{sub 2}/N{sub 2} mixtures have been obtained from in situ small-angle neutron scattering and neutron diffraction, combined with ex situ X-ray diffraction structure measurements. The role of structure in carbon capture functionality is discussed with reference to the ongoing characterization challenges and a possible materials-by-design approach. - Graphical abstract: We present in situ small-angle neutron scattering results for two flexible metal-organic frameworks (MOFs). The figure shows that for one (NiBpene, high CO{sub 2} adsorption) the intensity of the Bragg peak for the expandable d-spacing most associated with CO{sub 2} adsorption varies approximately with the isotherm, while for the other (NiDBM-Bpy, high CO{sub 2} selectivity) the d-spacing, itself, varies with the isotherm. The cartoons show the proposed modes of structural change. - Highlights: • Dynamic structures of two flexible MOF CO{sub 2} sorbent compounds are compared in situ. • These porous solid sorbents serve as models for pure & dual gas adsorption. • Different

  12. The application of in situ analytical transmission electron microscopy to the study of preferential intergranular oxidation in Alloy 600

    Energy Technology Data Exchange (ETDEWEB)

    Burke, M.G., E-mail: m.g.burke@manchester.ac.uk; Bertali, G.; Prestat, E.; Scenini, F.; Haigh, S.J.

    2017-05-15

    In situ analytical transmission electron microscopy (TEM) can provide a unique perspective on dynamic reactions in a variety of environments, including liquids and gases. In this study, in situ analytical TEM techniques have been applied to examine the localised oxidation reactions that occur in a Ni-Cr-Fe alloy, Alloy 600, using a gas environmental cell at elevated temperatures. The initial stages of preferential intergranular oxidation, shown to be an important precursor phenomenon for intergranular stress corrosion cracking in pressurized water reactors (PWRs), have been successfully identified using the in situ approach. Furthermore, the detailed observations correspond to the ex situ results obtained from bulk specimens tested in hydrogenated steam and in high temperature PWR primary water. The excellent agreement between the in situ and ex situ oxidation studies demonstrates that this approach can be used to investigate the initial stages of preferential intergranular oxidation relevant to nuclear power systems. - Highlights: • In situ analytical TEM has been performed in 1 bar H{sub 2}-H{sub 2}O vapor at 360–480 °C. • Nanoscale GB migration and solute partitioning correlate with ex situ data for Alloy 600 in H{sub 2}-steam. • This technique can provide new insights into localised reactions associated with localised oxidation.

  13. Demonstration testing and evaluation of in situ soil heating. Treatability study work plan, Revision 1

    Energy Technology Data Exchange (ETDEWEB)

    Sresty, G.C.

    1994-07-07

    A Treatability Study planned for the demonstration of the in situ electromagnetic (EM) heating process to remove organic solvents is described in this Work Plan. The treatability study will be conducted by heating subsurface vadose-zone soils in an organic plume adjacent to the Classified Burial Ground K-1070-D located at K-25 Site, Oak Ridge. The test is scheduled to start during the fourth quarter of FY94 and will be completed during the first quarter of FY95. The EM heating process for soil decontamination is based on volumetric heating technologies developed during the `70s for the recovery of fuels from shale and tar sands by IIT Research Institute (IITRI) under a co-operative program with the US Department of Energy (DOE). Additional modifications of the technology developed during the mid `80s are currently used for the production of heavy oil and waste treatment. Over the last nine years, a number of Government agencies (EPA, Army, AF, and DOE) and industries sponsored further development and testing of the in situ heating and soil decontamination process for the remediation of soils containing hazardous organic contaminants. In this process the soil is heated in situ using electrical energy. The contaminants are removed from the soil due to enhanced vaporization, steam distillation and stripping. IITRI will demonstrate the EM Process for in situ soil decontamination at K-25 Site under the proposed treatability study. Most of the contaminants of concern are volatile organics which can be removed by heating the soil to a temperature range of 85 to 95 C. The efficiency of the treatment will be determined by comparing the concentration of contaminants in soil samples. Samples will be obtained before and after the demonstration for a measurement of the concentration of contaminants of concern.

  14. In-situ oxidation study of Pd(100) by surface x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Kilic, Volkan; Franz, Dirk; Stierle, Andreas [AG Grenzflaechen, Universitaet Siegen (Germany); Martin, Natalia; Lundgren, Edvin [Department of Synchrotron Radiation Research, Lund University (Sweden); Mantilla, Miguel [MPI fuer Metallforschung, Stuttgart (Germany)

    2011-07-01

    The oxidation of the Pd(100) surface at oxygen pressures in the 10{sup -6} mbar to 10{sup 3} mbar range and temperatures up to 1000 K has been studied in-situ by surface x-ray diffraction (SXRD). The SXRD experiments were performed at the MPI beamline at the Angstrom Quelle Karlsruhe (ANKA). We present the surface and crystal truncation rod (CTR) data from the ({radical}(5) x {radical}(5)) surface layer. We show that the transformation from the surface oxide to PdO bulk oxide can be observed in-situ under specific pressure and temperature conditions. We compare our results with previously proposed structure models based on low energy electron diffraction (LEED) I(V) curves and density functional theory calculations. Finally, we elucidate the question of commensurability of the surface oxide layer with respect to the Pd(100) substrate.

  15. A case study of in situ oil contamination in a mangrove swamp (Rio De Janeiro, Brazil).

    Science.gov (United States)

    Brito, Elcia M S; Duran, Robert; Guyoneaud, Rémy; Goñi-Urriza, Marisol; García de Oteyza, T; Crapez, Miriam A C; Aleluia, Irene; Wasserman, Julio C A

    2009-08-01

    Mangroves are sensitive ecosystems of prominent ecological value that lamentably have lost much of their areas across the world. The vulnerability of mangroves grown in proximity to cities requires the development of new technologies for the remediation of acute oil spills and chronic contaminations. Studies on oil remediation are usually performed with in vitro microcosms whereas in situ experiments are rare. The aim of this work was to evaluate oil degradation on mangrove ecosystems using in situ microcosms seeded with an indigenous hydrocarbonoclastic bacterial consortium (HBC). Although the potential degradation of oil through HBC has been reported, their seeding directly on the sediment did not stimulate oil degradation during the experimental period. This is probably due to the availability of carbon sources that are easier to degrade than petroleum hydrocarbons. Our results emphasize the fragility of mangrove ecosystems during accidental oil spills and also the need for more efficient technologies for their remediation.

  16. Study on underground-water restoration of acid in-situ leaching process with electrodialytic desalination

    International Nuclear Information System (INIS)

    Huang Chongyuan; Meng Jin; Li Weicai

    2003-01-01

    The study focus undergrounder water restoration of acid in-situ leaching process with electrodialysis desalination in Yining Uranium Mine. It is shown in field test that electrodialysis desalination is an effective method for underground water restoration of acid in-situ leaching process. When TDS of underground-water at the decommissioning scope is 10-12 g/L, and TDS will be less than 1 g/L after the desalination process, the desalination rate is more than 90%, freshwater recovery 60%-70%, power consumption for freshwater recovery 5 kW·h/m 3 , the distance of the desalination flow 12-13 m, current efficiency 80%, and the throughput of the twin membrane 0.22-0.24 m 3 /(m 2 ·d)

  17. Compositional Simulation of In-Situ Combustion EOR: A Study of Process Characteristics

    DEFF Research Database (Denmark)

    Jain, Priyanka; Stenby, Erling Halfdan; von Solms, Nicolas

    2010-01-01

    In order to facilitate the study of the influence of reservoir process characteristics in In-Situ combustion modeling and advance the work of Kristensen et al. in this domain; a fully compositional In-situ combustion (ISC) model of Virtual Kinetic Cell (VKC; single-cell model) for laboratory scale....... This incorporates fourteen pseudo components and fourteen reactions (distributed amongst thermal cracking, low temperature oxidation and high temperature oxidation). The paper presents a set of derivative plots indicating that reservoir process characterization in terms of thermal behavior of oil can be well...... construed in terms of thermo-oxidative sensitivity of SARA fractions. It can be interpreted from the results that operating parameters like air injection rate, oxygen feed concentration and activation energy have significant influence on oil recovery; an increase in air injection rate can lead to cooling...

  18. XAS and XRF investigation of an actual HAWC glass fragment obtained from the Karlsruhe vitrification plant (VEK)

    Science.gov (United States)

    Dardenne, K.; González-Robles, E.; Rothe, J.; Müller, N.; Christill, G.; Lemmer, D.; Praetorius, R.; Kienzler, B.; Metz, V.; Roth, G.; Geckeis, H.

    2015-05-01

    Several sections of HAWC glass rods remaining at the end of glass pouring at the Karlsruhe Vitrification Plant (VEK) were retained during vitrification operation in 2009-2010 and transferred to the KIT-INE shielded box line for later glass product characterization. A mm sized fragment with a contact dose rate of ∼590 μSv/h was selected for pilot XAS/XRF investigations at the INE-Beamline for actinide science at the ANKA synchrotron radiation source. The experiment was aimed at elucidating the potential of direct radionuclide speciation with an emphasis on the fission products Se and Tc in highly active nuclear materials and at assessing the possible influence of the γ-radiation field surrounding highly active samples on the beamline instrumentation. While the influence of γ-radiation turned out to be negligible, initial radionuclide speciation studies by XAFS were most promising. In addition to Se and Tc speciation, the focus of these initial investigations was on the possibility for direct actinide speciation by recording corresponding L3-edge XAFS data. The registration of high quality XANES data was possible for the actinide elements U, Np, Pu and Am, as well as for Zr.

  19. Direct measurement of DX-centre related lattice relaxations in Al$_{x}$Ga$_{1-x}$As compounds

    CERN Multimedia

    2002-01-01

    Donor impurities from elements of group IV and VI form localized electronic states, so-called DX-centers, in AlGaAs and other semiconductors. One of the well known effects related to DX-centers is the persistent photoconductivity. In spite of extensive studies, the microscopic structure of the DX-center is still a matter of controversy. The direct determination of the donor lattice sites and their microscopical surrounding is a crucial point in understanding the relation of microscopic structure to the localized electronic state of the DX-center.\\\\ It is proposed to implant radioactive group VI elements $^{73}$Se (from $^{73}$Br) and $^{118}$Te (from $^{118}$Xe) into Al$_{x}$Ga$_{1-x}$As of different mole fractions ${x}$ and to determine (i) the lattice site of Te and Se impurities by emission channeling of decay positrons and electrons (ii) the local structure of Se impurities using the perturbed $\\gamma$-$\\gamma$-angular correlation technique (PAC). The appearance of the DX-center shall be check...

  20. Numerical study on core damage and interpretation of in situ state of stress

    Energy Technology Data Exchange (ETDEWEB)

    Hakala, M. [Gridpoint Finland Oy (Finland)

    1999-06-01

    Core disking is a phenomenon where a diamond cored core sample will be sliced when released from a stressed host rock. Ring disking is a similar phenomenon which takes place during overcoring with a pilot hole. Because of the uniform shape and spacing of disk fracturing, it has the potential to be used for estimating the in situ state of stress. If this is feasible, it could be used in high stress states where the traditional stress measuring techniques are not valid or even possible. In this work the both the core disking and ring disking phenomena were studied based on the elastic bottom hole stress application developed and a series of fracture growth stability simulations. The results-showed that both phenomena are very complicated and site specific, but the spacing, shape, extent and initiation point are clearly stress state dependent. Throughout the work, guidelines for the in situ stress field interpretation method were developed and implemented for the borehole aligned orthogonal stress field and Poisson`s ratio of 0.25. Based on this study, the in situ state of stress can be estimated with acceptable accuracy if information on both core disking and ring disking is available. On the other hand, as an indirect method, there are no reasons to use it if direct measurements can be used. (orig.) 35 refs.

  1. Development of new ultrafiltration techniques maintaining in-situ hydrochemical conditions for colloidal study

    International Nuclear Information System (INIS)

    Aosai, Daisuke; Yamamoto, Yuhei; Mizuno, Takashi

    2011-01-01

    Chemical state of elements in groundwater is one of the most important information for understanding behavior of elements in underground environment. Chemical state of elements controlled mainly by groundwater physico-chemical parameters. Because the change of physico-chemical parameters of groundwater, due to pressure release and oxidation during sampling, causes changes in chemical state of elements, systematic methodologies for understanding in situ chemical state is required. In this study, in order to understand chemical state of elements in groundwater, an ultrafiltration instrument for maintaining in-situ pressure and anaerobic conditions was developed. The instrument developed in this study for ultrafiltration made of passivated Stainless Used Steel (SUS) materials, was designed to keep groundwater samples maintaining in-situ pressure/anaerobic conditions. Ultrafiltration of groundwater was conducted at a borehole drilled from the 200 mbGL (meters below ground level) Sub-stage at a depth of 200 m at the Mizunami Underground Research Laboratory. Chemical analyses of groundwater were also conducted using samples filtered under both pressurized/anaerobic and atmospheric conditions and passivated SUS materials with different elapsed times after passivation. The results indicate that our ultrafiltration method is suitable for collection of filtered groundwater and passivation is an essential treatment before ultrafiltration. (author)

  2. Numerical study on core damage and interpretation of in situ state of stress

    International Nuclear Information System (INIS)

    Hakala, M.

    1999-06-01

    Core disking is a phenomenon where a diamond cored core sample will be sliced when released from a stressed host rock. Ring disking is a similar phenomenon which takes place during overcoring with a pilot hole. Because of the uniform shape and spacing of disk fracturing, it has the potential to be used for estimating the in situ state of stress. If this is feasible, it could be used in high stress states where the traditional stress measuring techniques are not valid or even possible. In this work the both the core disking and ring disking phenomena were studied based on the elastic bottom hole stress application developed and a series of fracture growth stability simulations. The results-showed that both phenomena are very complicated and site specific, but the spacing, shape, extent and initiation point are clearly stress state dependent. Throughout the work, guidelines for the in situ stress field interpretation method were developed and implemented for the borehole aligned orthogonal stress field and Poisson's ratio of 0.25. Based on this study, the in situ state of stress can be estimated with acceptable accuracy if information on both core disking and ring disking is available. On the other hand, as an indirect method, there are no reasons to use it if direct measurements can be used. (orig.)

  3. Mechanical properties enhancement and microstructure study of Al-Si-TiB2 in situ composites

    Science.gov (United States)

    Sahoo, S. K.; Majhi, J.; Pattnaik, A. B.; Sahoo, J. K.; Das, Swagat

    2018-03-01

    Al–Si alloy-based composite is one of the most promising MMC materials owing to its outstanding mechanical properties, wear and corrosion resistance, low cost and ability to be synthesized via conventional casting routes. Challenges in achieving clean interface between reinforced particles and matrix alloy have been overcome by means of in-situ techniques of fabrication. Present investigation is concerned with synthesizing Al-Si-TiB2 in-situ composites through stir casting route using K2TiF6 and KBF4 halide salts for exothermic salt metal reaction. X-Ray diffraction analysis revealed the existence of TiB2 in the prepared samples. Effect of TiB2in-situ particles in the Al-Si base alloy has been investigated from the results obtained from optical microscopy as well as SEM study and wear analysis with a pin on disc wear testing apparatus. Improved hardness and wear properties were observed with addition of TiB2.

  4. An in situ study of zirconium-based conversion treatment on zinc surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Taheri, P. [Materials innovation institute (M2i), Elektronicaweg 25, 2628 XG Delft (Netherlands); Delft University of Technology, Department of Materials Science and Engineering, Mekelweg 2, 2628 CD Delft (Netherlands); Laha, P. [Vrije Universiteit Brussel, Department of Electrochemical and Surface Engineering, Pleinlaan 2, B-1050 Brussels (Belgium); Terryn, H. [Delft University of Technology, Department of Materials Science and Engineering, Mekelweg 2, 2628 CD Delft (Netherlands); Vrije Universiteit Brussel, Department of Electrochemical and Surface Engineering, Pleinlaan 2, B-1050 Brussels (Belgium); Mol, J.M.C., E-mail: J.M.C.Mol@tudelft.nl [Delft University of Technology, Department of Materials Science and Engineering, Mekelweg 2, 2628 CD Delft (Netherlands)

    2015-11-30

    Highlights: • We investigated the deposition mechanism of zirconium conversion layer on zinc. • In situ FTIR and electrochemical measurements are conducted. • The initial hydroxyl fraction plays an important role in the deposition process. • Deposition starts with hydroxyl removal by fluoride ions. • An increase of alkalinity adjacent to the surface promotes deposition of Zr. - Abstract: This study is focused on the deposition process of zirconium-based conversion layers on Zn surfaces. The analysis approach is based on a Kretschmann configuration in which in situ ATR-FTIR spectroscopy is combined with open circuit potential (OCP) and near surface pH measurements. Differently pretreated Zn surfaces were subjected to conversion treatments, while the Zr-based deposition mechanism was probed in situ. It was found that the initial hydroxyl fraction promotes the overall Zr conversion process as the near surface pH values are influenced by the initial hydroxyl fraction. Kinetics of the early surface activation and the subsequent Zr-based conversion process are discussed and correlated to the initial hydroxyl fractions.

  5. Matrix diffusion studies by electrical conductivity methods. Comparison between laboratory and in-situ measurements

    International Nuclear Information System (INIS)

    Ohlsson, Y.; Neretnieks, I.

    1998-01-01

    Traditional laboratory diffusion experiments in rock material are time consuming, and quite small samples are generally used. Electrical conductivity measurements, on the other hand, provide a fast means for examining transport properties in rock and allow measurements on larger samples as well. Laboratory measurements using electrical conductivity give results that compare well to those from traditional diffusion experiments. The measurement of the electrical resistivity in the rock surrounding a borehole is a standard method for the detection of water conducting fractures. If these data could be correlated to matrix diffusion properties, in-situ diffusion data from large areas could be obtained. This would be valuable because it would make it possible to obtain data very early in future investigations of potentially suitable sites for a repository. This study compares laboratory electrical conductivity measurements with in-situ resistivity measurements from a borehole at Aespoe. The laboratory samples consist mainly of Aespoe diorite and fine-grained granite and the rock surrounding the borehole of Aespoe diorite, Smaaland granite and fine-grained granite. The comparison shows good agreement between laboratory measurements and in-situ data

  6. Role of Bi promotion and solvent in platinum-catalyzed alcohol oxidation probed by in situ X-ray absorption and ATR-IR spectroscopy

    DEFF Research Database (Denmark)

    Mondelli, C.; Grunwaldt, Jan-Dierk; Ferri, D.

    2010-01-01

    the catalysts under working conditions using in situ X-ray absorption spectroscopy (XAS) and attenuated total reflection infrared spectroscopy (ATR-IR), aiming at uncovering the roles of the metal promoter and the reaction medium. XAS confirms that Bi is oxidized more easily than Pt, maintaining the catalytic...... surfaces than on step or kink sites. Side products, CO and benzoate species, appearing during the reaction reveal that the geometric suppression of undesired reactions does not occur to the same extent on Pt-based catalysts as on Pd, suggesting that decarbonylation of the produced aldehyde on Pt may occur...

  7. Comparison between XAS, AWAXS and DAFS applied to nanometer scale supported metallic clusters. Pt.1; monometallic clusters

    International Nuclear Information System (INIS)

    Bazin, D.C.; Sayers, D.A.

    1993-01-01

    The structural information found using three techniques related to synchrotron radiation are compared. XAS (X-ray Absorption Spectroscopy), AWAXS (Anomalous Wide Angle X-ray Scattering) and DAFS (Diffraction Anomalous Fine Structure) are applied to nanometer scale metallic clusters. (author)

  8. In-situ x-ray absorption study of copper films in ground water solutions

    International Nuclear Information System (INIS)

    Kvashnina, K.O.; Butorin, S.M.; Modin, A.; Soroka, I.; Marcellini, M.; Nordgren, J.; Guo, J.-H.; Werme, L.

    2007-01-01

    This study illustrates how the damage from copper corrosion can be reduced by modifying the chemistry of the copper surface environment. The surface modification of oxidized copper films induced by chemical reaction with Cl - and HCO 3 - in aqueous solutions was monitored by in situ X-ray absorption spectroscopy. The results show that corrosion of copper can be significantly reduced by adding even a small amount of sodium bicarbonate. The studied copper films corroded quickly in chloride solutions, whereas the same solution containing 1.1 mM HCO 3 - prevented or slowed down the corrosion processes

  9. An in situ study of the adsorption behavior of functionalized particles on selfassembled monolayers via different chemical interactions

    NARCIS (Netherlands)

    Ling, X.Y.; Malaquin, Laurent; Reinhoudt, David; Wolf, Heiko; Huskens, Jurriaan

    2007-01-01

    The formation of particle monolayers by convective assembly was studied in situ with three different kinds of particle-surface interactions: adsorption onto native surfaces, with additional electrostatic interactions, and with supramolecular host-guest interactions. In the first case

  10. In situ treatment of arsenic contaminated groundwater by aquifer iron coating: Experimental study

    Energy Technology Data Exchange (ETDEWEB)

    Xie, Xianjun, E-mail: xjxie@cug.edu.cn [State Key Laboratory of Biogeology and Environmental Geology, School of Environmental Studies, China University of Geosciences, 430074 Wuhan (China); Wang, Yanxin, E-mail: yx.wang@cug.edu.cn [State Key Laboratory of Biogeology and Environmental Geology, School of Environmental Studies, China University of Geosciences, 430074 Wuhan (China); Pi, Kunfu [State Key Laboratory of Biogeology and Environmental Geology, School of Environmental Studies, China University of Geosciences, 430074 Wuhan (China); Liu, Chongxuan [State Key Laboratory of Biogeology and Environmental Geology, School of Environmental Studies, China University of Geosciences, 430074 Wuhan (China); Pacific Northwest National Laboratory, Richland, WA 99354 (United States); Li, Junxia; Liu, Yaqing; Wang, Zhiqiang; Duan, Mengyu [State Key Laboratory of Biogeology and Environmental Geology, School of Environmental Studies, China University of Geosciences, 430074 Wuhan (China)

    2015-09-15

    In situ arsenic removal from groundwater by an aquifer iron coating method has great potential to be a cost effective and simple groundwater remediation technology, especially in rural and remote areas where groundwater is used as the main water source for drinking. The in situ arsenic removal technology was first optimized by simulating arsenic removal in various quartz sand columns under anoxic conditions. The effectiveness was then evaluated in an actual high-arsenic groundwater environment. The arsenic removal mechanism by the coated iron oxide/hydroxide was investigated under different conditions using scanning electron microscopy (SEM)/X-ray absorption spectroscopy, electron probe microanalysis, and Fourier transformation infrared spectroscopy. Aquifer iron coating method was developed via a 4-step alternating injection of oxidant, iron salt and oxygen-free water. A continuous injection of 5.0 mmol/L FeSO{sub 4} and 2.5 mmol/L NaClO for 96 h can form a uniform goethite coating on the surface of quartz sand without causing clogging. At a flow rate of 7.2 mL/min of the injection reagents, arsenic (as Na{sub 2}HAsO{sub 4}) and tracer fluorescein sodium to pass through the iron-coated quartz sand column were approximately at 126 and 7 column pore volumes, respectively. The retardation factor of arsenic was 23.0, and the adsorption capacity was 0.11 mol As per mol Fe. In situ arsenic removal from groundwater in an aquifer was achieved by simultaneous injections of As(V) and Fe(II) reagents. Arsenic fixation resulted from a process of adsorption/co-precipitation with fine goethite particles by way of bidentate binuclear complexes. Therefore, the study results indicate that the high arsenic removal efficiency of the in situ aquifer iron coating technology likely resulted from the expanded specific surface area of the small goethite particles, which enhanced arsenic sorption capability and/or from co-precipitation of arsenic on the surface of goethite particles

  11. In situ treatment of arsenic contaminated groundwater by aquifer iron coating: Experimental study

    International Nuclear Information System (INIS)

    Xie, Xianjun; Wang, Yanxin; Pi, Kunfu; Liu, Chongxuan; Li, Junxia; Liu, Yaqing; Wang, Zhiqiang; Duan, Mengyu

    2015-01-01

    In situ arsenic removal from groundwater by an aquifer iron coating method has great potential to be a cost effective and simple groundwater remediation technology, especially in rural and remote areas where groundwater is used as the main water source for drinking. The in situ arsenic removal technology was first optimized by simulating arsenic removal in various quartz sand columns under anoxic conditions. The effectiveness was then evaluated in an actual high-arsenic groundwater environment. The arsenic removal mechanism by the coated iron oxide/hydroxide was investigated under different conditions using scanning electron microscopy (SEM)/X-ray absorption spectroscopy, electron probe microanalysis, and Fourier transformation infrared spectroscopy. Aquifer iron coating method was developed via a 4-step alternating injection of oxidant, iron salt and oxygen-free water. A continuous injection of 5.0 mmol/L FeSO 4 and 2.5 mmol/L NaClO for 96 h can form a uniform goethite coating on the surface of quartz sand without causing clogging. At a flow rate of 7.2 mL/min of the injection reagents, arsenic (as Na 2 HAsO 4 ) and tracer fluorescein sodium to pass through the iron-coated quartz sand column were approximately at 126 and 7 column pore volumes, respectively. The retardation factor of arsenic was 23.0, and the adsorption capacity was 0.11 mol As per mol Fe. In situ arsenic removal from groundwater in an aquifer was achieved by simultaneous injections of As(V) and Fe(II) reagents. Arsenic fixation resulted from a process of adsorption/co-precipitation with fine goethite particles by way of bidentate binuclear complexes. Therefore, the study results indicate that the high arsenic removal efficiency of the in situ aquifer iron coating technology likely resulted from the expanded specific surface area of the small goethite particles, which enhanced arsenic sorption capability and/or from co-precipitation of arsenic on the surface of goethite particles. - Highlights:

  12. Report on in-situ studies of flash sintering of uranium dioxide

    Energy Technology Data Exchange (ETDEWEB)

    Raftery, Alicia Marie [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2017-01-24

    Flash sintering is a novel type of field assisted sintering that uses an electric field and current to provide densification of materials on very short time scales. The potential for field assisted sintering techniques to be used in producing nuclear fuel is gaining recognition due to the potential economic benefits and improvements in material properties. The flash sintering behavior has so far been linked to applied and material parameters, but the underlying mechanisms active during flash sintering have yet to be identified. This report summarizes the efforts to investigate flash sintering of uranium dioxide using dilatometer studies at Los Alamos National Laboratory and two separate sets of in-situ studies at Brookhaven National Laboratory’s NSLS-II XPD-1 beamline. The purpose of the dilatometer studies was to understand individual parameter (applied and material) effects on the flash behavior and the purpose of the in-situ studies was to better understand the mechanisms active during flash sintering. As far as applied parameters, it was found that stoichiometry, or oxygen-to-metal ratio, has a significant effect on the flash behavior (time to flash and speed of flash). Composite systems were found to have degraded sintering behavior relative to pure UO2. The critical field studies are complete for UO2.00 and will be analyzed against an existing model for comparison. The in-situ studies showed that the strength of the field and current are directly related to the sample temperature, with temperature-driven phase changes occurring at high values. The existence of an ‘incubation time’ has been questioned, due to a continuous change in lattice parameter values from the moment that the field is applied. Some results from the in-situ experiments, which should provide evidence regarding ion migration, are still being analyzed. Some preliminary conclusions can be made from these results with regard to using field assisted sintering to

  13. The erosive effects of some mouthrinses on enamel. A study in situ.

    Science.gov (United States)

    Pontefract, H; Hughes, J; Kemp, K; Yates, R; Newcombe, R G; Addy, M

    2001-04-01

    There are both anecdotal clinical and laboratory experimental data suggesting that low pH mouthrinses cause dental erosion. This evidence is particularly relevant to acidified sodium chlorite (ASC) formulations since they have plaque inhibitory properties comparable to chlorhexidine but without the well known local side effects. Studies in situ and in vitro were planned to measure enamel erosion by low pH mouthrinses. The study in situ measured enamel erosion by ASC, essential oil and hexetidine mouthrinses over 15-day study periods. The study was a 5 treatment, single blind cross over design involving 15 healthy subjects using orange juice, as a drink, and water, as a rinse, as positive and negative controls respectively. 2 enamel specimens from unerupted human third molar teeth were placed in the palatal area of upper removable acrylic appliances which were worn from 9 a.m. to 5 p.m., Monday to Friday for 3 weeks. Rinses were used 2x daily and 250 ml volumes of orange juice were imbibed 4x daily. Enamel loss was determined by profilometry on days 5, 10 and 15. The study in vitro involved immersing specimens in the 4 test solutions together with a reduced acid ASC formulation for a period of 4 h under constant stirring; Enamel loss was measured by profilometry every hour. Enamel loss was in situ progressive over time with the 3 rinses and orange juice but negligible with water. ASC produced similar erosion to orange juice and significantly more than the two proprietary rinses and water. The essential oil and hexetidine rinses produced similar erosion and significantly more than water. Enamel loss in vitro was progressive over time, and the order from low to high erosion was reduced acid ASC, ASC, Essential oil, and hexetidine mouthrinses and orange juice. Based on the study in situ, it is recommended that low pH mouthrinses should not be considered for long term or continuous use and never as pre-brushing rinses. In view of the plaque inhibitory efficacy of ASC

  14. Novel in situ radiotracer methods for the direct and indirect study of chromate adsorption on alumina

    International Nuclear Information System (INIS)

    Gancs, L.; Nemeth, Z.; Horanyi, G.

    2002-01-01

    Radiotracer methods, particularly the radiotracer thin foil method, provide unique possibility of in situ monitoring of chromate adsorption on powdered adsorbents. Two different versions of the thin foil method can be distinguished. In the direct method, the species to be studied is labelled and the radiation measured gives direct information on the adsorption of this species. In the indirect method, a different labelled indicator species is added to the system and the adsorption of this species is followed and the adsorption of the species to be studied is determined based on analysis of the competitive adsorption processes. Both methods were used in the present study. In the in situ methods, the radiation measured consists of two main parts, one coming from the solution background, the other originating from the adsorption layer. In the case of the thin foil method using isotopes emitting soft β - radiation or low energy X-ray the solution background is governed and minimised by self-absorption of the radiation. In the direct study we applied an experimental methodology based on the energy selective measurement of the characteristic K α,β X-radiation emitted by the 51 Cr-labelled chromate species, whereas 35 S-labelled sulphate ions were used as the indicator species in the indirect study. (P.A.)

  15. Towards functionalization of graphene: in situ study of the nucleation of copper-phtalocyanine on graphene

    OpenAIRE

    Schwarz, Daniel; Henneke, Caroline; Kumpf, Christian

    2016-01-01

    Molecular films present an elegant way for the uniform functionalization or doping of graphene. Here, we present an in situ study on the initial growth of copper phthalocyanine (CuPc) on epitaxial graphene on Ir(111). We followed the growth up to a closed monolayer with low energy electron microscopy and selected area electron diffraction (μLEED). The molecules coexist on graphene in a disordered phase without long-range order and an ordered crystalline phase. The local topography of the grap...

  16. A STUDY ON MICROSTRUCTURE CHARACTERISTICS OF IN SITU FORMED TiC REINFORCED COMPOSITE COATINGS

    OpenAIRE

    PENG LIU; WEI GUO; HUI LUO

    2012-01-01

    In situ synthesized TiC reinforced composite coating was fabricated by laser cladding of Al-Ni-Cr-C powders on titanium alloys, which can greatly improve the surface performance of the substrate. In this study, the Al-Ni-Cr-C laser-cladded composite coatings have been researched by means of X-ray diffraction, scanning electron microscope (SEM) and electron probe micro-analyzer (EPMA). There was a metallurgical combination between the Al-Ni-Cr-C laser-cladded coating and the Ti-6Al-4V substrat...

  17. Development of conductivity probe and temperature probe for in-situ measurements in hydrological studies

    International Nuclear Information System (INIS)

    Chandra, U.; Galindo, B.J.; Castagnet, A.C.G.

    1981-05-01

    A conductivity probe and a temperature probe have been developed for in-situ measurements in various hydrological field studies. The conductivity probe has platinum electrodes and is powered with two 12 volt batteries. The sensing element of the temperature probe consists of a resistor of high coefficient of temperature. Response of the conductivity probe is measured in a milliampere mater while the resistance of the thermistor is read by a digital meter. The values of conductivity and temperature are derived from respective calibration. The probes are prototype and their range of measurement can be improved depending upon the requirement of the field problem. (Author) [pt

  18. Case studies illustrating in-situ remediation methods for soil and groundwater contaminated with petrochemicals

    Energy Technology Data Exchange (ETDEWEB)

    Dixon, Robert A.; Lance, P.E.; Downs, A.; Kier, Brian P. [EMCON Northwest Inc., Portland, OR (United States)

    1993-12-31

    Four case studies of successful in-situ remediation are summarized illustrating cost-effective methods to remediate soil and groundwater contaminated with volatile and non-volatile petrochemicals. Each site is in a different geologic environment with varying soil types and with and without groundwater impact. The methods described include vadose zone vapor extraction, high-vacuum vapor extraction combined with groundwater tab.le depression, air sparging with groundwater recovery and vapor extraction, and bio remediation of saturated zone soils using inorganic nutrient and oxygen addition

  19. Sintering of oxide-supported Pt and Pd nanoparticles in air studied by in situ TEM

    DEFF Research Database (Denmark)

    Simonsen, Søren Bredmose

    This thesis presents a fundamental study of the sintering of supported nanoparticles in relation to diesel oxidation catalysts. The sintering of supported nanoparticles is an important challenge in relation to this catalyst, as well as many other catalyst systems, and a fundamental understanding...... of Pt, Pd and bimetallic Pt-Pd nanoparticles supported on a flat and homogeneous Al2O3 or SiO2 surface. By using in situ TEM on the planar model catalysts it was possible to directly monitor the detailed dynamical changes of the individual nanoparticles during exposure to oxidizing conditions...

  20. Chlorophyll bleaching by UV-irradiation in vitro and in situ: Absorption and fluorescence studies

    International Nuclear Information System (INIS)

    Zvezdanovic, Jelena; Cvetic, Tijana; Veljovic-Jovanovic, Sonja; Markovic, Dejan

    2009-01-01

    Chlorophyll bleaching by UV-irradiation has been studied by absorbance and fluorescence spectroscopy in extracts containing mixtures of photosynthetic pigments, in acetone and n-hexane solutions, and in aqueous thylakoid suspensions. Chlorophyll undergoes destruction (bleaching) accompanied by fluorescent transient formation obeying first-order kinetics. The bleaching is governed by UV-photon energy input, as well as by different chlorophyll molecular organizations in solvents of different polarities (in vitro), and in thylakoids (in situ). UV-C-induced bleaching of chlorophylls in thylakoids is probably caused by different mechanisms compared to UV-A- and UV-B-induced bleaching

  1. Case studies illustrating in-situ remediation methods for soil and groundwater contaminated with petrochemicals

    Energy Technology Data Exchange (ETDEWEB)

    Dixon, Robert A; Lance, P E; Downs, A; Kier, Brian P [EMCON Northwest Inc., Portland, OR (United States)

    1994-12-31

    Four case studies of successful in-situ remediation are summarized illustrating cost-effective methods to remediate soil and groundwater contaminated with volatile and non-volatile petrochemicals. Each site is in a different geologic environment with varying soil types and with and without groundwater impact. The methods described include vadose zone vapor extraction, high-vacuum vapor extraction combined with groundwater tab.le depression, air sparging with groundwater recovery and vapor extraction, and bio remediation of saturated zone soils using inorganic nutrient and oxygen addition

  2. Design, installation and in-situ performance study of ultrasonic continuous level meter

    International Nuclear Information System (INIS)

    Surya Prakash, G.; Somayaji, K.M.

    1995-01-01

    The report discusses the design and the development of a continuous liquid level meter based on ultrasonic pulse-echo technique. A review of various methods for level measurement along with the details of pulse-echo technique are presented. Also discussed is the development of discrete level detectors based on ultrasonic techniques. Lastly, the procedures adopted for in-situ installation of these level meters in FBTR and RML are given along with the field performance study. Some of the typical merits and limitations of the method and the surface preparation procedure are also highlighted. (author) (author)

  3. Application of in-situ bioassays with macrophytes in aquatic mesocosm studies.

    Science.gov (United States)

    Coors, Anja; Kuckelkorn, Jochen; Hammers-Wirtz, Monika; Strauss, Tido

    2006-10-01

    Aquatic mesocosm studies assess ecotoxicological effects of chemicals by using small artificial ponds as models of lentic ecosystems. In this study, methods of controlled insertion of macrophytes within an outdoor mesocosm study were explored. Although analytically confirmed concentrations of the model herbicide terbuthylazine were high enough to expect direct effects on phytoplankton, functional parameters and dominant taxa abundance indicated only minor and transient effects. In-situ assays with Lemna minor, Myriophyllum spicatum, Potamogeton lucens and Chara globularis revealed adverse effects at concentrations in accordance with literature data. Complex interactions such as nutrient limitation and competition were possible reasons for the observed growth promotion at the lower concentration of about 5 microg/l terbuthylazine. The approach of macrophyte in-situ bioassays within a mesocosm study proved to be applicable. Presumed advantages are simultaneous acquisition of toxicity data for several species of aquatic plants under more realistic conditions compared to laboratory tests and inclusion of macrophytes as important structural and functional components in mesocosms while limiting their domination of the model ecosystem.

  4. In-situ Non-destructive Studies on Biofouling Processes in Reverse Osmosis Membrane Systems

    KAUST Repository

    Farhat, Nadia

    2016-12-01

    Reverse osmosis (RO) and nanofiltration (NF) membrane systems are high-pressure membrane filtration processes that can produce high quality drinking water. Biofouling, biofilm formation that exceeds a certain threshold, is a major problem in spiral wound RO and NF membrane systems resulting in a decline in membrane performance, produced water quality, and quantity. In practice, detection of biofouling is typically done indirectly through measurements of performance decline. Existing direct biofouling detection methods are mainly destructive, such as membrane autopsies, where biofilm samples can be contaminated, damaged and resulting in biofilm structural changes. The objective of this study was to test whether transparent luminescent planar oxygen sensing optodes, in combination with a simple imaging system, can be used for in-situ, non-destructive biofouling characterization. Aspects of the study were early detection of biofouling, biofilm spatial patterning in spacer filled channels, and the effect of feed cross-flow velocity, and feed flow temperature. Oxygen sensing optode imaging was found suitable for studying biofilm processes and gave detailed spatial and quantitative biofilm development information enabling better understanding of the biofouling development process. The outcome of this study attests the importance of in-situ, non-destructive imaging in acquiring detailed knowledge on biofilm development in membrane systems contributing to the development of effective biofouling control strategies.

  5. First-principles calculations of the structural, electronic and optical properties of cubic B{sub x}Ga{sub 1-x}As alloys

    Energy Technology Data Exchange (ETDEWEB)

    Guemou, M., E-mail: guemoumhamed7@gmail.com [Engineering Physics Laboratory, University Ibn Khaldoun of Tiaret, BP 78-Zaaroura, Tiaret 14000 (Algeria); Bouhafs, B. [Modelling and Simulation in Materials Science Laboratory, Physics Department, University of Sidi Bel-Abbes, 22000 Sidi Bel-Abbes (Algeria); Abdiche, A. [Applied Materials Laboratory, Research Center, University of Sidi Bel Abbes, 22000 Sidi Bel Abbes (Algeria); Khenata, R. [Laboratoire de Physique Quantique et de Modelisation Mathematique (LPQ3M), Departement de Technologie, Universite de Mascara, 29000 Mascara (Algeria); Al Douri, Y. [Institute of Nano Electronic Engineering, Universiti Malaysia Perlis, Perlis (Malaysia); Bin Omran, S. [Department of Physics and Astronomy, Faculty of Science, King Saud University, P.O. Box 2455, Riyadh 11451 (Saudi Arabia)

    2012-04-15

    Density functional calculations are performed to study the structural, electronic and optical properties of technologically important B{sub x}Ga{sub 1-x}As ternary alloys. The calculations are based on the total-energy calculations within the full-potential augmented plane-wave (FP-LAPW) method. For exchange-correlation potential, local density approximation (LDA) and the generalized gradient approximation (GGA) have been used. The structural properties, including lattice constants, bulk modulus and their pressure derivatives, are in very good agreement with the available experimental and theoretical data. The electronic band structure, density of states for the binary compounds and their ternary alloys are given. The dielectric function and the refractive index are also calculated using different models. The obtained results compare very well with previous calculations and experimental measurements.

  6. Methodology for studying strain inhomogeneities in polycrystalline thin films during in situ thermal loading using coherent x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Vaxelaire, N; Labat, S; Thomas, O [Aix-Marseille University, IM2NP, FST avenue Escadrille Normandie Niemen, F-13397 Marseille Cedex (France); Proudhon, H; Forest, S [MINES ParisTech, Centre des materiaux, CNRS UMR 7633, BP 87, 91003 Evry Cedex (France); Kirchlechner, C; Keckes, J [Erich Schmid Institute for Material Science, Austrian Academy of Science and Institute of Metal Physics, University of Leoben, Jahnstrasse 12, 8700 Leoben (Austria); Jacques, V; Ravy, S [Synchrotron SOLEIL, L' Orme des merisiers, Saint-Aubin BP 48, 91192 Gif-sur-Yvette Cedex (France)], E-mail: nicolas.vaxelaire@univ-cezanne.fr

    2010-03-15

    Coherent x-ray diffraction is used to investigate the mechanical properties of a single grain within a polycrystalline thin film in situ during a thermal cycle. Both the experimental approach and finite element simulation are described. Coherent diffraction from a single grain has been monitored in situ at different temperatures. This experiment offers unique perspectives for the study of the mechanical properties of nano-objects.

  7. Methodology for studying strain inhomogeneities in polycrystalline thin films during in situ thermal loading using coherent x-ray diffraction

    International Nuclear Information System (INIS)

    Vaxelaire, N; Labat, S; Thomas, O; Proudhon, H; Forest, S; Kirchlechner, C; Keckes, J; Jacques, V; Ravy, S

    2010-01-01

    Coherent x-ray diffraction is used to investigate the mechanical properties of a single grain within a polycrystalline thin film in situ during a thermal cycle. Both the experimental approach and finite element simulation are described. Coherent diffraction from a single grain has been monitored in situ at different temperatures. This experiment offers unique perspectives for the study of the mechanical properties of nano-objects.

  8. Chromogenic in situ hybridisation for the assessment of HER2 status in breast cancer: an international validation ring study

    OpenAIRE

    van de Vijver, Marc; Bilous, Michael; Hanna, Wedad; Hofmann, Manfred; Kristel, Petra; Penault-Llorca, Frédérique; Rüschoff, Josef

    2007-01-01

    Introduction Before any new methodology can be introduced into the routine diagnostic setting it must be technically validated against the established standards. To this end, a ring study involving five international pathology laboratories was initiated to validate chromogenic in situ hybridisation (CISH) against fluorescence in situ hybridisation (FISH) and immunohistochemistry (IHC) as a test for assessing human epidermal growth factor receptor 2 (HER2) status in breast cancer. Methods Each...

  9. An Equation-of-State Compositional In-Situ Combustion Model: A Study of Phase Behavior Sensitivity

    DEFF Research Database (Denmark)

    Kristensen, Morten Rode; Gerritsen, M. G.; Thomsen, Per Grove

    2009-01-01

    phase behavior sensitivity for in situ combustion, a thermal oil recovery process. For the one-dimensional model we first study the sensitivity to numerical discretization errors and provide grid density guidelines for proper resolution of in situ combustion behavior. A critical condition for success...... to ignition. For a particular oil we show that the simplified approach overestimates the required air injection rate for sustained front propagation by 17% compared to the equation of state-based approach....

  10. In Situ Synchrotron X-ray Study of Ultrasound Cavitation and Its Effect on Solidification Microstructures

    Energy Technology Data Exchange (ETDEWEB)

    Mi, Jiawei; Tan, Dongyue; Lee, Tung Lik (Hull)

    2014-12-11

    Considerable progress has been made in studying the mechanism and effectiveness of using ultrasound waves to manipulate the solidification microstructures of metallic alloys. However, uncertainties remain in both the underlying physics of how microstructures evolve under ultrasonic waves, and the best technological approach to control the final microstructures and properties. We used the ultrafast synchrotron X-ray phase contrast imaging facility housed at the Advanced Photon Source, Argonne National Laboratory, US to study in situ the highly transient and dynamic interactions between the liquid metal and ultrasonic waves/bubbles. The dynamics of ultrasonic bubbles in liquid metal and their interactions with the solidifying phases in a transparent alloy were captured in situ. The experiments were complemented by the simulations of the acoustic pressure field, the pulsing of the bubbles, and the associated forces acting onto the solidifying dendrites. The study provides more quantitative understanding on how ultrasonic waves/bubbles influence the growth of dendritic grains and promote the grain multiplication effect for grain refinement.

  11. Cutaneous melanoma in situ: translational evidence from a large population-based study.

    Science.gov (United States)

    Mocellin, Simone; Nitti, Donato

    2011-01-01

    Cutaneous melanoma in situ (CMIS) is a nosologic entity surrounded by health concerns and unsolved debates. We aimed to shed some light on CMIS by means of a large population-based study. Patients with histologic diagnosis of CMIS were identified from the Surveillance Epidemiology End Results (SEER) database. The records of 93,863 cases of CMIS were available for analysis. CMIS incidence has been steadily increasing over the past 3 decades at a rate higher than any other in situ or invasive tumor, including invasive skin melanoma (annual percentage change [APC]: 9.5% versus 3.6%, respectively). Despite its noninvasive nature, CMIS is treated with excision margins wider than 1 cm in more than one third of cases. CMIS is associated with an increased risk of invasive melanoma (standardized incidence ratio [SIR]: 8.08; 95% confidence interval [CI]: 7.66-8.57), with an estimated 3:5 invasive/in situ ratio; surprisingly, it is also associated with a reduced risk of gastrointestinal (SIR: 0.78, CI: 0.72-0.84) and lung (SIR: 0.65, CI: 0.59-0.71) cancers. Relative survival analysis shows that persons with CMIS have a life expectancy equal to that of the general population. CMIS is increasingly diagnosed and is often overtreated, although it does not affect the life expectancy of its carriers. Patients with CMIS have an increased risk of developing invasive melanoma (which warrants their enrollment in screening programs) but also a reduced risk of some epithelial cancers, which raises the intriguing hypothesis that genetic/environmental risk factors for some tumors may oppose the pathogenesis of others.

  12. Glycolate adsorption at gold and platinum electrodes: A theoretical and in situ spectroelectrochemical study

    International Nuclear Information System (INIS)

    Delgado, Jose Manuel; Blanco, Raquel; Orts, Jose Manuel; Perez, Juan Manuel; Rodes, Antonio

    2010-01-01

    The adsorption of glycolate anions at sputtered gold thin-film electrodes was studied in perchloric acid solutions by cyclic voltammetry experiments combined with in situ Surface Enhanced Raman Scattering (SERS) and Surface Enhanced Infrared Reflection Absorption Spectroscopy under attenuated total reflection conditions (ATR-SEIRAS). Theoretical harmonic vibrational frequencies and band intensities obtained from B3LYP/LANL2DZ,6-31+G(d) calculations for glycolate species adsorbed on Au clusters with (1 1 1) orientation were used to interpret the experimental spectra. Vibrational data confirm the bidentate bonding of glycolate anions through the oxygen atoms of the carboxylate group, in a bridge configuration with the OCO plane perpendicular to the metal surface. The DFT calculations show no significant effect of the total charge of the metal cluster-adsorbate adduct on the vibrational frequencies of adsorbed glycolate species. The infrared experimental study is extended to platinum films electrochemically deposited onto sputtered gold thin-film electrodes showing the potential-dependent formation of adsorbed CO upon dissociative adsorption of glycolate anions. As in the case of gold, the reversible adsorption of glycolate anions takes place in a bidentate configuration as predicted by DFT calculations for glycolate adsorbed on Pt(1 1 1) clusters. At low glycolic acid concentration, the in situ ATR-SEIRA spectra evidence the formation of adsorbed oxalate as reaction intermediate.

  13. Two US EPA bioremediation field initiative studies: Evaluation of in-situ bioventing

    International Nuclear Information System (INIS)

    Sayles, G.D.; Brenner, R.C.; Hinchee, R.E.; Vogel, C.M.; Miller, R.N.

    1992-01-01

    Bioventing is the process of supplying oxygen in-situ to oxygen-deprived soil microbes by forcing air through contaminated soil at low air flow rates. Unlike soil venting or soil vacuum extraction technologies, bioventing attempts to stimulate biodegradative activity while minimizing stripping of volatile organics. The process destroys the toxic compounds in the ground. Bioventing technology is especially valuable for treating contaminated soils in areas where structures and utilities cannot be disturbed because the equipment needed (air injection/withdrawal wells, air blower, and soil gas monitoring wells) is relatively non-invasive. The US EPA Risk Reduction Engineering Laboratory, with resources from the US EPA Bioremediation Field Initiative, began two parallel 2-year field studies of in-situ of 1991 in collaboration with the US Air Force. The field sites are located at Eielson Air Force Base (AFB) near Fairbanks, Alaska, and Hill AFB near Salt Lake City, Utah. Each site has jet fuel JP-4 contaminated unsaturated soil where a spill has occurred in association with a fuel distribution network. With the pilot-scale experience gained in these studies and others, bioventing should be available in the very near future as an inexpensive, unobtrusive means of treating large quantities of organically contaminated soils. 5 figs

  14. In situ X-ray diffraction studies on the piezoelectric response of PZT thin films

    Energy Technology Data Exchange (ETDEWEB)

    Davydok, A., E-mail: davydok@mpie.de [Aix Marseille Université, CNRS, Université de Toulon, IM2NP UMR 7334, 13397 Marseille (France); Max-Planck-Institut für Eisenforschung, Department Structure and Nano-/Micromechanics of Materials, D-40237 Düsseldorf (Germany); Cornelius, T.W. [Aix Marseille Université, CNRS, Université de Toulon, IM2NP UMR 7334, 13397 Marseille (France); Mocuta, C. [SOLEIL Synchrotron, DiffAbs beamline, L' Orme des Merisiers, Saint-Aubin - BP 48, 91192 Gif-sur-Yvette Cedex (France); Lima, E.C. [Universidade Federal do Tocantins, 77500-000 Porto Nacional, TO (Brazil); Araujo, E.B. [Departamento de Fisica e Quimica, Universidade Estadual Paulista, Av. Brasil, 56 Centro, 15385-000 Ilha Solteira, SP (Brazil); Thomas, O. [Aix Marseille Université, CNRS, Université de Toulon, IM2NP UMR 7334, 13397 Marseille (France)

    2016-03-31

    Piezoelectric properties of randomly oriented self-polarized PbZr{sub 0.50}Ti{sub 0.50}O{sub 3} (PZT) thin films were investigated using in situ synchrotron X-ray diffraction. Possibilities for investigating the piezoelectric effect using micro-sized hard X-ray beams are demonstrated and perspectives for future dynamical measurements on PZT samples with variety of compositions and thicknesses are given. Studies performed on the crystalline [100, 110] directions evidenced piezoelectric anisotropy. The piezoelectric coefficient d{sub 33} was calculated in terms of the lab reference frame (d{sub perp}) and found to be two times larger along the [100] direction than along the [110] direction. The absolute values for the d{sub perp} amount to 120 and 230 pm/V being in good agreement with experimental and theoretical values found in literature for bulk PZT ceramics. - Highlights: • We performed in situ synchrotron X-ray diffraction studies on (PZT) thin films. • We discuss anisotropy of piezo effect in different crystallographic directions. • Perpendicular component Piezo coefficient of thin PZT layer is defined.

  15. In situ synchrotron X-ray studies during metal-organic chemical vapor deposition of semiconductors

    Energy Technology Data Exchange (ETDEWEB)

    Thompson, Carol [Northern Illinois Univ., DeKalb, IL (United States); Argonne National Lab., Argonne, IL (United States); Highland, Matthew J.; Perret, Edith; Fuoss, Paul H.; Streiffer, Stephen K.; Stephenson, G. Brian [Argonne National Lab., Argonne, IL (United States); Richard, Marie-Ingrid [Universite Paul Cezanne Aix-Marseille, Marseille (France)

    2012-07-01

    In-situ, time-resolved techniques provide valuable insight into the complex interplay of surface structural and chemical evolution occurring during materials synthesis and processing of semiconductors. Our approach is to observe the evolution of surface structure and morphology at the atomic scale in real-time during metal organic vapor phase deposition (MOCVD) by using grazing incidence x-ray scattering and X-ray fluorescence, coupled with visible light scattering. Our vertical-flow MOCVD chamber is mounted on a 'z-axis' surface diffractometer designed specifically for these studies of the film growth, surface evolution and the interactions within a controlled growth environment. These techniques combine the ability of X-rays to penetrate a complex environment for measurements during growth and processing, with the sensitivity of surface scattering techniques to atomic and nanoscale structure. In this talk, we outline our program and discuss examples from our in-situ and real-time X-ray diffraction and fluorescence studies of InN, GaN, and InGaN growth on GaN(0001).

  16. In situ treatment of arsenic contaminated groundwater by aquifer iron coating: Experimental study.

    Science.gov (United States)

    Xie, Xianjun; Wang, Yanxin; Pi, Kunfu; Liu, Chongxuan; Li, Junxia; Liu, Yaqing; Wang, Zhiqiang; Duan, Mengyu

    2015-09-15

    In situ arsenic removal from groundwater by an aquifer iron coating method has great potential to be a cost effective and simple groundwater remediation technology, especially in rural and remote areas where groundwater is used as the main water source for drinking. The in situ arsenic removal technology was first optimized by simulating arsenic removal in various quartz sand columns under anoxic conditions. The effectiveness was then evaluated in an actual high-arsenic groundwater environment. The arsenic removal mechanism by the coated iron oxide/hydroxide was investigated under different conditions using scanning electron microscopy (SEM)/X-ray absorption spectroscopy, electron probe microanalysis, and Fourier transformation infrared spectroscopy. Aquifer iron coating method was developed via a 4-step alternating injection of oxidant, iron salt and oxygen-free water. A continuous injection of 5.0 mmol/L FeSO4 and 2.5 mmol/L NaClO for 96 h can form a uniform goethite coating on the surface of quartz sand without causing clogging. At a flow rate of 7.2 mL/min of the injection reagents, arsenic (as Na2HAsO4) and tracer fluorescein sodium to pass through the iron-coated quartz sand column were approximately at 126 and 7 column pore volumes, respectively. The retardation factor of arsenic was 23.0, and the adsorption capacity was 0.11 mol As per mol Fe. In situ arsenic removal from groundwater in an aquifer was achieved by simultaneous injections of As(V) and Fe(II) reagents. Arsenic fixation resulted from a process of adsorption/co-precipitation with fine goethite particles by way of bidentate binuclear complexes. Therefore, the study results indicate that the high arsenic removal efficiency of the in situ aquifer iron coating technology likely resulted from the expanded specific surface area of the small goethite particles, which enhanced arsenic sorption capability and/or from co-precipitation of arsenic on the surface of goethite particles. Copyright © 2015

  17. Fatty acid profile of the initial oral biofilm (pellicle): an in-situ study.

    Science.gov (United States)

    Reich, Marco; Kümmerer, Klaus; Al-Ahmad, Ali; Hannig, Christian

    2013-09-01

    The first step of bioadhesion on dental surfaces is the formation of the acquired pellicle. This mainly acellular layer is formed instantaneously on all solid surfaces exposed to oral fluids. It is composed of proteins, glycoproteins and lipids. However, information on the lipid composition is sparse. The aim of the present study was to evaluate the fatty acid (FA) profile of the in-situ pellicle for the first time. Furthermore, the impact of rinses with safflower oil on the pellicle's FA composition was investigated. Pellicles were formed in situ on bovine enamel slabs mounted on individual upper jaw splints. The splints were carried by ten subjects over durations of 3-240 min. After comprehensive sample preparation, gas chromatography coupled with electron impact ionization mass spectrometry (GC-EI/MS) was used in order to characterize qualitatively and quantitatively a wide range of FA (C12-C24). The relative FA profiles of the pellicle samples gained from different subjects were remarkably similar, whereas the amount of FA showed significant interindividual variability. An increase in FA in the pellicle was observed over time. The application of rinses with safflower oil resulted in an accumulation of its specific FA in the pellicle. Pellicle formation is a highly selective process that does not correlate directly with salivary composition, as shown for FA.

  18. Laboratory studies on natural restoration of ground water after in-situ leach uranium mining

    International Nuclear Information System (INIS)

    Bell, N.E.; Deutsch, W.J.; Serne, R.J.

    1983-05-01

    When uranium is mined using in-situ leach techniques, the chemical quality of the ground water in the ore-zone aquifer is affected. This could lead to long-term degradation of the ground water if restoration techniques are not applied after the leaching is completed. Pacific Northwest Laboratory (PNL), is conducting an NRC-sponsored research project on natural restoration and induced-restoration techniques. Laboratory studies were designed to evaluate the ability of the natural system (ore-zone sediments and groundwater) to mitigate the effects of mining on aquifer chemistry. Using batch and flow-through column experiments [performed with lixiviant (leaching solution) and sediments from the reduced zone of an ore-zone aquifer], we found that the natural system can lower uranium and bicarbonate concentrations in solutions and reduce the lixiviant redox potential (Eh). The change in redox potential could cause some of the contaminants that were dissolved during the uranium leaching operation to precipitate, thereby lowering their solution concentration. The concentrations of other species such as calcium, potassium, and sulfate increased, possibly as a result of mineral dissolution and ion exchange. In this paper, we describe the experimentally determined mobility of contaminants after in-situ leach mining, and discuss the possible chemical process affecting mobility

  19. Prioritising in situ conservation of crop resources: a case study of African cowpea (Vigna unguiculata).

    Science.gov (United States)

    Moray, C; Game, E T; Maxted, N

    2014-06-17

    Conserving crop wild relatives (CWR) is critical for maintaining food security. However, CWR-focused conservation plans are lacking, and are often based on the entire genus, even though only a few taxa are useful for crop improvement. We used taxonomic and geographic prioritisation to identify the best locations for in situ conservation of the most important (priority) CWR, using African cowpea (Vigna unguiculata (L.) Walp.) as a case study. Cowpea is an important crop for subsistence farmers in sub-Saharan Africa, yet its CWR are under-collected, under-conserved and under-utilised in breeding. We identified the most efficient sites to focus in situ cowpea CWR conservation and assessed whether priority CWR would be adequately represented in a genus-based conservation plan. We also investigated whether priority cowpea CWR are likely to be found in existing conservation areas and in areas important for mammal conservation. The genus-based method captured most priority CWR, and the distributions of many priority CWR overlapped with established conservation reserves and targets. These results suggest that priority cowpea CWR can be conserved by building on conservation initiatives established for other species.

  20. In-situ study of hydriding kinetics in Pd-based thin film systems

    Energy Technology Data Exchange (ETDEWEB)

    Delmelle, Renaud; Proost, Joris [Univ. Catholique de Louvain, Louvain-la-Neuve (Belgium). Div. of Materials and Process Engineering

    2010-07-01

    The hydriding kinetics of Pd thin films has been investigated in detail. The key experimental technique used in this work consists of a high resolution curvature measurement setup, which continuously monitors the reflections of multiple laser beams coming off a cantilevered sample. After mounting the sample inside a vacuum chamber, a H-containing gas mixture is introduced to instantaneously generate a given hydrogen partial pressure (p{sub H2}) inside the chamber. The resulting interaction of H with the Pd layer then leads to a volume expansion of the thin film system. This induces in turn changes in the sample curvature as a result of internal stresses developing in the Pd film during a hydriding cycle. Based on such curvature date obtained in-situ at different p{sub H2}, a two-step model for the kinetics of Pd-hydride formation has been proposed and expressions for the hydrogen adsorption and absorption velocities have been derived. The rate-limiting steps have been identified by studying the p{sub H2}-dependence of these velocities. Furthermore, from our in-situ experimental data, relevant kinetic parameters have been calculated. The effect of dry air exposure of the Pd films on the hydriding kinetics has been considered as well. (orig.)

  1. Fluorescence in situ hybridization and molecular studies in infertile men with dysplasia of the fibrous sheath.

    Science.gov (United States)

    Baccetti, Baccio; Collodel, Giulia; Gambera, Laura; Moretti, Elena; Serafini, Francesca; Piomboni, Paola

    2005-07-01

    To perform fluorescence in situ hybridization (FISH) and molecular analysis in patients with the genetic sperm defect "dysplasia of the fibrous sheath" (DFS). Retrospective study. Regional Referral Center for Male Infertility, Siena, Italy. Twelve infertile patients with DFS sperm defects. Family history, lymphocytic karyotype, physical and hormonal assays, semen analysis. The DFS sperm phenotype was defined by light, fluorescent, and electron microscopy. Sperm chromosomal constitution was examined by FISH. Gene deletions were tested by polymerase chain reaction. The genetic sperm defect DFS was determined by transmission and scanning electron microscopy. Immunofluorescence staining of A-kinase anchoring protein 4 (AKAP4) showed a moderate and diffuse signal, revealing a disorganized and incompletely assembled fibrous sheath. In 11 of 12 DFS patients, polymerase chain reaction for detecting the presence of partial sequence of AKAP4/AKAP3 binding regions gave positive results. Fluorescence in situ hybridization was performed in decondensed sperm nuclei with probes for chromosomes 18, X, and Y. The mean disomy frequency of chromosome 18 was in the normal range, whereas the mean disomy frequencies of sex chromosomes and diploidies were twice those of controls. These results should be considered when DFS sperm are used in assisted reproductive technology, owing to the high risk of transmission of chromosomal unbalance and of DFS sperm defects to male offspring.

  2. Laboratory studies on natural restoration of ground water after in-situ leach uranium mining

    Energy Technology Data Exchange (ETDEWEB)

    Bell, N.E.; Deutsch, W.J.; Serne, R.J.

    1983-05-01

    When uranium is mined using in-situ leach techniques, the chemical quality of the ground water in the ore-zone aquifer is affected. This could lead to long-term degradation of the ground water if restoration techniques are not applied after the leaching is completed. Pacific Northwest Laboratory (PNL), is conducting an NRC-sponsored research project on natural restoration and induced-restoration techniques. Laboratory studies were designed to evaluate the ability of the natural system (ore-zone sediments and groundwater) to mitigate the effects of mining on aquifer chemistry. Using batch and flow-through column experiments (performed with lixiviant (leaching solution) and sediments from the reduced zone of an ore-zone aquifer), we found that the natural system can lower uranium and bicarbonate concentrations in solutions and reduce the lixiviant redox potential (Eh). The change in redox potential could cause some of the contaminants that were dissolved during the uranium leaching operation to precipitate, thereby lowering their solution concentration. The concentrations of other species such as calcium, potassium, and sulfate increased, possibly as a result of mineral dissolution and ion exchange. In this paper, we describe the experimentally determined mobility of contaminants after in-situ leach mining, and discuss the possible chemical process affecting mobility.

  3. Growth studies of CVD-MBE by in-situ diagnostics

    Science.gov (United States)

    Maracas, George N.; Steimle, Timothy C.

    1992-10-01

    This is the final technical report for the three year DARPA-URI program 'Growth Studies of CVD-MBE by in-situ Diagnostics'. The goals of the program were to develop non-invasive, real time epitaxial growth monitoring techniques and combine them to gain an understanding of processes that occur during MBE growth from gas sources. We have adapted these techniques to a commercially designed gas source MBE system (Vacuum Generators Inc.) to facilitate technology transfer out of the laboratory into industrial environments. The in-situ measurement techniques of spectroscopic ellipsometry (SE) and laser induced fluorescence (LIF) have been successfully implemented to monitor the optical and chemical properties of the growing epitaxial film and the gas phase reactants. The ellipsometer was jointly developed with the J. Woolam Co. and has become a commercial product. The temperature dependence of group 3 and 5 desorption from GaAs and InP has been measured as well as the incident effusion cell fluxes. The temporal evolution of the growth has also been measured both by SE and LIF to show the smoothing of heterojunction surfaces during growth interruption. Complicated microcavity optical device structures have been monitored by ellipsometry in real time to improve device quality. This data has been coupled with the structural information obtained from reflection high energy electron diffraction (RHEED) to understand the growth processes in binary and ternary bulk 3-5 semiconductors and heterojunctions.

  4. Prevention of dental erosion of a sports drink by nano-sized hydroxyapatite in situ study.

    Science.gov (United States)

    Min, Ji Hyun; Kwon, Ho Keun; Kim, Baek Il

    2015-01-01

    To evaluate the inhibitory effects of the sports drink containing nano-sized hydroxyapatite (nano-HA) on dental erosion in situ. The study had a single-blind, two-treatment crossover design. The two treatment groups were a control group (CG; Powerade only) and an experimental group (EG; 0.25% wt/vol nano-HA was added to Powerade). Ten subjects wore removable palatal appliances containing bovine enamel specimens. The appliances were immersed in each drink for 10 mins, 4 times a day for 10 days. The tooth surface microhardness (SMH) was tested, and the erosion depth and the morphology of the tooth surface were observed. The data were analysed by repeated measures anova and t-test. Between the baseline and the 10th day, SMH was decreased by 80% in the specimens of the CG (P erosion depth of 12.70 ± 4.66 μm and an irregular tooth surface were observed on the 10th day in the specimens of the CG. No dental erosions, however, was observed in the specimens of the EG. The sports drink containing 0.25% nano-HA was effective in preventing dental erosion in situ. © 2014 BSPD, IAPD and John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

  5. Oxide ion diffusion mechanism related to Co and Fe ions in (Ba0.5Sr0.5)(Co0.8Fe0.2)O3-δ using in-situ X-ray absorption spectroscopy

    Science.gov (United States)

    Itoh, Takanori; Imai, Hideto

    2018-03-01

    The time changes of the white line and pre-edge intensities of Co and Fe K-edge in (Ba0.5Sr0.5)(Co0.8Fe0.2)O3-δ (BSCF) were observed to estimate the oxide ion diffusion related to Co and Fe ions by using in - situ X-ray absorption spectroscopy (XAS) during oxidation. The 20 μm self-standing BSCF film was prepared for in - situ XAS measurements. The time changes of absorption were fitted to the exponential decay function with two terms. The longer relaxation time (τ), related to the oxide ion diffusion during the oxidation of BSCF, is dependent on temperature. The oxide ion diffusion coefficients (D) were calculated from the τ s estimated by in - situ XAS. The values of the activation energy (Ea) for D related to Co K-edge white line, Co pre-edge, and Fe pre-edge were 1.8-2.0 eV. The value of Ea for D related to Fe K-edge white line, however, was higher than other absorption values at approximately 2.3 eV. We discussed the oxide ion diffusion mechanism related to Co and Fe ions in BSCF using in - situ XAS.

  6. Micro-CT in situ study of carbonate rock microstructural evolution for geologic CO2 storage

    DEFF Research Database (Denmark)

    Zheng, Yi; Yang, Yan; Rogowska, M.

    2017-01-01

    to achieve this is to find a suitable condition to create a stable 3D space in carbonate rock by injecting liquid to prepare space for the later CO2 injection. Micro-CT imaging is a non-destructive 3D method that can be used to study the property changes of carbonate rocks during and after CO2 injection....... The advance in lab source based micro-CT has made it capable of in situ experiments. We used a commercial bench top micro-CT (Zeiss Versa XRM410) to study the microstructure changes of chalk during liquid injection. Flexible temporal CT resolution is essential in this study because that the time scales...... of coupled physical and chemical processes can be very different. The results validated the feasibility of using a bench top CT system with a pressure cell to monitor the mesoscale multiphase interactions in chalk....

  7. HER-2 gene amplification by chromogenic in situ hybridisation (CISH) compared with fluorescence in situ hybridisation (FISH) in breast cancer-A study of two hundred cases.

    Science.gov (United States)

    Sáez, A; Andreu, F J; Seguí, M A; Baré, M L; Fernández, S; Dinarés, C; Rey, M

    2006-08-01

    The purpose of the study was to compare two methods used to analyse HER-2 gene amplification (fluorescence in situ hybridisation (FISH) and chromogenic in situ hybridisation (CISH)), and determine the accuracy of the antibodies CB11 and HercepTest for immunohistochemical detection of HER-2 overexpression from archival breast cancer tissue. Additionally, interobserver variability in the interpretation of CISH and immunohistochemical tests was measured. Two hundred cases of invasive breast carcinoma diagnosed between 2000 and 2003 were selected. Immunohistochemistry (IHC) was performed with HercepTest and CB11, and gene amplification was determined by FISH (PathVision, Vysis) and CISH (Zymed) using tissue macroarrays. An excellent concordance (94.8%) was found between CISH and FISH. Considering FISH as gold standard, sensitivity of CISH was 97.5% and specificity 94%. Overall interobserver agreement of CISH was 97.5% and of IHC 84%. Both antibodies showed a sensitivity of 95.2% and a specificity of 70.7% (CB11) and 81.2% (HercepTest). Our results show that CISH is a highly accurate, reproducible and practical technique to determine HER-2 gene amplification. CB11 and HercepTest are good screening methods with a high sensitivity. The performance of tissue macroarrays to test HER-2 status by IHC, FISH and CISH has demonstrated to be an available and effective method to study large series of tumours.

  8. In situ experimental study for the optimization of chlorine dosage in seawater cooling systems

    Energy Technology Data Exchange (ETDEWEB)

    Nebot, E.; Casanueva, T.; Fernandez-Baston, M.M.; Sales, D. [Department of Chemical Engineering, Food Technology and Environmental Technologies, University of Cadiz (Spain); Casanueva, J.F. [Department of Thermal Engines, University of Cadiz (Spain)

    2006-11-15

    The paper details an in situ study for the evaluation of the evolution of fouling heat transfer resistance and to optimize the antifouling chlorine dosage at a 550MW power station. A portable pilot plant has been designed to simulate the steam surface condenser and used as an accurate fouling monitor that takes the seawater from the same intake point as the power station. This study includes fouling extraction and its characterization for different dosage patterns. The residual chlorine concentration at the cooling-water discharge from the power station is 0.2mg/l and has been considered appropriate for the prevention of the formation of fouling, because with this concentration approximately 90% reduction in the amount of fouling is obtained. Residual chlorine dosages lower than 0.2ppm could be effective in controlling fouling development if mechanical techniques of fouling control are also available. (author)

  9. In situ experimental study of subduction zone fluids using diamond anvil cells

    Science.gov (United States)

    Bureau, H.; Foy, E.; Somogyi, A.; Munsch, P.; Simon, G.; Kubsky, S.

    2008-12-01

    Experiments carried out in diamond anvil cells combined with in situ synchrotron light source measurements represent the only one issue to observe and study fluid equilibria in real time, at the pressure and temperature conditions of the subduction zones. We will present new results recently obtained at the DIFFABS beam line (SOLEIL Synchrotron) aiming at studying equilibria between silica-rich hydrous melts and aqueous fluids in the presence of U, Th, Pb, Ba and Br. We used synchrotron X-Ray fluorescence analysis performed in situ in Bassett-modified hydrothermal diamond anvil cells in order to monitor the chemical transfers of the studied elements between the phases in equilibrium at different pressures (up to 1.6 GPa) and temperatures (up to 900°C). We have calculated the partition coefficients for each studied element (i): Difluid/melt = Cifluid/Cimelt. Results show that U and Th exhibit more affinities for the silica-rich hydrous fluids in the presence or absence of Br, considered here such as an analogue for Cl, (i.e. 0.4 > 10 after decompression) this coefficient decreases with pressure suggesting that Br would not be immediately washed out from the subducted plate during dehydration but may be recycled deeper in the mantle. These new data combined with previous ones obtained for Pb, Ba (Bureau et al., 2007, HPR vol 27, p. 235) and Rb, Sr, Zr (Bureau et al., 2004, Eos Trans. AGU, 85(47), V11C-05), allow us to propose a general outline of the fluid phase transfers through the subduction factory: (1) at shallow level: their nature and composition, the impact of the presence of halogens and the fertilizing role of such fluids in the mantle wedge, where the generation of arc magmas takes place (2) deeper in the mantle: where hydrous silica-rich supercritical fluids may also favour a deep recycling of a fraction of volatiles and trace elements present in the subducted oceanic crust.

  10. Multiphoton microscopy: an efficient tool for in-situ study of cultural heritage artifacts

    Science.gov (United States)

    Latour, Gaël.; Echard, Jean-Philippe; Didier, Marie; Schanne-Klein, Marie-Claire

    2013-05-01

    We present multimodal nonlinear optical imaging of historical artifacts by combining Two-Photon Excited Fluorescence (2PEF) and Second Harmonic Generation (SHG) microscopies. Three-dimensional (3D) non-contact laser-scanning imaging with micrometer resolution is performed without any preparation of the objects under study. 2PEF signals are emitted by a wide range of fluorophores such as pigments and binder, which can be discriminated thanks to their different emission spectral bands by using suitable spectral filters in the detection channel. SHG signals are specific for dense non-centrosymmetric organizations such as the crystalline cellulose within the wood cell walls. We also show that plaster particles exhibit SHG signals. These particles are bassanite crystals with a non-centrosymmetric crystalline structure, while the other types of calcium sulphates exhibit a centrosymmetric crystalline structure with no SHG signal. In our study, we first characterize model single-layered samples: wood, gelatin-based films containing plaster or cochineal lake and sandarac film containing cochineal lake. We then study multilayered coating systems on wood and show that multimodal nonlinear microscopy successfully reveals the 3D distribution of all components within the stratified sample. We also show that the fine structure of the wood can be assessed, even through a thick multilayered varnish coating. Finally, in situ multimodal nonlinear imaging is demonstrated in a historical violin. SHG/2PEF imaging thus appears as an efficient non-destructive and contactless 3D imaging technique for in situ investigation of historical coatings and more generally for wood characterization and coating analysis at micrometer scale.

  11. In situ and Ex situ Annealing Studies of Hydrothermally Synthesized SrFe12O19 Nano Platelets

    DEFF Research Database (Denmark)

    Gjørup, Frederik; Saura-Múzquiz, Matilde; Ahlburg, Jakob

    Strontium hexaferrite is a chemically stable and cheap magnetic compound, free of rare-earth metals. Previous studies have shown that nanostructuring can improve the magnetic performance of strontium hexaferrite, both as a powder and after pellet compaction, which allows for better bulk magnets f...

  12. Applications of in situ optical measurements in ecological and biogeochemical studies - a framework for a user-driven national network

    Science.gov (United States)

    Bergamaschi, B. A.; Pellerin, B. A.; Downing, B. D.; Saraceno, J.; Aiken, G.; Stumpner, P.

    2010-12-01

    A critical challenge for understanding the dynamics between water quality, and ecological processes is obtaining data at time scales in which changes occur. Traditional, discrete sampling, approaches for data collection are often limited by analytical and field costs, site access, and logistical challenges, for long-term sampling at a large number of sites. The timescales of change, however, are often minutes, hours, or years. In situ optical (absorbance and fluorescence) instruments offer opportunities to help overcome these difficulties by directly or indirectly measuring constituents of interest. In situ optical instrumentation have been in use in oceanographic studies for well over 50 years, and as advances in the science, engineering and technology of these sensors have improved, optical sensors have become more commercially viable and available for research. We present several examples that highlight applications of in situ optical measurements for understanding dynamics in stream, river, and estuary systems. Examples illustrate the utility of in situ optical sensors for studies over short-duration events of days to weeks (diurnal cycles, tidal cycles, storm events and snowmelt periods) as well as longer-term continuous monitoring for months to years. We also highlight applied in situ optical measurements as proxies for constituents that are difficult and expensive to measure at high spatiotemporal resolution, for example, dissolved organic carbon, dissolved organic nitrogen, mercury and methylmercury, trihalomethane precursors, harmful algal blooms, and others. We propose that relatively simple absorbance and fluorescence measurements made in situ could be incorporated into short and long-term ecological research and monitoring programs, resulting in advanced understanding of sources that contribute to water quality improvements or degradation, contaminant and carbon cycling, and the occurrence and persistence of harmful algal blooms. Linking these efforts

  13. 1913–2013 – The centennial of X-ray absorption spectroscopy (XAS): Evidences about a question still open

    Energy Technology Data Exchange (ETDEWEB)

    Mottana, Annibale, E-mail: annibale.mottana@uniroma3.it [Università degli Studi Roma Tre, Dipartimento di Scienze, Largo S. Leonardo Murialdo 1, I-00146 Roma (Italy); Istituto Nazionale di Fisica Nucleare, Laboratori Nazionali di Frascati, Via E. Fermi 40, I-00044 Frascati, RM (Italy)

    2014-10-15

    Highlights: • X-ray Absorption Spectroscopy (XAS) cannot be dated exactly as for its birth. • The assumed discoverer, M. de Broglie, was preceded by J. Herweg in the submission. • However, both their spectra were found to be mistaken. • Before the work of W. Stenström and H. Fricke no sure evidence of XAS is published. • The solution is, probably, taking October 1, 1918 as XAS fictitious birthday. - Abstract: In 1913 J. Herweg first (June 30) and M. de Broglie slightly later (November 17) claimed the discovery of a series of spots and lines closely following the main absorption edges of heavy metals, which they interpreted as the proof of the existence of X-ray spectra analogous to light spectra. In the following year they documented their discoveries via photographic plates. However, they were both discredited: Herweg by G.E.M. Jauncey, who showed that his spectra, taken on Pt and W, did not obey Moseley's rule; de Broglie by W.H. Bragg, M. Siegbahn and E. Wagner, who showed that his lines were in fact the fluorescence lines of the Ag and Br constituents of the photographic emulsion. Consequently, W. Stenström's description (sent to publisher on July 2, 1918) of certain photographically recorded and graphically rendered modulations near the M-series edges of heavy metals may possibly be the first published evidence of true X-ray absorption spectra. Indeed, they were interpreted as such by W. Kossel (1920) in his seminal theoretical paper. Otherwise, H. Fricke's table, although printed in 1920, which exhibits the photographic plate of sulphur absorption dated October 1, 1918, and its graphical rendering by a photometric method, is the first unequivocally dated evidence of recorded modulations at a XAS K-edge.

  14. In-situ TEM study of domain switching in GaN thin films

    Science.gov (United States)

    Wang, Baoming; Wang, Tun; Haque, Aman; Snure, Michael; Heller, Eric; Glavin, Nicholas

    2017-09-01

    Microstructural response of gallium nitride (GaN) films, grown by metal-organic chemical vapor deposition, was studied as a function of applied electrical field. In-situ transmission electron microscopy showed sudden change in the electron diffraction pattern reflecting domain switching at around 20 V bias, applied perpendicular to the polarization direction. No such switching was observed for thicker films or for the field applied along the polarization direction. This anomalous behavior is explained by the nanoscale size effects on the piezoelectric coefficients of GaN, which can be 2-3 times larger than the bulk value. As a result, a large amount of internal energy can be imparted in 100 nm thick films to induce domain switching at relatively lower voltages to induce such events at the bulk scale.

  15. Towards functionalization of graphene: in situ study of the nucleation of copper-phtalocyanine on graphene

    Science.gov (United States)

    Schwarz, Daniel; Henneke, Caroline; Kumpf, Christian

    2016-02-01

    Molecular films present an elegant way for the uniform functionalization or doping of graphene. Here, we present an in situ study on the initial growth of copper phthalocyanine (CuPc) on epitaxial graphene on Ir(111). We followed the growth up to a closed monolayer with low energy electron microscopy and selected area electron diffraction (μLEED). The molecules coexist on graphene in a disordered phase without long-range order and an ordered crystalline phase. The local topography of the graphene substrate plays an important role in the nucleation process of the crystalline phase. Graphene flakes on Ir(111) feature regions that are under more tensile stress than others. We observe that the CuPc molecules form ordered domains initially on those graphene regions that are closest to the fully relaxed lattice. We attribute this effect to a stronger influence of the underlying Ir(111) substrate for molecules adsorbed on those relaxed regions.

  16. Towards functionalization of graphene: in situ study of the nucleation of copper-phtalocyanine on graphene

    International Nuclear Information System (INIS)

    Schwarz, Daniel; Henneke, Caroline; Kumpf, Christian

    2016-01-01

    Molecular films present an elegant way for the uniform functionalization or doping of graphene. Here, we present an in situ study on the initial growth of copper phthalocyanine (CuPc) on epitaxial graphene on Ir(111). We followed the growth up to a closed monolayer with low energy electron microscopy and selected area electron diffraction (μLEED). The molecules coexist on graphene in a disordered phase without long-range order and an ordered crystalline phase. The local topography of the graphene substrate plays an important role in the nucleation process of the crystalline phase. Graphene flakes on Ir(111) feature regions that are under more tensile stress than others. We observe that the CuPc molecules form ordered domains initially on those graphene regions that are closest to the fully relaxed lattice. We attribute this effect to a stronger influence of the underlying Ir(111) substrate for molecules adsorbed on those relaxed regions. (paper)

  17. In situ surface and interface study of crystalline (3×1)-O on InAs

    Energy Technology Data Exchange (ETDEWEB)

    Qin, Xiaoye, E-mail: xxq102020@utdallas.edu; Wallace, Robert M., E-mail: rmwallace@utdallas.edu [Department of Materials Science and Engineering, University of Texas at Dallas, Richardson, Texas 75080 (United States); Wang, Wei-E.; Rodder, Mark S. [Advanced Logic Lab, Samsung Semiconductor, Inc., Austin, Texas 78754 (United States)

    2016-07-25

    The oxidation behavior of de-capped InAs (100) exposed to O{sub 2} gas at different temperatures is investigated in situ with high resolution of monochromatic x-ray photoelectron spectroscopy and low energy electron diffraction. The oxide chemical states and structure change dramatically with the substrate temperature. A (3 × 1) crystalline oxide layer on InAs is generated in a temperature range of 290–330 °C with a coexistence of In{sub 2}O and As{sub 2}O{sub 3}. The stability of the crystalline oxide upon the atomic layer deposition (ALD) of HfO{sub 2} is studied as well. It is found that the generated (3 × 1) crystalline oxide is stable upon ALD HfO{sub 2} growth at 100 °C.

  18. In-Situ TEM Study of Interface Sliding and Migration in an Ultrafine Lamellar Structure

    Energy Technology Data Exchange (ETDEWEB)

    Hsiung, L M

    2005-12-06

    The instability of interfaces in an ultrafine TiAl-({gamma})/Ti{sub 3}Al-({alpha}{sub 2}) lamellar structure by straining at room temperature has been investigated using in-situ straining techniques performed in a transmission electron microscope. The purpose of this study is to obtain experimental evidence to support the creep mechanisms based upon the interface sliding in association with a cooperative movement of interfacial dislocations previously proposed to interpret the nearly linear creep behavior observed from ultrafine lamellar TiAl alloys. The results have revealed that both the sliding and migration of lamellar interfaces can take place simultaneously as a result of the cooperative movement of interfacial dislocations.

  19. In-Situ X-ray Tomography Study of Cement Exposed to CO2 Saturated Brine

    DEFF Research Database (Denmark)

    Chavez Panduro, E. A.; Torsæter, M.; Gawel, K.

    2017-01-01

    For successful CO2 storage in underground reservoirs, the potential problem of CO2 leakage needs to be addressed. A profoundly improved understanding of the behavior of fractured cement under realistic subsurface conditions including elevated temperature, high pressure and the presence of CO2...... saturated brine is required. Here, we report in situ X-ray micro computed tomography (μ-CT) studies visualizing the microstructural changes upon exposure of cured Portland cement with an artificially engineered leakage path (cavity) to CO2 saturated brine at high pressure. Carbonation of the bulk cement......, self-healing of the leakage path in the cement specimen, and leaching of CaCO3 were thus directly observed. The precipitation of CaCO3, which is of key importance as a possible healing mechanism of fractured cement, was found to be enhanced in confined regions having limited access to CO2...

  20. In situ stresses in rock masses: methodology for its study in tunnel projects in Spain

    International Nuclear Information System (INIS)

    Madirolas Perez, G.; Perucho Martinez, A.

    2014-01-01

    In situ stress is one of the main factors to be taken into account in the design of tunnels, as it can cause inadmissible stresses and strains leading to high deviations in the budgets. For that reason, the stress state is directly introduced into the numerical models used for the design of tunnels. In Spain, although several tunnels have been carried out with an important overburden in tectonically relevant zones, a quantitative determination of the stresses has not been usually included in civil work projects. Therefore, it is considered necessary to implement a routine procedure of study of civil work projects involving tunnels excavated in rock, and a new detailed methodology is proposed. The challenge is that project managers, who face works in which stresses may play a determinant role, may have a practical reference enabling them to optimize available resources and to include the real stress information in the design of underground works. (Author)

  1. Spectroelectrochemical study of polyphenylene by in situ external reflection FT-IR spectroscopy. Pt. 2

    International Nuclear Information System (INIS)

    Kvarnstroem, C.; Ivaska, A.

    1994-01-01

    In situ external reflection FT-IR measurements are performed during cyclic voltammetric scans on electrochemically polymerized polyphenylene films. The films are polymerized either in 0.1 or 0.8 M biphenyl in 0.1 M TBABF 4 in acetonitrile. Changes in the IR spectrum of films of different thicknesses are studied when the films are potentially cycled from the neutral to the oxidized states of the polymer. No differences between films made in high or low dimer concentration can be observed in the spectra. The potential-dependent insertion and expulsion of solvent, residual water, anions and cations in and out of the film have different behaviour in films of different thicknesses. Changes in the structure of the segments in the film, from the benzenoid form into the quinoid form, can be followed. Differences between the first and subsequent cyclic potential scans are observed. (orig.)

  2. In situ Raman study of C60 polymerization during isothermal pressurizing at 800 K

    International Nuclear Information System (INIS)

    Talyzin, A V; Dubrovinsky, L S

    2004-01-01

    The first in situ Raman study of C 60 isothermal compression at 800 K and up to 32 GPa was performed using rhombohedral and tetragonal phases as starting materials. The rhombohedral phase shows a phase transition to 3D polymer above 10 GPa, similar to that in experiments where isobaric heating was used at pressures of 9-13 GPa. It is shown that the T-P diagram of C 60 polymeric phases (temperature increase followed by pressurizing) is significantly different from the known P-T diagram (pressurizing followed by heating). Tetragonal polymer exhibited significantly stronger stability and can be followed at least up to ∼15 GPa. Heating up to 800 K of tetragonal polymer at pressures of 6-8 GPa confirms that, due to geometrical frustrations, the tetragonal phase remains stable even at pressure and temperature conditions at which rhombohedral polymer is usually formed

  3. In situ neutron scattering study of nanostructured PbTe-PbS bulk thermoelectric material

    Energy Technology Data Exchange (ETDEWEB)

    Ren, Fei [Temple University; Schmidt, Robert D [ORNL; Case, Eldon D [Michigan State University, East Lansing; An, Ke [ORNL

    2016-01-01

    Nanostructures play an important role in thermoelectric materials. Their thermal stability, such as phase change and evolution at elevated temperatures, is thus of great interest to the thermoelectric community. In this study, in situ neutron diffraction was used to examine the phase evolution of nanostructured bulk PbTe-PbS materials fabricated using hot pressing and pulsed electrical current sintering (PECS). The PbS second phase was observed in all samples in the as-pressed condition. The temperature dependent lattice parameter and phase composition data show an initial formation of PbS precipitates followed by a redissolution during heating. The redissolution process started around 570 600 K, and completed at approximately 780 K. During cooling, the PECS sample followed a reversible curve while the heating/cooling behavior of the hot pressed sample was irreversible.

  4. In-situ studies of bulk deformation structures: Static properties under load and dynamics during deformation

    DEFF Research Database (Denmark)

    Jakobsen, Bo

    2006-01-01

    The main goal of the study presented in this thesis was to perform in-situ investigations on deformation structures in plastically deformed polycrystalline copper at low degrees of tensile deformation (model system for cell forming pure fcc metals. Anovel synchrotron...... grains in polycrystalline samples during tensile deformation. We have shown that the resulting 3D reciprocal space maps from tensile deformed copper comprise a pronounced structure, consisting of bright sharp peaks superimposed on a cloud of enhanced intensity. Based on the integrated intensity......, the width of the peaks, and spatial scanning experiments it is concluded that the individual peaks arise from individual dislocation-free regions (the subgrains) in the dislocation structure. The cloud is attributed to the dislocation rich walls. Samples deformed to 2% tensile strain were investigated under...

  5. In situ X-ray and neutron diffraction study of Ba2In2O5

    International Nuclear Information System (INIS)

    Speakman, S.A.; Misture, S.T.

    2001-01-01

    Order-disorder transitions in barium indate, Ba 2 In 2 O 5 , have been studied using in-situ X-ray and neutron diffraction. At room temperature, the crystal structure is an orthorhombic brownmillerite structure. At 706 C, the crystal structure is orthorhombic, possibly of the Imma or Ibm2 space groups. At 900 C, oxygen vacancies begin to disorder. The order-disorder transition occurs slowly in two steps over a temperature range of 900 - 925 C. Above this temperature range, the crystal structure is tetragonal, most likely belonging to the space group I 4/mcm. A second order-disorder transition begins at 1040 C, and proceeds over the temperature range 1040 - 1065 C. Above this temperature range, the crystal structure is a cubic, oxygen-deficient perovskite structure, with space group Pm3m. At an undetermined temperature above 1200 C, Ba 2 In 2 O 5 begins to decompose. (orig.)

  6. Reactive molecular beam epitaxial growth and in situ photoemission spectroscopy study of iridate superlattices

    Directory of Open Access Journals (Sweden)

    C. C. Fan

    2017-08-01

    Full Text Available High-quality (001-oriented perovskite [(SrIrO3m/(SrTiO3] superlattices (m=1/2, 1, 2, 3 and ∞ films have been grown on SrTiO3(001 epitaxially using reactive molecular beam epitaxy. Compared to previously reported superlattices synthesized by pulsed laser deposition, our superlattices exhibit superior crystalline, interface and surface structure, which have been confirmed by high-resolution X-ray diffraction, scanning transmission electron microscopy and atomic force microscopy, respectively. The transport measurements confirm a novel insulator-metal transition with the change of dimensionality in these superlattices, and our first systematic in situ photoemission spectroscopy study indicates that the increasing strength of effective correlations induced by reducing dimensionality would be the dominating origin of this transition.

  7. Donor-impurity related photoionization cross section in GaAs/Ga{sub 1−x}Al{sub x}As concentric double quantum rings: Effects of geometry and hydrostatic pressure

    Energy Technology Data Exchange (ETDEWEB)

    Baghramyan, H.M. [Department of Solid State Physics, Yerevan State University, Alex Manoogian 1, 0025 Yerevan (Armenia); Barseghyan, M.G., E-mail: mbarsegh@ysu.am [Department of Solid State Physics, Yerevan State University, Alex Manoogian 1, 0025 Yerevan (Armenia); Kirakosyan, A.A. [Department of Solid State Physics, Yerevan State University, Alex Manoogian 1, 0025 Yerevan (Armenia); Laroze, D. [Instituto de Alta Investigación, Universidad de Tarapacá, Casilla 7D, Arica (Chile); Duque, C.A. [Grupo de Materia Condensada-UdeA, Instituto de Física, Facultad de Ciencias Exactas y Naturales, Universidad de Antioquia UdeA, Calle 70 No. 52-21, Medellín (Colombia)

    2014-09-15

    The donor-impurity related photoionization cross section in GaAs/Ga{sub 1−x}Al{sub x}As three-dimensional concentric double quantum rings is investigated. The photoionization cross section dependence on the incident photon energy is studied considering the effects of hydrostatic pressure, variations of aluminum concentration, geometries of the structure, and impurity position. The interpretation of the dipole matrix element, which reflects the photoionization probability, is also given. We have found that these parameters can lead to both redshift and blueshift of the photoionization spectrum and also influence the cross section peak value.

  8. The effect of tissue decalcification on mRNA retention within bone for in-situ hybridization studies.

    Science.gov (United States)

    Walsh, L; Freemont, A J; Hoyland, J A

    1993-06-01

    Tissue decalcification is a routine part of the preparation of bone tissue for histological studies. Although in-situ hybridization has been employed to localize mRNA of collagenous and non-collagenous bone related proteins in skeletal tissue, little is known regarding the effects of decalcifying agents on mRNA retention within tissue. In this study in-situ hybridization using an oligonucleotide probe (i.e. a poly d(T) probe) to detect total messenger RNA has been employed to investigate the effects of the decalcifying agents nitric acid, formic acid and EDTA on mRNA retention compared to undeacalcified tissue. The results show that formalin fixation and EDTA decalcification preserve substantial amounts of mRNA within the tissue. In particular, this study illustrates that it is possible to perform in-situ hybridization on formalin fixed decalcified paraffin embedded tissue.

  9. [HER-2 oncogene amplification assessment in invasive breast cancer by dual-color in situ hybridization (dc-CISH): a comparative study with fluorescent in situ hybridization (FISH)].

    Science.gov (United States)

    Akhdar, Abbas; Bronsard, Marc; Lemieux, Renald; Geha, Sameh

    2011-12-01

    The amplification of the gene encoding for the human epidermal growth factor receptor 2 (HER-2 oncogene), located on chromosome 17 (17q21-q22), or the overexpression of this receptor have prognostic and therapeutic implications in invasive breast cancer. An evaluation of the HER-2 status by immunohistochemistry (IHC) is performed on all invasive breast cancer cases. Fluorescent in situ hybridization (FISH) is considered as the gold standard for the detection of HER-2 gene amplification for IHC equivocal cases (score 2+). A more recent in situ hybridization technique, the dual-color chromogenic in situ hybridization (dc-CISH), has been proposed as an alternative to FISH. The aim of this study was to measure the correlation between dc-CISH and FISH for HER-2 oncogene amplification assessment in invasive breast cancer. We built four tissue micro-array (TMA) blocs with 100 breast invasive cancer cases that had been previously tested by IHC for HER-2 detection: 10 score 0 cases, 10 score 3+cases, 39 score 1+and 41 score 2+cases. Both FISH and dc-CISH techniques were applied on all TMA cases as well as on two additional slides serving as controls. Interpretation of dc-CISH was carried out by a pathologist using an optical microscope. For FISH, the interpretation was done by a professional from the medical genetics department using a fluorescent microscope linked to a computer system for image capturing and analysis. The interpretation of the HER-2/CEN-17 ratio for both tests was in accordance with the values of the updated recommendations from the Canadian National Consensus Meeting on HER-2/neu testing in breast cancer and from the ASCO/CAP. Among the 100 cases initially included in the study, eight were excluded from the analysis due to sampling or technical flaws. From the 92 remaining cases, we obtained a concordance of 97.8% (90/92 cases) between the two techniques (Kappa coefficient 0.97, 95% confidence interval). The correlation coefficient (rho) between ratios

  10. [Study of the phase transformation of TiO2 with in-situ XRD in different gas].

    Science.gov (United States)

    Ma, Li-Jing; Guo, Lie-Jin

    2011-04-01

    TiO2 sample was prepared by sol-gel method from chloride titanium. The phase transformation of the prepared TiO2 sample was studied by in-situ XRD and normal XRD in different gas. The experimental results showed that the phase transformation temperatures of TiO2 were different under in-situ or normal XRD in different kinds of gas. The transformation of amorphous TiO2 to anatase was controlled by kinetics before 500 degrees C. In-situ XRD showed that the growth of anatase was inhibited, but the transformation of anatase to rutile was accelerated under inactive nitrogen in contrast to air. Also better crystal was obtained under hydrogen than in argon. These all showed that external oxygen might accelerate the growth of TiO2, but reduced gas might partly counteract the negative influence of lack of external oxygen. The mechanism of phase transformation of TiO2 was studied by in-situ XRD in order to control the structure in situ.

  11. Rheological Studies of Komatiite Liquids by In-Situ Falling Sphere Viscometry

    Science.gov (United States)

    O Dwyer, L.; Lesher, C. E.; Baxter, G.; Clark, A.; Fuss, T.; Tangeman, J.; Wang, Y.

    2005-12-01

    The rheological properties of komatiite liquids at high pressures and temperatures are being investigated by the in situ falling sphere technique, using the T-25 multianvil apparatus at the GSECARS 13 ID-D-D beamline at the Advanced Photon Source, ANL. The refractory and fluid nature of komatiite and other ultramafic liquids relevant to the Earth's deep interior, presents unique challenges for this approach. To reduce the density contrast between the melt and the marker sphere, and thus increase the Stoke's travel time, we have begun testing various composite spheres composed of refractory silicates and metals. Two successful custom designs are zirconia silicate mantled by Pt and Pt mantled by forsterite. These custom spheres contain sufficient Pt to absorb x-rays, while containing sufficient low-density refractory silicate so that marker sphere densities are in the range of 4-6 g/cc. These relatively more buoyant spheres increase travel time. These custom spheres, together with Re or Pt marker spheres, have been used to determine the viscosity of Gorgona anhydrous komatiite around 1600 ° C between 3.5 and 6 GPa. Initial experiments yield viscosities of 2.8 Pa s at 3.5 GPa, 5.3 Pa s at 4.6 GPa and 7.6 Pa s at 6 GPa. The observed positive pressure dependence of viscosity is consistent with recent results on pyrolite composition liquids and suggests that the activation volume for highly depolymerized melts will be positive for at least upper mantle conditions. The development of low-density, x-ray detectable marker spheres has applications in studies of melt density, whereby in situ detection of sink-float behavior during heating and compression cycles may be possible.

  12. In situ study of heavy ion induced radiation damage in NF616 (P92) alloy

    International Nuclear Information System (INIS)

    Topbasi, Cem; Motta, Arthur T.; Kirk, Mark A.

    2012-01-01

    Highlights: ► The ferritic–martensitic alloy NF616 was irradiated in situ with 1 MeV Kr ions at 50 K and 473 K. ► The defect cluster density increases with dose and saturates at ∼6 dpa at 50 K and 473 K. ► The defect size distributions do not change with dose at this temperature range. ► Results indicate that defect cluster formation and destruction is governed by cascade impact. - Abstract: NF616 is a nominal 9Cr ferritic–martensitic steel that is amongst the primary candidates for cladding and duct applications in the Sodium-Cooled Fast Reactor, one of the Generation IV nuclear energy systems. In this study, an in situ investigation of the microstructure evolution in NF616 under heavy ion irradiation has been conducted. NF616 was irradiated to 8.4 dpa at 50 K and to 7.6 dpa at 473 K with 1 MeV Kr ions. Nano-sized defects first appeared as white dots in dark-field TEM images and their areal density increased until saturation (∼6 dpa). Dynamic observations at 50 K and 473 K showed appearance and disappearance of TEM-visible defect clusters under irradiation that continued above saturation dose. Quantitative analysis showed no significant change in the average size (∼3–4 nm) and distribution of defect clusters with increasing dose at 50 K and 473 K. These results indicate a cascade-driven process of microstructure evolution under irradiation in these alloys that involves both the formation of TEM-visible defect clusters by various degrees of cascade overlap and cascade induced defect cluster elimination. According to this mechanism, saturation of defect cluster density is reached when the rate of defect cluster formation by overlap is equal to the rate of cluster elimination during irradiation.

  13. Corneal ectasia after myopic laser in situ keratomileusis: a long-term study

    Directory of Open Access Journals (Sweden)

    Spadea L

    2012-11-01

    Full Text Available Leopoldo Spadea,1 Emilia Cantera,2 Magdalena Cortes,2 Nicole Evangelista Conocchia,1 Charles WM Stewart11University of L’Aquila, Department of Biotechnological and Applied Clinical Sciences, Eye Clinic, L’Aquila, 2Villa Stuart Clinic, Department of Ophthalmic Sciences, Rome, ItalyBackground: The purpose of this study was to evaluate the long-term postoperative incidence of and key factors in the genesis of corneal ectasia after myopic laser-assisted in situ keratomileusis (LASIK in a large number of cases.Methods: A retrospective review of one surgeon's myopic LASIK database was performed. Patients were stratified into two groups based on date of surgery, ie, group 1 (1313 eyes from 1999 to 2001 and group 2 (2714 eyes from 2001 to 2003. Visual acuity, refraction, pachymetry, and corneal topography data were available for each patient from examinations performed both before and after the refractive procedures.Results: Of the 4027 surgically treated eyes, 23 (0.57% developed keratectasia during the follow-up period, which was a minimum seven years; nine eyes (0.69% were from group 1 and 14 eyes (0.51% were from group 2. The onset of corneal ectasia was at 2.57 ± 1.04 (range 1–4 years and 2.64 ± 1.29 (range 0.5–5 years, respectively, for groups 1 and 2. The most important preoperative risk factors using the Randleman Ectasia Risk Score System were manifest refractive spherical error in group 1 and a thin residual stromal bed in group 2. Each of the cases that developed corneal ectasia had risk factors that were identified.Conclusion: Ectasia was an uncommon outcome after an otherwise uncomplicated laser in situ keratomileusis procedure. The variables present in eyes developing postoperative LASIK ectasia can be better understood using the Randleman Ectasia Risk Score System.Keywords: corneal topography, Ectasia Risk Score System, keratectasia, myopia, LASIK

  14. Corrosion in Haas expanders with and without use of an antimicrobial agent: an in situ study

    Science.gov (United States)

    BAGATIN, Cristhiane Ristum; ITO, Izabel Yoko; ANDRUCIOLI, Marcela Cristina Damião; NELSON-FILHO, Paulo; FERREIRA, José Tarcísio Lima

    2011-01-01

    Objectives The purpose of this study was to evaluate in situ the occurrence of corrosion in the soldering point areas between the wire, silver brazing and band in Haas expanders. Material and Methods Thirty-four 7-12-year-old patients who needed maxillary expansion with a Haas expander were randomly assigned to two groups of 17 individuals each, according to the oral hygiene protocol adopted during the orthodontic treatment: Group I (control), toothbrushing with a fluoride dentifrice and Group II (experimental), toothbrushing with the same dentifrice plus 0.12% chlorhexidine gluconate (Periogard®) mouthrinses twice a week. The appliances were removed after approximately 4 months. Fragments of the appliances containing a metallic band with a soldered wire were sectioned at random for examination by stereomicroscopy, scanning electron microscopy (SEM) and energy dispersive x-ray spectroscopy (EDS). Data were analyzed statistically by Fisher's test at 5% significance level. Results The analysis by optical microscopy revealed areas with color change suggestive of corrosion in the soldering point areas joining the band and the wire in all specimens of both groups, with no statistically significant difference between the groups (p=1). The peaks of chemical elements (Ni, Fe, Cr, O, C and P) revealed by EDS were also similar in both groups. Conclusion: Color changes and peaks of chemical elements suggestive of corrosion were observed in the soldering point areas between the wire, silver brazing and band in both control and experimental groups, which indicate that the 0.12% chlorhexidine gluconate mouthrinses did not influence the occurrence of corrosion in situ. PMID:22231004

  15. In situ disinfection of sewage contaminated shallow groundwater: a feasibility study.

    Science.gov (United States)

    Bailey, Morgan M; Cooper, William J; Grant, Stanley B

    2011-11-01

    Sewage-contaminated shallow groundwater is a potential cause of beach closures and water quality impairment in marine coastal communities. In this study we set out to evaluate the feasibility of several strategies for disinfecting sewage-contaminated shallow groundwater before it reaches the coastline. The disinfection rates of Escherichia coli (EC) and enterococci bacteria (ENT) were measured in mixtures of raw sewage and brackish shallow groundwater collected from a coastal community in southern California. Different disinfection strategies were explored, ranging from benign (aeration alone, and aeration with addition of brine) to aggressive (chemical disinfectants peracetic acid (PAA) or peroxymonosulfate (Oxone)). Aeration alone and aeration with brine did not significantly reduce the concentration of EC and ENT after 6 h of exposure, while 4-5 mg L(-1) of PAA or Oxone achieved >3 log reduction after 15 min of exposure. Oxone disinfection was more rapid at higher salinities, most likely due to the formation of secondary oxidants (e.g., bromine and chlorine) that make this disinfectant inappropriate for marine applications. Using a Lagrangian modeling framework, we identify several factors that could influence the performance of in-situ disinfection with PAA, including the potential for bacterial regrowth, and the non-linear dependence of disinfection rate upon the residence time of water in the shallow groundwater. The data and analysis presented in this paper provide a framework for evaluating the feasibility of in-situ disinfection of shallow groundwater, and elucidate several topics that warrant further investigation. Copyright © 2011 Elsevier Ltd. All rights reserved.

  16. The Oxford-Diamond In Situ Cell for studying chemical reactions using time-resolved X-ray diffraction

    Science.gov (United States)

    Moorhouse, Saul J.; Vranješ, Nenad; Jupe, Andrew; Drakopoulos, Michael; O'Hare, Dermot

    2012-08-01

    A versatile, infrared-heated, chemical reaction cell has been assembled and commissioned for the in situ study of a range of chemical syntheses using time-resolved energy-dispersive X-ray diffraction (EDXRD) on Beamline I12 at the Diamond Light Source. Specialized reactor configurations have been constructed to enable in situ EDXRD investigation of samples under non-ambient conditions. Chemical reactions can be studied using a range of sample vessels such as alumina crucibles, steel hydrothermal autoclaves, and glassy carbon tubes, at temperatures up to 1200 °C.

  17. Characterization of Monodispersed Iron Oxide Nanocrystals by XAS and MCD measurement

    International Nuclear Information System (INIS)

    Kim, J.-Y.; Noh, H.-J.; Park, B.-G.; Kim, T.-Y.; Park, J.-H.; Hyeon, T.; Park, J.; Kang, E.

    2004-01-01

    Full text: Nanoparticles have attracted so much attention because of their potential technological applications and abundance of scientifically interesting issues. In particular, magnetic nanoparticles are considered to be applicable to various magnetic devices such as terabit memory, ferrofluids, magnetocaloric refrigeration systems, blood cells, etc. With the development of nano-technology, variation of physical properties as a function of particle size is one of the most important issues, but has been rarely explored because of difficulty of the size control in synthesizing nanoparticles. Recently, some of us successfully synthesized high crystalline and monodisperse maghemite nanoparticles without a size selection process and research in this field seems to be promoted by one step. In this report, we present a systematic characterization of the monodispersed nanocrystalline γ - Fe 2 O 3 with the diameter of 13, 8 and 4 nm by measuring the x-ray absorption spectroscopy (XAS) and the x-ray magnetic circular dichroism(XMCD) spectra on Fe L edge. The spectra of the 4 nm nanoparticles are very similar to those of maghemite (γ - Fe 2 O 3 ). However, the spectra become close to those of magnetite (Fe 3 O 4 ) as the particle size becomes 8 and 13 nm. Considering that the maghemite and magnetite have the same spinel structure with different Fe vacancies, these results can be explained that the surface of nanoparticles has more vacancies than the core part, indicating that surface disorder increases as the particle size decreases

  18. XAS Investigation of bio-relevant cobalt complexes in aqueous media

    International Nuclear Information System (INIS)

    Bresson, C.; Lamouroux, C.; Esnouf, S.; Solari, P.L.; Den Auwer, C.

    2006-01-01

    Cobalt is an essential element of biological cycles involved in numerous metallo-biomolecules, but it becomes a toxic element at high concentration or a radio-toxic element because of its use in the nuclear industry. 'Molecular speciation' in biological media is an essential prerequisite to evaluate its chemical behaviour as well as its toxic or beneficial effects. In this scheme, we have focused on the coordination properties of the thiol-containing amino acid cysteine (Cys) and the pseudo-peptide N-(2-mercapto-propionyl) glycine (MPG) towards the Co 2+ cation in aqueous media. XAS at the Co K edge and traditional spectroscopic techniques have been coupled in order to structurally characterize the cobalt coordination sphere. Oxidation states and geometries of the bis- and tris-cysteinato Co(III) complexes are in agreement with the literature data. In addition, bond lengths between the metallic centre and the donor atoms have been determined. The structure of a new dimeric N-(2-mercapto-propionyl) glycinato Co(II) complex in solution is also reported. The coordination of MPG to Co(II) through the thiolate and carboxylate functions is ascertained. This work provides fundamental structural information about bio-relevant complexes of cobalt, which will contribute to our understanding of the chemical behaviour and the biological role of this radionuclide. (authors)

  19. Development of Ta-based Superconducting Tunnel Junction X-ray Detectors for Fluorescence XAS

    International Nuclear Information System (INIS)

    Friedrich, S.; Drury, O.; Hall, J.; Cantor, R.

    2009-01-01

    We are developing superconducting tunnel junction (STJ) soft X-ray detectors for chemical analysis of dilute samples by fluorescence-detected X-ray absorption spectroscopy (XAS). Our 36-pixel Nb-based STJ spectrometer covers a solid angle (Omega)/4π ∼ 10 -3 , offers an energy resolution of ∼10-20 eV FWHM for energies up to ∼1 keV, and can be operated at total count rates of ∼10 6 counts/s. For increased quantum efficiency and cleaner response function, we have now started the development of Ta-based STJ detector arrays. Initial devices modeled after our Nb-based STJs have an energy resolution below 10 eV FWHM for X-ray energies below 1 keV, and pulse rise time discrimination can be used to improve their response function for energies up to several keV. We discuss the performance of the Ta-STJs and outline steps towards the next-generation of large STJ detector arrays with higher sensitivity.

  20. In situ optical emission study on the role of C2 in the synthesis of singlewalled carbon nanotubes

    CSIR Research Space (South Africa)

    Motaung, DE

    2010-01-01

    Full Text Available applications. In this study, the authors have applied in situ optical emission spectroscopy (OES) to study the plasma in the laser-furnace method to synthesize SWCNTs. In particular, the authors have investigated the temporal and spatial behavior of C2 as well...

  1. In situ X-ray probing reveals fingerprints of surface platinum oxide.

    Science.gov (United States)

    Friebel, Daniel; Miller, Daniel J; O'Grady, Christopher P; Anniyev, Toyli; Bargar, John; Bergmann, Uwe; Ogasawara, Hirohito; Wikfeldt, Kjartan Thor; Pettersson, Lars G M; Nilsson, Anders

    2011-01-07

    In situ X-ray absorption spectroscopy (XAS) at the Pt L(3) edge is a useful probe for Pt-O interactions at polymer electrolyte membrane fuel cell (PEMFC) cathodes. We show that XAS using the high energy resolution fluorescence detection (HERFD) mode, applied to a well-defined monolayer Pt/Rh(111) sample where the bulk penetrating hard X-rays probe only surface Pt atoms, provides a unique sensitivity to structure and chemical bonding at the Pt-electrolyte interface. Ab initio multiple-scattering calculations using the FEFF code and complementary extended X-ray absorption fine structure (EXAFS) results indicate that the commonly observed large increase of the white-line at high electrochemical potentials on PEMFC cathodes originates from platinum oxide formation, whereas previously proposed chemisorbed oxygen-containing species merely give rise to subtle spectral changes.

  2. Ultrahigh-vacuum in situ electrochemistry with solid polymer electrolyte and x-ray photoelectron spectroscopy studies of polypyrrole

    International Nuclear Information System (INIS)

    Skotheim, T.A.; Florit, M.I.; Melo, A.; O'Grady, W.E.

    1984-01-01

    A new in situ combined electrochemistry and x-ray-photoelectron-spectroscopy (XPS) technique using solid polymer electrolytes has been used to characterize electrically conducting films of polypyrrole perchlorate. The technique allows in situ electrochemical oxidation and reduction (doping and undoping) in ultrahigh vacuum and the simultaneous study of the polymer with XPS as a function of its electrochemical potential. We demonstrate that some anion species interact strongly electrostatically with the nitrogen heteroatoms. We also show conclusively that the electrochemistry of polypyrrole is highly irreversible

  3. Back to the Origin: In Situ Studies Are Needed to Understand Selection during Crop Diversification

    Directory of Open Access Journals (Sweden)

    Yolanda H. Chen

    2017-10-01

    Full Text Available Crop domestication has been embraced as a model system to study the genetics of plant evolution. Yet, the role of the environment, including biotic forces such as microbial and insect communities, in contributing to crop phenotypes under domestication and diversification has been poorly explored. In particular, there has been limited progress in understanding how human selection, agricultural cultivation (soil disturbance, fertilization, and irrigation, and biotic forces act as selective pressures on crop phenotypes. For example, geographically-structured pathogenic, pestiferous, and mutualistic interactions with crop plants have likely given rise to landraces that interact differently with local microbial and insect communities. In order to understand the adaptive role of crop traits, we argue that more studies should be conducted in the geographic centers of origin to test hypotheses on how abiotic, biotic, and human selective forces have shaped the phenotypes of domesticated plants during crop domestication and subsequent diversification into landraces. In these centers of origin, locally endemic species associated with wild ancestors have likely contributed to the selection on plant phenotypes. We address a range of questions that can only be studied in the geographic center of crop origin, placing emphasis on Mesoamerican polyculture systems, and highlight the significance of in situ studies for increasing the sustainability of modern agricultural systems.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-04-15

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

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

    International Nuclear Information System (INIS)

    Surrey, Alexander; Schultz, Ludwig; Rellinghaus, Bernd

    2017-01-01

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

  6. In-situ, time-lapse study of extracellular polymeric substance discharge in Streptococcus mutans biofilm.

    Science.gov (United States)

    Liu, Bernard Haochih; Yu, Li-Chieh

    2017-02-01

    Streptococcus mutans is one of the main pathogens that cause tooth decay. By metabolizing carbohydrates, S. mutans emits extracellular polymeric substance (EPS) that adheres to the tooth surface and forms layers of biofilm. Periodontal disease occurs due to the low pH environment created by S. mutans biofilm, and such an acidic environment gradually erodes tooth enamel. Since the existence of EPS is essential in the formation of biofilm, the in-situ investigation of its generation and distribution in real time is the key to the control and suppression of S. mutans biofilm. Prior studies of the biofilm formation process by fluorescence microscope, scanning electron microscope, or spectroscope have roughly divided the mechanism into three stages: (1) initial attachment; (2) microcolonies; and (3) maturation. However, these analytical methods are incapable to observe real-time changes in different locations of the extracellular matrix, and to analyze mechanical properties for single bacteria in micro and nanoscale. Since atomic force microscopy (AFM) operates by precise control of tip-sample interaction forces in liquid and in air, living microorganisms can be analyzed under near-physiological conditions. Thus, analytical techniques based on AFM constitute powerful tools for the study of biological samples, both qualitatively and quantitatively. In this study, we used AFM to quantitatively track the changes of multiple nanomechanical properties of S. mutans, including dissipation energy, adhesion force, deformation, and elastic modulus at different metabolic stages. The data revealed that the bacterial extracellular matrix has a gradient distribution in stickiness, in which different stickiness indicates the variation of EPS compositions, freshness, and metabolic stages. In-situ, time-lapse AFM images showed the local generation and distribution of EPS at different times, in which the highest adhesion distributed along sides of the S. mutans cells. Through time

  7. In situ degradation studies of two-dimensional WSe₂-graphene heterostructures.

    Science.gov (United States)

    Wang, B; Eichfield, S M; Wang, D; Robinson, J A; Haque, M A

    2015-09-14

    Heterostructures of two-dimensional materials can be vulnerable to thermal degradation due to structural and interfacial defects as well as thermal expansion mismatch, yet a systematic study does not exist in the literature. In this study, we investigate the degradation of freestanding WSe2-graphene heterostructures due to heat and charge flow by performing in situ experiments inside a transmission electron microscope. Experimental results show that purely thermal loading requires higher temperatures (>850 °C), about 150 °C higher than that under combined electrical and thermal loading. In both cases, selenium is the first element to decompose and migration of silicon atoms from the test structure to the freestanding specimen initiates rapid degradation through the formation of tungsten disilicide and silicon carbide. The role of the current flow is to enhance the migration of silicon from the sample holder and to knock-out the selenium atoms. The findings of this study provide fundamental insights into the degradation of WSe2-graphene heterostructures and inspire their application in electronics for use in harsh environments.

  8. Dual patch voltage clamp study of low membrane resistance astrocytes in situ.

    Science.gov (United States)

    Ma, Baofeng; Xu, Guangjin; Wang, Wei; Enyeart, John J; Zhou, Min

    2014-03-17

    Whole-cell patch clamp recording has been successfully used in identifying the voltage-dependent gating and conductance properties of ion channels in a variety of cells. However, this powerful technique is of limited value in studying low membrane resistance cells, such as astrocytes in situ, because of the inability to control or accurately measure the real amplitude of command voltages. To facilitate the study of ionic conductances of astrocytes, we have developed a dual patch recording method which permits membrane current and membrane potential to be simultaneously recorded from astrocytes in spite of their extraordinarily low membrane resistance. The utility of this technique is demonstrated by measuring the voltage-dependent activation of the inwardly rectifying K+ current abundantly expressed in astrocytes and multiple ionic events associated with astrocytic GABAA receptor activation. This protocol can be performed routinely in the study of astrocytes. This method will be valuable for identifying and characterizing the individual ion channels that orchestrate the electrical activity of low membrane resistance cells.

  9. Operable Unit 7-13/14 in situ thermal desorption treatability study work plan

    International Nuclear Information System (INIS)

    Shaw, P.; Nickelson, D.; Hyde, R.

    1999-01-01

    This Work Plan provides technical details for conducting a treatability study that will evaluate the application of in situ thermal desorption (ISTD) to landfill waste at the Subsurface Disposal Area (SDA) at the Idaho National Engineering and Environmental Laboratory (INEEL). ISTD is a form of thermally enhanced vapor vacuum extraction that heats contaminated soil and waste underground to raise its temperature and thereby vaporize and destroy most organics. An aboveground vapor vacuum collection and treatment system then destroys or absorbs the remaining organics and vents carbon dioxide and water to the atmosphere. The technology is a byproduct of an advanced oil-well thermal extraction program. The purpose of the ISTD treatability study is to fill performance-based data gaps relative to off-gas system performance, administrative feasibility, effects of the treatment on radioactive contaminants, worker safety during mobilization and demobilization, and effects of landfill type waste on the process (time to remediate, subsidence potential, underground fires, etc.). By performing this treatability study, uncertainties associated with ISTD as a selected remedy will be reduced, providing a better foundation of remedial recommendations and ultimate selection of remedial actions for the SDA

  10. An in-situ IR study on the adsorption of CO2 and H2O on hydrotalcites

    NARCIS (Netherlands)

    Coenen, K.T.; Gallucci, F.; Mezari, B.; Hensen, E.J.M.; van Sint Annaland, M.

    2018-01-01

    In-situ IR technique was used to study the reversible adsorption of CO2 and H2O at elevated temperatures on a potassium-promoted hydrotalcite for its use in sorption-enhanced water-gas shift (SEWGS). It was found that mainly bidentate carbonate species are responsible for the reversible (cyclic)

  11. ATR-IR spectroscopic cell for in situ studies at solid-liquid interface at elevated temperatures and pressures

    NARCIS (Netherlands)

    Koichumanova, Kamila; Visan, Aura; Geerdink, Bert; Lammertink, Rob G.H.; Mojet, Barbara; Seshan, Kulathuiyer; Lefferts, Leonardus

    2017-01-01

    An in situ ATR-IR spectroscopic cell suitable for studies at solid-liquid interface is described including the design and experimental details in continuous flow mode at elevated temperatures (230 °C) and pressures (30 bar). The design parameters considered include the cell geometry, the procedure

  12. Weldon Spring, Missouri, Raffinate Pits 1, 2, 3, and 4: Preliminary grout development screening studies for in situ waste immobilization

    International Nuclear Information System (INIS)

    McDaniel, E.W.; Gilliam, T.M.; Dole, L.R.; West, G.A.

    1987-04-01

    Results of Oak Ridge National Laboratory's initial support program to develop a preliminary grout formula to solidify in situ the Weldon Spring waste are presented. The screening study developed preliminary formulas based on a simulated composite waste and then tested the formulas on actual waste samples. Future data needs are also discussed. 1 ref., 6 figs., 9 tabs

  13. Expression and localization of ionotropic glutamate receptor subunits in the goldfish retina--an in situ hybridization and immunocytochemical study

    NARCIS (Netherlands)

    Vandenbranden, C. A.; Kamphuis, W.; Nunes Cardozo, B.; Kamermans, M.

    2000-01-01

    The expression and distribution of AMPA, kainate and NMDA glutamate receptor subunits was studied in the goldfish retina. For the immunocytochemical localization of the AMPA receptor antisera against GluR2, GluR2/3 and GluR4 were used, and for in situ hybridization rat specific probes for GluR1 and

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

    Science.gov (United States)

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

    2013-02-01

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

  15. Hybrid aerogels and bioactive aerogels under uniaxial compression: an in situ SAXS study

    Directory of Open Access Journals (Sweden)

    Esquivias, L.

    2010-12-01

    Full Text Available The complex structure of hybrid organic/inorganic aerogels is composed by an inorganic phase covalently bonded to an organic chain forming a copolymer. Conventional hybrid aerogels were studied as well as bioactive hybrid aerogels, that is, aerogels with a calcium active phase added. In this work, the relationship between mechanical response and nanostructure was studied, using a specifically designed sample-holder for in situ uniaxial compression obtaining at the same time the small-angle X-ray pattern from synchrotron radiation (SAXS. Structural elements can be described as a particulated silica core surrounded by the organic chains. These chains are compressed on the direction parallel to the load, and a relationship between macroscopic uniaxial compression and particle and pore deformations can be established.

    La compleja estructura de los aerogeles híbridos orgánico/inorgánicos está compuesta por una fase inorgánica de sílice, unida mediante enlaces covalentes a una red de cadenas orgánicas. Se han estudiado composites híbridos convencionales y bioactivos, esto es, con una fase activa de calcio añadida. En este trabajo se ha investigado la relación entre la respuesta mecánica y la nanoestructura, con ayuda de un portamuestras específicamente diseñado para el estudio in situ de muestras bajo compresión uniaxial, a la vez que se obtiene el espectro de rayos-X a bajo-ángulo de radiación sincrotrón (SAXS. Los elementos estructurales se pueden describir como núcleos particulados de sílice rodeados de las cadenas orgánicas. Estas, se comprimen en la dirección paralela a la carga pudiéndose establecer una relación entre la compresión uniaxial macroscópica y la deformación de las partículas y poros que forman la estructura.

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

  17. Diffusion of Radionuclides in Bentonite Clay - Laboratory and in situ Studies

    International Nuclear Information System (INIS)

    Jansson, Mats

    2002-12-01

    This thesis deals with the diffusion of ions in compacted bentonite clay. Laboratory experiments were performed to examine in detail different processes that affect the diffusion. To demonstrate that the results obtained from the laboratory investigations are valid under in situ conditions, two different kinds of in situ experiments were performed. Laboratory experiments were performed to better understand the impact of ionic strength on the diffusion of S 2+ and Cs + ions, which sorb to mineral surfaces primarily by ion exchange. Furthermore, surface related diffusion was examined and demonstrated to take place for Sr 2+ and Cs + but not for Co 2+ , which sorbs on mineral surfaces by complexation. The diffusion of anions in bentonite clay compacted to different dry densities was also investigated. The results indicate that anion diffusion in bentonite clay consists of two processes, one fast and another slower. We ascribe the fast diffusive process to intralayer diffusion and the slow process to diffusion in interparticle water, where anions are to some extent sorbed to edge sites of the montmorillonite. Two different types of in situ experiments were performed, CHEMLAB and LOT. CHEMLAB is a borehole laboratory, where cation (Cs + , Sr 2+ and Co 2+ ) and anion (I- and TcO 4 - ) diffusion experiments were performed using groundwater from a fracture in the borehole. In the LOT experiments cylindrical bentonite blocks surrounding a central copper rod were placed in a 4 m deep vertical borehole. The borehole was then sealed and the blocks are left for 1, 5 or >> 5 years. When the bentonite was water saturated the central copper rod is heated to simulate the temperature increase due to radioactive decay of the spent fuel. Bentonite doped with radioactive Cs and Co was placed in one of the lower blocks. Interestingly, the redox-sensitive pertechnetate ion (TcO 4 - ) which thermodynamically should be reduced and precipitate as TcO 2 n H 2 O, travelled unreduced through

  18. Cricothyroidotomy In Situ Simulation Curriculum (CRIC Study): Training Residents for Rare Procedures.

    Science.gov (United States)

    Petrosoniak, Andrew; Ryzynski, Agnes; Lebovic, Gerald; Woolfrey, Karen

    2017-04-01

    Technical skill acquisition for rare procedures can be challenging given the few real-life training opportunities. In situ simulation (ISS), a training technique that takes place in the actual workplace, is a promising method to promote environmental fidelity for rare procedures. This study evaluated a simulation-based technical skill curriculum for cricothyroidotomy using deliberate practice, followed by an ISS evaluation session. Twenty emergency medicine residents participated in a two-part curriculum to improve cricothryoidotomy performance. A pretest established participant baseline technical skill. The training session consisted of two parts, didactic teaching followed by deliberate practice using a task-training manikin. A posttest consisted of an unannounced, high-fidelity ISS, during an emergency department shift. The primary outcome was the mean performance time between the pretest and posttest sessions. Skill performance was also evaluated using a checklist scale and global rating scale. Cricothyroidotomy performance time improved significantly from pretest to posttest sessions (mean difference, 59 seconds; P training session consisting of didactic learning and deliberate practice, improved cricothyroidotomy skill performance was observed during an unannounced ISS in the emergency department. The integration of ISS in cricothyroidotomy training represents a promising approach; however, further study is needed to establish its role.

  19. In situ X-ray studies of film cathodes for solid oxide fuel cells

    International Nuclear Information System (INIS)

    Fuoss, Paul; Chang, Kee-Chul; You, Hoydoo

    2013-01-01

    Highlights: •Synchrotron X-rays are used to study in operando the structural and chemical changes of LSM and LSCF film cathodes during half-cell operations. •A-site and B-site cations actively segregate or desegregate on the changes of temperature, pO 2 , and electrochemical potential. •Chemical lattice expansions show that oxygen-cathode interface is the primary source of rate-limiting processes. •The surface and subsurface of the LSM and LSCF films have different oxidation-states due to vacancy concentration changes. •Liquid-phase infiltration and coarsening processes of cathode materials into porous YSZ electrolyte backbone were monitored by USAXS. -- Abstract: Synchrotron-based X-ray techniques have been used to study in situ the structural and chemical changes of film cathodes during half-cell operations. The X-ray techniques used include X-ray reflectivity (XR), total-reflection X-ray fluorescence (TXRF), high-resolution diffraction (HRD), ultra-small angle X-ray scattering (USAXS). The epitaxial thin film model cathodes for XR, TXRF, and HRD measurements are made by pulse laser deposition and porous film cathodes for USAX measurements are made by screen printing technique. The experimental results reviewed here include A-site and B-site segregations, lattice expansion, oxidation-state changes during cell operations and liquid-phase infiltration and coarsening of cathode to electrolyte backbone

  20. In-situ EXAFS study on the thermal decomposition of TiH2

    International Nuclear Information System (INIS)

    Zhou Yingli; Wu Min; An Pengfei; Zheng Lirong; Chu Shengqi; Zhang Jing; Hu Tiandou

    2014-01-01

    Thermal decomposition behaviors of TiH 2 powder under a flowing helium atmosphere and in a low vacuum condition have been studied using an in situ EXAFS technique. By an EXAFS analysis containing the multiple scattering paths including H atoms, the changes of the hydrogen stoichiometric ratio and the phase transformation sequence are obtained. The results demonstrate that the initial decomposition temperature is dependent on experimental conditions, which occurs, respectively, at about 300 and 400 °C in a low vacuum condition and under a flowing helium atmosphere. During the decomposition process of TiH 2 in a low vacuum condition, the sample experiences a phase change process: δ(TiH 2 ) → δ (TiH x ) → δ(TiH x )+ β(TiH x ) → δ(TiH x )+ β(TiH x ) + α(Ti) → β(TiH x ) + α(Ti) → α(Ti) + β(Ti). This study offers a way to detect the structural information of hydrogen. A detailed discussion about the decomposition process of TiH 2 is given in this paper. (authors)

  1. Bioreactor tests preliminary to landfill in situ aeration: A case study

    Energy Technology Data Exchange (ETDEWEB)

    Raga, Roberto, E-mail: roberto.raga@unipd.it [ICEA Department, University of Padova. Via Marzolo, 9, 35131 Padova (Italy); Cossu, Raffaello [ICEA Department, University of Padova. Via Marzolo, 9, 35131 Padova (Italy)

    2013-04-15

    Highlights: ► Carbon and nitrogen mass balances in aerated landfill simulation reactors. ► Waste stabilization in aerated landfill simulation reactors. ► Effect of temperature on biodegradation processes in aerated landfills. - Abstract: Lab scale tests in bioreactor were carried out in the framework of the characterization studies of a landfill where in situ aeration (possibly followed by landfill mining) had been proposed as part of the novel waste management strategy in a region in northern Italy. The tests were run to monitor the effects produced by aerobic conditions at different temperatures on waste sampled at different depths in the landfill, with focus on the carbon and nitrogen conversion during aeration. Temperatures ranging from 35 to 45 °C were chosen, in order to evaluate possible inhibition of biodegradation processes (namely nitrification) at 45 °C in the landfill. The results obtained showed positive effects of the aeration on leachate quality and a significant reduction of waste biodegradability. Although a delay of biodegradation processes was observed in the reactor run at 45 °C, biodegradation rates increased after 2 months of aeration, providing very low values of the relevant parameters (as in the other aerated reactors) by the end of the study. Mass balances were carried out for TOC and N-NH{sub 4}{sup +}; the findings obtained were encouraging and provided evidence of the effectiveness of carbon and nitrogen conversion processes in the aerated landfill simulation reactors.

  2. Contribution of in situ acoustic emission analysis coupled with thermogravimetry to study zirconium alloy oxidation

    International Nuclear Information System (INIS)

    Al Haj, O.; Peres, V.; Serris, E.; Cournil, M.; Grosjean, F.; Kittel, J.; Ropital, F.

    2015-01-01

    Zirconium alloy (zircaloy-4) corrosion behavior under oxidizing atmosphere at high temperature was studied using thermogravimetric experiment associated with acoustic emission analysis. Under a mixture of oxygen and air in helium, an acceleration of the corrosion is observed due to the detrimental effect of nitrogen which produces zirconium nitride. The kinetic rate increases significantly after a kinetic transition (breakaway). This acceleration is accompanied by an acoustic emission (AE) activity. Most of the acoustic emission bursts were recorded after the kinetic transition or during the cooling of the sample. Acoustic emission signals analysis allows us to distinguish different populations of cracks in the ZrO 2 layer. These cracks have also been observed by SEM on post mortem cross section of oxidized samples and by in-situ microscopy observations on the top surface of the sample during oxidation. The numerous small convoluted thin cracks observed deeper in the zirconia scale are not detected by the AE technique. From these studies we can conclude that mechanisms as irreversible mechanisms, as cracks initiation and propagation, generate AE signals

  3. Deformation of nanotubes in peeling contact with flat substrate: An in situ electron microscopy nanomechanical study

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Xiaoming; Zheng, Meng; Wei, Qing; Ke, Changhong, E-mail: cke@binghamton.edu [Department of Mechanical Engineering, State University of New York at Binghamton, Binghamton, New York 13902-6000 (United States); Signetti, Stefano [Laboratory of Bio-Inspired and Graphene Nanomechanics, Department of Civil, Environmental and Mechanical Engineering, University of Trento, Trento (Italy); Pugno, Nicola M. [Laboratory of Bio-Inspired and Graphene Nanomechanics, Department of Civil, Environmental and Mechanical Engineering, University of Trento, Trento (Italy); Centre for Materials and Microsystems, Fondazione Bruno Kessler, Povo (Trento) (Italy); School of Engineering and Materials Science, Queen Mary University of London, London (United Kingdom)

    2016-04-21

    Peeling of one-dimensional (1D) nanostructures from flat substrates is an essential technique in studying their adhesion properties. The mechanical deformation of the nanostructure in the peeling experiment is critical to the understanding of the peeling process and the interpretation of the peeling measurements, but it is challenging to measure directly and quantitatively at the nanoscale. Here, we investigate the peeling deformation of a bundled carbon nanotube (CNT) fiber by using an in situ scanning electron microscopy nanomechanical peeling technique. A pre-calibrated atomic force microscopy cantilever is utilized as the peeling force sensor, and its back surface acts as the peeling contact substrate. The nanomechanical peeling scheme enables a quantitative characterization of the deformational behaviors of the CNT fiber in both positive and negative peeling configurations with sub-10 nm spatial and sub-nN force resolutions. Nonlinear continuum mechanics models and finite element simulations are employed to interpret the peeling measurements. The measurements and analysis reveal that the structural imperfections in the CNT fiber may have a substantial influence on its peeling deformations and the corresponding peeling forces. The research findings reported in this work are useful to the study of mechanical and adhesion properties of 1D nanostructures by using nanomechanical peeling techniques.

  4. Bioreactor tests preliminary to landfill in situ aeration: A case study

    International Nuclear Information System (INIS)

    Raga, Roberto; Cossu, Raffaello

    2013-01-01

    Highlights: ► Carbon and nitrogen mass balances in aerated landfill simulation reactors. ► Waste stabilization in aerated landfill simulation reactors. ► Effect of temperature on biodegradation processes in aerated landfills. - Abstract: Lab scale tests in bioreactor were carried out in the framework of the characterization studies of a landfill where in situ aeration (possibly followed by landfill mining) had been proposed as part of the novel waste management strategy in a region in northern Italy. The tests were run to monitor the effects produced by aerobic conditions at different temperatures on waste sampled at different depths in the landfill, with focus on the carbon and nitrogen conversion during aeration. Temperatures ranging from 35 to 45 °C were chosen, in order to evaluate possible inhibition of biodegradation processes (namely nitrification) at 45 °C in the landfill. The results obtained showed positive effects of the aeration on leachate quality and a significant reduction of waste biodegradability. Although a delay of biodegradation processes was observed in the reactor run at 45 °C, biodegradation rates increased after 2 months of aeration, providing very low values of the relevant parameters (as in the other aerated reactors) by the end of the study. Mass balances were carried out for TOC and N-NH 4 + ; the findings obtained were encouraging and provided evidence of the effectiveness of carbon and nitrogen conversion processes in the aerated landfill simulation reactors

  5. Chloride influence on the formation of lanthanum hexaboride: An in-situ diffraction study

    Science.gov (United States)

    Mattox, Tracy M.; Groome, Chloe; Doran, Andrew; Beavers, Christine M.; Urban, Jeffrey J.

    2018-03-01

    LaB6 has been a material of interest for decades due to its thermionic emission, plasmonic properties, and low work function, and researchers continue to discover new properties even now. In order to meet growing interest in customizing these properties, it is important to gain better control over the system and a better understanding of the fundamental mechanism of LaB6 crystal growth and formation. Traditional synthetic methods require very high temperatures, at which point crystallization happens too quickly to be readily studied. Our discovery that LaB6 may be made using lower temperatures has made it possible to slow down crystal formation enough for lattice growth to be observed. We report here an in situ diffraction study of the reaction between LaCl3 and NaBH4. In observing the evolution of the (1 1 1), (1 1 0), and (2 0 0) lattice planes of LaB6, we have discovered that the Cl of LaCl3 has a strong influence on crystal formation, and that excess Cl, temperature and heating rate may all be used as tools to control the LaB6 final product.

  6. An in situ Raman study of the intercalation of supercapacitor-type electrolyte into microcrystalline graphite

    International Nuclear Information System (INIS)

    Hardwick, Laurence J.; Hahn, Matthias; Ruch, Patrick; Holzapfel, Michael; Scheifele, Werner; Buqa, Hilmi; Krumeich, Frank; Novak, Petr; Koetz, Ruediger

    2006-01-01

    An initial Raman study on the effects of intercalation for aprotic electrolyte-based electrochemical double-layer capacitors (EDLCs) is reported. In situ Raman microscopy is employed in the study of the electrochemical intercalation of tetraethylammonium (Et 4 N + ) and tetrafluoroborate (BF 4 - ) into and out of microcrystalline graphite. During cyclic voltammetry experiments, the insertion of Et 4 N + into graphite for the negative electrode occurs at an onset potential of +1.0 V versus Li/Li + . For the positive electrode, BF 4 - was shown to intercalate above +4.3 V versus Li/Li + . The characteristic G-band doublet peak (E 2g2 (i) (1578 cm -1 ) and E 2g2 (b) (1600 cm -1 )) showed that various staged compounds were formed in both cases and the return of the single G-band (1578 cm -1 ) demonstrates that intercalation was fully reversible. The disappearance of the D-band (1329 cm -1 ) in intercalated graphite is also noted and when the intercalant is removed a more intense D-band reappears, indicating possible lattice damage. For cation intercalation, such irreversible changes of the graphite structure are confirmed by scanning electron microscopy (SEM)

  7. Effect of different frequencies of fluoride dentifrice and mouthrinse administration: an in situ study

    Directory of Open Access Journals (Sweden)

    Daniela Correia Cavalcante Souza

    2010-12-01

    Full Text Available The effect of a combination of topical fluoridation methods for inhibition of enamel demineralization in the face of a cariogenic challenge has not been clearly established. This in situ crossover study aimed to assess whether the addition of daily use of fluoride mouthrinse (FR to that of fluoride dentifrice (FD is equivalent to increasing the frequency of FD application in terms of the effect on enamel demineralization and fluoride content. Over 3 phases of 14 days each, 12 volunteers wore appliances containing enamel blocks exposed to a 20 % sucrose solution 8 times/day. During each phase the blocks underwent one of the following treatments: 2x/day FD, 2x/day FD + 1x/day FR, and 3x/day FD. The blocks were assessed for hardness and fluoride content. Three x/day FD did not differ from 2x/day + 1x/day FR, however it enhanced demineralization protection when compared to 2x/day FD. All treatments produced an increase in enamel fluoride content compared to no treatment (sound blocks (p < 0.05, but the differences between them were not significant. The results of this study suggest that the daily use of fluoride mouthrinse combined with that of fluoride dentifrice has similar effects on enamel demineralization and fluoride content when compared to increasing the frequency of fluoride dentifrice use.

  8. In-Situ Synchrotron X-ray Study of the Phase and Texture Evolution of Ceria and Superconductor Films Deposited by Chemical Solution Method

    DEFF Research Database (Denmark)

    Yue, Zhao; Grivel, Jean-Claude; He, Dong

    2012-01-01

    In situ synchrotron x-ray diffraction is used to study the phase and texture formation of ceria based films and superconductor films deposited by the chemical solution method on technical substrates. Combined analysis using in situ synchrotron x-ray diffraction, thermogravimetry/differential ther......In situ synchrotron x-ray diffraction is used to study the phase and texture formation of ceria based films and superconductor films deposited by the chemical solution method on technical substrates. Combined analysis using in situ synchrotron x-ray diffraction, thermogravimetry...

  9. Field study of nitrous oxide production with in situ aeration in a closed landfill site.

    Science.gov (United States)

    Nag, Mitali; Shimaoka, Takayuki; Nakayama, Hirofumi; Komiya, Teppei; Xiaoli, Chai

    2016-03-01

    Nitrous oxide (N(2)O) has gained considerable attention as a contributor to global warming and depilation of stratospheric ozone layer. Landfill is one of the high emitters of greenhouse gas such as methane and N(2)O during the biodegradation of solid waste. Landfill aeration has been attracted increasing attention worldwide for fast, controlled and sustainable conversion of landfills into a biological stabilized condition, however landfill aeration impel N(2)O emission with ammonia removal. N(2)O originates from the biodegradation, or the combustion of nitrogen-containing solid waste during the microbial process of nitrification and denitrification. During these two processes, formation of N(2)O as a by-product from nitrification, or as an intermediate product of denitrification. In this study, air was injected into a closed landfill site and investigated the major N(2)O production factors and correlations established between them. The in-situ aeration experiment was carried out by three sets of gas collection pipes along with temperature probes were installed at three different distances of one, two and three meter away from the aeration point; named points A-C, respectively. Each set of pipes consisted of three different pipes at three different depths of 0.0, 0.75 and 1.5 m from the bottom of the cover soil. Landfill gases composition was monitored weekly and gas samples were collected for analysis of nitrous oxide concentrations. It was evaluated that temperatures within the range of 30-40°C with high oxygen content led to higher generation of nitrous oxide with high aeration rate. Lower O(2) content can infuse N(2)O production during nitrification and high O(2) inhibit denitrification which would affect N(2)O production. The findings provide insights concerning the production potentials of N(2)O in an aerated landfill that may help to minimize with appropriate control of the operational parameters and biological reactions of N turnover. Investigation of

  10. Photosynthetic activity, photoprotection and photoinhibition in intertidal microphytobenthos as studied in situ using variable chlorophyll fluorescence

    Science.gov (United States)

    Serôdio, João; Vieira, Sónia; Cruz, Sónia

    2008-06-01

    The photosynthetic activity of microphytobenthos biofilms was studied in situ on an intertidal mudflat of the Ria de Aveiro, Portugal. Time series of physical variables characterizing the microenvironment at the sediment photic zone (incident solar irradiance, temperature, salinity), photophysiological parameters and productive biomass of undisturbed microalgal assemblages were measured during daytime low-tide periods along one spring-neap tidal cycle, with the objective of (1) characterizing the short-term variability in photosynthetic activity in situ, (2) relating it with the changing environmental conditions and (3) with the operation of physiologically (xanthophyll cycle) and behaviorally (vertical migration) based photoprotective processes, and (4) assessing the occurrence of photoinhibition. Pulse Amplitude Modulated (PAM) fluorometry was applied to measure photosynthetic activity (the effective and maximum quantum yield of photosystem II, Δ F/ Fm' and Fv/ Fm; the photosynthesis index EFY; rapid light-response curves (RLC)), the photoprotective operation of the xanthophyll cycle and photoinhibition (non-photochemical quenching, NPQ; quantum efficiency of open RCs, Fv'/ Fm'), and vertical migration (productive biomass, Fo). The photosynthetic activity was found to be strongly affected by the cumulative light dose received during the morning low-tide periods. The fluorescence indices Δ F/ Fm', EFY, Fv'/ Fm' and RLC parameters were more depressed under high irradiances when clear sky was present during the morning low tide than when foggy conditions reduced the light dose received during a comparable period. Productive biomass exhibited maximum values in the first hours of the morning, followed by a steep decrease when irradiance reached moderate levels, due to the downward migration of the microalgae. This photophobic migratory response appeared to display a photoprotective role, allowing Δ F/ Fm' to remain near optimum values until irradiance reached

  11. Nuclear Waste Package Mockups: A Study of In-situ Redox State

    Science.gov (United States)

    Helean, K.; Anderson, B.; Brady, P. V.

    2006-05-01

    The Yucca Mountain Repository (YMR), located in southern Nevada, is to be the first facility in the U.S. for the permanent disposal of high-level radioactive waste and spent nuclear fuels. Total system performance assessment(TSPA) has indicated that among the major radionuclides contributing to dose are Np, Tc, and I. These three radionuclides are mobile in most geochemical settings, and therefore sequestering them within the repository horizon is a priority for the Yucca Mountain Project (YMP). Corroding steel may offset radionuclide transport processes within the proposed waste packages at YMR by retaining radionuclides, creating locally reducing conditions, and reducing porosity. Ferrous iron has been shown to reduce UO22+ to UO2s, and some ferrous iron-bearing ion-exchange materials have been shown to adsorb radionuclides and heavy metals. Locally reducing conditions may lead to the reduction and subsequent immobilization of problematic dissolved species such as TcO4-, NpO2+, and UO22+ and can also inhibit corrosion of spent nuclear fuel. Water occluded during corrosion produces bulky corrosion products, and consequently less porosity is available for water and radionuclide transport. The focus of this study is on the nature of Yucca Mountain waste package corrosion products and their effects on local redox conditions, radionuclide transport, and porosity. In order to measure in-situ redox, six small-scale (1:40) waste package mockups were constructed using A516 and 316 stainless steel, the same materials as the proposed Yucca Mountain waste packages. The mockups are periodically injected with a simulated groundwater and the accumulated effluent and corrosion products are evaluated for their Fe(II)/Fe(III) content and mineralogy. Oxygen fugacities are then calculated and, thus, in-situ redox conditions are determined. Early results indicate that corrosion products are largely amorphous Fe-oxyhydroxides, goethite and magnetite. That information together with the

  12. First in situ TOF-PET study using digital photon counters for proton range verification.

    Science.gov (United States)

    Cambraia Lopes, P; Bauer, J; Salomon, A; Rinaldi, I; Tabacchini, V; Tessonnier, T; Crespo, P; Parodi, K; Schaart, D R

    2016-08-21

    Positron emission tomography (PET) is the imaging modality most extensively tested for treatment monitoring in particle therapy. Optimal use of PET in proton therapy requires in situ acquisition of the relatively strong (15)O signal due to its relatively short half-life (~2 min) and high oxygen content in biological tissues, enabling shorter scans that are less sensitive to biological washout. This paper presents the first performance tests of a scaled-down in situ time-of-flight (TOF) PET system based on digital photon counters (DPCs) coupled to Cerium-doped Lutetium Yttrium Silicate (LYSO:Ce) crystals, providing quantitative results representative of a dual-head tomograph that complies with spatial constraints typically encountered in clinical practice (2  ×  50°, of 360°, transaxial angular acceptance). The proton-induced activity inside polymethylmethacrylate (PMMA) and polyethylene (PE) phantoms was acquired within beam pauses (in-beam) and immediately after irradiation by an actively-delivered synchrotron pencil-beam, with clinically relevant 125.67 MeV/u, 4.6  ×  10(8) protons s(-1), and 10(10) total protons. 3D activity maps reconstructed with and without TOF information are compared to FLUKA simulations, demonstrating the benefit of TOF-PET to reduce limited-angle artefacts using a 382 ps full width at half maximum coincidence resolving time. The time-dependent contributions from different radionuclides to the total count-rate are investigated. We furthermore study the impact of the acquisition time window on the laterally integrated activity depth-profiles, with emphasis on 2 min acquisitions starting at different time points. The results depend on phantom composition and reflect the differences in relative contributions from the radionuclides originating from carbon and oxygen. We observe very good agreement between the shapes of the simulated and measured activity depth-profiles for post-beam protocols. However, our results

  13. An in situ caries study on the interplay between fluoride dose and concentration in milk.

    Science.gov (United States)

    Lippert, F; Martinez-Mier, E A; Zero, D T

    2014-07-01

    This randomized, cross-over in situ study investigated the impact of sodium fluoride dose and concentration in milk on caries lesion rehardening, fluoridation and acid resistance. Twenty-eight subjects wore two gauze-covered enamel specimens with preformed lesions placed buccally on their mandibular partial dentures for three weeks. Participants used fluoride-free dentifrice throughout the study and consumed once daily one of the five study treatments: no fluoride in 200 ml milk (0F-200), 1.5 or 3 mg fluoride in either 100 (1.5F-100; 3F-100) or 200 ml milk (1.5F-200; 3F-200). After three weeks, specimens were retrieved. Knoop hardness was used to determine rehardening and resistance to a secondary acid challenge. Enamel fluoride uptake (EFU) was determined using a microbiopsy technique. A linear fluoride dose-response was observed for all study variables which exhibited similar overall patterns. All the treatments resulted in rehardening, with 0F-200 inducing the least and 3F-100 the most. Apart from 1.5F-200, all the treatments resulted in statistically significantly more rehardening compared to 0F-200. The fluoride doses delivered in 100 ml provided directionally although not statistically significantly more rehardening than those delivered in 200 ml milk. EFU data exhibited better differentiation between treatments: all fluoridated milk treatments delivered more fluoride to lesions than 0F-200; fluoride in 100 ml demonstrated statistically significantly higher EFU than fluoride in 200 ml milk. Findings for acid resistance were also more discerning than rehardening data. The present study has provided further evidence for the anti-caries benefits of fluoridated milk. Both fluoride dose and concentration appear to impact the cariostatic properties of fluoride in milk. Copyright © 2014 Elsevier Ltd. All rights reserved.

  14. a Study on Microstructure Characteristics of IN SITU Formed TiC Reinforced Composite Coatings

    Science.gov (United States)

    Liu, Peng; Guo, Wei; Luo, Hui

    2012-04-01

    In situ synthesized TiC reinforced composite coating was fabricated by laser cladding of Al-Ni-Cr-C powders on titanium alloys, which can greatly improve the surface performance of the substrate. In this study, the Al-Ni-Cr-C laser-cladded composite coatings have been researched by means of X-ray diffraction, scanning electron microscope (SEM) and electron probe micro-analyzer (EPMA). There was a metallurgical combination between the Al-Ni-Cr-C laser-cladded coating and the Ti-6Al-4V substrate, and the micro-hardness of the Al-Ni-Cr-C laser-cladded coating was in the range of 1200-1450 HV0.2, which was 3-4 times higher than that of Ti-6Al-4V substrate. Furthermore, the reinforcement of theAl-Ni-Cr-C laser-cladded coating were mainly contributed to the action of the TiC, Ti3Al, Cr7C3, Al8Cr5 phases and the solution strengthening.

  15. Studies on in situ magnetic alignment of bonded anisotropic Nd-Fe-B alloy powders

    Energy Technology Data Exchange (ETDEWEB)

    Nlebedim, I.C. [Ames Laboratory, Ames, IA 50011 (United States); Ucar, Huseyin; Hatter, Christine B. [Oak Ridge National Laboratory, Oak Ridge, TN 37831 (United States); McCallum, R.W. [Ames Laboratory, Ames, IA 50011 (United States); McCall, Scott K. [Lawrence Livermore National Laboratory, Livermore, CA 94550 (United States); Kramer, M.J. [Ames Laboratory, Ames, IA 50011 (United States); Paranthaman, M. Parans [Oak Ridge National Laboratory, Oak Ridge, TN 37831 (United States)

    2017-01-15

    Considerations for achieving high degree of alignment in polymer bonded permanent magnets are presented via the results of a study on in situ magnetic alignment of anisotropic Nd-Fe-B magnet powders. Contributions from effect of the alignment temperature, alignment magnetic field and the properties of the polymer on the hard magnetic properties of the bonded magnet were considered. The thermo-rheological properties of the polymer and the response of the magnet powders to the applied magnetic field indicate that hard magnetic properties were optimized at an alignment temperature just above the melting temperature of the EVA co-polymer. This agrees with an observed correlation between the change in magnetization due to improved magnetic alignment of the anisotropic powders and the change in viscosity of the binder. Manufacturing cost can be minimized by identifying optimum alignment temperatures and magnetic field strengths. - Highlights: • Optimum alignment of anisotropic magnet powders can enable high performance bonded magnets. • The viscoelastic state of polymer binders determines the dominating coercivity mechanism. • The minimum deviation in coercivity and remanence, with magnetic field, can occur at different temperatures. • Melting characteristics of polymer binders and the change in magnetization during alignment can be correlated.

  16. In situ TEM study of microplasticity and Bauschinger effect in nanocrystalline metals

    International Nuclear Information System (INIS)

    Rajagopalan, Jagannathan; Rentenberger, Christian; Peter Karnthaler, H.; Dehm, Gerhard; Saif, M. Taher A.

    2010-01-01

    In situ transmission electron microscopy straining experiments with concurrent macroscopic stress-strain measurements were performed to study the effect of microstructural heterogeneity on the deformation behavior of nanocrystalline metal films. In microstructurally heterogeneous gold films (mean grain size d m = 70 nm) comprising randomly oriented grains, dislocation activity is confined to relatively larger grains, with smaller grains deforming elastically, even at applied strains approaching 1.2%. This extended microplasticity leads to build-up of internal stresses, inducing a large Bauschinger effect during unloading. Microstructurally heterogeneous aluminum films (d m = 140 nm) also show similar behavior. In contrast, microstructurally homogeneous aluminum films comprising mainly two grain families, both favorably oriented for dislocation glide, show limited microplastic deformation and minimal Bauschinger effect despite having a comparable mean grain size (d m = 120 nm). A simple model is proposed to describe these observations. Overall, our results emphasize the need to consider both microstructural size and heterogeneity in modeling the mechanical behavior of nanocrystalline metals.

  17. Pyrophosphate-Inhibition of Apatite Formation Studied by In Situ X-Ray Diffraction

    Directory of Open Access Journals (Sweden)

    Casper Jon Steenberg Ibsen

    2018-02-01

    Full Text Available The pathways to crystals are still under debate, especially for materials relevant to biomineralization, such as calcium phosphate apatite known from bone and teeth. Pyrophosphate is widely used in biology to control apatite formation since it is a potent inhibitor of apatite crystallization. The impacts of pyrophosphate on apatite formation and crystallization kinetics are, however, not fully understood. Therefore, we studied apatite crystallization in water by synchrotron in situ X-ray diffraction. Crystallization was conducted from calcium chloride (0.2 M and sodium phosphate (0.12 M at pH 12 where hydrogen phosphate is the dominant phosphate species and at 60 °C to allow the synchrotron measurements to be conducted in a timely fashion. Following the formation of an initial amorphous phase, needle shaped crystals formed that had an octacalcium phosphate-like composition, but were too small to display the full 3D periodic structure of octacalcium phosphate. At later growth stages the crystals became apatitic, as revealed by changes in the lattice constant and calcium content. Pyrophosphate strongly inhibited nucleation of apatite and increased the onset of crystallization from minute to hour time scales. Pyrophosphate also reduced the rate of growth. Furthermore, when the pyrophosphate concentration exceeded ~1% of the calcium concentration, the resultant crystals had reduced size anisotropy suggesting that pyrophosphate interacts in a site-specific manner with the formation of apatite crystals.

  18. In Situ Test Study of Characteristics of Coal Mining Dynamic Load

    Directory of Open Access Journals (Sweden)

    Jiang He

    2015-01-01

    Full Text Available Combination of coal mining dynamic load and high static stress can easily induce such dynamic disasters as rock burst, coal and gas outburst, roof fall, and water inrush. In order to obtain the characteristic parameters of mining dynamic load and dynamic mechanism of coal and rock, the stress wave theory is applied to derive the relation of mining dynamic load strain rate and stress wave parameters. The in situ test was applied to study the stress wave propagation law of coal mine dynamic load by using the SOS microseismic monitoring system. An evaluation method for mining dynamic load strain rate was proposed, and the statistical evaluation was carried out for the range of strain rate. The research results show that the loading strain rate of mining dynamic load is in direct proportion to the seismic frequency of coal-rock mass and particle peak vibration velocity and is in inverse proportion to wave velocity. The high-frequency component damps faster than the low-frequency component in the shockwave propagating process; and the peak particle vibration velocity has a power functional relationship with the transmitting distance. The loading strain rate of mining dynamic load is generally less than class 10−1/s.

  19. An in-situ FTIR study of the side-chain alkylation of toluene with methanol

    International Nuclear Information System (INIS)

    King, S.T.; Garces, J.

    1985-01-01

    The side-chain alkylation of toluene with methanol to styrene and ethylbenzene can be an economically attractive industrial process if it has high enough conversion and selectivity. This process has been investigated by many others using zeolites or metal oxides as the catalyst. It has been generally accepted that high basicity in certain size pores in the catalyst is required for such side-chain alkylation. However, the actual reaction mechanism is still not understood. In this paper the results of an in-situ FT-IR study of the side-chain alkylation in Li, Na, K, Rb and Cs exchanged X zeolites is discussed. It was found that the KX, RbX and CsX zeolites, which are capable of side-chain alkylation, also form surface formate and a surface precursor of formate from methanol decomposition. While the surface formate itself is not the alkylation agent, the observed formate precursor may be the intermediate for side-chain alkylation

  20. In-situ high-temperature Raman spectroscopic studies of aluminosilicate liquids

    Science.gov (United States)

    Daniel, Isabelle; Gillet, Philippe; Poe, Brent T.; McMillan, Paul F.

    1995-03-01

    We have measured in-situ Raman spectra of aluminosilicate glasses and liquids with albite (NaAlSi3 O8) and anorthite (CaAl2Si2O8) compositions at high temperatures, through their glass transition range up to 1700 and 2000 K, respectively. For these experiments, we have used a wire-loop heating device coupled with micro-Raman spectroscopy, in order to achieve effective spatial filtering of the extraneous thermal radiation. A major concern in this work is the development of methodology for reliably extracting the first and second order contributions to the Raman scattering spectra of aluminosilicate glasses and liquids from the high temperature experimental data, and analyzing these in terms of vibrational (anharmonic) and configurational changes. The changes in the first order Raman spectra with temperature are subtle. The principal low frequency band remains nearly constant with increasing temperature, indicating little change in the T-O-T angle, and that the angle bending vibration is quite harmonic. This is in contrast to vitreous SiO2, studied previously. Above Tg, intensity changes in the 560 590 cm-1 regions of both sets of spectra indicate configurational changes in the supercooled liquids, associated with formation of additional Al-O-Al linkages, or 3-membered (Al, Si)-containing rings. Additional intensity at 800 cm-1 reflects also some rearrangement of the Si-O-Al network.

  1. Spectroelectrochemical study of polyphenylene by in situ external reflection FT-IR spectroscopy. Pt. 1

    International Nuclear Information System (INIS)

    Kvarnstroem, C.; Ivaska, A.

    1994-01-01

    In situ spectroelectrochemical measurements with external reflection FT-IR are performed at different stages of polymerization of 0.05, 0.1 and 0.8 M biphenyl in 0.1 M TBABF 4 in acetonitrile. The biphenyl concentration is not found to have any effect on the structure of the polymer formed. Formation of oligomers and the ratio of ortho/para-substituted polymer chains during film growth are studied. The first coupling of dimers to oligomers is found to take place in the vicinity of the electrode surface and at a later stage of polymerization the oligomers start to form polymer film on the electrode. A mixed para and ortho coupling resulting in crosslinking between chains is observed already at the early stage of polymerization. However, when a lower current density is used a more ordered polymer structure is obtained. A breakdown of the polymer film due to overoxidation can be seen when the potential is increased to 2.0 V. (orig.)

  2. Benzalkonium runoff from roofs treated with biocide products - In situ pilot-scale study.

    Science.gov (United States)

    Gromaire, M C; Van de Voorde, A; Lorgeoux, C; Chebbo, G

    2015-09-15

    Roof maintenance practices often involve the application of biocide products to fight against moss, lichens and algae. The main component of these products is benzalkonium chloride, a mixture of alkyl benzyl dimethyl ammonium chlorides with mainly C12 and C14 alkyl chain lengths, which is toxic for the aquatic environment. This paper describes, on the basis of an in-situ pilot scale study, the evolution of roof runoff contamination over a one year period following the biocide treatment of roof frames. Results show a major contamination of roof runoff immediately after treatment (from 5 to 30 mg/L), followed by an exponential decrease. 175-375 mm of cumulated rainfall is needed before the runoff concentrations become less than EC50 values for fish (280 μg/l). The residual concentration in the runoff water remains above 4 μg/L even after 640 mm of rainfall. The level of benzalkonium ions leaching depends on the roofing material, with lower concentrations and total mass leached from ceramic tiles than from concrete tiles, and on the state of the tile (new or worn out). Mass balance calculations indicate that a large part of the mass of benzalkonium compounds applied to the tiles is lost, probably due to biodegradation processes. Copyright © 2015 Elsevier Ltd. All rights reserved.

  3. In situ neutron diffraction studies of high density amorphous ice under pressure

    International Nuclear Information System (INIS)

    Klotz, Stefan; Straessle, Th; Saitta, A M; Rousse, G; Hamel, G; Nelmes, R J; Loveday, J S; Guthrie, M

    2005-01-01

    We review recent in situ neutron diffraction studies on the structural pressure dependence and the recrystallization of dense amorphous ices up to 2 GPa. Progress in high pressure techniques and data analysis methods allows the reliable determination of all three partial structure factors of amorphous ice under pressure. The strong pressure dependence of the g OO (r) correlation function shows that the isothermal compression of high density amorphous ice (HDA) at 100 K is achieved by a contraction (∼ 20%) of the second-neighbour coordination shell leading to a strong increase in coordination. The g DD (r) and g OD (r) structure factors are, in contrast, only weakly sensitive to pressure. These data allow a comparison with structural features of the recently reported 'very high density amorphous ice' (VHDA) which indicates that VHDA at ambient pressure is very similar to compressed HDA, at least up to the second-neighbour shell. The recrystallization of HDA has been investigated in the range 0.3-2 GPa. It is shown that hydrogen-disordered phases are produced which normally grow only from the liquid, such as ice XII, and in particular ice IV. These findings are in good agreement with results on quench-recovered samples

  4. In situ TEM study of microplasticity and Bauschinger effect in nanocrystalline metals

    Energy Technology Data Exchange (ETDEWEB)

    Rajagopalan, Jagannathan [Mechanical Science and Engineering Department, University of Illinois at Urbana-Champaign, 1206 W Green Street, Urbana, IL 61801 (United States); Rentenberger, Christian; Peter Karnthaler, H. [Physics of Nanostructured Materials, Faculty of Physics, University of Vienna, Boltzmanngasse 5, A-1090 Wien (Austria); Dehm, Gerhard [Erich Schmid Institute of Materials Science, Austrian Academy of Sciences, and Dept. Materials Physics, University of Leoben, Jahnstr.12, 8700 Leoben (Austria); Saif, M. Taher A., E-mail: saif@illinois.edu [Mechanical Science and Engineering Department, University of Illinois at Urbana-Champaign, 1206 W Green Street, Urbana, IL 61801 (United States)

    2010-08-15

    In situ transmission electron microscopy straining experiments with concurrent macroscopic stress-strain measurements were performed to study the effect of microstructural heterogeneity on the deformation behavior of nanocrystalline metal films. In microstructurally heterogeneous gold films (mean grain size d{sub m} = 70 nm) comprising randomly oriented grains, dislocation activity is confined to relatively larger grains, with smaller grains deforming elastically, even at applied strains approaching 1.2%. This extended microplasticity leads to build-up of internal stresses, inducing a large Bauschinger effect during unloading. Microstructurally heterogeneous aluminum films (d{sub m} = 140 nm) also show similar behavior. In contrast, microstructurally homogeneous aluminum films comprising mainly two grain families, both favorably oriented for dislocation glide, show limited microplastic deformation and minimal Bauschinger effect despite having a comparable mean grain size (d{sub m} = 120 nm). A simple model is proposed to describe these observations. Overall, our results emphasize the need to consider both microstructural size and heterogeneity in modeling the mechanical behavior of nanocrystalline metals.

  5. Study of the Radical Chain Mechanism of Hydrocarbon Oxidation for In Situ Combustion Process

    Directory of Open Access Journals (Sweden)

    Alexandra Ushakova

    2017-01-01

    Full Text Available Despite the abundance of in situ combustion models of oil oxidation, many of the effects are still beyond consideration. For example, until now, initial stages of oxidation were not considered from a position of radical chain process. This is a serious difficulty for the simulation of oil recovery process that involves air injection. To investigate the initial stages of oxidation, the paper considers the sequence of chemical reactions, including intermediate short-living compounds and radicals. We have attempted to correlate the main stages of the reaction with areas of heat release observed in the experiments. The system of differential equations based on the equations of oxidation reactions was solved. Time dependence of peroxides formation and start of heat release is analytically derived for the initial stages. We have considered the inhibition of initial oxidation stages by aromatic oil compounds and have studied the induction time in dependence on temperature. Chain ignition criteria for paraffins and crude oil in presence of core samples were obtained. The calculation results are compared with the stages of oxidation that arise by high-pressure differential scanning calorimetry. According to experimental observations we have determined which reactions are important for the process and which can be omitted or combined into one as insignificant.

  6. In situ diffraction studies of electrode surface structure during gold electrodeposition

    International Nuclear Information System (INIS)

    Magnussen, O.M.; Krug, K.; Ayyad, A.H.; Stettner, J.

    2008-01-01

    Surface X-ray scattering (SXS) in transmission geometry provides a valuable tool for in situ structural studies of electrochemical interfaces under reaction conditions, as illustrated here for homoepitaxial electrodeposition on Au(1 0 0) and Au(1 1 1) electrodes. Employing diffusion-limited deposition conditions to separate the effects of potential and deposition rate, a mutual interaction between the interface structure and the growth behavior is found. Time-dependent SXS measurements during Au(1 0 0) homoepitaxy show with decreasing potential transitions from step flow to layer-by-layer growth, then to multilayer growth, and finally back to layer-by-layer growth. This complex growth behavior can be explained within the framework of kinetic growth theory by the effect of potential, Cl adsorbates and the Au surface structure, specifically the presence of the surface reconstruction, on the Au surface mobility. Conversely, the electrodeposition process influences the structure of the reconstructed Au surface, as illustrated for Au(1 1 1), where a significant deposition-induced compression of the Au surface layer as compared to Au(1 1 1) surfaces under ultrahigh vacuum conditions or in Au-free electrolyte is found. This compression increases towards more negative potentials, which may be explained by a release of potential-induced surface stress

  7. In situ synchrotron X-ray diffraction study of hydrides in Zircaloy-4 during thermomechanical cycling

    Energy Technology Data Exchange (ETDEWEB)

    Cinbiz, Mahmut N., E-mail: cinbizmn@ornl.gov [Department of Mechanical and Nuclear Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Koss, Donald A., E-mail: koss@ems.psu.edu [Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Motta, Arthur T., E-mail: atm2@psu.edu [Department of Mechanical and Nuclear Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Park, Jun-Sang, E-mail: parkjs@aps.anl.gov [Advanced Photon Source, Argonne National Laboratory, Argonne, IL, 60439 (United States); Almer, Jonathan D., E-mail: almer@aps.anl.gov [Advanced Photon Source, Argonne National Laboratory, Argonne, IL, 60439 (United States)

    2017-04-15

    The d-spacing evolution of both in-plane and out-of-plane hydrides has been studied using in situ synchrotron radiation X-ray diffraction during thermo-mechanical cycling of cold-worked stress-relieved Zircaloy-4. The structure of the hydride precipitates is such that the δ{111} d-spacing of the planes aligned with the hydride platelet face is greater than the d-spacing of the 111 planes aligned with the platelet edges. Upon heating from room temperature, the δ{111} planes aligned with hydride plate edges exhibit bi-linear thermally-induced expansion. In contrast, the d-spacing of the (111) plane aligned with the hydride plate face initially contracts upon heating. These experimental results can be understood in terms of a reversal of stress state associated with precipitating or dissolving hydride platelets within the α-zirconium matrix. - Highlights: •The δ{111} d-spacings aligned with the hydride plate edges exhibit a bi-linear thermal expansion. •Stress state reversal is predicted with the onset of hydride dissolution. •During dissolution, the δ{111} planes oriented parallel to the hydride plate face initially contract upon heating. •Hydride d-spacings indicate that both in-plane (circumferential) and out-of-plane (radial) hydrides are in the same strain-state and likely in the same stress state as well.

  8. Studies on in situ magnetic alignment of bonded anisotropic Nd-Fe-B alloy powders

    International Nuclear Information System (INIS)

    Nlebedim, I.C.; Ucar, Huseyin; Hatter, Christine B.; McCallum, R.W.; McCall, Scott K.; Kramer, M.J.; Paranthaman, M. Parans

    2017-01-01

    Considerations for achieving high degree of alignment in polymer bonded permanent magnets are presented via the results of a study on in situ magnetic alignment of anisotropic Nd-Fe-B magnet powders. Contributions from effect of the alignment temperature, alignment magnetic field and the properties of the polymer on the hard magnetic properties of the bonded magnet were considered. The thermo-rheological properties of the polymer and the response of the magnet powders to the applied magnetic field indicate that hard magnetic properties were optimized at an alignment temperature just above the melting temperature of the EVA co-polymer. This agrees with an observed correlation between the change in magnetization due to improved magnetic alignment of the anisotropic powders and the change in viscosity of the binder. Manufacturing cost can be minimized by identifying optimum alignment temperatures and magnetic field strengths. - Highlights: • Optimum alignment of anisotropic magnet powders can enable high performance bonded magnets. • The viscoelastic state of polymer binders determines the dominating coercivity mechanism. • The minimum deviation in coercivity and remanence, with magnetic field, can occur at different temperatures. • Melting characteristics of polymer binders and the change in magnetization during alignment can be correlated.

  9. Field test for treatment verification of an in-situ enhanced bioremediation study

    International Nuclear Information System (INIS)

    Taur, C.K.; Chang, S.C.

    1995-01-01

    Due to a leakage from a 12-inch pressurized diesel steel pipe four years ago, an area of approximately 30,000 square meters was contaminated. A pilot study applying the technology of in-situ enhanced bioremediation was conducted. In the study, a field test kit and on-site monitoring equipment were applied for site characterization and treatment verification. Physically, the enhanced bioremediation study consisted of an air extraction and air supply system, and a nutrition supply network. Certain consistent sampling methodology was employed. Progress was verified by daily monitoring and monthly verification. The objective of this study was to evaluate the capabilities of indigenous microorganisms to biodegrade the petroleum hydrocarbons with provision of oxygen and nutrients. Nine extraction wells and eight air sparging wells were installed. The air sparging wells injected the air into geoformation and the extraction wells provided the underground air circulation. The soil samples were obtained monthly for treatment verification by a Minuteman drilling machine with 2.5-foot-long hollow-stem augers. The samples were analyzed on site for TPH-diesel concentration by a field test kit manufactured by HNU-Hanby, Houston, Texas. The analytical results from the field test kit were compared with the results from an environmental laboratory. The TVPH concentrations of the air extracted from the vadose zone by a vacuum blower and the extraction wells were routinely monitored by a Foxboro FID and Cosmos XP-311A combustible air detector. The daily monitoring of TVPH concentrations provided the reliable data for assessing the remedial progress

  10. Annealing of hydrogen-induced defects in RF-plasma-treated Si wafers: ex situ and in situ transmission electron microscopy studies

    International Nuclear Information System (INIS)

    Ghica, C; Nistor, L C; Vizireanu, S; Dinescu, G

    2011-01-01

    The smart-cut(TM) process is based on inducing and processing structural defects below the free surface of semiconductor wafers. The necessary defects are currently induced by implantation of light elements such as hydrogen or helium. An alternative softer way to induce shallow subsurface defects is by RF-plasma hydrogenation. To facilitate the smart-cut process, the wafers containing the induced defects need to be subjected to an appropriate thermal treatment. In our experiments, (0 0 1) Si wafers are submitted to 200 and 50 W hydrogen RF-plasma and are subsequently annealed. The samples are studied by transmission electron microscopy (TEM), before and after annealing. The plasma-introduced defects are {1 1 1} and {1 0 0} planar-like defects and nanocavities, all of them involving hydrogen. Many nanocavities are aligned into strings almost parallel to the wafer surface. The annealing is performed either by furnace thermal treatment at 550 deg. C, or by in situ heating in the electron microscope at 450, 650 and 800 deg. C during the TEM observations. The TEM microstructural studies indicate a partial healing of the planar defects and a size increase of the nanometric cavities by a coalescence process of the small neighbouring nanocavities. By annealing, the lined up nanometric voids forming chains in the as-hydrogenated sample coalesced into well-defined cracks, mostly parallel to the wafer surface.

  11. Setup for in situ X-ray diffraction studies of thin film growth by magnetron sputtering

    CERN Document Server

    Ellmer, K; Weiss, V; Rossner, H

    2001-01-01

    A novel method is described for the in situ-investigation of nucleation and growth of thin films during magnetron sputtering. Energy dispersive X-ray diffraction with synchrotron light is used for the structural analysis during film growth. An in situ-magnetron sputtering chamber was constructed and installed at a synchrotron radiation beam line with a bending magnet. The white synchrotron light (1-70 keV) passes the sputtering chamber through Kapton windows and hits one of the substrates on a four-fold sample holder. The diffracted beam, observed under a fixed diffraction angle between 3 deg. and 10 deg., is energy analyzed by a high purity Ge-detector. The in situ-EDXRD setup is demonstrated for the growth of tin-doped indium oxide (ITO) films prepared by reactive magnetron sputtering from a metallic target.

  12. Exposure to contaminated sediments induces alterations in the gill epithelia in juvenile Solea senegalensis: a comparative in situ and ex situ study

    Directory of Open Access Journals (Sweden)

    Carla Martins

    2014-06-01

    contaminated sediments. Hypertrophied chloride cells are a consequence of a hindered osmotic regulation by the impairment of ionic active transport, leading to loss-of-function and excessive fluid retention in the cytoplasm. On its turn, a reduction in number and size of gill mucous cells likely reduced the protection provided by mucous to these delicate structures. In general, the alterations were more pronounced in the ex situ study than in situ bioassays, which is probably linked to differences in contaminant bioavailability between laboratory and field scenarios. This variation is likely related to, for instance, estuarine hydrodynamics and sediment steady-state parameters. Interestingly, the results suggest that time of exposure is a key factor, since fewer alterations were observed in animals sampled at the end of the assay (28 days compared to the mid-term (14 days, revealing adaptation to toxicological challenge. In conclusion, mixed sediment contamination can cause physiological alterations in fish gill epithelia that can be determined histologically. These subtle changes may affect the health status of animals by impairing key vital functions such as osmotic balance. As such, physiological alterations to fish gill epithelia may reflect, as in the present case, estuarine sediment contamination even when severe gill lesions are reduced or absent, which mandates caution when interpreting histopathological data in fish for the purpose of environmental risk assessment.

  13. In-situ Spectroscopic Studies and Modelling of Crystallization Processes of Sulphuric Acid Catalysts

    DEFF Research Database (Denmark)

    Oehlers, C.; Fehrmann, Rasmus; Masters, Stephen Grenville

    1996-01-01

    Deactivation of commercial and prototype sulphuric acid catalysts has been investigated in-situ by ESR spectroscopy. The influence of support pore structure,and the chemical composition of the catalyst and the gas phase was dicussed.A statistical lattice model was applied to describe the crystall......Deactivation of commercial and prototype sulphuric acid catalysts has been investigated in-situ by ESR spectroscopy. The influence of support pore structure,and the chemical composition of the catalyst and the gas phase was dicussed.A statistical lattice model was applied to describe...

  14. Evaluating in situ thermal transmittance of green buildings masonries—A case study

    Directory of Open Access Journals (Sweden)

    Francesco Asdrubali

    2014-01-01

    The paper presents the results of a measurement campaign of in situ thermal transmittance, performed in some buildings in the Umbria Region (Italy, designed implementing bio-architecture solutions. The analyzed walls were previously monitored with thermographic surveys in order to assess the correct application of the sensors. Results of the investigation show that in situ thermal transmittance measurements and theoretical calculated U-value are not in perfect agreement. The mismatch becomes important for monolithic structures such as walls made of thermal blocks without insulating layers.

  15. In-situ TEM study of dislocation patterning during deformation in single crystal aluminum

    International Nuclear Information System (INIS)

    Landau, P; Shneck, R Z; Makov, G; Venkert, A

    2010-01-01

    The evolution of dislocation patterns in single crystal aluminum was examined using transmission electron microscopy (TEM). In-situ tensile tests of single crystals were carried out in a manner that activated double slip. Cross slip of dislocations, which is prominent in all stages of work hardening, plays an important role in dislocation motion and microstructural evolution. In spite of the limitations of in-situ straining to represent bulk phenomena, due to surface effects and the thickness of the samples, it is shown that experiments on prestrained samples can represent the early stages of deformation. Transition between stage I and stage II of work hardening and evolution during stage III were observed.

  16. In situ x-ray diffraction studies of three-dimensional C60 polymers

    International Nuclear Information System (INIS)

    Wood, R A; Lewis, M H; Bennington, S M; Cain, M G; Kitamura, N; Fukumi, A K

    2002-01-01

    In situ investigations into the P/T field of C 60 fullerene were performed using energy-dispersive x-ray diffraction techniques. Isobars were obtained at 11 and 9 GPa accompanied by isotherms at 750 and 800 K with pressure reaching 13 GPa. The P/T history and pressure isotropy were investigated with the aim of optimizing conditions for 3D polymer formation. Confirmation of the formation of 3D polymers was performed in situ; however, the reclaimed sample did not exhibit the expected high hardness value, due to depolymerization on pressure release. Isotropy in the pressure field promoted formation and retention of the face-centred-cubic structure

  17. An animal model for instructing and the study of in situ arterial bypass.

    Science.gov (United States)

    Saifi, J; Chang, B B; Paty, P S; Kaufman, J; Leather, R P; Shah, D M

    1990-11-01

    A canine model that used the cephalic vein to bypass from the brachial to the ulnar artery was designed for use in instructing and evaluating surgical technique needed for constructing an in situ arterial bypass. This model was used for instructing vascular residents in the in situ vein bypass technique. The use of this model enabled the resident to become more adept with the instruments for valve incision and construction of small vessel anastomosis. The improvement in the resident's operative technique was reflected by a decrease in the number of technical complications (missed valves, missed arteriovenous fistulas, poorly constructed anastomoses) and improved patency rate.

  18. Effects of higher-coordination shells in garnets detected by XAS at the Al K-edge

    International Nuclear Information System (INIS)

    Marcelli, A.; Wu, Z.; Mottana, A.; Giuli, G.; Paris, E.; Seifert, F.

    1996-03-01

    The aluminium 1 s x-ray-absorption spectra of a series of garnets, pyrope, almandine, spessartine and grossular, are compared to full multiple-scattering calculation using cluster models. An overall good agreement between experiment and calculation, extended also to the edge region,is obtained in the energy range in up to 60 e V above the threshold, provided cluster containing at least 40 atoms are used. The analysis of these garnet XAS spectra provides clear evidence on the effect of probe, XANES spectroscopy at the edge of low Z elements appears to be a perfect tool to investigate the role played by atoms located in higher-coordination shells

  19. Effects of higher-coordination shells in garnets detected by XAS at the Al K-edge

    Energy Technology Data Exchange (ETDEWEB)

    Marcelli, A. [Istituto Nazionale di Fisica Nucleare, Frascati (Italy). Lab. Nazionale di Frascati; Wu, Z. [CNRS UMR 110, Laboratoire de Chimie des Solides, Nantes Cedex (France). Institut de materiaux de Nantes; Mottana, A. [Roma III Univ., Rome (Italy). Dipartimento di Scienze Geologiche; Giuli, G.; Paris, E. [Camerino Univ., Camerino (Italy).Diparimento di Scienze della Terra; Seifert, F [Univ. Bayreuth, Bayreuth (Italy). Bayerisches Geoinstitut (Germany)

    1996-03-01

    The aluminium 1 s x-ray-absorption spectra of a series of garnets, pyrope, almandine, spessartine and grossular, are compared to full multiple-scattering calculation using cluster models. An overall good agreement between experiment and calculation, extended also to the edge region,is obtained in the energy range in up to 60 e V above the threshold, provided cluster containing at least 40 atoms are used. The analysis of these garnet XAS spectra provides clear evidence on the effect of probe, XANES spectroscopy at the edge of low Z elements appears to be a perfect tool to investigate the role played by atoms located in higher-coordination shells.

  20. PySpline: A Modern, Cross-Platform Program for the Processing of Raw Averaged XAS Edge and EXAFS Data

    International Nuclear Information System (INIS)

    Tenderholt, Adam; Hedman, Britt; Hodgson, Keith O.

    2007-01-01

    PySpline is a modern computer program for processing raw averaged XAS and EXAFS data using an intuitive approach which allows the user to see the immediate effect of various processing parameters on the resulting k- and R-space data. The Python scripting language and Qt and Qwt widget libraries were chosen to meet the design requirement that it be cross-platform (i.e. versions for Windows, Mac OS X, and Linux). PySpline supports polynomial pre- and post-edge background subtraction, splining of the EXAFS region with a multi-segment polynomial spline, and Fast Fourier Transform (FFT) of the resulting k3-weighted EXAFS data

  1. A study of the methane hydrate formation by in situ turbidimetry

    Energy Technology Data Exchange (ETDEWEB)

    Herri, J M

    1996-02-02

    The study of the Particle Size Distribution (PSD) during the processes of crystallization is a subject of considerable interest, notably in the offshore exploitation of liquid fuels where the gas hydrate crystallization can plug production, treatment and transport facilities. The classical remedy to this problem is mainly thermodynamic additives such as alcohols or salts, but a new way of research is the use of dispersant additives which avoid crystals formation. In this paper, we show an original apparatus that is able to measure in situ the polychromatic UV-Visible turbidity spectrum in a pressurised reactor. We apply this technology to the calculation of the PSD during the crystallization of methane hydrate particles in a stirred semi-batch tank reactor. We discuss the mathematics treatment of the turbidity spectrum in order to determine the PSD and especially the method of matrix inversion with constraint. Moreover, we give a method to calculate theoretically the refractive index of the hydrate particles and we validate it experimentally with the methane hydrate particles. We apply this technology to the study of the crystallization of methane hydrate from pure liquid water and methane gas into the range of temperature [0-2 deg. C], into the range of pressure [30-100 bars] and into the range of stirring rate [0-600 rpm]. We produce a set of experiments concerning these parameters. Then we realize a model of the crystallization taking into account the processes of nucleation, of growth, of agglomeration and flotation. We compare this model with the experimental results concerning the complex influence of stirring rate at 1 deg. C and 30 bars. Then, we investigate the influence of additives such as Fontainebleau Sand, Potassium Chloride and a surfactant such as Poly-Vinyl-Pyrrolydone. (authors). 133 refs., 210 figs., 54 tabs.

  2. Phase transformation in delta Pu alloys at low temperature: in situ dilatometric study

    Energy Technology Data Exchange (ETDEWEB)

    Texier, G.; Oudot, B.; Platteau, C.; Ravat, B.; Delaunay, F. [CEA Valduc, 21 - Is-sur-Tille (France)

    2010-07-01

    The purpose of this work is to precisely study the martensitic transformation in a plutonium-gallium alloy. Thus, the thermodynamics and kinetics of the {delta} {yields} {alpha}' + {delta} transformation in a Pu-Ga alloy were studied under isochronal and isothermal conditions. The activation energy of the {delta} {yields} {alpha}' + {delta} phase transformation at a constant cooling rate (0.5 K. min{sup -1}) was determined by using Kissinger and Ozawa models. The average value of the activation energy was found to be at -56 kJ.mol{sup -1}. Dilatometry measurement was also used to trace 'in situ' the entire transformation for several temperatures. The kinetics of the {delta} {yields} {alpha}' + {delta} transformation were modelled under isothermal conditions in the theoretical frame of the Johnson-Mehl-Avrami-Kolmogorov (JMAK) theory. It is proposed that the transformation consists of three stages. The {alpha}' transformation begins with a nucleation of pre-existing embryos. Then, both nucleation and rapid growth of {alpha}' occurs simultaneously and finally, the plates width expend. Apparent activation energies for nucleation and growth transformation were determined from the temperature dependence of the constant K at respectively -34 kJ.mol{sup -1} and -60 kJ.mol{sup -1}. Dler et al. [1] investigated also the thermodynamics and the kinetics of the martensitic transformation in Pu alloys. These nucleation energies were found by modelling of heterogeneous martensitic nucleation via strain interaction with observed superdislocation-like nucleation sites in PuGa alloys. The values obtain by this model was very close to those we find. Investigations in steels alloys indicate that these energies are of the same order for nucleation near dislocation. Then, it could be indicating a strong relationship between these dislocations and martensitic nucleation sites. (authors)

  3. Phase transformation in {delta} Pu alloys at low temperature: In situ dilatometric study

    Energy Technology Data Exchange (ETDEWEB)

    Texier, G; Oudot, B; Platteau, C; Ravat, B; Delaunay, F, E-mail: gwenael.texier@cea.fr, E-mail: benoit.oudot@cea.fr [CEA, DAM, Valduc, Is sur Tille 21120 (France)

    2010-03-15

    The purpose of this work is to precisely study the martensitic transformation in a plutonium-gallium alloy. Thus, the thermodynamics and kinetics of the {delta}{yields}{alpha}'+{delta} phase transformation in a Pu-Ga alloy were studied under isochronal and isothermal conditions. The activation energy of the {delta}{yields}{alpha}'+{delta} phase transformation at a constant cooling rate (0.5 K.min{sup -1}) was determined by using Kissinger and Ozawa models. The average value of the activation energy was found to be at -56 kJ.mol{sup -1}. Dilatometry measurement was also used to trace 'in situ' the entire transformation for several temperatures. The kinetics of the {delta}{yields}{alpha}'+{delta} transformation were modelled under isothermal conditions in the theoretical frame of the Johnson-Mehl-Avrami-Kolmogorov (JMAK) theory. It is proposed that the transformation consists of three stages. The {alpha}' transformation begins with a nucleation of pre-existing embryos. Then, both nucleation and rapid growth of {alpha}' occurs simultaneously and finally, the plates width expend. Apparent activation energies for nucleation and growth transformation were determined from the temperature dependence of the constant K at respectively -34 kJ.mol{sup -1} and -60 kJ.mol{sup -1}. Adler et al. [1] investigated also the thermodynamics and the kinetics of the martensitic transformation in Pu alloys. These nucleation energies were found by modelling of heterogeneous martensitic nucleation via strain interaction with observed superdislocation-like nucleation sites in PuGa alloys. The values obtain by this model was very close to those we find. Investigations in steels alloys indicate that these energies are of the same order for nucleation near dislocation. Then, it could be indicating a strong relationship between these dislocations and martensitic nucleation sites.

  4. Effect of ozone to remineralize initial enamel caries: in situ study.

    Science.gov (United States)

    Samuel, S R; Dorai, S; Khatri, S G; Patil, S T

    2016-06-01

    Effect of ozonated water in remineralizing artificially created initial enamel caries was investigated using laser fluorescence and polarized light microscopy in an in situ study. Teeth specimens (buccal sections) were immersed in 5-ml solution of 2 mM CaCl2, 2 mM NaH2P04, and 50 mM CH3COOH at pH of 4.55 for 5 h in an incubator at 37° to create subsurface demineralization. After which, they were randomly allocated into one of the following remineralization regimens: ozone (ozonated water 0.1 mg/l and 10 % nano-hydroxyapatite paste, Aclaim(TM)), without ozone (only 10 % nano-hydroxyapatite paste, Aclaim(TM)), and control (subjects' saliva alone). Specimens were embedded in acrylic retainers worn by orthodontic patients throughout the 21-day study duration and constantly exposed to their saliva. Laser fluorescence was recorded for all the specimens at baseline, after demineralization, and remineralization using DIAGNOdent, and the results were validated using polarized microscopic examination. The results were analyzed using repeated measures, one-way ANOVA with post hoc multiple comparisons. Reduced DIAGNOdent scores and greater depth of remineralization following application of ozonated water and nano-hydroxyapatite were found compared to those of the without ozone and control groups (P nano-hydroxyapatite compared to nano-hydroxyapatite alone and saliva. Ozone water can be used to remineralize incipient carious lesions, and it enhances the remineralizing potential of nano-hydroxyapatite thereby preventing the tooth from entering into the repetitive restorative cycle.

  5. Efficiency of consortium for in-situ bioremediation and CO2 evolution method of refines petroleum oil in microcosms study

    OpenAIRE

    Dutta, Shreyasri; Singh, Padma

    2017-01-01

    An in-situ bioremediation study was conducted in a laboratory by using mixed microbial consortium. An indigenous microbial consortium was developed by assemble of two Pseudomonas spp. and two Aspergillus spp. which were isolated from various oil contaminated sites of India. The laboratory feasibility study was conducted in a 225 m2 block. Six treatment options-Oil alone, Oil+Best remediater, Oil+Bacterial consortium, Oil+Fungal consortium, Oil+Mixed microbial consortium, Oil+Indigenous microf...

  6. In situ transmission electron microscope studies of ion irradiation-induced and irradiation-enhanced phase changes

    International Nuclear Information System (INIS)

    Allen, C.W.

    1992-01-01

    Motivated at least initially by materials needs for nuclear reactor development, extensive irradiation effects studies employing transmission electron microscopes (TEM) have been performed for several decades, involving irradiation-induced and irradiation-enhanced microstructural changes, including phase transformations such as precipitation, dissolution, crystallization, amorphization, and order-disorder phenomena. From the introduction of commercial high voltage electron microscopes (HVEM) in the mid-1960s, studies of electron irradiation effects have constituted a major aspect of HVEM application in materials science. For irradiation effects studies two additional developments have had particularly significant impact; the development of TEM specimen holder sin which specimen temperature can be controlled in the range 10-2200 K and the interfacing of ion accelerators which allows in situ TEM studies of irradiation effects and the ion beam modification of materials within this broad temperature range. This paper treats several aspects of in situ studies of electron and ion beam-induced and enhanced phase changes and presents two case studies involving in situ experiments performed in an HVEM to illustrate the strategies of such an approach of the materials research of irradiation effects

  7. A comparative study of the character and complexation properties of in-situ and extracted humic and fulvic substances

    International Nuclear Information System (INIS)

    Warwick, P.; Hall, A.; Patterson, M.

    1992-12-01

    The character and complexation properties of humic and fulvic acids, derived from a moorland water, have been studied, both under ''in-situ'' conditions and also after extraction. The characterisation studies involved determinations of UV-visible properties, fluorescence properties. size ranges, molecular weights and proton capacities. Complexation studies were conducted using High Performance Size Exclusion Chromatography, Fluorescence Reduction and the Schubert Ion Exchange Method. A strong and weak site ligand model was used to interpret the data. The effects of pH, ionic strength, side reactions, ligand type, purity and nature of the cation were considered. No major differences in the character or complexation properties of the in-situ and extracted materials were found. (Author)

  8. In-situ leaching of crownpoint, NM, uranium ore: Part 7 - Laboratory study of chemical agents for molybdenum restoration

    International Nuclear Information System (INIS)

    Strom, E.T.; Vogt, T.C.

    1987-01-01

    One possible drawback to the use of an in-situ leaching to recover uranium is the potential release of previously insoluble chemical species into the formation water. Before a pilot test of in-situ uranium leaching at Crownpoint, NM, was begun, extensive laboratory studies were undertaken to develop chemical methods for treating one possible contaminant, molybdenum (Mo). New Mexico regulations restrict the amount of Mo permissable in formation waters after leaching to less than 1 ppm. Two techniques to restore Mo after leaching were studied with core and pack tests. These studies suggest that if Mo restoration problems occur in the field, the use of precipitating agents such as Ca/sup 2+/ or reducing agents such as Fe/sup 2+/ may be helpful in ameliorating such problems

  9. Seed conservation in ex situ genebanks - genetic studies on longevity in barley

    NARCIS (Netherlands)

    Nagel, M.; Vogel, H.; Landjeva, S.; Buck-Sorlin, G.H.; Lohwasser, U.; Scholz, U.; Börner, A.

    2009-01-01

    Recognizing the danger due to a permanent risk of loss of the genetic variability of cultivated plants and their wild relatives in response to changing environmental conditions and cultural practices, plant ex situ genebank collections were created since the beginning of the last century. World-wide

  10. Applications of ribosomal in situ hybridization for the study of bacterial cells in the mouse intestine

    DEFF Research Database (Denmark)

    Licht, Tine Rask; Poulsen, Lars Kongsbak; Molin, Søren

    1997-01-01

    Localization of E. coli and S. typhimurium in the large and small intestine of streptomycin-treated mice was visualized by in situ hybridization with specific rRNA target probes and epi-fluorescence microscopy. Growth rates of E. coli BJ4 colonizing the large intestine of streptomycin-treated mic...

  11. In situ study starch gelatinization under ultra-high hydrostatic pressure using synchrotron SAXS

    KAUST Repository

    Yang, Zhi; Gu, Qinfen; Lam, Elisa; Tian, Feng; Chaieb, Saharoui; Hemar, Yacine

    2015-01-01

    The gelatinization of waxy (very low amylose) corn and potato starches by high hydrostatic pressure (HHP) (up to ∼1 GPa) was investigated in situ using synchrotron small-angle X-ray scattering (SAXS) on samples held in a diamond anvil cell (DAC

  12. A study on prediction of uranium concentration in pregnant solution from in-situ leaching

    International Nuclear Information System (INIS)

    Yi Weiping; Zhou Quan; Yu Yunzhen; Wang Shude; Yang Yihan; Lei Qifeng

    2005-01-01

    The modeling course on prediction of uranium concentration in pregnant solution from in-situ leaching of uranium is described, a mathematical model based on grey system theory is put forward, and a set of computer application software is correspondingly developed. (authors)

  13. Deformation processes in functional materials studied by in situ neutron diffraction and ultrasonic techniques

    International Nuclear Information System (INIS)

    Sittner, P.; Novak, V.; Landa, M.; Lukas, P.

    2007-01-01

    The unique thermomechanical functions of shape memory alloys (hysteretic stress-strain-temperature responses) not their structural properties (as strength, fatigue, corrosion resistance, etc.) are primarily utilized in engineering applications. In order to better understand and predict the functional behavior, we have recently employed two dedicated non-invasive in situ experimental methods capable to follow the deformation/transformation processes in thermomechanically loaded polycrystalline samples. The in situ neutron diffraction method takes advantage of the ability of thermal neutrons to penetrate bulk samples. As a diffraction technique sensitive to interplanar spacings in crystalline solids, it provides in situ information on the changes in crystal structure, phase composition, phase stress and texture in the transforming samples. The combined in situ ultrasonic and electric resistance method follows variations of the electric resistance as well as speed and attenuation of acoustic waves propagating through the transforming sample. The acoustic waves are mainly sensitive to changes of elastic properties accompanying the deformation/transformation processes. The latter method thus follows the changes in interatomic bonds rather than changes in the interplanar lattice spacings focused in the neutron diffraction method. The methods are thus complementary. They are briefly described and selected experimental results obtained recently on NiTi alloys are presented and discussed

  14. In-situ nanomechanical study on bending characteristics of individual multi-walled carbon nanotubes

    Energy Technology Data Exchange (ETDEWEB)

    Tsai, Ping-Chi, E-mail: pctjbenchen@yahoo.com.tw [Department of Mechanical Engineering, National Chung Cheng University, Chia-Yi 621, Taiwan (China); Advanced Institute of Manufacturing with High-Tech Innovations, National Chung Cheng University, Chia-Yi 621, Taiwan (China); Jeng, Yeau-Ren, E-mail: imeyrj@ccu.edu.tw [Department of Mechanical Engineering, National Chung Cheng University, Chia-Yi 621, Taiwan (China); Advanced Institute of Manufacturing with High-Tech Innovations, National Chung Cheng University, Chia-Yi 621, Taiwan (China)

    2016-03-21

    Bending characteristics of individual thin-walled carbon nanotubes (CNTs) are investigated through a novel in-situ nanoindentation in transmission electron microscopy. Unlike thick-walled CNTs, the graphitic layers of thin ones buckle into V-shaped kinks rather than Yoshimura ripples. These kinks are found to be entirely reversible without residual plastic deformation following unloading.

  15. In situ study of radionuclide diffusion into clays with specific device: Autolab probe

    International Nuclear Information System (INIS)

    Porcheron, J.

    1993-01-01

    The aim of this shared cost contract between the French Atomic Energy Commissariat, Nuclear Safety and Protection Institute and the Commission of the European Communities was to build and use an experimental drilling probe, the AUTOLAB prob, which was designed to measure the diffusion into clay of radioactive pollutants originating from a high activity waste storage. The measurement was carried out in-situ during drilling. The probe is equipped a new operating mode which involves using the pressure of the drilling water as its source of energy. The probe is autonomous and can stay in the bore hole for an extensive period of time without requiring any monitoring and without introducing any pollution. The diffusion experiment was carried out in a bore-hole at the JRC in ISPRA (ITALY). Two diffusion experiments were carried out in identical conditions (clay, 85Sr tracer, water samples), one in Laboratory, (ISPRA JRC Radiochemistry Laboratory, ITALY), and the other in-situ. The results displayed that 85Sr diffusion was considerably faster in the in-situ experiment than in that conducted in Laboratory. The explanation for this phenomenon, which could be due to the balance of carbonates, has not yet been clearly established. This test shows the value of comparing laboratory tests with in-situ tests conducted accurately using well adapted equipment. 9 refs., 10 figs

  16. In Situ Study of Live Specimens in an Environmental Scanning Electron Microscope

    Czech Academy of Sciences Publication Activity Database

    Tihlaříková, Eva; Neděla, Vilém; Shiojiri, M.

    2013-01-01

    Roč. 19, č. 4 (2013), s. 914-918 ISSN 1431-9276 R&D Projects: GA ČR GAP102/10/1410 Institutional support: RVO:68081731 Keywords : live biological sample * high-pressure environment * hydration system * in situ observation * Monte Carlo simulation * methodology Subject RIV: JA - Electronics ; Optoelectronics, Electrical Engineering Impact factor: 1.757, year: 2013

  17. In situ nuclear magnetic resonance study of defect dynamics during deformation of materials

    NARCIS (Netherlands)

    Murty, K.L.; Detemple, K.; Kanert, O.; Peters, G; de Hosson, J.T.M.

    1996-01-01

    Nuclear magnetic resonance techniques can be used to monitor in situ the dynamical behaviour of point and line defects in materials during deformation. These techniques are non-destructive and non-invasive. We report here the atomic transport, in particular the enhanced diffusion during deformation

  18. In Situ X-ray Diffraction Studies of (De)lithiation Mechanism in Silicon Nanowire Anodes

    KAUST Repository

    Misra, Sumohan; Liu, Nian; Nelson, Johanna; Hong, Seung Sae; Cui, Yi; Toney, Michael F.

    2012-01-01

    -Si product has been observed. In this work, we use an X-ray transparent battery cell to perform in situ synchrotron X-ray diffraction on SiNWs in real time during electrochemical cycling. At deep lithiation voltages the known metastable Li 15Si 4 phase forms

  19. First in situ TOF-PET study using digital photon counters for proton range verification

    NARCIS (Netherlands)

    Cambraia Lopes Ferreira da Silva, P.; Bauer, J.; Salomon, A.; Rinaldi, I; Tabacchini, V.; Tessonnier, T.; Crespo, P; Parodi, K; Schaart, D.R.

    2016-01-01

    Positron emission tomography (PET) is the imaging modality most extensively tested for treatment monitoring in particle therapy. Optimal use of PET in proton therapy requires in situ acquisition of the relatively strong 15O signal due to its relatively short half-life (∼2 min) and high

  20. In situ bioremediation of petroleum hydrocarbons and chlorinated hydrocarbons: Three case studies

    International Nuclear Information System (INIS)

    Bost, R.C.; Perry, R.G.; Barber, T.

    1997-01-01

    In situ biodegradation of organic contaminants is one of the most cost-effective means of site remediation. This method has proven successful in soils, ground water, and slurries. Bacteria capable of degrading organic contaminants within an aquifer include many species from a wide spectrum of genera, e.g. Pseudomonas, Corynebacterium, Bacillus, etc. In most cases, a mixture of bacterial strains is required to completely oxidize a complex organic contaminant. Each strain of an organism may target a specific compound, working together with other organisms to ultimately degrade each intermediate until complete degradation, also known as mineralization, occurs. One or more of the following mechanisms are utilized by bacteria for organic chemical degradation: (1) aerobic, (2) anaerobic, and (3) co-metabolic. During aerobic oxidation of organic chemicals, bacteria utilize the pollutant as an electron and hydrogen source and oxygen acts as the electron and hydrogen acceptor, resulting in water. As the bacterial enzymes cleave the compound, oxidized products are produced along with energy for the reaction to proceed. This is the most rapid and widely utilized mechanism. Dehalogenation occurs under aerobic, or perhaps more often, under anoxic conditions. This process occurs in the presence of alternate electron acceptors and replaces chlorine with hydrogen. The mechanism of co-metabolism can be aerobic or anaerobic, but is more often aerobic. This process requires a separate energy source for the bacterial cell because the pollutant is not utilized as an energy source. The role of bioremediation in site remediation is demonstrated below by three case studies: (1) a refinery, (2) a municipal landfill and (3) a pesticide formulation plant

  1. Conductivity percolation in loosely compacted microcrystalline cellulose: An in situ study by dielectric spectroscopy during densification.

    Science.gov (United States)

    Nilsson, Martin; Frenning, Göran; Gråsjö, Johan; Alderborn, Göran; Strømme, Maria

    2006-10-19

    The present study aims at contributing to a complete understanding of the water-induced ionic charge transport in cellulose. The behavior of this transport in loosely compacted microcrystalline cellulose (MCC) powder was investigated as a function of density utilizing a new type of measurement setup, allowing for dielectric spectroscopy measurement in situ during compaction. The ionic conductivity in MCC was found to increase with increasing density until a leveling-out was observed for densities above approximately 0.7 g/cm3. Further, it was shown that the ionic conductivity vs density followed a percolation type behavior signifying the percolation of conductive paths in a 3D conducting network. The density percolation threshold was found to be between approximately 0.2 and 0.4 g/cm3, depending strongly on the cellulose moisture content. The observed percolation behavior was attributed to the forming of interparticulate bonds in the MCC and the percolation threshold dependence on moisture was linked to the moisture dependence of particle rearrangement and plastic deformation in MCC during compaction. The obtained results add to the understanding of the density-dependent water-induced ionic transport in cellulose showing that, at given moisture content, the two major parameters determining the magnitude of the conductivity are the connectedness of the interparticluate bonds and the connectedness of pores with a diameter in the 5-20 nm size range. At densities between approximately 0.7 and 1.2 g/cm3 both the bond and the pore networks have percolated, facilitating charge transport through the MCC compact.

  2. "In Situ Vascular Nerve Graft" for Restoration of Intrinsic Hand Function: An Anatomical Study.

    Science.gov (United States)

    Mozaffarian, Kamran; Zemoodeh, Hamid Reza; Zarenezhad, Mohammad; Owji, Mohammad

    2018-06-01

    In combined high median and ulnar nerve injury, transfer of the posterior interosseous nerve branches to the motor branch of the ulnar nerve (MUN) is previously described in order to restore intrinsic hand function. In this operation a segment of sural nerve graft is required to close the gap between the donor and recipient nerves. However the thenar muscles are not innervated by this nerve transfer. The aim of the present study was to evaluate whether the superficial radial nerve (SRN) can be used as an "in situ vascular nerve graft" to connect the donor nerves to the MUN and the motor branch of median nerve (MMN) at the same time in order to address all denervated intrinsic and thenar muscles. Twenty fresh male cadavers were dissected in order to evaluate the feasibility of this modification of technique. The size of nerve branches, the number of axons and the tension at repair site were evaluated. This nerve transfer was technically feasible in all specimens. There was no significant size mismatch between the donor and recipient nerves Conclusions: The possible advantages of this modification include innervation of both median and ulnar nerve innervated intrinsic muscles, preservation of vascularity of the nerve graft which might accelerate the nerve regeneration, avoidance of leg incision and therefore the possibility of performing surgery under regional instead of general anesthesia. Briefly, this novel technique is a viable option which can be used instead of conventional nerve graft in some brachial plexus or combined high median and ulnar nerve injuries when restoration of intrinsic hand function by transfer of posterior interosseous nerve branches is attempted.

  3. Reduction of mixed Mn-Zr oxides: in situ XPS and XRD studies.

    Science.gov (United States)

    Bulavchenko, O A; Vinokurov, Z S; Afonasenko, T N; Tsyrul'nikov, P G; Tsybulya, S V; Saraev, A A; Kaichev, V V

    2015-09-21

    A series of mixed Mn-Zr oxides with different molar ratios Mn/Zr (0.1-9) have been prepared by coprecipitation of manganese and zirconium nitrates and characterized by X-ray diffraction (XRD) and BET methods. It has been found that at concentrations of Mn below 30 at%, the samples are single-phase solid solutions (MnxZr1-xO2-δ) based on a ZrO2 structure. X-ray photoelectron spectroscopy (XPS) measurements showed that manganese in these solutions exists mainly in the Mn(4+) state on the surface. An increase in Mn content mostly leads to an increase in the number of Mn cations in the structure of solid solutions; however, a part of the manganese cations form Mn2O3 and Mn3O4 in the crystalline and amorphous states. The reduction of these oxides with hydrogen was studied by a temperature-programmed reduction technique, in situ XRD, and near ambient pressure XPS in the temperature range from 100 to 650 °C. It was shown that the reduction of the solid solutions MnxZr1-xO2-δ proceeds via two stages. During the first stage, at temperatures between 100 and 500 °C, the Mn cations incorporated into the solid solutions MnxZr1-xO2-δ undergo partial reduction. During the second stage, at temperatures between 500 and 700 °C, Mn cations segregate on the surface of the solid solution. In the samples with more than 30 at% Mn, the reduction of manganese oxides was observed: Mn2O3 → Mn3O4 → MnO.

  4. An in situ Study of NiTi Powder Sintering Using Neutron Diffraction

    Directory of Open Access Journals (Sweden)

    Gang Chen

    2015-04-01

    Full Text Available This study investigates phase transformation and mechanical properties of porous NiTi alloys using two different powder compacts (i.e., Ni/Ti and Ni/TiH2 by a conventional press-and-sinter means. The compacted powder mixtures were sintered in vacuum at a final temperature of 1373 K. The phase evolution was performed by in situ neutron diffraction upon sintering and cooling. The predominant phase identified in all the produced porous NiTi alloys after being sintered at 1373 K is B2 NiTi phase with the presence of other minor phases. It is found that dehydrogenation of TiH2 significantly affects the sintering behavior and resultant microstructure. In comparison to the Ni/Ti compact, dehydrogenation occurring in the Ni/TiH2 compact leads to less densification, yet higher chemical homogenization, after high temperature sintering but not in the case of low temperature sintering. Moreover, there is a direct evidence of the eutectoid decomposition of NiTi at ca. 847 and 823 K for Ni/Ti and Ni/TiH2, respectively, during furnace cooling. The static and cyclic stress-strain behaviors of the porous NiTi alloys made from the Ni/Ti and Ni/TiH2 compacts were also investigated. As compared with the Ni/Ti sintered samples, the samplessintered from the Ni/TiH2 compact exhibited a much higher porosity, a higher close-to-total porosity, a larger pore size and lower tensile and compressive fracture strength.

  5. Intracellular distribution of histone mRNAs in human fibroblasts studied by in situ hybridization

    International Nuclear Information System (INIS)

    Lawrence, J.B.; Singer, R.H.; Villnave, C.A.; Stein, J.L.; Stein, G.S.

    1988-01-01

    We have used in situ hybridization to study the intracellular distribution of mRNAs for cell cycle-dependent core and H1 histone proteins in human WI-38 fibroblasts. Because histones are abundant nuclear proteins and histone mRNA expression is tightly coupled to DNA synthesis, it was of interest to determine whether histone mRNAs are localized near the nucleus. Cells were hybridized with tritiated DNA probes specific for either histone H1, histone H4, actin, or poly(A)+ mRNA and were processed for autoradiography. In exponentially growing cultures, the fraction of histone mRNA-positive cells correlated well with the fraction of cells in S phase and was eliminated by hydroxyurea inhibition of DNA synthesis. Within individual cells the label for histone mRNA was widely distributed throughout the cytoplasm and did not appear to be more heavily concentrated near the nucleus. However, histone mRNA appeared to exhibit patchy, nonhomogeneous localization, and a quantitative evaluation confirmed that grain distributions were not as uniform as they were after hybridizations to poly(A)+ mRNA. Actin mRNA in WI-38 cells was also widely distributed throughout the cytoplasm but differed from histone mRNA in that label for actin mRNA was frequently most dense at the outermost region of narrow cell extensions. The localization of actin mRNA was less pronounced but qualitatively very similar to that previously described for chicken embryonic myoblasts and fibroblasts. We conclude that localization of histones in WI-38 cells is not facilitated by localization of histone protein synthesis near the nucleus and that there are subtle but discrete and potentially functional differences in the distributions of histone, actin, and poly(A)+ mRNAs

  6. Wavefront-guided versus wavefront-optimized laser in situ keratomileusis: contralateral comparative study.

    Science.gov (United States)

    Padmanabhan, Prema; Mrochen, Michael; Basuthkar, Subam; Viswanathan, Deepa; Joseph, Roy

    2008-03-01

    To compare the outcomes of wavefront-guided and wavefront-optimized treatment in fellow eyes of patients having laser in situ keratomileusis (LASIK) for myopia. Medical and Vision Research Foundation, Tamil Nadu, India. This prospective comparative study comprised 27 patients who had wavefront-guided LASIK in 1 eye and wavefront-optimized LASIK in the fellow eye. The Hansatome (Bausch & Lomb) was used to create a superior-hinged flap and the Allegretto laser (WaveLight Laser Technologie AG), for photoablation. The Allegretto wave analyzer was used to measure ocular wavefront aberrations and the Functional Acuity Contrast Test chart, to measure contrast sensitivity before and 1 month after LASIK. The refractive and visual outcomes and the changes in aberrations and contrast sensitivity were compared between the 2 treatment modalities. One month postoperatively, 92% of eyes in the wavefront-guided group and 85% in the wavefront-optimized group had uncorrected visual acuity of 20/20 or better; 93% and 89%, respectively, had a postoperative spherical equivalent refraction of +/-0.50 diopter. The differences between groups were not statistically significant. Wavefront-guided LASIK induced less change in 18 of 22 higher-order Zernike terms than wavefront-optimized LASIK, with the change in positive spherical aberration the only statistically significant one (P= .01). Contrast sensitivity improved at the low and middle spatial frequencies (not statistically significant) and worsened significantly at high spatial frequencies after wavefront-guided LASIK; there was a statistically significant worsening at all spatial frequencies after wavefront-optimized LASIK. Although both wavefront-guided and wavefront-optimized LASIK gave excellent refractive correction results, the former induced less higher-order aberrations and was associated with better contrast sensitivity.

  7. The impact of in situ breast cancer and family history on risk of subsequent breast cancer events and mortality - a population-based study from Sweden

    NARCIS (Netherlands)

    Sackey, Helena; Hui, Miao; Czene, Kamila; Verkooijen, Helena; Edgren, Gustaf; Frisell, Jan; Hartman, Mikael

    2016-01-01

    BACKGROUND: The clinical behavior of in situ breast cancer is incompletely understood and several factors have been associated with invasive recurrence. The purpose of this study was to evaluate long-term risk of subsequent breast cancer and mortality among women diagnosed with in situ breast

  8. A Next-Generation Hard X-Ray Nanoprobe Beamline for In Situ Studies of Energy Materials and Devices

    Science.gov (United States)

    Maser, Jörg; Lai, Barry; Buonassisi, Tonio; Cai, Zhonghou; Chen, Si; Finney, Lydia; Gleber, Sophie-Charlotte; Jacobsen, Chris; Preissner, Curt; Roehrig, Chris; Rose, Volker; Shu, Deming; Vine, David; Vogt, Stefan

    2014-01-01

    The Advanced Photon Source is developing a suite of new X-ray beamlines to study materials and devices across many length scales and under real conditions. One of the flagship beamlines of the APS upgrade is the In Situ Nanoprobe (ISN) beamline, which will provide in situ and operando characterization of advanced energy materials and devices under varying temperatures, gas ambients, and applied fields, at previously unavailable spatial resolution and throughput. Examples of materials systems include inorganic and organic photovoltaic systems, advanced battery systems, fuel cell components, nanoelectronic devices, advanced building materials and other scientifically and technologically relevant systems. To characterize these systems at very high spatial resolution and trace sensitivity, the ISN will use both nanofocusing mirrors and diffractive optics to achieve spots sizes as small as 20 nm. Nanofocusing mirrors in Kirkpatrick-Baez geometry will provide several orders of magnitude increase in photon flux at a spatial resolution of 50 nm. Diffractive optics such as zone plates and/or multilayer Laue lenses will provide a highest spatial resolution of 20 nm. Coherent diffraction methods will be used to study even small specimen features with sub-10 nm relevant length scale. A high-throughput data acquisition system will be employed to significantly increase operations efficiency and usability of the instrument. The ISN will provide full spectroscopy capabilities to study the chemical state of most materials in the periodic table, and enable X-ray fluorescence tomography. In situ electrical characterization will enable operando studies of energy and electronic devices such as photovoltaic systems and batteries. We describe the optical concept for the ISN beamline, the technical design, and the approach for enabling a broad variety of in situ studies. We furthermore discuss the application of hard X-ray microscopy to study defects in multi-crystalline solar cells, one

  9. Petroleum Science and Technology Institute with the TeXas Earth and Space Science (TXESS) Revolution

    Science.gov (United States)

    Olson, H. C.; Olson, J. E.; Bryant, S. L.; Lake, L. W.; Bommer, P.; Torres-Verdin, C.; Jablonowski, C.; Willis, M.

    2009-12-01

    The TeXas Earth and Space Science (TXESS) Revolution, a professional development program for 8th- thru 12th-grade Earth Science teachers, presented a one-week Petroleum Science and Technology Institute at The University of Texas at Austin campus. The summer program was a joint effort between the Jackson School of Geosciences and the Department of Petroleum and Geosystems Engineering. The goal of the institute was to focus on the STEM components involved in the petroleum industry and to introduce teachers to the larger energy resources theme. The institute kicked off with a welcoming event and tour of a green, energy-efficient home (LEED Platinum certified) owned by one of the petroleum engineering faculty. Tours of the home included an introduction to rainwater harvesting, solar energy, sustainable building materials and other topics on energy efficiency. Classroom topics included drilling technology (including a simulator lab and an overview of the history of the technology), energy use and petroleum geology, well-logging technology and interpretation, reservoir engineering and volumetrics (including numerous labs combining chemistry and physics), risk assessment and economics, carbon capture and storage (CO2 sequestration technology) and hydraulic fracturing. A mid-week field trip included visiting the Ocean Star offshore platform in Galveston, the Weiss Energy Hall at the Houston Museum of Science and Schlumberger (to view 3-D visualization technology) in Houston. Teachers remarked that they really appreciated the focused nature of the institute and especially found the increased use of mathematics both a tool for professional growth, as well as a challenge for them to use more math in their science classes. STEM integration was an important feature of the summer institute, and teachers found the integration of science (earth sciences, geophysics), technology, engineering (petroleum, chemical and reservoir) and mathematics particularly valuable. Pre

  10. Nucleation and growth of elastin-like peptide fibril multilayers: an in situ atomic force microscopy study

    International Nuclear Information System (INIS)

    Yang Guocheng; Yip, Christopher M; Wong, Michael K; Lin, Lauren E

    2011-01-01

    Controlling how molecules assemble into complex supramolecular architectures requires careful consideration of the subtle inter- and intra-molecular interactions that control their association. This is particularly crucial in the context of assembly at interfaces, where both surface chemistry and structure can play a role in directing structure formation. We report here the results of a study into the self-assembly of the elastin-like peptide EP I on structurally modified highly ordered pyrolytic graphite, including the role of spatial confinement on fibril nucleation and the growth of oriented fibril multilayers. In situ atomic force microscopy performed in fluid and at elevated temperature provided direct evidence of frustrated fibril nuclei and oriented growth of independent fibril domains. These results portend the application of this in situ strategy for studies of the nucleation and growth mechanisms of other fibril- and amyloid-forming proteins.

  11. A new in situ technique for studying deformation and fracture in thin film ductile/brittle laminates

    International Nuclear Information System (INIS)

    Hackney, S.A.; Milligan, W.W.

    1991-01-01

    A new technique for studying deformation and fracture of thin film ductile/brittle laminates is described. The laminates are prepared by sputtering a brittle coating on top of an electropolished TEM thin foil. The composites are then strained in situ in the TEM. In this preliminary investigation, the composites consisted of a ductile aluminum substrate and a brittle silicon coating. Cracks in the brittle film grew discontinuously in bursts several micrometers in length. The crack opening displacement initiated plastic deformation in the ductile film, thus dissipating energy and allowing crack arrest. The interface was well bonded, and delamination was not observed. Due to the good interfacial bond and the crack opening behind the crack tip, it was possible to study very large plastic deformations and ductile fracture in the aluminum in situ, without buckling of the foil. The possibility of micromechanical modeling of the fracture behavior is briefly discussed. (orig.)

  12. In situ AFM study of pitting corrosion and corrosion under strain on a 304L stainless steel

    International Nuclear Information System (INIS)

    Martin, F.A.; Cousty, J.; Masson, J-L.; Bataillon, C.

    2004-01-01

    Our study is centred on surface localised corrosion under strain of a standard stainless steel (304L). The interest we take in these corrosion phenomena is led by the general misunderstanding of its primary initiation steps. The goal of this study is to determine precisely the relationships between local geometrical defects (grain boundaries, dislocation lines, etc) or chemical defects (inclusions) with the preferential sites of corrosion on the strained material. By combining three techniques at the same time: Atomic Force Microscopy, an electrochemical cell and a traction plate, we can observe in situ the effect of localised stress and deformation on the sample surface exposed to a corrosive solution. We managed to build an original set-up compatible with all the requirements of these three different techniques. Furthermore, we prepared the surface of our sample as flat as possible to decrease at maximum the topographical noise in order to observe the smallest defect on the surface. By using a colloidal suspension of SiO 2 , we obtained surfaces with a typical corrugation (RMS) of about 1 A for areas of at least 1 μm 2 . Our experimental study has been organised in two primary investigations: - In situ study of the morphology evolution of the surface under a corrosive chloride solution (borate buffer with NaCl salt). The influence of time, NaCl concentration, and potential was investigated; - In situ exploration of a 304L strained surface. It revealed the first stages of the surface plastic evolutions like activation of sliding dislocations, materialized by parallel steps of about 2 nm high in the same grain. The secondary sliding plane systems were also noticeable for higher deformation rates. Recent results concerning in situ AFM observation of corroded surfaces under strain in a chloride media will be presented. (authors)

  13. In situ AFM study of pitting corrosion and corrosion under strain on a 304L stainless steel

    Energy Technology Data Exchange (ETDEWEB)

    Martin, F.A. [CEA de Saclay, DRECAM/SPCSI, 91191 Gif-sur-Yvette cedex (France); Cousty, J.; Masson, J-L. [CEA de Saclay, DRECAM/SPCSI, 91191 Gif-sur-Yvette cedex (France); Bataillon, C. [CEA de Saclay, DEN/DPC/LECA, 91191 Gif-sur-Yvette cedex (France)

    2004-07-01

    Our study is centred on surface localised corrosion under strain of a standard stainless steel (304L). The interest we take in these corrosion phenomena is led by the general misunderstanding of its primary initiation steps. The goal of this study is to determine precisely the relationships between local geometrical defects (grain boundaries, dislocation lines, etc) or chemical defects (inclusions) with the preferential sites of corrosion on the strained material. By combining three techniques at the same time: Atomic Force Microscopy, an electrochemical cell and a traction plate, we can observe in situ the effect of localised stress and deformation on the sample surface exposed to a corrosive solution. We managed to build an original set-up compatible with all the requirements of these three different techniques. Furthermore, we prepared the surface of our sample as flat as possible to decrease at maximum the topographical noise in order to observe the smallest defect on the surface. By using a colloidal suspension of SiO{sub 2}, we obtained surfaces with a typical corrugation (RMS) of about 1 A for areas of at least 1 {mu}m{sup 2}. Our experimental study has been organised in two primary investigations: - In situ study of the morphology evolution of the surface under a corrosive chloride solution (borate buffer with NaCl salt). The influence of time, NaCl concentration, and potential was investigated; - In situ exploration of a 304L strained surface. It revealed the first stages of the surface plastic evolutions like activation of sliding dislocations, materialized by parallel steps of about 2 nm high in the same grain. The secondary sliding plane systems were also noticeable for higher deformation rates. Recent results concerning in situ AFM observation of corroded surfaces under strain in a chloride media will be presented. (authors)

  14. In-situ high temperature irradiation setup for temperature dependent structural studies of materials under swift heavy ion irradiation

    International Nuclear Information System (INIS)

    Kulriya, P.K.; Kumari, Renu; Kumar, Rajesh; Grover, V.; Shukla, R.; Tyagi, A.K.; Avasthi, D.K.

    2015-01-01

    An in-situ high temperature (1000 K) setup is designed and installed in the materials science beam line of superconducting linear accelerator at the Inter-University Accelerator Centre (IUAC) for temperature dependent ion irradiation studies on the materials exposed with swift heavy ion (SHI) irradiation. The Gd 2 Ti 2 O 7 pyrochlore is irradiated using 120 MeV Au ion at 1000 K using the high temperature irradiation facility and characterized by ex-situ X-ray diffraction (XRD). Another set of Gd 2 Ti 2 O 7 samples are irradiated with the same ion beam parameter at 300 K and simultaneously characterized using in-situ XRD available in same beam line. The XRD studies along with the Raman spectroscopic investigations reveal that the structural modification induced by the ion irradiation is strongly dependent on the temperature of the sample. The Gd 2 Ti 2 O 7 is readily amorphized at an ion fluence 6 × 10 12 ions/cm 2 on irradiation at 300 K, whereas it is transformed to a radiation-resistant anion-deficient fluorite structure on high temperature irradiation, that amorphized at ion fluence higher than 1 × 10 13 ions/cm 2 . The temperature dependent ion irradiation studies showed that the ion fluence required to cause amorphization at 1000 K irradiation is significantly higher than that required at room temperature irradiation. In addition to testing the efficiency of the in-situ high temperature irradiation facility, the present study establishes that the radiation stability of the pyrochlore is enhanced at higher temperatures

  15. In Situ Atomic Force Microscopy Studies on Nucleation and Self-Assembly of Biogenic and Bio-Inspired Materials

    Directory of Open Access Journals (Sweden)

    Cheng Zeng

    2017-08-01

    Full Text Available Through billions of years of evolution, nature has been able to create highly sophisticated and ordered structures in living systems, including cells, cellular components and viruses. The formation of these structures involves nucleation and self-assembly, which are fundamental physical processes associated with the formation of any ordered structure. It is important to understand how biogenic materials self-assemble into functional and highly ordered structures in order to determine the mechanisms of biological systems, as well as design and produce new classes of materials which are inspired by nature but equipped with better physiochemical properties for our purposes. An ideal tool for the study of nucleation and self-assembly is in situ atomic force microscopy (AFM, which has been widely used in this field and further developed for different applications in recent years. The main aim of this work is to review the latest contributions that have been reported on studies of nucleation and self-assembly of biogenic and bio-inspired materials using in situ AFM. We will address this topic by introducing the background of AFM, and discussing recent in situ AFM studies on nucleation and self-assembly of soft biogenic, soft bioinspired and hard materials.

  16. Combining in situ transmission electron microscopy irradiation experiments with cluster dynamics modeling to study nanoscale defect agglomeration in structural metals

    International Nuclear Information System (INIS)

    Xu Donghua; Wirth, Brian D.; Li Meimei; Kirk, Marquis A.

    2012-01-01

    We present a combinatorial approach that integrates state-of-the-art transmission electron microscopy (TEM) in situ irradiation experiments and high-performance computing techniques to study irradiation defect dynamics in metals. Here, we have studied the evolution of visible defect clusters in nanometer-thick molybdenum foils under 1 MeV krypton ion irradiation at 80 °C through both cluster dynamics modeling and in situ TEM experiments. The experimental details are reported elsewhere; we focus here on the details of model construction and comparing the model with the experiments. The model incorporates continuous production of point defects and/or small clusters, and the accompanying interactions, which include clustering, recombination and loss to the surfaces that result from the diffusion of the mobile defects. To account for the strong surface effect in thin TEM foils, the model includes one-dimensional spatial dependence along the foil depth, and explicitly treats the surfaces as black sinks. The rich amount of data (cluster number density and size distribution at a variety of foil thickness, irradiation dose and dose rate) offered by the advanced in situ experiments has allowed close comparisons with computer modeling and permitted significant validation and optimization of the model in terms of both physical model construct (damage production mode, identities of mobile defects) and parameterization (diffusivities of mobile defects). The optimized model exhibits good qualitative and quantitative agreement with the in situ TEM experiments. The combinatorial approach is expected to bring a unique opportunity for the study of radiation damage in structural materials.

  17. Exciton confinement in strain-engineered metamorphic InAs/I nxG a1 -xAs quantum dots

    Science.gov (United States)

    Khattak, S. A.; Hayne, M.; Huang, J.; Vanacken, J.; Moshchalkov, V. V.; Seravalli, L.; Trevisi, G.; Frigeri, P.

    2017-11-01

    We report a comprehensive study of exciton confinement in self-assembled InAs quantum dots (QDs) in strain-engineered metamorphic I nxG a1 -xAs confining layers on GaAs using low-temperature magnetophotoluminescence. As the lattice mismatch (strain) between QDs and confining layers (CLs) increases from 4.8% to 5.7% the reduced mass of the exciton increases, but saturates at higher mismatches. At low QD-CL mismatch there is clear evidence of spillover of the exciton wave function due to small localization energies. This is suppressed as the In content x in the CLs decreases (mismatch and localization energy increasing). The combined effects of low effective mass and wave-function spillover at high x result in a diamagnetic shift coefficient that is an order of magnitude larger than for samples where In content in the barrier is low (mismatch is high and localization energy is large). Finally, an anomalously small measured Bohr radius in samples with the highest x is attributed to a combination of thermalization due to low localization energy, and its enhancement with magnetic field, a mechanism which results in small dots in the ensemble dominating the measured Bohr radius.

  18. Nucleation and Nanometric Inhomogeneity in Niobiogermanate Glass: In-Situ Inelastic Light Scattering and TEM Studies

    International Nuclear Information System (INIS)

    Takahashi, Y; Ihara, R; Fujiwara, T; Osada, M; Masai, H

    2011-01-01

    We performed in-situ inelastic light scattering measurement in KNbGeO 5 glass with a high nucleation ability during heating in order to elucidate nanocrystallization dynamics. The results of the in-situ measurement and TEM observation revealed that nanometric heterogeneous region (∼1-2 nm) consisting of the Nb-richer phase develops, i.e., K 3 Nb 7 O 19 , at the temperature, in which glassy-supercooled-liquid (SCL) phase-transition occurs, i.e., precursive stage of nanocrystallization. This strongly suggests that evolution of the nanometric Nb-richer phase in the SCL phase corresponds to nucleation in the KNbGeO 5 glass.

  19. Solid oxide electrode kinetics in light of in situ surface studies

    DEFF Research Database (Denmark)

    Mogensen, Mogens Bjerg

    2014-01-01

    The combination of in situ and in particular in operando characterization methods such as electrochemical impedance spectroscopy (EIS) on both technical and model electrode are well known ways to gain some practical insight in electrode reaction kinetics. Yet, is has become clear that in spite...... of the strengths it is not sufficient to reveal much details of the electrode mechanisms mainly because it provide average values only. Therefore it has to be combined with surface science methods in order to reveal the interface structure and composition. Ex situ methods have been very useful over the latest....... Furthermore, it seems that detailed mathematical modeling using new tools like COMSOL is necessary for the synthesis of the large amount of data for a well-characterized electrode into one physical meaningful picture. A brief review of literature an own data will be presented with a practical example of SOFC...

  20. Design of in-situ reactive wall systems - a combined hydraulical-geochemical-economical simulation study

    International Nuclear Information System (INIS)

    Teutsch, G.; Tolksdorff, J.; Schad, H.

    1997-01-01

    The paper presents a coupled hydraulical-geochemical-economical simulation model for the design of in-situ reactive wall systems. More specific, the model is used for cost-optimization and sensitivity analysis of a funnel-and-gate system with an in-situ sorption reactor. The groundwater flow and advective transport are simulated under steady-state conditions using a finite-difference numerical model. This model is coupled to an analytical solution describing the sorption kinetics of hydrophobic organic compounds within the reactor (gate). The third part of the model system is an economical model which calculates (a) the investment costs for the funnel-and-gate construction and (b) the operation cost based on the number of reactor refills, which depends on the breakthrough time for a given contaminant and the anticipated total operation time. For practical applications a simplified approximation of the cost-function is derived and tested

  1. An in situ Fourier transform infrared spectroelectrochemical study on ethanol electrooxidation on Pd in alkaline solution

    Energy Technology Data Exchange (ETDEWEB)

    Fang, Xiang; Wang, Lianqin; Shen, Pei Kang [The State Key Laboratory of Optoelectronic Materials and Technologies, School of Physics and Engineering, Sun Yat-Sen University, Guangzhou 510275 (China); Cui, Guofeng [School of Chemistry and Chemical Engineering, Sun Yat-Sen University, Guangzhou 510275 (China); Bianchini, Claudio [Istituto di Chimica dei Composti Organometallici (ICCOM-CNR), via Madonna del Piano 10, 50019 Sesto Fiorentino (Italy)

    2010-03-01

    The mechanism of ethanol electrooxidation on a palladium electrode in alkaline solution (from 0.01 to 5 M NaOH) has been investigated by cyclic voltammetry and in situ Fourier transform infrared spectroelectrochemistry. The electrode performance has been found to depend on the pH of the fuel solution. The best performance was observed in 1 M NaOH solution (pH = 14), while the electrochemical activity decreased by either increasing or decreasing the NaOH concentration. In situ FTIR spectroscopic measurements showed the main oxidation product to be sodium acetate at NaOH concentrations higher than 0.5 M. The C-C bond cleavage of ethanol, put in evidence by the formation of CO{sub 2}, occurred at pH values {<=}13. In these conditions, however, the catalytic activity for ethanol oxidation was quite low. No CO formation was detected along the oxidation of ethanol by FTIR spectroscopy. (author)

  2. Ion scattering spectroscopy studies of zirconium dioxide thin films prepared in situ

    International Nuclear Information System (INIS)

    Martin, P.J.; Netterfield, R.P.

    1987-01-01

    Low energy Ion Scattering Spectroscopy has been used to investigate, in situ, thin films of zirconium dioxide deposited by evaporation and ion-assisted deposition. It is shown that when a film is deposited to an average thickness of 0.3 nm +- 0.03, as measured by in situ ellipsometry, complete coverage of the substrate occurs. 'Ion-assisted films have detectably higher Zr surface concentrations and reduced low-energy sputter peaks. Inelastic tailing effects in the Zr scattering peak for 2 keV 4 He + are found to come from particles scattered from approximately the first 7 nm of the oxide surface. The influence of primary ion energy on the Zr/O ratio is also examined. (author)

  3. In-situ white beam microdiffraction study of the deformation behavior in polycrystalline magnesium alloy during uniaxial loading

    International Nuclear Information System (INIS)

    Advanced Light Source; Tamura, Nobumichi; Lynch, P.A.; Stevenson, A.W.; Liang, D.; Parry, D.; Wilkins, S.; Madsen, I.C.; Bettles, C.; Tamura, N.; Geandier, G.

    2007-01-01

    Scanning white beam X-ray microdiffraction has been used to study the heterogeneous grain deformation in a polycrystalline Mg alloy (MgAZ31). The high spatial resolution achieved on beamline 7.3.3 at the Advanced Light Source provides a unique method to measure the elastic strain and orientation of single grains as a function of applied load. To carry out in-situ measurements a light weight (∼0.5kg) tensile stage, capable of providing uniaxial loads of up to 600kg, was designed to collect diffraction data on the loading and unloading cycle. In-situ observation of the deformation process provides insight about the crystallographic deformation mode via twinning and dislocation slip

  4. Laboratory study on leaching of a sandstone-type uranium deposit for acid in-situ leaching

    International Nuclear Information System (INIS)

    Wen Zhenqian; Yao Yixuan; Zheng Jianping; Jiang Yan; Cui Xin; Xing Yongguo; Hao Jinting; Tang Huazhang

    2013-01-01

    Ore samples were took from in-situ leaching experiment boreholes in a sandstone-type uranium deposit. Technological mineralogy study, agitating leaching and column leaching experiments were carried. The results show that the content of minerals consuming acid and deoxidized minerals is low. When sulfuric acid concentration was 1O g/L, initial uranium content was 0.0224%, and liquid-to-solid ratio was l.91, leaching rate of column leaching experiments is 89.19%, acid consumption is 8.2 kg/t ore, acid consumption is 41.88 t/tU. Acid leaching, technology is recommend for field in-situ leaching experiment, sulfuric acid concentration in confecting solution is 10 g/L, and oxidizing agent is needless during leaching process. (authors)

  5. In-situ XRD and EDS method study on the oxidation behaviour of Ni-Cu sulphide ore.

    Science.gov (United States)

    Li, Guangshi; Cheng, Hongwei; Xiong, Xiaolu; Lu, Xionggang; Xu, Cong; Lu, Changyuan; Zou, Xingli; Xu, Qian

    2017-06-12

    The oxidation mechanism of sulfides is the key issue during the sulphide-metallurgy process. In this study, the phase transformation and element migration were clearly demonstrated by in-situ laboratory-based X-ray diffraction (XRD) and energy-dispersive X-ray spectroscopy (EDS), respectively. The reaction sequence and a four-step oxidation mechanism were proposed and identified. The elemental distribution demonstrated that at a low temperature, the Fe atoms diffused outward and the Ni/Cu atoms migrated toward the inner core, whereas the opposite diffusion processes were observed at a higher temperature. Importantly, the unique visual presentation of the oxidation behaviour provided by the combination of in-situ XRD and EDS might be useful for optimising the process parameters to improve the Ni/Cu extraction efficiency during Ni-Cu sulphide metallurgy.

  6. Study of the inhomogeneity of critical current under in-situ tensile stress for YBCO tape

    Science.gov (United States)

    Zhu, Y. P.; Chen, W.; Zhang, H. Y.; Liu, L. Y.; Pan, X. F.; Yang, X. S.; Zhao, Y.

    2018-07-01

    A Hall sensor system was used to measure the local critical current of YBCO tape with high spatial resolution under in-situ tensile stress. The hot spot generation and minimum quench energy of YBCO tape, which depended on the local critical current, was calculated through the thermoelectric coupling model. With the increase in tensile stress, the cracks which have different dimensions and critical current degradation arose more frequently and lowered the thermal stability of the YBCO tape.

  7. Studies on electrochemical hydrodebromination mechanism of 2,5-dibromobenzoic acid on Ag electrode by in situ FTIR spectroscopy

    International Nuclear Information System (INIS)

    Li Meichao; Bao Dandan; Ma Chunan

    2011-01-01

    Research highlights: → Silver is a good catalyst for the hydrodebromination of 2,5-dibromobenzoic acid. → 3-Bromobenzoic acid as main intermediate product. → The finally product is benzoic acid. → In situ FTIR is useful to study the electrochemical hydrodebromination mechanism. - Abstract: Cyclic voltammetry and in situ FTIR were employed to study the electrochemical hydrodebromination (EHB) mechanism of 2,5-dibromobenzoic acid (2,5-DBBA) in NaOH solution. Compared with titanium and graphite electrodes, silver electrode exhibited a high electrocatalytic activity for the hydrodebromination reaction of 2,5-DBBA. On the basis of in situ FTIR data, EHB reaction of 2,5-DBBA on Ag cathode might be represented as a sequence of electron additions and bromine expulsions. Firstly, from potential at approximately -1100 mV, 2,5-DBBA received an electron to form 2,5-DBBA radical anion, which lost a bromine ion in the 2-position to form 3-bromobenzoic acid (3-BBA) free radical. Then the free radical received a proton to give 3-BBA. Finally, 3-BBA further took off another bromine ion to produce benzoic acid free radical and the end product benzoic acid was obtained by receiving another electron and a proton with the potential shifting to more negative values.

  8. In-situ Transmission Electron Microscopy and Spectroscopy Studies of Interfaces in Li-ion Batteries: Challenges and Opportunities

    International Nuclear Information System (INIS)

    Wang, Chong M.; Xu, Wu; Liu, Jun; Choi, Daiwon; Arey, Bruce W.; Saraf, Laxmikant V.; Zhang, Jiguang; Yang, Zhenguo; Thevuthasan, Suntharampillai; Baer, Donald R.; Salmon, Norman

    2010-01-01

    The critical challenge facing the lithium ion battery development is the basic understanding of the structural evolution during the cyclic operation of the battery and the consequence of the structural evolution on the properties of the battery. Although transmission electron microscopy (TEM) and spectroscopy have been evolved to a stage such that it can be routinely used to probe into both the structural and chemical composition of the materials with a spatial resolution of a single atomic column, a direct in-situ TEM observation of structural evolution of the materials in lithium ion battery during the dynamic operation of the battery has never been reported. This is related to three factors: high vacuum operation of a TEM; electron transparency requirement of the region to be observed, and the difficulties dealing with the liquid electrolyte of lithium ion battery. In this paper, we report the results of exploring the in-situ TEM techniques for observation of the interface in lithium ion battery during the operation of the battery. A miniature battery was fabricated using a nanowire and an ionic liquid electrolyte. The structure and chemical composition of the interface across the anode and the electrolyte was studied using TEM imaging, electron diffraction, and electron energy loss spectroscopy. In addition, we also explored the possibilities of carrying out in-situ TEM studies of lithium ion batteries with a solid state electrolyte.

  9. In situ scanning tunneling microscopy study of Ca-modified rutile TiO2(110 in bulk water

    Directory of Open Access Journals (Sweden)

    Giulia Serrano

    2015-02-01

    Full Text Available Despite the rising technological interest in the use of calcium-modified TiO2 surfaces in biomedical implants, the Ca/TiO2 interface has not been studied in an aqueous environment. This investigation is the first report on the use of in situ scanning tunneling microscopy (STM to study calcium-modified rutile TiO2(110 surfaces immersed in high purity water. The TiO2 surface was prepared under ultrahigh vacuum (UHV with repeated sputtering/annealing cycles. Low energy electron diffraction (LEED analysis shows a pattern typical for the surface segregation of calcium, which is present as an impurity on the TiO2 bulk. In situ STM images of the surface in bulk water exhibit one-dimensional rows of segregated calcium regularly aligned with the [001] crystal direction. The in situ-characterized morphology and structure of this Ca-modified TiO2 surface are discussed and compared with UHV-STM results from the literature. Prolonged immersion (two days in the liquid leads to degradation of the overlayer, resulting in a disordered surface. X-ray photoelectron spectroscopy, performed after immersion in water, confirms the presence of calcium.

  10. Grain Nucleation and Growth in Deformed NiTi Shape Memory Alloys: An In Situ TEM Study

    Science.gov (United States)

    Burow, J.; Frenzel, J.; Somsen, C.; Prokofiev, E.; Valiev, R.; Eggeler, G.

    2017-12-01

    The present study investigates the evolution of nanocrystalline (NC) and ultrafine-grained (UFG) microstructures in plastically deformed NiTi. Two deformed NiTi alloys were subjected to in situ annealing in a transmission electron microscope (TEM) at 400 and 550 °C: an amorphous material state produced by high-pressure torsion (HPT) and a mostly martensitic partly amorphous alloy produced by wire drawing. In situ annealing experiments were performed to characterize the microstructural evolution from the initial nonequilibrium states toward energetically more favorable microstructures. In general, the formation and evolution of nanocrystalline microstructures are governed by the nucleation of new grains and their subsequent growth. Austenite nuclei which form in HPT and wire-drawn microstructures have sizes close to 10 nm. Grain coarsening occurs in a sporadic, nonuniform manner and depends on the physical and chemical features of the local environment. The mobility of grain boundaries in NiTi is governed by the local interaction of each grain with its microstructural environment. Nanograin growth in thin TEM foils seems to follow similar kinetic laws to those in bulk microstructures. The present study demonstrates the strength of in situ TEM analysis and also highlights aspects which need to be considered when interpreting the results.

  11. The adhesion behavior of carbon coating studied by re-indentation during in situ TEM nanoindentation

    Energy Technology Data Exchange (ETDEWEB)

    Fan, Xue; Diao, Dongfeng, E-mail: dfdiao@szu.edu.cn

    2016-01-30

    Graphical abstract: Nanoscale adhesion induced response in terms of re-indentation was directly observed. During unloading (start from B), the re-indentation phenomenon with the displacement sudden drop and the external loading force change from tension (C) to compression (D) within 0.1 s was captured by in situ TEM nanoindentation. - Highlights: • In situ TEM nanoindentation was performed on carbon coating. • Adhesion induced nano-response of re-indentation was directly observed. • Adhesive forces were measured from the load–displacement curves. • Adhesion energies released for re-indentation were quantitatively analyzed. • Carbon coating reduced the impact of adhesion for silicon substrate. - Abstract: We report a nanoscale adhesion induced nano-response in terms of re-indentation during in situ transmission electron microscope (TEM) nanoindentation on the carbon coating with silicon substrate. The adhesive force generated with nanoindentation was measured, and re-indentation phenomenon during unloading with displacement sudden drop and external loading force change from tension to compression was found. The occurrence of re-indentation during unloading was ascribed to the adhesive force of the contact interface between the indenter and the coating surface. Adhesion energies released for re-indentation processes were quantitatively analyzed from the re-indentation load–displacement curves, and carbon coating reduced the impact of adhesion for silicon substrate. The adhesion induced nano-response of contact surfaces would affect the reliability and performance of nano devices.

  12. Capillary based Li-air batteries for in situ synchrotron X-ray powder diffraction studies

    DEFF Research Database (Denmark)

    Storm, Mie Møller; Johnsen, Rune E.; Younesi, Reza

    2015-01-01

    For Li-air batteries to reach their full potential as energy storage system, a complete understanding of the conditions and reactions in the battery during operation is needed. To follow the reactions in situ a capillary-based Li-O2 battery has been developed for synchrotron-based in situ X......-ray powder diffraction (XRPD). In this article, we present the results for the analysis of 1st and 2nd deep discharge and charge for a cathode being cycled between 2 and 4.6 V. The crystalline precipitation of Li2O2 only is observed in the capillary battery. However, there are indications of side reactions...... of constant exposure of X-ray radiation to the electrolyte and cathode during charge of the battery was also investigated. X-ray exposure during charge leads to changes in the development of the intensity and the FWHM of the Li2O2 diffraction peaks. The X-ray diffraction results are supported by ex situ X...

  13. In situ FT-IR spectroelectrochemical study of electrooxidation of pyridoxol on a gold electrode

    International Nuclear Information System (INIS)

    Wang Meiling; Zhang Youyu; Xie Qingji; Yao Shouzhuo

    2005-01-01

    The electrochemical oxidation of pyridoxol (PN) on a polycrystalline gold electrode was investigated by cyclic voltammetry and in situ Fourier transform infrared spectroscopy (FTIRS). In 0.1 M aqueous NaOH solution, the gold electrode showed a high catalytic activity for the irreversible oxidation process of PN. The individual ionic species and the major tautomeric equilibria of PN molecules in aqueous solutions were evidenced well from the pH-dependent attenuated total reflectance (ATR) spectra, and the results were in good agreement with the voltammetric observations. In situ single potential alteration infrared reflectance spectroscopy (SPAIRS) demonstrated that a lactone form of PN, rather than pyridoxal aldehyde, was likely formed, which was subsequently diffused into the thin layer solution and underwent hydrolysis slowly to pyridoxic acid (PA) as the final product. In addition, the adsorption of PN at Au electrode was characterized by in situ subtractively normalized interfacial Fourier transform infrared reflectance spectroscopy (SNIFTIRS) method, which revealed that the adsorption of deprotonated PN, via nitrogen atom in vertical configuration on electrode surface, occurred from -0.5 V versus Ag vertical bar AgCl vertical bar KCl(sat), which was much lower than the potential of PN electrooxidation observed from ca. 0 V

  14. Hydration of swelling clay and bacteria interaction. An experimental in situ reaction study

    International Nuclear Information System (INIS)

    Berger, J.

    2008-01-01

    This study reports on the physical-chemical behaviour of swelling di-octahedral clays (smectites) and their interaction with aqueous solutions and bacteria (Shewanella putrefaciens). Experimental results are presented for compacted clays, hydrated under confined volume conditions, using a new type of reaction-cell (the 'wet-cell' of Warr and Hoffman, 2004) that was designed for in situ X-ray diffraction (XRD) measurement. For comparison, dispersed clay systems were studied using standard batch solutions subjected to varying degrees of agitation. The combination of time-dependent in situ XRD measurements with gravimetric measurements and calculated diffraction patterns using the CALCMIX software (Plancon and Drits, 1999) allowed to successful quantification of the dynamics of water uptake and storage. This analytical procedure combined with published water vapour adsorption data enabled determination of the abundance of structured water layers, developed in the interlayer space, and the amount of water contained in different storage sites (interlayers, surfaces and pore spaces). Qualitative information on surface area and textural organization was also estimated based on calculated changes in the average particle thickness and the organization of water layer structures (ordering). Abiotic smectite hydration experiments, using a range of natural and industrial bentonites (SWy-2, IBECO, MX80, TIXOTON), focused on defining the role of the interlayer cation, variable clay packing densities and the ionic strength of the infiltrating solution. The rate of smectite hydration, as expected, was seen to be highly dependent on the type of interlayer cation (enhanced for Ca as opposed to Na) and the ionic strength of solution (enhanced uptake rates with saline solutions, particularly as they infiltrate Na-smectite). A range of dynamic changes in micro textural state occurred as a function of packing density. These changes explain the differences in hydration behaviour observed

  15. Spin injection into semiconductors: the role of Fe/AlxGa1-xAs interface

    International Nuclear Information System (INIS)

    Fitzsimmons, M.R.; Park, S.

    2004-01-01

    The influence of the growth and post-growth annealing temperatures of Fe/Al x Ga 1-x As-based spin light-emitting diodes (LEDs) on the spin injection efficiency is discussed. The extent of interfacial reactions during molecular beam epitaxial growth of Fe on GaAs was determined from in-situ x-ray photoelectron spectroscopy studies. The Fe/GaAs interface results in ≤ 3 monolayers of reaction for Fe grown at -15 C. Intermediate growth temperatures (95 C) lead to ∼5 monolayers of interfacial reactions, and high growth temperatures of 175 C lead to a ∼9 monolayer thick reacted layer. Polarized neutron reflectivity was used to determine the interfacial magnetic properties of epitaxial Fe 0.5 Co 0.5 /GaAs heterostructures grown under identical conditions. No interfacial magnetic dead layer is detected at the interface for Fe 0.5 Co 0.5 films grown at -15 C, an ∼6 (angstrom) thick nonmagnetic layer formed at the interface for 95 C growth and an ∼5 (angstrom) thick magnetic interfacial reacted layer formed for growth at 175 C. Spin injection from Fe contacts into spin LEDs decreases sharply when reactions result in a nonmagnetic interfacial layer. Significant spin injection signals are obtained from Fe contacts grown between -5 C and 175 C, although the higher Fe growth temperatures resulted in a change in the sign of the spin polarization. Post-growth annealing of the spin LEDs is found to increase spin injection efficiency for low Fe growth temperatures and to a sign reversal of the spin polarization for high growth temperature (175 C). An effective Schottky barrier height increase indicates that post growth annealing modifies the Fe/Al x Ga 1-x As interface.

  16. XAS studies of the effectiveness of iron chelating treatments of Mary Rose timbers

    International Nuclear Information System (INIS)

    Berko, A; Schofield, E J; Chadwick, A V; Smith, A D; Jones, A M; Mosselmans, J F W

    2009-01-01

    The oxidation of sulfur in marine archaeological timbers under museum storage conditions is a recently identified problem, particularly for major artefacts such as historic ships excavated from the seabed. Recent work on the Vasa has stressed the role of iron in catalysing the oxidative degradation of the wood cellulose and the polyethylene glycols used to restore mechanical integrity to the timbers. In developing new treatment protocols for the long term preservation of Henry VIII of England's flagship, the Mary Rose, we are investigating the potential of chelating agents to neutralise and remove the iron products from the ships timbers. We have explored the use of aqueous solutions of chelating agents of calcium phytate, ethylenediaminetetraacetic acid (EDTA), diethylenetriaminepentaacetic acid (DTPA) and ammonium citrate to extract the iron compounds. All of these solutions exhibit some level of iron removal; however the key is to find the most effective concentration at pH of around 7 of the reagent solution, to minimise the treatment time and find the most cost-effective treatment for the whole of the Mary Rose hull. Fe K-edge XAFS data from samples of Mary Rose timbers, before and after treatment by the chelating agents mentioned has been collected. The data collected provide valuable insights into the effectiveness of the treatment solutions.

  17. In Situ Apparatus to Study Gas-Metal Reactions and Wettability at High Temperatures for Hot-Dip Galvanizing Applications

    Science.gov (United States)

    Koltsov, A.; Cornu, M.-J.; Scheid, J.

    2018-02-01

    The understanding of gas-metal reactions and related surface wettability at high temperatures is often limited due to the lack of in situ surface characterization. Ex situ transfers at low temperature between annealing furnace, wettability device, and analytical tools induce noticeable changes of surface composition distinct from the reality of the phenomena.Therefore, a high temperature wettability device was designed in order to allow in situ sample surface characterization by x-rays photoelectron spectroscopy after gas/metal and liquid metal/solid metal surface reactions. Such airless characterization rules out any contamination and oxidation of surfaces and reveals their real composition after heat treatment and chemical reaction. The device consists of two connected reactors, respectively, dedicated to annealing treatments and wettability measurements. Heat treatments are performed in an infrared lamp furnace in a well-controlled atmosphere conditions designed to reproduce gas-metal reactions occurring during the industrial recrystallization annealing of steels. Wetting experiments are carried out in dispensed drop configuration with the precise control of the deposited droplets kinetic energies. The spreading of drops is followed by a high-speed CCD video camera at 500-2000 frames/s in order to reach information at very low contact time. First trials have started to simulate phenomena occurring during recrystallization annealing and hot-dip galvanizing on polished pure Fe and FeAl8 wt.% samples. The results demonstrate real surface chemistry of steel samples after annealing when they are put in contact with liquid zinc alloy bath during hot-dip galvanizing. The wetting results are compared to literature data and coupled with the characterization of interfacial layers by FEG-Auger. It is fair to conclude that the results show the real interest of such in situ experimental setup for interfacial chemistry studies.

  18. In situ synchrotron X-ray diffraction study on epitaxial-growth dynamics of III–V semiconductors

    Science.gov (United States)

    Takahasi, Masamitu

    2018-05-01

    The application of in situ synchrotron X-ray diffraction (XRD) to the molecular-beam epitaxial (MBE) growth of III–V semiconductors is overviewed along with backgrounds of the diffraction theory and instrumentation. X-rays are sensitive not only to the surface of growing films but also to buried interfacial structures because of their large penetration depth. Moreover, a spatial coherence length up to µm order makes X-rays widely applicable to the characterization of low-dimensional structures, such as quantum dots and wires. In situ XRD studies during growth were performed using an X-ray diffractometer, which was combined with an MBE chamber. X-ray reciprocal space mapping at a speed matching a typical growth rate was achieved using intense X-rays available from a synchrotron light source and an area detector. The importance of measuring the three-dimensional distribution of XRD intensity in a reciprocal space map is demonstrated for the MBE growth of two-, one-, and zero-dimensional structures. A large amount of information about the growth process of two-dimensional InGaAs/GaAs(001) epitaxial films has been provided by three-dimensional X-ray reciprocal mappings, including the anisotropic strain relaxation, the compositional inhomogeneity, and the evolution of surface and interfacial roughness. For one-dimensional GaAs nanowires grown in a Au-catalyzed vapor-liquid–solid mode, the relationship between the diameter of the nanowires and the formation of polytypes has been suggested on the basis of in situ XRD measurements. In situ three-dimensional X-ray reciprocal space mapping is also shown to be useful for determining the lateral and vertical sizes of self-assembled InAs/GaAs(001) quantum dots as well as their internal strain distributions during growth.

  19. Dynamics of electrochemical lithiation/delithiation of graphene-encapsulated silicon nanoparticles studied by in-situ TEM.

    Science.gov (United States)

    Luo, Langli; Wu, Jinsong; Luo, Jiayan; Huang, Jiaxing; Dravid, Vinayak P

    2014-01-24

    The incorporation of nanostructured carbon has been recently reported as an effective approach to improve the cycling stability when Si is used as high-capacity anodes for the next generation Li-ion battery. However, the mechanism of such notable improvement remains unclear. Herein, we report in-situ transmission electron microscopy (TEM) studies to directly observe the dynamic electrochemical lithiation/delithiation processes of crumpled graphene-encapsulated Si nanoparticles to understand their physical and chemical transformations. Unexpectedly, in the first lithiation process, crystalline Si nanoparticles undergo an isotropic to anisotropic transition, which is not observed in pure crystalline and amorphous Si nanoparticles. Such a surprising phenomenon arises from the uniformly distributed localized voltage around the Si nanoparticles due to the highly conductive graphene sheets. It is observed that the intimate contact between graphene and Si is maintained during volume expansion/contraction. Electrochemical sintering process where small Si nanoparticles react and merge together to form large agglomerates following spikes in localized electric current is another problem for batteries. In-situ TEM shows that graphene sheets help maintain the capacity even in the course of electrochemical sintering. Such in-situ TEM observations provide valuable phenomenological insights into electrochemical phenomena, which may help optimize the configuration for further improved performance.

  20. In situ X-ray diffraction study of the electrochemical reaction on lead electrodes in sulphate electrolytes

    International Nuclear Information System (INIS)

    Angerer, P.; Mann, R.; Gavrilovic, A.; Nauer, G.E.

    2009-01-01

    The anodic oxidation of pure lead in two acidic sulphate electrolytes with identical ionic strength (pH ∼ 0 and pH ∼ -0.1) was studied by in situ grazing incidence X-ray diffraction method (GIXD). Crystalline products such as lead sulphate (anglesite, PbSO 4 , orthorhombic), α- and β-lead dioxide (α-PbO 2 , orthorhombic, and β-PbO 2 , tetragonal), and tribasic lead sulphate hydrate with the stoichiometric composition 3PbO.PbSO 4 .H 2 O (triclinic) were detected at defined potentials. A method for the semi-quantitative determination of the thickness of the deposited layer from diffraction data is described. After the in situ measurement, the washed and dried working electrodes were additionally characterized ex situ by GIXD measurements at different angles of incidence. The phase litharge (lead oxide, t-PbO, tetragonal) and lead sulphate were observed at the surface of the lead substrate. The quantitative evaluation of the diffraction intensity of this measurement series enables the modelling of a qualitative depth profile of the layer generated during the electrochemical treatment. The anglesite phase is located in the uppermost layer, while the litharge phase was detected closer to the lead substrate

  1. In-situ leaching of Crownpoint, New Mexico, uranium ore: Part 7 - laboratory study of chemical agents for molybdenum restoration

    International Nuclear Information System (INIS)

    Strom, E.T.; Vogt, T.C.

    1985-01-01

    While in-situ leaching has significant advantages over conventional uranium recovery methods, one possible drawback to its use is the potential release of previously insoluble chemical species into the formation water. Before Mobil began a pilot test of in-situ uranium leaching at Crownpoint, New Mexico, extensive laboratory studies were undertaken to develop chemical methods for treating one possible contaminant, molybdenum (Mo). In-situ production of uranium entails oxidizing uranium from the insoluble +4 oxidation state to the soluble, readily complexed +6 state. However, this process also transforms insoluble Mo +4 compounds such as molybdenite or jordesite, MoS 2 , into the soluble T6 form, molybdate, Mo0 4 2- . New Mexico regulations restrict the amount of Mo permissible in formation waters after leaching to less than one ppm. Conceptually, Mo restoration after leaching can be dealt with in one of two ways. (1) The oxidizing environment can be left unchanged with something added to render the molybdate ion insoluble or (2) the environment can be changed to a reducing one, converting the Mo back to the less soluble +4 oxidation state

  2. Feasibility study of the in-situ combustion in shallow, thin, and multi-layered heavy oil reservoir

    Energy Technology Data Exchange (ETDEWEB)

    Zhong, L. [Society of Petroleum Engineers, Kuala Lumpur (Malaysia)]|[Daqing Petroleum Inst., Beijing (China); Yu, D. [Daqing Petroleum Inst., Beijing (China); Gong, Y. [China National Petroleum Corp., Beijing (China). Liaohe Oilfield; Wang, P.; Zhang, L. [China National Petroleum Corp., Beijing (China). Huabei Oilfield; Liu, C. [China National Petroleum Corp., Beijing (China). JiLin Oilfield

    2008-10-15

    In situ combustion is a process where oxygen is injected into oil reservoirs in order to oxidize the heavier components of crude oil. The oil is driven towards the production wells by the combustion gases and steam generated by the combustion processes. This paper investigated dry and wet forward in situ combustion processes designed for an oil reservoir with thin sand layers. Laboratory and numerical simulations were conducted to demonstrate the feasibility of the processes in a shallow, thin, heterogenous heavy oil reservoir in China. Combustion tube experiments were conducted in order to determine fuel consumption rates. A numerical geological model was constructed to represent the reservoir conditions. Gas, water, oil and solid phases were modelled. Four processes were considered: cracking; pyrolysis of heavy fractions; the combustion of light and heavy fractions; and the combustion of coke. Oil recovery rates were calculated for a period of 10 years. Reactor experiments were conducted to investigate igniting temperatures and air injection rates using an apparatus comprised of an electric heater, oil sand pack tube and a computerized control system. Experiments were performed at different temperature and injection rates. The experiments demonstrated that ignition times and air volumes decreased when air temperature was increased. Results of the study showed that a 20 per cent increase in oil recovery using the in situ combustion processes. It was concluded that adequate air injection rates are needed to ensure effective combustion front movement. 4 refs., 6 tabs., 4 figs.

  3. Support effects in catalysis studied by in-situ sum frequency generation vibrational spectroscopy and in-situ x-ray spectroscopies

    Energy Technology Data Exchange (ETDEWEB)

    Kennedy, Griffin John [Univ. of California, Berkeley, CA (United States)

    2017-04-14

    Here, kinetic measurements are paired with in-situ spectroscopic characterization tools to investigate colloidally based, supported Pt catalytic model systems in order to elucidate the mechanisms by which metal and support work in tandem to dictate activity and selectivity. The results demonstrate oxide support materials, while inactive in absence of Pt nanoparticles, possess unique active sites for the selective conversion of gas phase molecules when paired with an active metal catalyst.

  4. Applicability study of using in-situ gamma-ray spectrometry technique for 137Cs and 210Pbex inventories measurement in grassland environments

    International Nuclear Information System (INIS)

    Li Junjie; Li Yong; Wang Yanglin; Wu Jiansheng

    2010-01-01

    In-situ measurement of fallout radionuclides 137 Cs and 210 Pb ex has the potential to assess soil erosion and sedimentation rapidly. In this study, inventories of 137 Cs and 210 Pb ex in the soil of Inner Mongolia grassland were measured using an In-situ Object Counting System (ISOCS). The results from the field study indicate that in-situ gamma-ray spectrometry has the following advantages over traditional laboratory measurements: no extra time is required for sample collection, no reference inventories are required, more economic, prompt availability of the results, the ability to average radionuclide inventory over a large area, and high precision.

  5. Hydration of swelling clay and bacteria interaction. An experimental in situ reaction study; Hydratation des argiles gonflantes et influence des bacteries. Etude experimentale de reaction in situ

    Energy Technology Data Exchange (ETDEWEB)

    Berger, J

    2008-01-15

    This study reports on the physical-chemical behaviour of swelling di-octahedral clays (smectites) and their interaction with aqueous solutions and bacteria (Shewanella putrefaciens). Experimental results are presented for compacted clays, hydrated under confined volume conditions, using a new type of reaction-cell (the 'wet-cell' of Warr and Hoffman, 2004) that was designed for in situ X-ray diffraction (XRD) measurement. For comparison, dispersed clay systems were studied using standard batch solutions subjected to varying degrees of agitation. The combination of time-dependent in situ XRD measurements with gravimetric measurements and calculated diffraction patterns using the CALCMIX software (Plancon and Drits, 1999) allowed to successful quantification of the dynamics of water uptake and storage. This analytical procedure combined with published water vapour adsorption data enabled determination of the abundance of structured water layers, developed in the interlayer space, and the amount of water contained in different storage sites (interlayers, surfaces and pore spaces). Qualitative information on surface area and textural organization was also estimated based on calculated changes in the average particle thickness and the organization of water layer structures (ordering). Abiotic smectite hydration experiments, using a range of natural and industrial bentonites (SWy-2, IBECO, MX80, TIXOTON), focused on defining the role of the interlayer cation, variable clay packing densities and the ionic strength of the infiltrating solution. The rate of smectite hydration, as expected, was seen to be highly dependent on the type of interlayer cation (enhanced for Ca as opposed to Na) and the ionic strength of solution (enhanced uptake rates with saline solutions, particularly as they infiltrate Na-smectite). A range of dynamic changes in micro textural state occurred as a function of packing density. These changes explain the differences in hydration behaviour

  6. Phase diagram of a two-dimensional liquid in GaAs/AlxGa1-xAs biased double quantum wells

    DEFF Research Database (Denmark)

    Timofeev, V. B.; Larionov, A. V.; Alessi, M. G.

    2000-01-01

    Photoluminescence (PL) and PL excitation (PLE) measurements have been performed in GaAs/AlxGa1-xAs biased double quantum well heterostructures. The recombination of electrons, e, with holes, h, located in the same or in two adjacent wells, has been investigated for different exciting power...

  7. Electron microscopic and optical investigations of the indium distribution GaAs capped InxGa1-xAs islands

    DEFF Research Database (Denmark)

    Woggon, U.; Langbein, Wolfgang Werner; Hvam, Jørn Märcher

    1997-01-01

    Results from a structural and optical analysis of buried InxGa1-xAs islands carried out after the process of GaAs overgrowth are presented. It is found that during the growth process, the indium concentration profile changes and the thickness of the wetting layer emanating from a Stranski-Krastan...

  8. The time-resolved and extreme conditions XAS (TEXAS) facility at the European Synchrotron Radiation Facility: the general-purpose EXAFS bending-magnet beamline BM23

    Energy Technology Data Exchange (ETDEWEB)

    Mathon, O., E-mail: mathon@esrf.fr; Beteva, A.; Borrel, J.; Bugnazet, D.; Gatla, S.; Hino, R.; Kantor, I.; Mairs, T. [European Synchrotron Radiation Facility, CS 40220, 38043 Grenoble Cedex 9 (France); Munoz, M. [European Synchrotron Radiation Facility, CS 40220, 38043 Grenoble Cedex 9 (France); Université Joseph Fourier, 1381 rue de la Piscine, BP 53, 38041 Grenoble Cedex 9 (France); Pasternak, S.; Perrin, F.; Pascarelli, S. [European Synchrotron Radiation Facility, CS 40220, 38043 Grenoble Cedex 9 (France)

    2015-10-17

    BM23 is the general-purpose EXAFS bending-magnet beamline at the ESRF, replacing the former BM29 beamline in the framework of the ESRF upgrade. Its mission is to serve the whole XAS user community by providing access to a basic service in addition to the many specialized instruments available at the ESRF. BM23 offers high-signal-to-noise ratio EXAFS in a large energy range (5–75 keV), continuous energy scanning for quick-EXAFS on the second timescale and a micro-XAS station delivering a spot size of 4 µm × 4 µm FWHM. BM23 is the general-purpose EXAFS bending-magnet beamline at the ESRF, replacing the former BM29 beamline in the framework of the ESRF upgrade. Its mission is to serve the whole XAS user community by providing access to a basic service in addition to the many specialized instruments available at the ESRF. BM23 offers high signal-to-noise ratio EXAFS in a large energy range (5–75 keV), continuous energy scanning for quick-EXAFS on the second timescale and a micro-XAS station delivering a spot size of 4 µm × 4 µm FWHM. It is a user-friendly facility featuring a high degree of automation, online EXAFS data reduction and a flexible sample environment.

  9. An assessment of some theoretical models used for the calculation of the refractive index of InXGa1-xAs

    Science.gov (United States)

    Engelbrecht, J. A. A.

    2018-04-01

    Theoretical models used for the determination of the refractive index of InXGa1-XAs are reviewed and compared. Attention is drawn to some problems experienced with some of the models. Models also extended to the mid-infrared region of the electromagnetic spectrum. Theoretical results in the mid-infrared region are then compared to previously published experimental results.

  10. Optimization of the confinement energy of quantum-wire states in T-shaped GaAs/AlxGa1-xAs structures

    DEFF Research Database (Denmark)

    Langbein, Wolfgang Werner; Gislason, Hannes; Hvam, Jørn Märcher

    1996-01-01

    We report on an optimization of the wire confinement energies of the confined electronic states at the T-shaped intersection of GaAs and AlxGa1-xAs quantum wells. These structures can be produced by the cleaved edge overgrowth technique. We present an analytical model for the confinement to give ...

  11. In-situ irradiation of cerium precursors in TEM to study nanocrystal formation

    Science.gov (United States)

    Asghar, Muhammad Sajid Ali; Sabri, Mohammed Mohammed; Tian, Zijian; Möbus, Günter

    2017-09-01

    Three of the most commonly used precursor chemicals for wet-chemical nano-ceria synthesis are examined by means of direct dry electron irradiation in TEM. Transformation reactions of micron-size carbonate, chloride, and nitrate grains into nanocrystallites (internal or external) are recorded in situ. Progress of possible redox-changes of cerium is tracked by EELS. We find a straight local oxidation reaction for carbonates, but external nanorod formation by condensation in the case of chlorides, while nitrates show a multi-stage complex redox behaviour.

  12. In-situ neutron diffraction study of Zircaloy 4 subjected to biaxial tension

    Energy Technology Data Exchange (ETDEWEB)

    Gharghouri, M.A. [Canadian Neutron Beam Centre, Chalk River Laboratories, Chalk River, ON (Canada); McDonald, D.; Xiao, L. [Atomic Energy of Canada Limited, Chalk River, ON (Canada)

    2014-07-01

    Zircaloy-4 is widely used as fuel element cladding in nuclear reactors. Pellet-clad interaction (PCI) failure is a concern for many water reactor fuel designs. Extensive work on the mechanism of PCI failure has led to the conclusion that stress corrosion cracking (SCC) induced by iodine vapour in the temperature range relevant to fuel operation is the most probable cause of PCI failure in zirconium alloy fuel element cladding. In-situ neutron diffraction measurements performed on tubular Zircaloy-4 specimens simultaneously pulled in tension and pressurized internally will provide information on the effects of stress biaxiality on the distribution of stresses at the crystal level during loading. (author)

  13. In situ SAXS study on cationic and non-ionic surfactant liquid crystals using synchrotron radiation.

    Science.gov (United States)

    Fritscher, C; Hüsing, N; Bernstorff, S; Brandhuber, D; Koch, T; Seidler, S; Lichtenegger, H C

    2005-11-01

    In situ synchrotron small-angle X-ray scattering was used to investigate various surfactant/water systems with hexagonal and lamellar structures regarding their structural behaviour upon heating and cooling. Measurements of the non-ionic surfactant Triton X-45 (polyethylene glycol 4-tert-octylphenyl ether) at different surfactant concentrations show an alignment of the lamellar liquid-crystalline structure close to the wall of the glass capillaries and also a decrease in d-spacing following subsequent heating/cooling cycles. Additionally, samples were subjected to a weak magnetic field (0.3-0.7 T) during heating and cooling, but no influence of the magnetic field was observed.

  14. Stability of Porous Platinum Nanoparticles: Combined In Situ TEM and Theoretical Study

    DEFF Research Database (Denmark)

    Chang, Shery L. Y.; Barnard, Amanda S.; Dwyer, Christian

    2012-01-01

    Porous platinum nanoparticles provide a route for the development of catalysts that use less platinum without sacrificing catalytic performance. Here, we examine porous platinum nanoparticles using a combination of in situ transmission electron microscopy and calculations based on a first-principles......-parametrized thermodynamic model. Our experimental observations show that the initially irregular morphologies of the as-sythesized porous nanoparticles undergo changes at high temperatures to morphologies having faceted external surfaces with voids present in the interior of the particles. The increasing size of stable...

  15. In situ EPR studies of reaction pathways in Titania photocatalyst-promoted alkylation of alkenes.

    Science.gov (United States)

    Rhydderch, Shona; Howe, Russell F

    2015-03-03

    In situ EPR spectroscopy at cryogenic temperatures has been used to observe and identify paramagnetic species produced when titania is irradiated in the presence of reactants used in the photocatalytic alkylation of maleimide with t-butyl carboxylic acid or phenoxyacetic acid. It is shown that maleimide acts as an acceptor of conduction band electrons. Valence band holes oxidise t-butyl carboxylic acid to the t-butyl radical and phenoxyacetic acid to the phenoxyacetic acid radical cation. In the presence of maleimide, the phenoxymethyl radical is formed from phenoxyacetic acid. The relevance of these observations to the mechanisms of titania photocatalyst-promoted alkylation of alkenes is discussed.

  16. Network of Nano-Landers for In-Situ Characterization of Asteroid Impact Studies

    OpenAIRE

    Kalita, Himangshu; Asphaug, Erik; Schwartz, Stephen; Thangavelautham, Jekanthan

    2017-01-01

    Exploration of asteroids and comets can give insight into the origins of the solar system and can be instrumental in planetary defence and in-situ resource utilization (ISRU). Asteroids, due to their low gravity are a challenging target for surface exploration. Current missions envision performing touch-and-go operations over an asteroid surface. In this work, we analyse the feasibility of sending scores of nano-landers, each 1 kg in mass and volume of 1U, or 1000 cm3. These landers would hop...

  17. In situ TEM study on elastic interaction between a prismatic loop and a gliding dislocation

    International Nuclear Information System (INIS)

    Matsukawa, Yoshitaka; Liu, Grace S.

    2012-01-01

    In situ straining in a transmission electron microscope was performed in order to investigate dislocation interactions with a prismatic loop, which as a mobile obstacle is expected to be displaced by the strain-field of dislocation prior to physical contact. It was found that when a gliding dislocation approached a critical distance, the prismatic loop was certainly attracted to the dislocation. The captured loop disrupted the dislocation motion and was not dragged along with the mobile dislocation. Instead, the dislocation bypassed the loop via cross-slip to another slip plane with a resolved shear stress estimated to be 40% lower than that of the original plane.

  18. In situ TEM study of deformation twinning in Ni-Mn-Ga non-modulated martensite

    Czech Academy of Sciences Publication Activity Database

    Zárubová, Niva; Ge, Y.; Heczko, Oleg; Hannula, S.-P.

    2013-01-01

    Roč. 61, č. 14 (2013), s. 5290-5299 ISSN 1359-6454 R&D Projects: GA ČR(CZ) GAP107/11/0391; GA MŠk(CZ) LM2011026; GA ČR GAP107/12/0800; GA AV ČR IAA100100920 Institutional support: RVO:68378271 Keywords : Ni-Mn-Ga * in situ TEM * magnetic shape memory * deformation twinning * twinning dislocation Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 3.940, year: 2013

  19. Experimental methods for in situ studies of morphology development during flow

    DEFF Research Database (Denmark)

    Lyngaae-Jørgensen, Jørgen

    1996-01-01

    A short overview of in situ methods is given. Multiple laminates of thin films is believed to represent unstable transition structures in many processing operations. A hypotesis for the break up is that first thin cylinders are formed . At a later stage these cylinders break up to spheres...... breakup mechanism involving creation of parallel layers of thin, filmlike formations parallel with the original film is observed. These layers then break up to a final state encompasing nearly spherical drops spread over a thickness much larger (by orders of magnitude) than the original film thickness....

  20. Photorefractive keratectomy versus laser in situ keratomileusis for moderate to high myopia. A randomized prospective study.

    Science.gov (United States)

    Hersh, P S; Brint, S F; Maloney, R K; Durrie, D S; Gordon, M; Michelson, M A; Thompson, V M; Berkeley, R B; Schein, O D; Steinert, R F

    1998-08-01

    This report presents the results of a randomized clinical trial of photorefractive keratectomy (PRK) and laser-assisted in situ keratomileusis (LASIK). A randomized, prospective multicenter clinical trial. A total of 220 eyes of 220 patients entered the study cohort: 105 randomized to PRK and 115 to LASIK. The mean preoperative manifest refraction spherical equivalent was -9.23 diopters (D) in the PRK group and -9.30 D in the LASIK group. All patients received a one-pass, multizone excimer laser ablation as part of either a PRK or LASIK procedure using the Summit Apex excimer laser. Attempted corrections ranged from 6.00 to 15.00 D. Data on uncorrected and spectacle-corrected visual acuity, predictability,and stability of refraction, corneal haze, and flap complications were analyzed. Patients were observed for up to 6 months. One day after surgery, 0 (0.0%) and 3 (4.5%) eyes in the PRK group saw 20/20 and 20/40 or better uncorrected, respectively, while 7 (10%) and 48 (68.6%) eyes in the LASIK group saw 20/20 and 20/40 or better, respectively. At 6 months after PRK, 13 (19.1%) and 45 (66.2%) eyes saw 20/20 and 20/40 or better, respectively, while after LASIK, 16 (26.2%) and 34 (55.7%) eyes saw 20/20 and 20/40 or better, respectively (odds ratio = 0.56 for likelihood of uncorrected visual acuity PRK vs. LASIK, 95% confidence interval [CI] = 0.31-1.19). After PRK, 39 eyes (57.4%) were within 1.0 D of attempted correction compared with 24 eyes (40.7%) in the LASIK group (odds ratio = 0.50 for likelihood fo undercorrection 1.0 D for PRK vs. LASIK, 95% CI = 0.24-1.04); however, the standard deviation of the predictability was similar between groups: 1.01 D for PRK and 1.22 D for LASIK. From months 1 to 6, there was an average regression of 0.89 D in the PRK group and 0.55 D in the LASIK group. After PRK, eight eyes (11.8%) had a decrease in spectacle-corrected visual acuity of two Snellen lines or more; after LASIK, two eyes (3.2%) had a decrease of two lines or more

  1. In situ chemical fixation of arsenic-contaminated soils: Anexperimental study

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Li; Donahoe, Rona J.; Redwine, James C.

    2007-03-27

    This paper reports the results of an experimentalstudytesting a low-cost in situ chemical fixation method designed to reclaimarsenic-contaminated subsurface soils. Subsurface soils from severalindustrial sites in southeastern U.S. were contaminated with arsenicthrough heavy application of herbicide containing arsenic trioxide. Themean concentrations of environmentally available arsenic in soilscollected from the two study sites, FW and BH, are 325 mg/kg and 900mg/kg, respectively. The soils are sandy loams with varying mineralogicaland organic contents. The previous study [Yang L, Donahoe RJ. The form,distribution and mobility of arsenic in soils contaminated by arsenictrioxide, at sites in Southeast USA. Appl Geochem 2007;22:320 341]indicated that a large portion of the arsenic in both soils is associatedwith amorphous aluminum and iron oxyhydroxides and shows very slowrelease against leaching by synthetic precipitation. The soil's amorphousaluminum and iron oxyhydroxides content was found to have the mostsignificant effect on its ability to retain arsenic.Based on thisobservation, contaminated soils were reacted with different treatmentsolutions in an effort to promote the formation of insolublearsenic-bearing phases and thereby decrease the leachability of arsenic.Ferrous sulfate, potassium permanganate and calcium carbonate were usedas the reagents for the chemical fixation solutions evaluated in threesets of batch experiments: (1) FeSO4; (2) FeSO4 and KMnO4; (3) FeSO4,KMnO4 and CaCO3. The optimum treatment solutions for each soil wereidentified based on the mobility of arsenic during sequential leaching oftreated and untreated soils using the fluids described in EPA Method 1311[USEPA. Method 1311: toxicity characteristic leaching procedure. Testmethods for evaluating solid waste, physical/chemical methods. 3rd ed.Washington, DC: U.S. Environmental Protection Agency, Office of SolidWaste. U.S. Government Printing Office; 1992]toxic characteristicsleaching

  2. A study of computational dosimetry and boron biodistribution for ex – situ lung BNCT at RA-3 Reactor

    International Nuclear Information System (INIS)

    Garabalino, M.A.; Trivillin, V. A.; Monti Hughes, A.; Pozzi, E.C.C.; Thorp, S.; Curotto, P; Miller, M.; Santa Cruz, G.A.; Saint Martin, G.; Schwint, A.E.; González, S.J.; Farías, R.O; Portu, A.; Ferraris, S.; Santa María, J.; Lange, F.; Bortolussi, S.; Altieri, S.

    2013-01-01

    Within the context of the preclinical ex-situ BNCT Project for the treatment of diffuse lung metastases, we performed boron biodistribution studies in a sheep model and computational dosimetry studies in human lung to evaluate the potential therapeutic efficacy of the proposed technique. Herein we report preliminary data that supports the use of the sheep model as an adequate human surrogate in terms of boron kinetics and uptake in clinically relevant tissues. Furthermore, the estimation of the potential therapeutic efficacy of the proposed treatment in humans, based on boron uptake values in the large animal model, yields promising tumor control probability values even in the most conservative scenario considered. (author)

  3. Prediction of CP and starch concentrations in ruminal in situ studies and ruminal degradation of cereal grains using NIRS.

    Science.gov (United States)

    Krieg, J; Koenzen, E; Seifried, N; Steingass, H; Schenkel, H; Rodehutscord, M

    2018-03-01

    Ruminal in situ incubations are widely used to assess the nutritional value of feedstuffs for ruminants. In in situ methods, feed samples are ruminally incubated in indigestible bags over a predefined timespan and the disappearance of nutrients from the bags is recorded. To describe the degradation of specific nutrients, information on the concentration of feed samples and undegraded feed after in situ incubation ('bag residues') is needed. For cereal and pea grains, CP and starch (ST) analyses are of interest. The numerous analyses of residues following ruminal incubation contribute greatly to the substantial investments in labour and money, and faster methods would be beneficial. Therefore, calibrations were developed to estimate CP and ST concentrations in grains and bag residues following in situ incubations by using their near-infrared spectra recorded from 680 to 2500 nm. The samples comprised rye, triticale, barley, wheat, and maize grains (20 genotypes each), and 15 durum wheat and 13 pea grains. In addition, residues after ruminal incubation were included (at least from four samples per species for various incubation times). To establish CP and ST calibrations, 620 and 610 samples (grains and bag residues after incubation, respectively) were chemically analysed for their CP and ST concentration. Calibrations using wavelengths from 1250 to 2450 nm and the first derivative of the spectra produced the best results (R 2 Validation=0.99 for CP and ST; standard error of prediction=0.47 and 2.10% DM for CP and ST, respectively). Hence, CP and ST concentration in cereal grains and peas and their bag residues could be predicted with high precision by NIRS for use in in situ studies. No differences were found between the effective ruminal degradation calculated from NIRS estimations and those calculated from chemical analyses (P>0.70). Calibrations were also calculated to predict ruminal degradation kinetics of cereal grains from the spectra of ground grains

  4. Experimental study and numerical modelling of geochemical reactions occurring during uranium in situ recovery (ISR) mining

    International Nuclear Information System (INIS)

    Ben Simon, R.

    2011-09-01

    The in situ Recovery (ISR) method consists of ore mining by in situ chemical leaching with acid or alkaline solutions. ISR takes place underground and is therefore limited to the analysis of the pumped solutions, hence ISR mine management is still empirical. Numerical modelling has been considered to achieve more efficient management of this process. Three different phenomena have to be taken into account for numerical simulations of uranium ISR mining: (1) geochemical reactions; (2) the kinetics of these reactions, and (3) hydrodynamic transport with respect to the reaction kinetics. Leaching tests have been conducted on ore samples from an uranium mine in Tortkuduk (Kazakhstan) where ISR is conducted by acid leaching. Two types of leaching experiments were performed: (1) tests in batch reactors; and (2) extraction in flow through columns. The assumptions deduced from the leaching tests were tested and validated by modelling the laboratory experiments with the numerical codes CHESS and HYTEC, both developed at the Geosciences research center of Mines ParisTech. A well-constrained 1D hydrogeochemical transport model of the ISR process at laboratory-scale was proposed. It enables to translate the chemical release sequence that is observed during experiments into a geochemical reaction sequence. It was possible to highlight the controlling factors of uranium dissolution, and the precipitation of secondary mineral phase in the deposit, as well as the determination of the relative importance of these factors. (author)

  5. Studies in earth sciences using in-situ produced cosmogenic radioisotopes

    International Nuclear Information System (INIS)

    Fink, D.

    1998-01-01

    The geological processes of glaciation and surface weathering which have moulded and continue to shape our landscape, are inextricably related to the dynamics of climate change. Earth Scientists have long sought an analytical technique based on radiometric methods that would quantify both temporally and spatially, the chronology of glacial cycles and erosion rates. Such a technique is now developing based on the in-situ production by cosmic rays of the long-lived cosmogenic radionuclides 10 Be (T 1 / 2 =1.5 Ma), 26 Al (0.7 Ma) and 36 Cl (0.3a) in exposed rocks, surfaces and within the first meter or so of the Earth's crust. Although only a million atoms of 10 Be are produced during a 100 ka exposure period per gram of rock, AMS can be applied to measure this telltale signal. Their build-up over time can be utilised as radiometric clocks to elucidate the exposure history of geomorphic formations and surfaces. Alternatively, if exposure has been sufficiently long for the in-situ signal to reach equilibrium, an average erosion rate can be determined. The applicability of the technique depends on the radioisotope half-life - in simple terms it works best over exposure periods of 5ka to 5 Ma (for 10 Be) and can identify erosion rates from 0.1 to 10 mm/ka

  6. In situ hybridization studies of hepatitis A viral RNA in patients with acute hepatitis A

    Energy Technology Data Exchange (ETDEWEB)

    Taylor, M; Goldin, R D; Ladva, S [Department of Histopathology, St. Mary' s Hospital Medical School, Imperial College of Science, Technology and Medicine, London (United Kingdom); Scheuer, P J [Department of Histopathology, Royal Free Hospital and School of Medicine, London (United Kingdom); Thomas, H C [Department of Medicine, St. Mary' s Hospital Medical School, Imperial College of Science, Technology and Medicine, London (United Kingdom)

    1994-01-01

    In situ hybridization with oligonucleotide probes has been used to localise hepatitis A virus RNA genomic sequences in formalin-fixed and routinely processed human liver biopsies from three patients. Using radiolabelled Sulphur-35 antisense probes, viral genomic sequences were found in all three cases, but signal intensity was greatest in cases 1 and 2 with fulminant hepatitis, and was minimal in the third case of resolving hepatitis biopsied 2 months after acute illness. Localisation showed the viral RNA to be present in hepatocytes, sinusoidal cells and inflammatory cells in and around the portal tracts. Both cases showed signal in similar cell types, but the distribution of staining was predominantly periportal in case 1, whereas lobular staining was more apparent in case 2. Hybridization with sense polarity probes failed to detect any evidence of replicative intermediates of antigenomic viral RNA. The presence of hepatitis A RNA in phagocytic cells was confirmed using immunohistochemistryfor a macrophage marker, CD68, combined with in situ hybridization. In all cases the signal was predominantly cytoplasmic, and this was confirmed with the use of tritiated probes. (au).

  7. In situ hybridization studies of hepatitis A viral RNA in patients with acute hepatitis A

    International Nuclear Information System (INIS)

    Taylor, M.; Goldin, R.D.; Ladva, S.; Scheuer, P.J.; Thomas, H.C.

    1994-01-01

    In situ hybridization with oligonucleotide probes has been used to localise hepatitis A virus RNA genomic sequences in formalin-fixed and routinely processed human liver biopsies from three patients. Using radiolabelled Sulphur-35 antisense probes, viral genomic sequences were found in all three cases, but signal intensity was greatest in cases 1 and 2 with fulminant hepatitis, and was minimal in the third case of resolving hepatitis biopsied 2 months after acute illness. Localisation showed the viral RNA to be present in hepatocytes, sinusoidal cells and inflammatory cells in and around the portal tracts. Both cases showed signal in similar cell types, but the distribution of staining was predominantly periportal in case 1, whereas lobular staining was more apparent in case 2. Hybridization with sense polarity probes failed to detect any evidence of replicative intermediates of antigenomic viral RNA. The presence of hepatitis A RNA in phagocytic cells was confirmed using immunohistochemistryfor a macrophage marker, CD68, combined with in situ hybridization. In all cases the signal was predominantly cytoplasmic, and this was confirmed with the use of tritiated probes. (au)

  8. Silver in geological fluids from in situ X-ray absorption spectroscopy and first-principles molecular dynamics

    Science.gov (United States)

    Pokrovski, Gleb S.; Roux, Jacques; Ferlat, Guillaume; Jonchiere, Romain; Seitsonen, Ari P.; Vuilleumier, Rodolphe; Hazemann, Jean-Louis

    2013-04-01

    The molecular structure and stability of species formed by silver in aqueous saline solutions typical of hydrothermal settings were quantified using in situ X-ray absorption spectroscopy (XAS) measurements, quantum-chemical modeling of near-edge absorption spectra (XANES) and extended fine structure spectra (EXAFS), and first-principles molecular dynamics (FPMD). Results show that in nitrate-bearing acidic solutions to at least 200 °C, silver speciation is dominated by the hydrated Ag+ cation surrounded by 4-6 water molecules in its nearest coordination shell with mean Ag-O distances of 2.32 ± 0.02 Å. In NaCl-bearing acidic aqueous solutions of total Cl concentration from 0.7 to 5.9 mol/kg H2O (m) at temperatures from 200 to 450 °C and pressures to 750 bar, the dominant species are the di-chloride complex AgCl2- with Ag-Cl distances of 2.40 ± 0.02 Å and Cl-Ag-Cl angle of 160 ± 10°, and the tri-chloride complex AgCl32- of a triangular structure and mean Ag-Cl distances of 2.60 ± 0.05 Å. With increasing temperature, the contribution of the tri-chloride species decreases from ˜50% of total dissolved Ag in the most concentrated solution (5.9m Cl) at 200 °C to less than 10-20% at supercritical temperatures for all investigated solutions, so that AgCl2- becomes by far the dominant Ag-bearing species at conditions typical of hydrothermal-magmatic fluids. Both di- and tri-chloride species exhibit outer-sphere interactions with the solvent as shown by the detection, using FPMD modeling, of H2O, Cl-, and Na+ at distances of 3-4 Å from the silver atom. The species fractions derived from XAS and FPMD analyses, and total AgCl(s) solubilities, measured in situ in this work from the absorption edge height of XAS spectra, are in accord with thermodynamic predictions using the stability constants of AgCl2- and AgCl32- from Akinfiev and Zotov (2001) and Zotov et al. (1995), respectively, which are based on extensive previous AgCl(s) solubility measurements. These data

  9. Mutual alloying of XAs (X=Ga, In, Al) materials: Tuning the optoelectronic and thermodynamic properties for solar energy applications

    KAUST Repository

    Haq, Bakhtiar Ul

    2014-02-01

    In the present work we did mutual alloying of the versatile XAs (X=Ga, In, Al) materials in order to improve their efficiency and enhance their range of technological applications using state of the art first principles method. We investigate the structural, electronic and thermodynamic properties of Ga1-xAlxAs, Ga1-xInxAs and In1-xAlxAs for x=0.25, 0.50, and 0.75. Calculations have been performed using the density functional theory (DFT) as implemented within the full potential linearized augmented plane wave plus local orbital (FP-LAPW+lo) method. For exchange and correlation energy treatment, we employed the local density approximations (LDA) as proposed by Wang and Perdew and the generalized gradient approximation (GGA) from Perdew et al. proposed. To calculate the accurate band structure, recently modified Becke Johnson (mBJ) potential was suggested as an alternative. Our calculations show a linear fall in the lattice constant in contrast to linear rise in bulk moduli of Ga1-xAlxAs and In1-xAlxAs with the increase of Al concentration. However the change of indium concentration in Ga1-xInxAs is displaying a reverse effect. The energy band gap of Ga1-xAlxAs and In1-xAlxAs was found to be increased, where a crossover from direct to indirect band gap has been observed with the increase of Al concentration. This direct to indirect crossover was found at 93.4% of Al concentration for Ga1-xAlxAs and at 84.63% of Al concentration for In1-xAlxAs. The effect of the mutual alloying of XAs materials on the thermodynamic properties is comprehensively reported. © 2013 Elsevier Ltd.

  10. Mutual alloying of XAs (X=Ga, In, Al) materials: Tuning the optoelectronic and thermodynamic properties for solar energy applications

    KAUST Repository

    Haq, Bakhtiar Ul; Ahmed, Rashid; El Haj Hassan, Fouad; Khenata, Rabah; Kasmin, Mohd Khalid; Goumri-Said, Souraya

    2014-01-01

    In the present work we did mutual alloying of the versatile XAs (X=Ga, In, Al) materials in order to improve their efficiency and enhance their range of technological applications using state of the art first principles method. We investigate the structural, electronic and thermodynamic properties of Ga1-xAlxAs, Ga1-xInxAs and In1-xAlxAs for x=0.25, 0.50, and 0.75. Calculations have been performed using the density functional theory (DFT) as implemented within the full potential linearized augmented plane wave plus local orbital (FP-LAPW+lo) method. For exchange and correlation energy treatment, we employed the local density approximations (LDA) as proposed by Wang and Perdew and the generalized gradient approximation (GGA) from Perdew et al. proposed. To calculate the accurate band structure, recently modified Becke Johnson (mBJ) potential was suggested as an alternative. Our calculations show a linear fall in the lattice constant in contrast to linear rise in bulk moduli of Ga1-xAlxAs and In1-xAlxAs with the increase of Al concentration. However the change of indium concentration in Ga1-xInxAs is displaying a reverse effect. The energy band gap of Ga1-xAlxAs and In1-xAlxAs was found to be increased, where a crossover from direct to indirect band gap has been observed with the increase of Al concentration. This direct to indirect crossover was found at 93.4% of Al concentration for Ga1-xAlxAs and at 84.63% of Al concentration for In1-xAlxAs. The effect of the mutual alloying of XAs materials on the thermodynamic properties is comprehensively reported. © 2013 Elsevier Ltd.

  11. Flow-induced corrosion of absorbable magnesium alloy: In-situ and real-time electrochemical study.

    Science.gov (United States)

    Wang, Juan; Jang, Yongseok; Wan, Guojiang; Giridharan, Venkataraman; Song, Guang-Ling; Xu, Zhigang; Koo, Youngmi; Qi, Pengkai; Sankar, Jagannathan; Huang, Nan; Yun, Yeoheung

    2016-03-01

    An in-situ and real-time electrochemical study in a vascular bioreactor was designed to analyze corrosion mechanism of magnesium alloy (MgZnCa) under mimetic hydrodynamic conditions. Effect of hydrodynamics on corrosion kinetics, types, rates and products was analyzed. Flow-induced shear stress (FISS) accelerated mass and electron transfer, leading to an increase in uniform and localized corrosions. FISS increased the thickness of uniform corrosion layer, but filiform corrosion decreased this layer resistance at high FISS conditions. FISS also increased the removal rate of localized corrosion products. Impedance-estimated and linear polarization-measured polarization resistances provided a consistent correlation to corrosion rate calculated by computed tomography.

  12. Study of the morphology exhibited by exfoliated polyurethane/montmorillonite nano composites during in situ recovery tests

    Energy Technology Data Exchange (ETDEWEB)

    Pereira, Iaci M., E-mail: iaci@ctex.eb.br [Divisao Belica do Centro Tecnologico do Exercito. CTEx, Rio de Janeiro, RJ (Brazil); Orefice, Rodrigo L. [Universidade Federal de Minas Gerais Departamento de Metalurgia e Materiais. UFMG, Belo Horizonte, MG (Brazil)

    2011-07-01

    By using small-angle X-ray scattering, this study aims to examine the SM behavior of montmorillonite polyurethane nano composites. To investigate the phase morphology, a deformed specimen was placed on a heating stage mounted at the Synchrotron beamline; the shape recovery was measured during 15 min. As temperature increases, the crystalline fraction rapidly decreases. The degree of clay delamination within the matrix increases, disturbing the formation of hard and soft segments. Deformation induces changes in the phase proportion, increasing the disperse phase contribution. During in situ tests, the ratio between matrix and disperse phase reaches an equilibrium controlled by the temperature. (author)

  13. A Rotational and Axial Motion System Load Frame Insert for In Situ High Energy X-Ray Studies (Postprint)

    Science.gov (United States)

    2015-09-08

    Paul A. Shade, Jay C. Schuren, and Todd J. Turner AFRL/RX Basil Blank PulseRay Peter Kenesei, Kurt Goetze, Ulrich Lienert, and Jonathan Almer...AFRL/RX 2) Basil Blank – PulseRay (continued on page 2) 5d. PROJECT NUMBER 4349 5e. TASK NUMBER 0001 5f...2015) A rotational and axial motion system load frame insert for in situ high energy x-ray studies Paul A. Shade,1,a) Basil Blank,2 Jay C. Schuren,1,b

  14. Neutron reflectivity as method to study in-situ adsorption of phospholipid layers to solid-liquid interfaces

    DEFF Research Database (Denmark)

    Gutberlet, Thomas; Klösgen, Beate Maria; Krastev, Rumen

    2004-01-01

    variation. It was observed that the method was capable of visualizing the adsorption of phospholipid layers to different solid-liquid interfaces and to resolve structural details at Angstroem resolution. The results depended strongly on a sufficiently good signal-to-noise ratio of the specific measurements......The use of neutron reflectivity as a method to study in-situ adsorption of phospholipid layers to solid-liquid interfaces was analyzed. The most important advantage of neutron reflectometry is the possibility to very the refractive index of the specific sample by isotope exchange, called contrast...

  15. Comparative study of in situ methods for potential and actual evapotranspiration determination and their calculation by simulation model

    International Nuclear Information System (INIS)

    Kolev, B.

    2006-01-01

    Four in situ methods for potential and actual evapotranspiration determining were compared: neutron gauge, tensiometers, gypsum blocks and lysimeters. The actual and potential evapotranspiration were calculated by water balance equation and by using a simulation model for their determination. The aim of this study was mainly pointed on calculations of water use efficiency and transpiration coefficient in potential production situation. This makes possible to choose the best way for water consumption optimization for a given crop. The final results find with the best of the methods could be used for applying the principles of sustainable agricultural production in random object of Bulgarian agricultural area

  16. Study in situ of the natural uranium, 60 Co and 137 Cs bioaccumulation factor in fish (Cyprinus carpio)

    International Nuclear Information System (INIS)

    Todoran, A.; Toma, A.; Dulama, C.; Horhoianu, V.; Hirica, O.; Patriche, N.; Tenciu, M.; Talpes, M.; Cristea, V.

    2006-01-01

    The paper presents the results of the 'in situ' research, aiming to determine the bioaccumulation factor of natural uranium, 60 Co and 137 Cs in fish (Cyprinus carpio) - the find link in aquatic ecosystems. The work performed is a part of a radioecological study achieved in the experimental pool of S.C.N. Pitesti. The objective of the research was to evaluate the release of the radioactive materials in the environment as well as to establish the transfer mechanisms of the radionuclides in the trophic chains from the aquatic ecosystem. (authors)

  17. Study in situ of the natural uranium, 60 Co and 137 Cs bioaccumulation factor in fish (Cyprinus carpio)

    Energy Technology Data Exchange (ETDEWEB)

    Todoran, A.; Toma, A.; Dulama, C.; Horhoianu, V.; Hirica, O. [Institute for Nuclear Research, Pitesti (Romania); Patriche, N.; Tenciu, M.; Talpes, M. [CPPPPIP, Galati (Romania); Cristea, V. [Galati Univ. (Romania)

    2006-07-01

    The paper presents the results of the 'in situ' research, aiming to determine the bioaccumulation factor of natural uranium, {sup 60}Co and {sup 137}Cs in fish (Cyprinus carpio) - the find link in aquatic ecosystems. The work performed is a part of a radioecological study achieved in the experimental pool of S.C.N. Pitesti. The objective of the research was to evaluate the release of the radioactive materials in the environment as well as to establish the transfer mechanisms of the radionuclides in the trophic chains from the aquatic ecosystem. (authors)

  18. Association of Serpulina hyodysenteriae with the colonic mucosa in experimental swine dysentery studied by fluorescent in situ hybridization

    DEFF Research Database (Denmark)

    Jensen, Tim Kåre; Boye, Mette; Møller, Kristian

    1998-01-01

    The localization of Serpulina hyodysenteriae in experimental swine dysentery was studied by fluorescent in situ hybridization (FISH) using an oligonucleotide probe targeting the 23S rRNA of S. hyodysenteriae. Nine 8-week-old pigs were challenged. Seven of the pigs were intragastrically dosed with 1......x10(9) cfu S. hyodysenteriae for 3 consecutive days, whereas two pigs were infected by contact. Six non-challenged pigs served as negative controls. The challenged pigs developed clinical swine dysentery from 8 to 14 days postinfection with typical gross lesions. By FISH S. hyodysenteriae cells...

  19. Beamline electrostatic levitator for in situ high energy x-ray diffraction studies of levitated solids and liquids

    Energy Technology Data Exchange (ETDEWEB)

    Gangopadhyay, A.K.; Lee, G.W.; Kelto, K.F.; Rogers, J.R.; Goldman, A.I.; Robinson, D.S.; Rathz, T.J.; Hyers, R.W. (WU); (UAB); (NASA); (UMASS, Amherst)

    2010-07-19

    Determinations of the phase formation sequence, crystal structures and the thermo-physical properties of materials at high temperatures are hampered by contamination from the sample container and environment. Containerless processing techniques, such as electrostatic (ESL), electromagnetic, aerodynamic, and acoustic levitation, are most suitable for these studies. An adaptation of ESL for in situ structural studies of a wide range of materials using high energy (30-130 keV) x rays at a synchrotron source is described here. This beamline ESL (BESL) allows the in situ determination of the atomic structures of equilibrium solid and liquid phases, undercooled liquids and time-resolved studies of solid-solid and liquid-solid phase transformations. The use of area detectors enables the rapid acquisition of complete diffraction patterns over a wide range (0.5-14 {angstrom}{sup -1}) of reciprocal space. The wide temperature range (300-2500 K), containerless processing environment under high vacuum (10{sup -7}-10{sup -8} Torr), and fast data acquisition capability, make BESL particularly well suited for phase stability studies of high temperature solids and liquids. An additional, but important, feature of BESL is the capability for simultaneous measurements of a host of thermo-physical properties including the specific heat, enthalpy of transformation, solidus and liquidus temperatures, density, viscosity, and surface tension, all on the same sample during the structural measurements.

  20. In situ characterization of uranium and americium oxide solid solution formation for CRMP process: first combination of in situ XRD and XANES measurements.

    Science.gov (United States)

    Caisso, Marie; Picart, Sébastien; Belin, Renaud C; Lebreton, Florent; Martin, Philippe M; Dardenne, Kathy; Rothe, Jörg; Neuville, Daniel R; Delahaye, Thibaud; Ayral, André

    2015-04-14

    Transmutation of americium in heterogeneous mode through the use of U1-xAmxO2±δ ceramic pellets, also known as Americium Bearing Blankets (AmBB), has become a major research axis. Nevertheless, in order to consider future large-scale deployment, the processes involved in AmBB fabrication have to minimize fine particle dissemination, due to the presence of americium, which considerably increases the risk of contamination. New synthesis routes avoiding the use of pulverulent precursors are thus currently under development, such as the Calcined Resin Microsphere Pelletization (CRMP) process. It is based on the use of weak-acid resin (WAR) microspheres as precursors, loaded with actinide cations. After two specific calcinations under controlled atmospheres, resin microspheres are converted into oxide microspheres composed of a monophasic U1-xAmxO2±δ phase. Understanding the different mechanisms during thermal conversion, that lead to the release of organic matter and the formation of a solid solution, appear essential. By combining in situ techniques such as XRD and XAS, it has become possible to identify the key temperatures for oxide formation, and the corresponding oxidation states taken by uranium and americium during mineralization. This paper thus presents the first results on the mineralization of (U,Am) loaded resin microspheres into a solid solution, through in situ XAS analysis correlated with HT-XRD.

  1. In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide

    International Nuclear Information System (INIS)

    Storm, Mie Møller; Johnsen, Rune E.; Norby, Poul

    2016-01-01

    Graphene oxide (GO) and reduced graphene oxide (rGO) are important materials in a wide range of fields. The modified Hummers methods, for synthesizing GO, and subsequent thermal reduction to rGO, are often employed for production of rGO. However, the mechanism behinds these syntheses methods are still unclear. We present an in situ X-ray diffraction study of the synthesis of GO and thermal reduction of GO. The X-ray diffraction revealed that the Hummers method includes an intercalation state and finally formation of additional crystalline material. The formation of GO is observed during both the intercalation and the crystallization stage. During thermal reduction of GO three stages were observed: GO, a disordered stage, and the rGO stage. The appearance of these stages depends on the heating ramp. The aim of this study is to provide deeper insight into the chemical and physical processes during the syntheses. - Graphical abstract: In situ X-ray diffraction results for of the modified Hummers synthesis and the thermal reduction of graphene oxide, revealing three stages for both syntheses as well as new GO diffraction peaks and unidentified crystalline material for the Hummers synthesis and a disordered stage for the thermal reduction of graphene oxide. Display Omitted - Highlights: • Hummers synthesis consists of three stages: dissolution, intercalation and crystal. • GO is produced early on during the synthesis and display new diffraction peaks. • An unidentified triclinic phase is observed for the Hummers synthesis. • Thermal reduction of GO display three stages: GO, a disordered stage and rGO. • In situ XRD indicate reformation of rGO even for fast heated thermal reduction.

  2. In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide

    Energy Technology Data Exchange (ETDEWEB)

    Storm, Mie Møller, E-mail: mmst@dtu.dk; Johnsen, Rune E.; Norby, Poul

    2016-08-15

    Graphene oxide (GO) and reduced graphene oxide (rGO) are important materials in a wide range of fields. The modified Hummers methods, for synthesizing GO, and subsequent thermal reduction to rGO, are often employed for production of rGO. However, the mechanism behinds these syntheses methods are still unclear. We present an in situ X-ray diffraction study of the synthesis of GO and thermal reduction of GO. The X-ray diffraction revealed that the Hummers method includes an intercalation state and finally formation of additional crystalline material. The formation of GO is observed during both the intercalation and the crystallization stage. During thermal reduction of GO three stages were observed: GO, a disordered stage, and the rGO stage. The appearance of these stages depends on the heating ramp. The aim of this study is to provide deeper insight into the chemical and physical processes during the syntheses. - Graphical abstract: In situ X-ray diffraction results for of the modified Hummers synthesis and the thermal reduction of graphene oxide, revealing three stages for both syntheses as well as new GO diffraction peaks and unidentified crystalline material for the Hummers synthesis and a disordered stage for the thermal reduction of graphene oxide. Display Omitted - Highlights: • Hummers synthesis consists of three stages: dissolution, intercalation and crystal. • GO is produced early on during the synthesis and display new diffraction peaks. • An unidentified triclinic phase is observed for the Hummers synthesis. • Thermal reduction of GO display three stages: GO, a disordered stage and rGO. • In situ XRD indicate reformation of rGO even for fast heated thermal reduction.

  3. Particle and liquid motion in semi-solid aluminium alloys: A quantitative in situ microradioscopy study

    International Nuclear Information System (INIS)

    Zabler, S.; Ershov, A.; Rack, A.; Garcia-Moreno, F.; Baumbach, T.; Banhart, J.

    2013-01-01

    Semi-solid melts exhibit a very unpredictable rheology and filling dynamics, when injected into thin-walled components. Optimization of the process requires an insight into the casting process during injection. For this purpose we injected semi-solid an Al–Ge alloy into two different thin channel geometries while recording high resolution radiographs at fast frame rates (up to 1000 images per s). Comparison of a bottleneck channel, which has previously been used for slower experiments, with a right-angle turn geometry reveals a significant influence of the channel shape on the flow behaviour of the particle–liquid mixture. While the bottleneck is quickly sealed with densified solid, turbulences in the right-angle turn apparently permit solid particles and clusters to move conjointly with the liquid and thus achieve a more complete filling. Single particle trajectories and rapid break-up of solid skeletons in such a system have been observed for the first time in situ

  4. In situ TEM study of the coarsening of carbon black supported Pt nanoparticles in hydrogen

    DEFF Research Database (Denmark)

    Simonsen, Søren Bredmose; Wang, Yan; Jensen, Jens Oluf

    2017-01-01

    The control of sizes and shapes of nanostructures is of tremendous importance for the catalytic activity in electrochemistry and in catalysis more generally. However, due to relatively large surface free energies, nanostructures often sinter to form coarser and more stable structures that may...... not have the intended physicochemical properties. Pt is known to be a very active catalyst in several chemical reactions and for example as carbon supported nanoparticles in fuel cells. The presentation focusses on coarsening mechanisms of Pt nanoparticles supported on carbon black during exposure...... to hydrogen. By means of in situ transmission electron microscopy (TEM), Pt nanoparticle coarsening was monitored in 6 mbar 20 % H2/Ar while ramping up the temperature to ca. 900 °C. Time-resolved TEM images directly reveal that separated ca. 3 nm sized Pt nanoparticles in the pure hydrogen environment...

  5. CHEMLAB. A probe for in-situ radionuclide experiments. Diffusion studies

    Energy Technology Data Exchange (ETDEWEB)

    Jansson, Mats; Eriksen, Trygve E. [Royal Inst. of Technology, Stockholm (Sweden). Dept. of Chemistry

    2001-06-01

    CHEMLAB is a borehole laboratory built into a probe, in which in situ experiments can be carried out under ambient conditions with respect to pressure and temperature with the use of natural groundwater from the surrounding rock. The first CHEMLAB experiments, diffusion of cations and anions in compacted bentonite clay, have been carried out in borehole KA2512A at a depth of 320 m in Aespoe Hard Rock Laboratory. Diffusant solutions of Co{sup 2+}, Sr{sup 2+}, Cs{sup +}, I{sup -} and TcO{sup 4-} with {sup 57}Co, {sup 85}Sr, {sup 134}Cs, {sup 131}I and {sup 99}Tc as tracers were used. measured profiles for the radionuclides in the bentonite are in good agreement with profiles predicted from modelling based on apparent diffusivities and sorption coefficients obtained in laboratory experiments with clay compacted to corresponding dry density and synthetic ground water with the same composition as in borehole KA2512A.

  6. CHEMLAB. A probe for in-situ radionuclide experiments. Diffusion studies

    International Nuclear Information System (INIS)

    Jansson, Mats; Eriksen, Trygve E.

    2001-06-01

    CHEMLAB is a borehole laboratory built into a probe, in which in situ experiments can be carried out under ambient conditions with respect to pressure and temperature with the use of natural groundwater from the surrounding rock. The first CHEMLAB experiments, diffusion of cations and anions in compacted bentonite clay, have been carried out in borehole KA2512A at a depth of 320 m in Aespoe Hard Rock Laboratory. Diffusant solutions of Co 2+ , Sr 2+ , Cs + , I - and TcO 4- with 57 Co, 85 Sr, 134 Cs, 131 I and 99 Tc as tracers were used. measured profiles for the radionuclides in the bentonite are in good agreement with profiles predicted from modelling based on apparent diffusivities and sorption coefficients obtained in laboratory experiments with clay compacted to corresponding dry density and synthetic ground water with the same composition as in borehole KA2512A

  7. Dynamical properties of nano-structured catalysts for methane conversion: an in situ scattering study

    DEFF Research Database (Denmark)

    Kehres, Jan

    /NiO particles in a fresh catalyst sample showed a Ni/NiO core shell structure. The Ni lattice parameter decreased during the reduction due to the release of stress between the Ni core and the NiO shell. Ni particles sintered during heating in hydrogen after the reduction of the NiO shell. Dry reforming......The reactivity of catalyst particles can be radically enhanced by decreasing their size down to the nanometer range. The nanostructure of a catalyst can have an enormous and positive influence on the reaction rate, for example strong structure sensitivity was observed for methane reforming...... range from 298 - 1023 K. Correlated crystallite and particle growth due to sintering were observed after the decomposition of the surfactant. Furthermore transformations from rod to spherical particle shape were observed. In situ reduction experiments of a Ni/MgAl2O4 catalyst were performed. The Ni...

  8. Photoinduced electron transfer to fullerene C70 (An in situ EPR study)

    International Nuclear Information System (INIS)

    Brezova, V.; Dvoranova, D.; Kostova, B.; Stasko, A.

    1999-01-01

    The photoexcitation of fullerene C 70 by monochromatic light (λ = 546 nm) in the presence of electron donating substrate 3,3',5,5'-tetramethyl-benzidine (TMB) resulted in the charge-transfer, quenching the fullerene triplet state and forming corresponding C 70 anion-radicals. Analogously to the photo-reduction of C 60 , two EPR signal were observed upon in situ irradiation in the cavity of EPR spectrometer. EPR singlet A characterized by g-value, g A = 2.0009 and peak-to-peak line-width, pp A = 0.013 mT was assigned to the C 70 mono-anion. Signal B (g B = 2.0011; pp B = 0.011 mT) was tentatively attributed to the C 70 di-anion or to the associated forms of mono-anions. The stabilization of photo-generated anion-radicals significantly depends on solvent polarity. (authors)

  9. In situ x-ray diffraction study on AgI nanowire arrays

    International Nuclear Information System (INIS)

    Wang Yinhai; Ye Changhui; Wang Guozhong; Zhang Lide; Liu Yanmei; Zhao Zhongyan

    2003-01-01

    The AgI nanowire arrays were prepared in the ordered porous alumina membrane by an electrochemical method. Transmission electron microscopy observation shows that the AgI nanowires are located in the channels of the alumina membrane. In situ x-ray diffractions show that the nanowire arrays possess hexagonal close-packed structure (β-AgI) at 293 K, orienting along the (002) plane, whereas at 473 K, the nanowire arrays possess a body-centered cubic structure (α-AgI), orienting along the (110) plane. The AgI nanowire arrays exhibit a negative thermal expansion property from 293 to 433 K, and a higher transition temperature from the β to α phase. We ascribe the negative thermal expansion behavior to the phase transition from the β to α phase, and the elevated transition temperature to the radial restriction by the channels of alumina membrane

  10. Raman mapping and in situ SERS spectroelectrochemical studies of 6-mercaptopurine SAMs on the gold electrode.

    Science.gov (United States)

    Yang, Haifeng; Liu, Yanli; Liu, Zhimin; Yang, Yu; Jiang, Jianhui; Zhang, Zongrang; Shen, Guoli; Yu, Ruqin

    2005-02-24

    The self-assembled monolayers (SAMs) of 6-mercaptopurine (6MP) were formed at the roughened polycrystalline gold surfaces in acid and alkaline media. The time-dependent Raman mapping spectral analysis in conjunction with the quantum calculations for the vibrational modes using ab initio BLYP/6-31G method suggested that both of the resulted 6MP SAMs adopted the same adsorption mode through the S atom of pyrimidine moiety and the N7 atom of the imidazole moiety anchoring the gold surface in a vertical way. The in situ surface-enhanced Raman scattering spectroelectrochemical experiment was conducted to examine the stability of the SAMs at various bias potentials. It was found that the detaching process of the 6MP SAMs from the surface involved one electron reduction as the voltage was applied at ca. 0.7 V vs a standard calomel electrode.

  11. In Situ High Resolution Synchrotron X-Ray Powder Diffraction Studies of Lithium Batteries

    DEFF Research Database (Denmark)

    Amri, Mahrez; Fitch, Andy; Norby, Poul

    2015-01-01

    allowing diffraction information to be obtained from only the active material during battery operation [2]. High resolution synchrotron x-ray powder diffraction technique has been undertaken to obtain detailed structural and compositional information during lithiation/delithiation of commercial LiFePO4...... materials [3]. We report results from the first in situ time resolved high resolution powder diffraction experiments at beamline ID22/31 at the European Synchrotron Radiation Facility, ESRF. We follow the structural changes during charge of commercial LiFePO4 based battery materials using the Rietveld...... method. Conscientious Rietveld analysis shows slight but continuous deviation of lattice parameters from those of the fully stoichiometric end members LiFePO4 and FePO4 indicating a subsequent variation of stoichiometry during cathode delithiation. The application of an intermittent current pulses during...

  12. In Situ X-ray Diffraction Studies of (De)lithiation Mechanism in Silicon Nanowire Anodes

    KAUST Repository

    Misra, Sumohan

    2012-06-26

    Figure Persented: Silicon is a promising anode material for Li-ion batteries due to its high theoretical specific capacity. From previous work, silicon nanowires (SiNWs) are known to undergo amorphorization during lithiation, and no crystalline Li-Si product has been observed. In this work, we use an X-ray transparent battery cell to perform in situ synchrotron X-ray diffraction on SiNWs in real time during electrochemical cycling. At deep lithiation voltages the known metastable Li 15Si 4 phase forms, and we show that avoiding the formation of this phase, by modifying the SiNW growth temperature, improves the cycling performance of SiNW anodes. Our results provide insight on the (de)lithiation mechanism and a correlation between phase evolution and electrochemical performance for SiNW anodes. © 2012 American Chemical Society.

  13. Quantitative in situ magnetization reversal studies in Lorentz microscopy and electron holography.

    Science.gov (United States)

    Rodríguez, L A; Magén, C; Snoeck, E; Gatel, C; Marín, L; Serrano-Ramón, L; Prieto, J L; Muñoz, M; Algarabel, P A; Morellon, L; De Teresa, J M; Ibarra, M R

    2013-11-01

    A generalized procedure for the in situ application of magnetic fields by means of the excitation of the objective lens for magnetic imaging experiments in Lorentz microscopy and electron holography is quantitatively described. A protocol for applying magnetic fields with arbitrary in-plane magnitude and orientation is presented, and a freeware script for Digital Micrograph(™) is provided to assist the operation of the microscope. Moreover, a method to accurately reconstruct hysteresis loops is detailed. We show that the out-of-plane component of the magnetic field cannot be always neglected when performing quantitative measurements of the local magnetization. Several examples are shown to demonstrate the accuracy and functionality of the methods. © 2013 Elsevier B.V. All rights reserved.

  14. In situ observation of Cu-Ni alloy nanoparticle formation by X-ray diffraction, X-ray absorption spectroscopy, and transmission electron microscopy: Influence of Cu/Ni ratio

    DEFF Research Database (Denmark)

    Wu, Qiongxiao; Duchstein, Linus Daniel Leonhard; Chiarello, Gian Luca

    2014-01-01

    Silica-supported, bimetallic Cu-Ni nanomaterials were prepared with different ratios of Cu to Ni by incipient wetness impregnation without a specific calcination step before reduction. Different in situ characterization techniques, in particular transmission electron microscopy (TEM), X-ray...... diffraction (XRD), and X-ray absorption spectroscopy (XAS), were applied to follow the reduction and alloying process of Cu-Ni nanoparticles on silica. In situ reduction of Cu-Ni samples with structural characterization by combined synchrotron XRD and XAS reveals a strong interaction between Cu and Ni species......, which results in improved reducibility of the Ni species compared with monometallic Ni. At high Ni concentrations silica-supported Cu-Ni alloys form a homogeneous solid solution of Cu and Ni, whereas at lower Ni contents Cu and Ni are partly segregated and form metallic Cu and Cu-Ni alloy phases. Under...

  15. In-situ study of pn-heterojunction interface states in organic thin film transistors

    International Nuclear Information System (INIS)

    Ye, Rongbin; Ohta, Koji; Baba, Mamoru

    2014-01-01

    In this paper, we have investigated the density of pn-heterojunction interface states by evaluating the threshold voltage shift with in-situ measurement of electrical characteristics of a sandwich fluorinated copper phthalocyanine/pentacene thin film transistor with various thicknesses of pentacene thin films. A threshold voltage (V T ) undergoes a significant shift from + 20.6 to + 0.53 V with increasing the thickness of pentacene. When the thickness of pentacene is more than a critical thickness of 15 nm, V T undergoes hardly any shift. On the other hand, the value of mobility is lightly decreased with increasing the thickness of pentacene due to the effect of the bulk current. Thus the V T shift is attributed to the increase of drain current in the sandwich device. In order to explain the V T shift, a model was assumed in the linear region of thin film transistor operation and the V T shift agrees with a tan −1 function of film thickness. The total charge density (Q 0 ) of 1.53 × 10 −7 C/cm 2 (9.56 × 10 11 electrons or holes/cm 2 ) was obtained. Furthermore, the V T shift and Q 0 could be adjusted by selecting a p-type semiconductor. - Highlights: • A threshold voltage was in-situ measured in an organic sandwich thin film transistor. • Density of pn-heterojunction interface states by evaluating the threshold voltage shift. • The threshold voltage shift attributes to the increase of drain current. • In order to explain the threshold voltage shift, a model was assumed

  16. In-situ study of pn-heterojunction interface states in organic thin film transistors

    Energy Technology Data Exchange (ETDEWEB)

    Ye, Rongbin, E-mail: ye@iwate-u.ac.jp; Ohta, Koji; Baba, Mamoru

    2014-03-03

    In this paper, we have investigated the density of pn-heterojunction interface states by evaluating the threshold voltage shift with in-situ measurement of electrical characteristics of a sandwich fluorinated copper phthalocyanine/pentacene thin film transistor with various thicknesses of pentacene thin films. A threshold voltage (V{sub T}) undergoes a significant shift from + 20.6 to + 0.53 V with increasing the thickness of pentacene. When the thickness of pentacene is more than a critical thickness of 15 nm, V{sub T} undergoes hardly any shift. On the other hand, the value of mobility is lightly decreased with increasing the thickness of pentacene due to the effect of the bulk current. Thus the V{sub T} shift is attributed to the increase of drain current in the sandwich device. In order to explain the V{sub T} shift, a model was assumed in the linear region of thin film transistor operation and the V{sub T} shift agrees with a tan{sup −1} function of film thickness. The total charge density (Q{sub 0}) of 1.53 × 10{sup −7} C/cm{sup 2} (9.56 × 10{sup 11} electrons or holes/cm{sup 2}) was obtained. Furthermore, the V{sub T} shift and Q{sub 0} could be adjusted by selecting a p-type semiconductor. - Highlights: • A threshold voltage was in-situ measured in an organic sandwich thin film transistor. • Density of pn-heterojunction interface states by evaluating the threshold voltage shift. • The threshold voltage shift attributes to the increase of drain current. • In order to explain the threshold voltage shift, a model was assumed.

  17. A feasibility study on geological and hydrogeological setting or in-situ leaching mining in a sandstone-type uranium deposit

    International Nuclear Information System (INIS)

    Guo Sanmin.

    1992-01-01

    A comparative study is made of various conditions for in-situ leaching mining in a sandstone-type uranium deposit in Inner Mongolia with those of same types at home and abroad based on a large number of practical information. It is concluded that the deposit basically exhibits the geological conditions for in-situ leaching mining, and tentative plan and suggestion for further work are presented

  18. New Rhizon in situ sampler for pore water studies in aquatic sediments: For example nutrient input from submarine groundwater discharge in costal areas.

    OpenAIRE

    Seeberg-Elverfeldt, J.; Schlüter, Michael; Kölling, M.; Feseker, T.

    2005-01-01

    To investigate coastal biogeochemical cycles, especially at the sediment/water interface,improved sampling methods are necessary. For this purpose, we developed apore water in situ sampler with miniature sampling devices, so called Rhizons. Rhizonsoil moisture samplers have been used as sampling devices in unsaturated soilsfor the last ten years. In aquatic science they have been rarely used to extract porewater from sediments. This study presents a new developed Rhizon In Situ Sampler(RISS) ...

  19. Microbiological aspects of an in situ model to study effects of antimicrobial agents on dental plaque ecology.

    Science.gov (United States)

    Giertsen, E; Guggenheim, B; Thurnheer, T; Gmür, R

    2000-10-01

    This study validates an in situ model for ecological studies of dental plaque exposed to various antimicrobial agents with different modes of action on plaque bacteria. Eleven subjects wore two acrylic appliances, each containing two bovine enamel discs, during two 1-wk test periods. Using a split-mouth crossover design, the appliances were dipped twice daily for 1 min into water (control; treatment A), fluoride (26.3 mM NaF; B), zinc acetate (20.0 mM; C), or fluoride plus zinc acetate (D). Four of the subjects used also chlorhexidine diacetate (2.2 mM; E) and chlorhexidine plus fluoride (F). At the end of each period, plaque was collected from the discs, after which the microbiota were analyzed by culture, automated quantitative immunofluorescence, and a viability fluorescence stain. As compared to control, treatments B, C, and D resulted in a significant reduction of individual taxa as detected by immunofluorescence, whereas similar bacterial viability and total bacterial numbers were observed. In contrast, chlorhexidine significantly reduced bacterial viability, total cell numbers, and the abundance of most of the enumerated taxa. We conclude that this in situ model is well suited to study effects of antimicrobial agents on dental plaque ecology. Combined with viability testing, immunofluorescence is obviously superior to culture in detecting taxa-specific shifts caused by antimicrobial agents.

  20. Study on development of evaluation technique of in-situ tracer test in Horonobe Underground Research Laboratory project (Contract research)

    International Nuclear Information System (INIS)

    Yokota, Hideharu; Amano, Kenji; Maekawa, Keisuke; Kunimaru, Takanori; Naemura, Yumi; Ijiri, Yuji; Motoshima, Takayuki; Suzuki, Shunichi; Teshima, Kazufumi

    2013-06-01

    In the Horonobe Underground Research Laboratory Project, in-situ tracer tests are valuable and important as the investigations to obtain the mass transportation data of fractures in hostrock. However, it is difficult that the in-situ tests are executed under various conditions due to long test period and the tests results are evaluated about permeable heterogeneity in a fracture and/or scale effects. In this study, a number of tracer tests are simulated in a fictitious single plate fracture generated on computer. And the transport parameters are identified by fitting one- and two-dimensional models to the breakthrough curves obtained from the simulations in order to investigate the applicability of these models to the evaluation of in-situ tracer test. As a result, one-dimensional model yields larger longitudinal dispersion length than two-dimensional model in the both cases of homogeneous and heterogeneous hydraulic conductivity fields of the fictitious fracture. This is because that the effect of transverse dispersion has to be included in the longitudinal dispersion length parameter in the one-dimensional model. It is also found that the larger dipole ratio and the larger natural groundwater flow crossing the flow generated between two boreholes make the identified longitudinal dispersion length larger. And, the longitudinal dispersion length identified from a tracer test is smaller and/or larger than the macroscopic longitudinal dispersion length identified from whole fracture. It is clarified that these are occurred by shorter or longer distance between boreholes compare to the correlation length of geostatistical heterogeneity of fictitious fracture. (author)

  1. Support Effects in Catalysis Studied by in-situ Sum Frequency Generation Vibrational Spectroscopy and in-situ X-Ray Spectroscopies

    Science.gov (United States)

    Kennedy, Griffin John

    Kinetic measurements are paired with in-situ spectroscopic characterization tools to investigate colloidally based, supported Pt catalytic model systems in order to elucidate the mechanisms by which metal and support work in tandem to dictate activity and selectivity. The results demonstrate oxide support materials, while inactive in absence of Pt nanoparticles, possess unique active sites for the selective conversion of gas phase molecules when paired with an active metal catalyst. In order to establish a paradigm for metal-support interactions using colloidally synthesized Pt nanoparticles the ability of the organic capping agent to inhibit reactivity and interaction with the support must first be assessed. Pt nanoparticles capped by poly(vinylpyrrolidone) (PVP), and those from which the PVP is removed by UV light exposure, are investigated for two reactions, the hydrogenation of ethylene and the oxidation of methanol. It is shown that prior to PVP removal the particles are moderately active for both reactions. Following removal, the activity for the two reactions diverges, the ethylene hydrogenation rate increases 10-fold, while the methanol oxidation rate decreases 3-fold. To better understand this effect the capping agent prior to, and the residual carbon remaining after UV treatment are probed by sum frequency generation vibrational spectroscopy. Prior to removal no major differences are observed when the particles are exposed to alternating H2 and O2 environments. When the PVP is removed, carbonaceous fragments remain on the surface that dynamically restructure in H2 and O2. These fragments create a tightly bound shell in an oxygen environment and a porous coating of hydrogenated carbon in the hydrogen environment. Reaction rate measurements of thermally cleaned PVP and oleic acid capped particles show this effect to be independent of cleaning method or capping agent. In all this demonstrates the ability of the capping agent to mediate nanoparticle catalysis

  2. Model test study on propagation law of plane stress wave in jointed rock mass under different in-situ stresses

    Science.gov (United States)

    Dong, Qian

    2017-12-01

    The study of propagation law of plane stress wave in jointed rock mass under in-situ stress has important significance for safety excavation of underground rock mass engineering. A model test of the blasting stress waves propagating in the intact rock and jointed rock mass under different in-situ stresses was carried out, and the influencing factors on the propagation law, such as the scale of static loads and the number of joints were studied respectively. The results show that the transmission coefficient of intact rock is larger than that of jointed rock mass under the same loading condition. With the increase of confining pressure, the transmission coefficients of intact rock and jointed rock mass both show an trend of increasing first and then decreasing, and the variation of transmission coefficients in intact rock is smaller than that of jointed rock mass. Transmission coefficient of jointed rock mass decreases with the increase of the number of joints under the same loading condition, when the confining pressure is relatively small, the reduction of transmission coefficients decreases with the increasing of the number of joints, and the variation law of the reduction of transmission coefficients is contrary when the confining pressure is large.

  3. In-situ, real-time, studies of film growth processes using ion scattering and direct recoil spectroscopy techniques.

    Energy Technology Data Exchange (ETDEWEB)

    Smentkowski, V. S.

    1999-04-22

    Time-of-flight ion scattering and recoil spectroscopy (TOF-ISARS) enables the characterization of the composition and structure of surfaces with 1-2 monolayer specificity. It will be shown that surface analysis is possible at ambient pressures greater than 3 mTorr using TOF-ISARS techniques; allowing for real-time, in situ studies of film growth processes. TOF-ISARS comprises three analytical techniques: ion scattering spectroscopy (ISS), which detects the backscattered primary ion beam; direct recoil spectroscopy (DRS), which detects the surface species recoiled into the forward scattering direction; and mass spectroscopy of recoiled ions (MSRI), which is 3 variant of DRS capable of isotopic resolution for all surface species--including H and He. The advantages and limitations of each of these techniques will be discussed. The use of the three TOF-ISARS methods for real-time, in situ film growth studies at high ambient pressures will be illustrated. It will be shown that MSRI analysis is possible during sputter deposition. It will be also be demonstrated that the analyzer used for MSRI can also be used for time of flight secondary ion mass spectroscopy (TOF-SIMS) under high vacuum conditions. The use of a single analyzer to perform the complimentary surface analytical techniques of MSRI and SIMS is unique. The dwd functionality of the MSRI analyzer provides surface information not obtained when either MSRI or SIMS is used independently.

  4. Formation and texture of palladium germanides studied by in situ X-ray diffraction and pole figure measurements

    Energy Technology Data Exchange (ETDEWEB)

    Geenen, F.A., E-mail: Filip.Geenen@UGent.be [Ghent University, Department of Solid-State Sciences, Krijgslaan 281 (S1), 9000 Gent (Belgium); Knaepen, W.; De Keyser, K. [Ghent University, Department of Solid-State Sciences, Krijgslaan 281 (S1), 9000 Gent (Belgium); Opsomer, K. [Interuniversitair Micro-Electronica Centrum (IMEC), Kapeldreef 75, 3001 Leuven (Belgium); Vanmeirhaeghe, R.L. [Ghent University, Department of Solid-State Sciences, Krijgslaan 281 (S1), 9000 Gent (Belgium); Jordan-Sweet, J.; Lavoie, C. [IBM T.J. Watson Research Center, Yorktown (United States); Detavernier, C. [Ghent University, Department of Solid-State Sciences, Krijgslaan 281 (S1), 9000 Gent (Belgium)

    2014-01-31

    The solid state reaction between 30 nm Pd films and various Ge substrates (Ge(100), Ge(111), polycrystalline Ge and amorphous Ge) was studied by means of in situ X-ray diffraction and in situ sheet resistance measurements. The reported phase sequence of Pd{sub 2}Ge followed by PdGe was verified on all substrates. The texture of the germanides was analysed by pole figure measurements on samples quenched in the Pd{sub 2}Ge and in the PdGe phase on both Ge(100) and (111) substrates. We report an epitaxial growth of Pd{sub 2}Ge on Ge(111) and on Ge(100). The formed PdGe has an axiotaxial alignment on Ge(111). On Ge(100), the axiotaxial texture is observed together with a fibre texture. The higher formation temperature of PdGe on Ge(111) could be related to the epitaxial alignment of the Pd{sub 2}Ge parent phase on Ge(111). - Highlights: • Solid-state reaction is studied on a Pd film with Ge substrates. • Pd2Ge grains have an epitaxial texture on both Ge 100 and Ge 111. • PdGe grains are found to grow with an axiotaxial texture. • Retarded PdGe formation on Ge111 is related with strong epitaxy of Pd2Ge.

  5. In Situ X-ray Diffraction Study of Cesium Exchange in Synthetic Umbite

    International Nuclear Information System (INIS)

    Fewox, C.; Clearfield, A.; Celestian, A.

    2011-01-01

    The exchange of Cs + into H 1.22 K 0.84 ZrSi 3 O 9 · 2.16H 2 O (umbite-(HK)) was followed in situ using time-resolved X-ray diffraction at the National Synchrotron Light Source. The umbite framework (space group P2 1 /c with cell dimensions of a = 7.2814(3) (angstrom), b = 10.4201(4) (angstrom), c = 13.4529(7) (angstrom), and β = 90.53(1) o ) consists of wollastonite-like silicate chains linked by isolated zirconia octahedra. Within umbite-(HK) there are two unique ion exchange sites in the tunnels running parallel to the a-axis. Exchange Site 1 is marked by 8 member-ring (MR) windows in the bc-plane and contains K + cations. Exchange Site 2 is marked by a larger 8-MR channel parallel to [100], and contains H 2 O molecules. The occupancy of the Cs + cations through these channels was modeled by Rietveld structure refinements of the diffraction data and demonstrated that there is a two-step exchange process. The incoming Cs + ions populated the larger 8-MR channel (Exchange Site 2) first and then migrated into the smaller 8-MR channel. During the exchange process a structural change occurs, transforming the exchanger from monoclinic P2 1 /c to orthorhombic P2 1 2 1 2 1 . This structural change occurs when Cs + occupancy in the small cavity becomes greater than 0.50. The final in situ ion exchange diffraction pattern was refined to yield umbite-(CsK) with the molecular formula H 0.18 K 0.45 Cs 1.37 ZrSi 3 O 9 · 0.98H 2 O and possessing an orthorhombic unit cell with dimensions a = 10.6668(8) (angstrom), b = 13.5821(11) (angstrom), c = 7.3946(6) (angstrom). Solid state 133 Cs MAS NMR showed there is only a slight difference between the two cavities electronically. Valence bond sums for the completely occupied Exchange Site 1 demonstrate that Cs-O bonds of up to 3.8 (angstrom) contribute to the coordination of the Cs + cation.

  6. Magnetic monolayers on semiconducting substrates. An in situ FMR study of Fe-based heterostructures

    Energy Technology Data Exchange (ETDEWEB)

    Zakeri Lori, K.

    2007-10-18

    The growth, magnetic anisotropy, g-factor, and magnetization of Fe monolayers grown on GaAs(001), InAs(001), and InP(001) are investigated by a combination of in situ ferromagnetic resonance and SQUID magnetometry as a function of temperature and film thickness. The effect of stress caused by the lattice mismatch and the surface reconstruction on the magnetic anisotropy is quantified. An in-plane spin reorientation transition as a function of film thickness is observed at room temperature for all systems. A magneto-elastic model is used to explain the direction of the easy axis, the spin reorientation transition, and the contributions to the magnetic anisotropy terms using the stress components measured directly by in situ IV-low-energy electron diffraction. While the model gives a quantitative explanation of the out-of-plane magnetic anisotropy, changes of the electronic interface structure have to be taken into account for the in-plane magnetic anisotropy. The influence of Ag and Au buffer and cap layers on the magnetic anisotropy terms are determined. The temperature dependence of the total magnetic anisotropy, as well as the surface-interface and volume contribution to the magnetic anisotropy are determined for Fe monolayers on GaAs(001). It is demonstrated that the temperature dependence of the magnetic anisotropy is correlated with the temperature dependence of the magnetization according to the Callen-Callen model. The temperature dependence of the volume contribution to the perpendicular magnetic anisotropy is fully explained by the temperature dependence of the magneto-elastic anisotropy. A temperature-driven morphological transformation occurring at a temperature higher than 550 K depending on the film thickness is observed. The thin Fe3Si binary Heusler structure epitaxially grown on MgO(001) is investigated. In addition to the structural properties, magnetic anisotropy, magnetization, g-factor, spin, and orbital magnetism, the magnetic relaxation

  7. Simultaneous FTIR/UV-Vis study of reactions over metallo-zeolites. Approach to quantitative in situ studies

    Czech Academy of Sciences Publication Activity Database

    Sobalík, Zdeněk; Jíša, Kamil; Jirglová, Hana; Bernauer, B.

    2007-01-01

    Roč. 126, 1-2 (2007), s. 73-80 ISSN 0920-5861 R&D Projects: GA AV ČR 1ET400400413; GA ČR GA104/06/1254; GA ČR GA203/05/2309 Institutional research plan: CEZ:AV0Z40400503 Keywords : metallo-zeolites * FTIR/UV-Vis * adsorption * modeling * in-situ Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 2.764, year: 2007

  8. In situ spectroscopic evidence for neptunium(V)-carbonate inner-sphere and outer-sphere ternary surface complexes on hematite surfaces.

    Science.gov (United States)

    Arai, Yuji; Moran, P B; Honeyman, B D; Davis, J A

    2007-06-01

    Np(V) surface speciation on hematite surfaces at pH 7-9 under pC2 = 10(-3.45) atm was investigated using X-ray absorption spectroscopy (XAS). In situ XAS analyses suggest that bis-carbonato inner-sphere and tris-carbonato outer-sphere ternary surface species coexist at the hematite-water interface at pH 7-8.8, and the fraction of outer-sphere species gradually increases from 27 to 54% with increasing pH from 7 to 8.8. The results suggest that the heretofore unknown Np(V)-carbonato ternary surface species may be important in predicting the fate and transport of Np(V) in the subsurface environment down gradient of high-level nuclear waste respositories.

  9. Powder metallurgical nanostructured medium carbon bainitic steel: Kinetics, structure, and in situ thermal stability studies

    Energy Technology Data Exchange (ETDEWEB)

    Lonardelli, I., E-mail: il244@cam.ac.uk [University of Cambridge, Materials Science and Metallurgy, Pembroke Street, Cambridge CB2 3QZ (United Kingdom); University of Trento, Materials Engineering and Industrial Technologies, via Mesiano 77, 38123 Trento (Italy); Bortolotti, M. [Fondazione Bruno Kessler, via Sommarive 18, 38123 Trento (Italy); Beek, W. van [Swiss-Norwegian Beamlines, ESRF, BP 220, 38043 Grenoble Cedex (France); Girardini, L.; Zadra, M. [K4-Sint, via Dante 300, 38057 Pergine Valsugana (Italy); Bhadeshia, H.K.D.H. [University of Cambridge, Materials Science and Metallurgy, Pembroke Street, Cambridge CB2 3QZ (United Kingdom)

    2012-10-15

    It has been possible to produce incredibly fine plates of bainitic ferrite separated by a percolating network of retained austenite in a medium carbon steel produced by mechanical alloying followed by spark plasma sintering and isothermal heat treatment. This is because the sintering process limits the growth of the austenite grains to such an extent that the martensite-start temperature is suppressed in spite of the medium carbon concentration. Furthermore, the fine austenite grain size accelerates the bainite transformation, which can therefore be suppressed to low temperatures to obtain a nanostructure. Microscopy and in situ synchrotron X-ray diffraction were used to investigate the morphology and the thermal stability of the retained austenite during continuous heating. These latter experiments revealed a gradient of carbon concentration in the retained austenite and a reduced thermal stability in high carbon film-austenite. It was also possible to correlate the evolution of defect density and carbon depletion in both retained austenite and bainitic ferrite during tempering.

  10. An in situ Raman spectroscopy study of stress transfer between carbon nanotubes and polymer

    International Nuclear Information System (INIS)

    Mu Minfang; Winey, Karen I; Osswald, Sebastian; Gogotsi, Yury

    2009-01-01

    The transfer mechanism of applied stress in single-wall carbon nanotube (SWCNT)/poly(methyl methacrylate) (PMMA) nanocomposites was investigated using in situ Raman spectroscopy on composite fibers. These SWCNT/PMMA nanocomposite fibers have no specific SWCNT-polymer interactions and the high degree of nanotube alignment minimizes the contributions from nanotube-nanotube interactions. Although tensile testing found significantly improved overall mechanical properties of the fibers, effective stress transfer to SWCNTs is limited to a small strain regime (ε<0.2%). At higher strains, the stress on the SWCNTs decreases due to the slippage at the nanotube-polymer interface. Slippage was also evident in scanning electron micrographs of fracture surfaces produced by tensile testing of the composite fibers. Above ε = 0.2%, the strain-induced slippage was accompanied by irreversible responses in stress and Raman peak shifts. This paper shows that efficient stress transfer to nanotubes as monitored by Raman spectroscopy is crucial to improving the mechanical properties of polymer nanocomposites and to detecting internal damage in nanocomposites.

  11. In situ study starch gelatinization under ultra-high hydrostatic pressure using synchrotron SAXS

    KAUST Repository

    Yang, Zhi

    2015-12-13

    The gelatinization of waxy (very low amylose) corn and potato starches by high hydrostatic pressure (HHP) (up to ∼1 GPa) was investigated in situ using synchrotron small-angle X-ray scattering (SAXS) on samples held in a diamond anvil cell (DAC). The starch pastes, made by mixing starch and water in a 1:1 ratio (by weight), were pressurized and measured at room temperature. During HHP, both SAXS peak areas (corresponding to the lamellar phase) of waxy corn and potato starches decreased suggesting the starch gelatinization increases with increasing pressure. As pressure increased, lamellar peak broadened and the power law exponent increased in low q region. 1D linear correlation function was further employed to analyse SAXS data. For both waxy potato and waxy corn starches, the long period length and the average thickness of amorphous layers decreased when the pressure increased. While for both of waxy starches, the thickness of the crystalline layer first increased, then decreased when the pressure increased. The former is probably due to the out-phasing of starch molecules, and the latter is due to the water penetrating into the crystalline region during gelatinization and to pressure induced compression.

  12. In situ infrared spectroscopic study of the electrochromic reactions of tungsten trioxide films

    International Nuclear Information System (INIS)

    Habib, M.A.; Maheswari, S.P.

    1991-01-01

    This paper reports on thin WO 3 films which are transparent in the oxidized state and colored in the reduced state. These changes in optical properties are associated with compositional variations of the material. Changes in vibrational intensities of W double-bond O, W emdash O, and W double-bond O emdash H bonds in the electrochromic WO 3 film were detected by an in situ FTIR technique at various stages of reduction (coloration). The absorbance due to O emdash H stretching and bending vibrations was found to increase during the electrochemical reduction of the film, indicating the incorporation of water into the film along with the formation of H x WO 3 bronze during coloration. The absorbance due to W double-bond O vibration decreased while that due to W emdash O vibration increased during reduction. These observations suggest that during the coloration process W double-bond O bonds break and new W emdash O bonds form in the film, and thus, provide direct evidence for the electrochromic reaction. O 2 W double-bond O + xH + + xe - ↔ O 2 W emdash O emdash H x

  13. In situ studies of oxide nucleation, growth, and transformation using slow electrons

    Science.gov (United States)

    Flege, Jan Ingo; Grinter, David C.

    2018-05-01

    Surface processes such as metal oxidation and metal oxide growth invariably influence the physical and chemical properties of materials and determine their interaction with their surroundings and hence their functionality in many technical applications. On a fundamental level, these processes are found to be governed by a complex interplay of thermodynamic variables and kinetic constraints, resulting in a rich variety of material-specific phenomena. In this review article, we discuss recent results and insights on transition metal oxidation and rare-earth oxide growth acquired by low-energy electron microscopy and related techniques. We demonstrate that the use of in situ surface sensitive methods is a prerequisite to gaining a deeper understanding of the underlying concepts and the mechanisms responsible for the emerging oxide structure and morphology. Furthermore, examples will be provided on how structural and chemical modifications of the oxide films and nanostructures can be followed in real-time and analyzed in terms of local reactivity and cooperative effects relevant for heterogeneous model catalysis.

  14. An in situ infrared study of dimethyl carbonate synthesis from carbon dioxide and methanol over zirconia

    International Nuclear Information System (INIS)

    Jung, Kyeong Taek; Bell, Alexis T.

    2001-01-01

    The mechanism of dimethyl carbonate (DMC) synthesis from methanol and carbon dioxide over monoclinic zirconia has been investigated using in situ infrared spectroscopy. The dissociative adsorption of methanol occurs more slowly than the adsorption of carbon dioxide, but the species formed from methanol are bound more strongly. Upon adsorption, the oxygen atom of methanol binds to coordinately unsaturated Zr4+ cations present at the catalyst surface. Rapid dissociation of the adsorbed methanol leads to the formation of a methoxide group (Zr-OCH3) and the release of a proton, which reacts with a surface hydroxyl group to produce water. Carbon dioxide inserts in the Zr-O bond of the methoxide to form a mondentate methyl carbonate group (Zr-OC(O)OCH3). This process is facilitated by the interactions of C and O atoms in CO2 with Lewis acid-base pairs of sites (Zr4+O2-) on the surface of the catalyst. Methyl carbonate species can also be produced via the reaction of methanol with carbon dioxide adsorbed in the form of bicarbonate species with methanol, a process that results in the transfer of a methyl group to the carbonate and restores a hydroxyl group to the zirconia surface. The decomposition of DMC on monoclinic zirconia has also been investigated and has been observed to occur via the reverse of the processes described for the synthesis of DMC

  15. Quantitative in situ magnetization reversal studies in Lorentz microscopy and electron holography

    International Nuclear Information System (INIS)

    Rodríguez, L.A.; Magén, C.; Snoeck, E.; Gatel, C.; Marín, L.; Serrano-Ramón, L.

    2013-01-01

    A generalized procedure for the in situ application of magnetic fields by means of the excitation of the objective lens for magnetic imaging experiments in Lorentz microscopy and electron holography is quantitatively described. A protocol for applying magnetic fields with arbitrary in-plane magnitude and orientation is presented, and a freeware script for Digital Micrograph ™ is provided to assist the operation of the microscope. Moreover, a method to accurately reconstruct hysteresis loops is detailed. We show that the out-of-plane component of the magnetic field cannot be always neglected when performing quantitative measurements of the local magnetization. Several examples are shown to demonstrate the accuracy and functionality of the methods. - Highlights: • Generalized procedure for application of magnetic fields with the TEM objective lens. • Arbitrary in-plane magnetic field magnitude and orientation can be applied. • Method to accurately reconstruct hysteresis loops by electron holography. • Out-of-plane field component should be considered in quantitative measurements. • Examples to illustrate the method in Lorentz microscopy and electron holography

  16. Growth of pentacene on α -Al2O3 (0001) studied by in situ optical spectroscopy

    Science.gov (United States)

    Zhang, Lei; Fu, X.; Hohage, M.; Zeppenfeld, P.; Sun, L. D.

    2017-09-01

    The growth of pentacene thin films on a sapphire α -Al2O3 (0001) surface was investigated in situ using differential reflectance spectroscopy (DRS). Two different film structures are observed depending on the substrate temperature. If pentacene is deposited at room temperature, a wetting layer consisting of flat-lying molecules is formed after which upright-standing molecular layers with a herringbone structure start to grow. At low substrate temperature of 100 K, the long molecular axis of the pentacene molecules remains parallel to the surface plane throughout the entire growth regime up to rather large thicknesses. Heating thin films deposited at 100 K to room temperature causes the pentacene molecules beyond the wetting layer to stand up and assemble into a herringbone structure. Another interesting observation is the dewetting of the first flat-lying monolayer upon exposure to air, leading to the condensation of islands consisting of upright-standing molecules. Our results emphasize the interplay between growth kinetics and thermodynamics and its influence on the molecular orientation in organic thin films.

  17. An in situ USAXS-SAXS-WAXS study of precipitate size distribution evolution in a model Ni-based alloy.

    Science.gov (United States)

    Andrews, Ross N; Serio, Joseph; Muralidharan, Govindarajan; Ilavsky, Jan

    2017-06-01

    Intermetallic γ' precipitates typically strengthen nickel-based superalloys. The shape, size and spatial distribution of strengthening precipitates critically influence alloy strength, while their temporal evolution characteristics determine the high-temperature alloy stability. Combined ultra-small-, small- and wide-angle X-ray scattering (USAXS-SAXS-WAXS) analysis can be used to evaluate the temporal evolution of an alloy's precipitate size distribution (PSD) and phase structure during in situ heat treatment. Analysis of PSDs from USAXS-SAXS data employs either least-squares fitting of a preordained PSD model or a maximum entropy (MaxEnt) approach, the latter avoiding a priori definition of a functional form of the PSD. However, strong low- q scattering from grain boundaries and/or structure factor effects inhibit MaxEnt analysis of typical alloys. This work describes the extension of Bayesian-MaxEnt analysis methods to data exhibiting structure factor effects and low- q power law slopes and demonstrates their use in an in situ study of precipitate size evolution during heat treatment of a model Ni-Al-Si alloy.

  18. Texture evolution and microstructural changes during solid-state dewetting: A correlative study by complementary in situ TEM techniques

    International Nuclear Information System (INIS)

    Niekiel, Florian; Kraschewski, Simon M.; Schweizer, Peter; Butz, Benjamin; Spiecker, Erdmann

    2016-01-01

    The transition of a thin film into an energetically favorable set of particles at temperatures below the melting point of the bulk material is known as solid-state dewetting. In this work the dewetting behavior of 16 nm thick discontinuous Au thin films on amorphous silicon nitride membranes is quantitatively studied by complementary in situ transmission electron microscopy techniques taking advantage of the unique capabilities of a chip-based heating system. The combination of dedicated imaging and diffraction techniques is used to investigate the interplay of grain growth and texture evolution with the process of dewetting. The results show an initial coarsening of the microstructure preceding the other processes. Texture evolution is highly correlated to material retraction and agglomeration during the following dewetting process. In-plane grain rotation has been observed, acting as an additional mechanism for orientation changes. From a methodological perspective this work demonstrates the capabilities of today’s transmission electron microscopy in combination with state-of-the-art in situ instrumentation. In particular the combination of complementary information from different dedicated techniques in one and the same setup is demonstrated to be highly beneficial.

  19. Hydrodistillation and in situ microwave-generated hydrodistillation of fresh and dried mint leaves: a comparison study.

    Science.gov (United States)

    Orio, Laura; Cravotto, Giancarlo; Binello, Arianna; Pignata, Giuseppe; Nicola, Silvana; Chemat, Farid

    2012-12-01

    Hydrodistillation (HD) has been used since ancient times for the extraction of essential oils (EO). Despite the intrinsic limitations of this technique, it remains the most common method both in the laboratory and on an industrial scale. The main drawbacks are the long extraction time involved and the risk of thermal degradation. Over the last decade, microwave-assisted extraction (MAE) and in situ microwave-generated hydrodistillation (MGH) have been shown to be the most promising techniques in improving plant extraction and hydrodistillation. In this study we compare HD with MGH in the extraction of several mint species cultivated in Piedmont: Mentha spicata L. var. rubra, Mentha spicata L. var. viridis and Mentha piperita L. MGH requires either fresh plant or rehydrated material, it is extremely fast and allows a reduction in energy consumption and overall cost. All the EO have been analyzed by gas chromatography-mass spectrometry. A mechanism of microwave-generated essential oil extraction has been proposed to explain the differences in the composition of the oil obtained from this environmentally friendly technique. The yields and composition percentages of the EO obtained by HD and in situ MGH of fresh and dried mint leaves lie in a relatively narrow range, although MGH is faster. MW polarization effects and the water solubility of the components influence extract composition. Copyright © 2012 Society of Chemical Industry.

  20. Use of in situ FT-Raman spectroscopy to study the kinetics of the transformation of carbamazepine polymorphs.

    Science.gov (United States)

    O'Brien, Laura E; Timmins, Peter; Williams, Adrian C; York, Peter

    2004-10-29

    The solid-state transformation of carbamazepine from form III to form I was examined by Fourier Transform Raman spectroscopy. Using a novel environmental chamber, the isothermal conversion was monitored in situ at 130 degrees C, 138 degrees C, 140 degrees C and 150 degrees C. The rate of transformation was monitored by taking the relative intensities of peaks arising from two CH bending modes; this approach minimised errors due to thermal artefacts and variations in power intensities or scattering efficiencies from the samples in which crystal habit changed from a characteristic prism morphology (form III) to whiskers (form I). The solid-state transformation at the different temperatures was fitted to various solid-state kinetic models of which four gave good fits, thus indicating the complexity of the process which is known to occur via a solid-gas-solid mechanism. Arrhenius plots from the kinetic models yielded activation energies from 344 kJ mol(-1) to 368 kJ mol(-1) for the transformation. The study demonstrates the value of a rapid in situ analysis of drug polymorphic type which can be of value for at-line in-process control.

  1. In situ ESEM study of the thermal decomposition of chrysotile asbestos in view of safe recycling of the transformation product

    International Nuclear Information System (INIS)

    Gualtieri, Alessandro F.; Gualtieri, Magdalena Lassinantti; Tonelli, Massimo

    2008-01-01

    The thermal transformation of asbestos into non-hazardous crystalline phases and their recycling is a promising solution for the 'asbestos problem'. The most common asbestos-containing industrial material produced worldwide is cement-asbestos. Knowledge of the kinetics of thermal transformation of asbestos fibers in cement-asbestos is of paramount importance for the optimization of the firing process at industrial scale. Here, environmental scanning electron microscopy (ESEM) was used for the first time to follow in situ the thermal transformation of chrysotile fibers present in cement-asbestos. It was found that the reaction kinetics of thermal transformation of chrysotile was highly slowed down in the presence of water vapor in the experimental chamber with respect to He. This was explained by chemisorbed water on the surface of the fibers which affected the dehydroxylation reaction and consequently the recrystallization into Mg-silicates. In the attempt to investigate alternative and faster firing routes for the decomposition of asbestos, a low melting glass was mixed with cement-asbestos and studied in situ to assess to which extent the decomposition of asbestos is favored. It was found that the addition of a low melting glass to cement-asbestos greatly improved the decomposition reaction and decreased the transformation temperatures

  2. Use of multiple sensor technologies for quality control of in situ biogeochemical measurements: A SeaCycler case study

    Science.gov (United States)

    Atamanchuk, Dariia; Koelling, Jannes; Lai, Jeremy; Send, Uwe; Wallace, Douglas

    2017-04-01

    Over the last two decades observing capacity for the global ocean has increased dramatically. Emerging sensor technologies for dissolved gases, nutrients and bio-optical properties in seawater are allowing extension of in situ observations beyond the traditionally measured salinity, temperature and pressure (CTD). However the effort to extend observations using autonomous instruments and platforms carries the risk of losing the level of data quality achievable through conventional water sampling techniques. We will present results from a case study with the SeaCycler profiling winch focusing on quality control of the in-situ measurements. A total of 13 sensors were deployed from May 2016 to early 2017 on SeaCycler's profiling sensor float, including CTD, dissolved oxygen (O2, 3 sensors), carbon dioxide (pCO2, 2 sensors), nutrients, velocity sensors, fluorometer, transmissometer, single channel PAR sensor, and others. We will highlight how multiple measurement technologies (e.g. for O2 and CO2) complement each other and result in a high quality data product. We will also present an initial assessment of the bio-optical data, their implications for seasonal phytoplankton dynamics and comparisons to climatologies and ocean-color data products obtained from the MODIS satellite.

  3. An in situ grazing incidence x-ray scattering study of block copolymer thin films during solvent vapor annealing

    Science.gov (United States)

    Gu, Xiaodan; Gunkel, Ilja; Hexemer, Alexander; Russell, Thomas

    2014-03-01

    Although solvent vapor annealing (SVA) has been widely applied to block copolymer (BCP) thin films to obtain well-ordered microdomains, the mechanism of enhancing lateral order is not well understood. Here, we used real time in situ grazing-incidence small-angle x-ray scattering (in situGISAXS) to study the self-assembly of PS-b-P2VP BCP BCPs with different molecular weights thin films in THF vapor, a near neutral solvent for both blocks. Both swelling and deswelling behavior of BCP thin films were examined. The extent of swellingand the solvent removal rate not only affect the domain spacing of BCPs but also dictate the extent of lateral ordering of the BCP microdomains. Larger grains were observed at higher values of the swelling ratio (close to disordering). To preserve the maximal lateral ordering of the microdomains in the swollen state, the fastest solvent removal rate is required to freeze in the ordered microdomain structure of the swollen BCP film. We thanks support from U.S. Department of Energy BES under contract BES-DE-FG02-96ER45612 and ALS doctoral fellowship.

  4. Study of the Integration of LIDAR and Photogrammetric Datasets by in Situ Camera Calibration and Integrated Sensor Orientation

    Science.gov (United States)

    Mitishita, E.; Costa, F.; Martins, M.

    2017-05-01

    Photogrammetric and Lidar datasets should be in the same mapping or geodetic frame to be used simultaneously in an engineering project. Nowadays direct sensor orientation is a common procedure used in simultaneous photogrammetric and Lidar surveys. Although the direct sensor orientation technologies provide a high degree of automation process due to the GNSS/INS technologies, the accuracies of the results obtained from the photogrammetric and Lidar surveys are dependent on the quality of a group of parameters that models accurately the user conditions of the system at the moment the job is performed. This paper shows the study that was performed to verify the importance of the in situ camera calibration and Integrated Sensor Orientation without control points to increase the accuracies of the photogrammetric and LIDAR datasets integration. The horizontal and vertical accuracies of photogrammetric and Lidar datasets integration by photogrammetric procedure improved significantly when the Integrated Sensor Orientation (ISO) approach was performed using Interior Orientation Parameter (IOP) values estimated from the in situ camera calibration. The horizontal and vertical accuracies, estimated by the Root Mean Square Error (RMSE) of the 3D discrepancies from the Lidar check points, increased around of 37% and 198% respectively.

  5. STUDY OF THE INTEGRATION OF LIDAR AND PHOTOGRAMMETRIC DATASETS BY IN SITU CAMERA CALIBRATION AND INTEGRATED SENSOR ORIENTATION

    Directory of Open Access Journals (Sweden)

    E. Mitishita

    2017-05-01

    Full Text Available Photogrammetric and Lidar datasets should be in the same mapping or geodetic frame to be used simultaneously in an engineering project. Nowadays direct sensor orientation is a common procedure used in simultaneous photogrammetric and Lidar surveys. Although the direct sensor orientation technologies provide a high degree of automation process due to the GNSS/INS technologies, the accuracies of the results obtained from the photogrammetric and Lidar surveys are dependent on the quality of a group of parameters that models accurately the user conditions of the system at the moment the job is performed. This paper shows the study that was performed to verify the importance of the in situ camera calibration and Integrated Sensor Orientation without control points to increase the accuracies of the photogrammetric and LIDAR datasets integration. The horizontal and vertical accuracies of photogrammetric and Lidar datasets integration by photogrammetric procedure improved significantly when the Integrated Sensor Orientation (ISO approach was performed using Interior Orientation Parameter (IOP values estimated from the in situ camera calibration. The horizontal and vertical accuracies, estimated by the Root Mean Square Error (RMSE of the 3D discrepancies from the Lidar check points, increased around of 37% and 198% respectively.

  6. Flow-induced corrosion of absorbable magnesium alloy: In-situ and real-time electrochemical study

    International Nuclear Information System (INIS)

    Wang, Juan; Jang, Yongseok; Wan, Guojiang; Giridharan, Venkataraman; Song, Guang-Ling; Xu, Zhigang; Koo, Youngmi; Qi, Pengkai; Sankar, Jagannathan; Huang, Nan; Yun, Yeoheung

    2016-01-01

    Highlights: • An in-situ and real-time electrochemical monitoring of flow-induced corrosion of Mg alloy is designed in a vascular bioreactor. • Effect of hydrodynamics on corrosion kinetics, types, rates and products is analyzed. • Flow accelerates mass and electron transfer, leading to an increase in uniform and localized corrosions. • Flow increases not only the thickness of uniform corrosion product layer, but the removal rate of localized corrosion products. • Electrochemical impedance spectroscopy and linear polarization-measured polarization resistances provide a consistent correlation to corrosion rate calculated by computed tomography. - Abstract: An in-situ and real-time electrochemical study in a vascular bioreactor was designed to analyze corrosion mechanism of magnesium alloy (MgZnCa) under mimetic hydrodynamic conditions. Effect of hydrodynamics on corrosion kinetics, types, rates and products was analyzed. Flow-induced shear stress (FISS) accelerated mass and electron transfer, leading to an increase in uniform and localized corrosions. FISS increased the thickness of uniform corrosion layer, but filiform corrosion decreased this layer resistance at high FISS conditions. FISS also increased the removal rate of localized corrosion products. Impedance-estimated and linear polarization-measured polarization resistances provided a consistent correlation to corrosion rate calculated by computed tomography.

  7. In Situ complement activation and T-cell immunity in leprosy spectrum: An immunohistological study on leprosy lesional skin.

    Science.gov (United States)

    Bahia El Idrissi, Nawal; Iyer, Anand M; Ramaglia, Valeria; Rosa, Patricia S; Soares, Cleverson T; Baas, Frank; Das, Pranab K

    2017-01-01

    Mycobacterium leprae (M. leprae) infection causes nerve damage and the condition worsens often during and long after treatment. Clearance of bacterial antigens including lipoarabinomannan (LAM) during and after treatment in leprosy patients is slow. We previously demonstrated that M. leprae LAM damages peripheral nerves by in situ generation of the membrane attack complex (MAC). Investigating the role of complement activation in skin lesions of leprosy patients might provide insight into the dynamics of in situ immune reactivity and the destructive pathology of M. leprae. In this study, we analyzed in skin lesions of leprosy patients, whether M. leprae antigen LAM deposition correlates with the deposition of complement activation products MAC and C3d on nerves and cells in the surrounding tissue. Skin biopsies of paucibacillary (n = 7), multibacillary leprosy patients (n = 7), and patients with erythema nodosum leprosum (ENL) (n = 6) or reversal reaction (RR) (n = 4) and controls (n = 5) were analyzed. The percentage of C3d, MAC and LAM deposition was significantly higher in the skin biopsies of multibacillary compared to paucibacillary patients (p = leprosy patients (r = 0.9578, pleprosy patients (p = leprosy patients, suggesting that inflammation driven by complement activation might contribute to nerve damage in the lesions of these patients. This should be regarded as an important factor in M. leprae nerve damage pathology.

  8. Non-invasive in-situ investigations versus micro-sampling: a comparative study on a Renoirs painting

    International Nuclear Information System (INIS)

    Miliani, C.; Sgamellotti, A.; Universita degli Studi di Perugia . Centro di Eccellenza SMAArt; Scientific Methodologies applied to Archaeology and Art)

    2007-01-01

    In this paper, a multi-technique in-situ non-invasive approach has been followed for the study of the materials used for a painting by Pierre-Auguste Renoir, ''A woman at her toilette''. The study was carried out using five portable spectroscopic techniques, namely X-ray fluorescence, mid-infrared reflectance spectroscopy, near infrared reflectance spectroscopy, and UV-Vis spectroscopy in absorption and emission. The painting was selected as a case study because it was examined in advance of the current investigation using conventional micro-sampling techniques. This provided the opportunity to evaluate potential and limitations of the non-invasive approach to the complex case of the modern painting. (orig.)

  9. In situ ATR FTIR studies of SO4 adsorption on goethite in the presence of copper ions.

    Science.gov (United States)

    Beattie, D A; Chapelet, J K; Gräfe, M; Skinner, W M; Smith, E

    2008-12-15

    Despite the existence of many single ion sorption studies on iron and aluminum oxides, fewer studies have been reported that describe cosorption reactions. In this work, we present an in situ ATR FTIR study of synergistic adsorption of sulfate (SO4) and copper (Cu) on goethite, which is representative of the minerals and ions present in mine wastes, acid sulfate soils, and other industrial and agricultural settings. Sulfate adsorption was studied as a function of varying pH, and as a function of increasing concentration in the absence and presence of Cu. The presence of Cu ions in solution had a complex effect on the ability of SO4 ions to be retained on the goethite surface with increasing pH, with complete desorption occurring near pH 7 and 9 in the absence and presence of Cu, respectively. In addition, Cu ions altered the balance of inner vs outer sphere adsorbed SO4. The solid phase partitioning of SO4 at pH 3 and pH 5 was elevated by the presence of Cu; in both cases Cu increased the affinity of SO4 for the goethite surface. Complementary ex situ sorption edge studies of Cu on goethite in the absence and presence of SO4 revealed that the Cu adsorption edge shifted to lower pH (6.3 --> 5.6) in the presence of SO4, consistent with a decrease of the electrostatic repulsion between the goethite surface and adsorbing Cu. Based on the ATR FTIR and bulk sorption data we surmise that the cosorption products of SO4 and Cu at the goethite-water interface were not in the nature of ternary complexes under the conditions studied here. This information is critical for the evaluation of the onset of surface precipitates of copper-hydroxy sulfates as a function of pH and solution concentration.

  10. In-Situ Simulation

    DEFF Research Database (Denmark)

    Bjerregaard, Anders Thais; Slot, Susanne; Paltved, Charlotte

    2015-01-01

    , and organisational characteristic. Therefore, it might fail to fully mimic real clinical team processes. Though research on in situ simulation in healthcare is in its infancy, literature is abundant on patient safety and team training1. Patient safety reporting systems that identify risks to patients can improve......Introduction: In situ simulation offers on-site training to healthcare professionals. It refers to a training strategy where simulation technology is integrated into the clinical encounter. Training in the simulation laboratory does not easily tap into situational resources, e.g. individual, team...... patient safety if coupled with training and organisational support. This study explored the use of critical incidents and adverse events reports for in situ simulation and short-term observations were used to create learning objectives and training scenarios. Method: This study used an interventional case...

  11. Low temperature hydrogen plasma-assisted atomic layer deposition of copper studied using in situ infrared reflection absorption spectroscopy

    International Nuclear Information System (INIS)

    Chaukulkar, Rohan P.; Rai, Vikrant R.; Agarwal, Sumit; Thissen, Nick F. W.

    2014-01-01

    Atomic layer deposition (ALD) is an ideal technique to deposit ultrathin, conformal, and continuous metal thin films. However, compared to the ALD of binary materials such as metal oxides and metal nitrides, the surface reaction mechanisms during metal ALD are not well understood. In this study, the authors have designed and implemented an in situ reflection-absorption infrared spectroscopy (IRAS) setup to study the surface reactions during the ALD of Cu on Al 2 O 3 using Cu hexafluoroacetylacetonate [Cu(hfac) 2 ] and a remote H 2 plasma. Our infrared data show that complete ligand-exchange reactions occur at a substrate temperature of 80 °C in the absence of surface hydroxyl groups. Based on infrared data and previous studies, the authors propose that Cu(hfac) 2 dissociatively chemisorbs on the Al 2 O 3 surface, where the Al-O-Al bridge acts as the surface reactive site, leading to surface O-Cu-hfac and O-Al-hfac species. Surface saturation during the Cu(hfac) 2 half-cycle occurs through blocking of the available chemisorption sites. In the next half-reaction cycle, H radicals from an H 2 plasma completely remove these surface hfac ligands. Through this study, the authors have demonstrated the capability of in situ IRAS as a tool to study surface reactions during ALD of metals. While transmission and internal reflection infrared spectroscopy are limited to the first few ALD cycles, IRAS can be used to probe all stages of metal ALD starting from initial nucleation to the formation of a continuous film

  12. In situ FTIR and UV-visible spectroelectrochemical studies of iron nitrosyl porphyrins in nonaqueous media

    International Nuclear Information System (INIS)

    Mu, X.H.; Kadish, K.M.

    1988-01-01

    The techniques of in situ FTIR and UV-visible spectroelectrochemistry were combined with microvoltammetry in order to elucidate the prevailing mechanism for electrooxidation of (P)Fe(NO), where P is the dianion of tetraphenylporphyrin (TPP), meso-tetrakis(2,4,6-trimethylphenyl)porphyrin (TMP), or octaethylporphurin (OEP). Each metalloporphyrin undergoes three reversible oxidations at a Pt microelectrode of 25-μm diameter. These oxidations were examined with respect to the site of electron transfer and to the fate of the NO group on the time scales of thin-layer cyclic voltammetry and bulk controlled-potential electrolysis. The NO group remains coordinated to the Fe(III) center after electrooxidation of (P)Fe(NO) and a 166-187-cm -1 shift in NO vibration is observed upon going from (P)Fe(NO) to [(P)Fe(NO)] + in CH 2 Cl 2 , 0.1 M TMAP. However, the bound NO ligand dissociates from [(P)Fe(NO)] 2+ , which is electrogenerated at more positive potentials. The effects of bound halide ion or neutral ligand coordination on γ NO of [(P)Fe(NO)] + were also examined. γ NO of (P)Fe(NO)X, where X = Cl - , Br - , or I - , is linearly related to the ionization potential of HX while γ NO of [(P)Fe(NO)(S)] + (where S is a bound solvent molecule) is linearly correlated with the Gutmann solvent number (DN) of the trans-lighted solvent molecule in bulk CH 2 Cl 2

  13. Effect of dentifrice containing fluoride and/or baking soda on enamel demineralization/remineralization: an in situ study.

    Science.gov (United States)

    Cury, J A; Hashizume, L N; Del Bel Cury, A A; Tabchoury, C P

    2001-01-01

    The additive effect of baking soda on the anticariogenic effect of fluoride dentifrice is not well established. To evaluate it, a crossover in situ study was done in three phases of 28 days. Volunteers, using acrylic palatal appliances containing four human enamel blocks, two sound (to evaluate demineralization) and two with artificial caries lesions (to evaluate remineralization), took part in this study. During each phase, 10% sucrose solution was dripped (3 times a day) only onto the sound blocks. After 10 min, a slurry of placebo, fluoride (F) or fluoride and baking soda (F+NaHCO(3)) dentifrice was dripped onto all enamel blocks. The results showed a higher F concentration in dental plaque formed during treatment with F+NaHCO(3) than placebo (pbaking soda neither improves nor impairs the effect of F dentifrice on reduction of demineralization and enhancement of remineralization of enamel.

  14. Studies on In-situ Chelation/Supercritical Fluid Extraction of Lanthanides and Actinides Using a Radiotracer Technique

    International Nuclear Information System (INIS)

    Lin, Yuehe; Wu, Hong; Smart, Neil G.; Wai, Chien M.

    2001-01-01

    Radioisotope tracer techniques were used to study the process of in-situ chelation/supercritical fluid extraction(SFE) of La3+ and Lu3+ from solid matrix using mixed ligand hexafluoroacetylacetone (HFA) and tributylphosphate (TBP) as chelating agents. A lab-built SFE extactor was used in this study and the extractor design was optimized based on the experimental results. Quantitative recovery of La and Lu was achieved when the extrator design was optimized. Extraction of uranium from real world samples was also investigated to demonstrate the capability of this chelation/SFE technology for environmental remediation applications. A novel on-line back extraction technique for the recovery of metal ions and regeneration of ligands is also reported.

  15. High-temperature dehydration of talc: a kinetics study using in situ X-ray powder diffraction

    Science.gov (United States)

    Wang, Duojun; Yi, Li; Huang, Bojin; Liu, Chuanjiang

    2015-06-01

    High-temperature in situ X-ray powder diffraction patterns were used to study the dehydration kinetics of natural talc with a size of 10-15 µm. The talc was annealed from 1073 to 1223 K, and the variations in the characteristic peaks corresponding to talc with the time were recorded to determine the reaction progress. The decomposition of talc occurred, and peaks corresponding to talc and peaks corresponding to enstatite and quartz were observed. The enstatite and talc exhibited a topotactic relationship. The dehydration kinetics of talc was studied as a function of temperature between 1073 and 1223 K. The kinetics data could be modeled using an Avrami equation that considers nucleation and growth processes ? where n varies from 0.4 to 0.8. The rate constant (k) equation for the natural talc is ? The reaction mechanism for the dehydration of talc is a heterogeneous nucleation and growth mechanism.

  16. Establishment of 60Co dose calibration curve using fluorescent in situ hybridization assay technique: Result of preliminary study

    International Nuclear Information System (INIS)

    Rahimah Abdul Rahim; Noriah Jamal; Noraisyah Mohd Yusof; Juliana Mahamad Napiah; Nelly Bo Nai Lee

    2010-01-01

    This study aims at establishing an in-vitro 60 Co dose calibration curve using Fluorescent In-Situ Hybridization assay technique for the Malaysian National Bio dosimetry Laboratory. Blood samples collected from a female healthy donor were irradiated with several doses of 60 Co radiation. Following culturing of lymphocytes, microscopic slides are prepared, denatured and hybridized. The frequencies of translocation are estimated in the metaphases. A calibration curve was then generated using a regression technique. It shows a good fit to a linear-quadratic model. The results of this study might be useful in estimating absorbed dose for the individual exposed to ionizing radiation retrospectively. This information may be useful as a guide for medical treatment for the assessment of possible health consequences. (author)

  17. In-situ early stage electromigration study in Al line using synchrotron polychromatic X-ray microdiffraction

    International Nuclear Information System (INIS)

    Chen, Kai; Tamura, Nobumichi; Tu, King-Ning

    2007-01-01

    Electromigration is a phenomenon that has attracted much attention in the semiconductor industry because of its deleterious effects on electronic devices (such as interconnects) as they become smaller and current density passing through them increases. However, the effect of the electric current on the microstructure of interconnect lines during the very early stage of electromigration is not well documented. In the present report, we used synchrotron radiation based polychromatic X-ray microdiffraction for the in-situ study of the electromigration induced plasticity effects on individual grains of an Al (Cu) interconnect test structure. Dislocation slips which are activated by the electric current stressing are analyzed by the shape change of the diffraction peaks. The study shows polygonization of the grains due to the rearrangement of geometrically necessary dislocations (GND) in the direction of the current. Consequences of these findings are discussed

  18. In-situ early stage electromigration study in Al line using synchrotron polychromatic X-ray microdiffraction

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Kai; Tamura, Nobumichi; Tu, King-Ning

    2007-10-31

    Electromigration is a phenomenon that has attracted much attention in the semiconductor industry because of its deleterious effects on electronic devices (such as interconnects) as they become smaller and current density passing through them increases. However, the effect of the electric current on the microstructure of interconnect lines during the very early stage of electromigration is not well documented. In the present report, we used synchrotron radiation based polychromatic X-ray microdiffraction for the in-situ study of the electromigration induced plasticity effects on individual grains of an Al (Cu) interconnect test structure. Dislocation slips which are activated by the electric current stressing are analyzed by the shape change of the diffraction peaks. The study shows polygonization of the grains due to the rearrangement of geometrically necessary dislocations (GND) in the direction of the current. Consequences of these findings are discussed.

  19. The Development of an In-Situ TEM Technique for Studying Corrosion Behavior as Applied to Zirconium-Based Alloys

    Science.gov (United States)

    Harlow, Wayne

    Zirconium-based alloys are a commonly used material for nuclear fuel rod cladding, due to its low neutron cross section and good corrosion properties. However, corrosion is still a limiting factor in fuel rod lifespan, which restricts burn up levels, and thus efficiency, that can be achieved. While long-term corrosion behavior has been studied through both reactor and autoclave samples, the oxide nucleation and growth behavior has not been extensively studied. This work develops a new technique to study the initial stages of corrosion in zirconium-based alloys and the microstructural effects on this process by developing an environmental cell system for the TEM. Nanoscale oxidation parameters are developed, as is a new FIB technique to support this method. Precession diffraction is used in conjunction with in-situ TEM to observe the initial stages of corrosion in these alloys, and oxide thickness is estimated using low-loss EELS. In addition, the stress stabilization of tetragonal ZrO 2 is explored in the context of sample preparation for TEM. It was found that in-situ environmental TEM using an environmental cell replicates the oxidation behavior observed in autoclaved samples in both oxide structure and phases. Utilizing this technique, it was shown that cracking of the oxide layer in zirconium-based alloys is related to oxide relaxation, and not thermal changes. The effect of secondary phase particles on oxidation behavior did not present significant results, however a new method for studying initial oxidation rates using low-loss EELS was developed.

  20. Some properties of Ga-As-Alsub(x)Gasub(1-x)As heterojunction grown by low temperature liquid phase epitaxy

    International Nuclear Information System (INIS)

    Yu Lisheng; Liu Hongxun; Zhang Bei; Wang Shumin

    1986-03-01

    GaAs-Alsub(x)Gasub(1-x)As heterojunction was grown by liquid phase epitaxy at low growth temperature 650-700 deg. C. The series resistance of heterojunction with DH laser structure was measured. Doping properties of Mg in GaAs and Alsub(x)Gasub(1-x)As were investigated. It is found that impurity concentration of Mg as high as 10 18 cm -3 can be doped easily. The Shubnikov-de-Haas oscillation was observed in GaAs-N Alsub(0.35)Gasub(0.65)As heterointerface. It is demonstrated that in these heterointerfaces there exists 2DEG with some contribution from 3D electron of N-AlGaAs layer. (author)

  1. Multiscale structural characterizations of mixed U(iv)-An(iii) oxalates (An(iii) = Pu or Am) combining XAS and XRD measurements.

    Science.gov (United States)

    Arab-Chapelet, B; Martin, P M; Costenoble, S; Delahaye, T; Scheinost, A C; Grandjean, S; Abraham, F

    2016-04-28

    Mixed actinide(III,IV) oxalates of the general formula M2.2UAn(C2O4)5·nH2O (An = Pu or Am and M = H3O(+) and N2H5(+)) have been quantitatively precipitated by oxalic precipitation in nitric acid medium (yield >99%). Thorough multiscale structural characterization using XRD and XAS measurements confirmed the existence of mixed actinide oxalate solid solutions. The XANES analysis confirmed that the oxidation states of the metallic cations, tetravalent for uranium and trivalent for plutonium and americium, are maintained during the precipitation step. EXAFS measurements show that the local environments around U(+IV), Pu(+III) and Am(+III) are comparable, and the actinides are surrounded by ten oxygen atoms from five bidentate oxalate anions. The mean metal-oxygen distances obtained by XAS measurements are in agreement with those calculated from XRD lattice parameters.

  2. The time-resolved and extreme conditions XAS (TEXAS) facility at the European Synchrotron Radiation Facility: the general-purpose EXAFS bending-magnet beamline BM23.

    Science.gov (United States)

    Mathon, O; Beteva, A; Borrel, J; Bugnazet, D; Gatla, S; Hino, R; Kantor, I; Mairs, T; Munoz, M; Pasternak, S; Perrin, F; Pascarelli, S

    2015-11-01

    BM23 is the general-purpose EXAFS bending-magnet beamline at the ESRF, replacing the former BM29 beamline in the framework of the ESRF upgrade. Its mission is to serve the whole XAS user community by providing access to a basic service in addition to the many specialized instruments available at the ESRF. BM23 offers high signal-to-noise ratio EXAFS in a large energy range (5-75 keV), continuous energy scanning for quick-EXAFS on the second timescale and a micro-XAS station delivering a spot size of 4 µm × 4 µm FWHM. It is a user-friendly facility featuring a high degree of automation, online EXAFS data reduction and a flexible sample environment.

  3. In Situ and Ex Situ Studies of Molybdenum Thin Films Deposited by rf and dc Magnetron Sputtering as a Back Contact for CIGS Solar Cells

    Directory of Open Access Journals (Sweden)

    K. Aryal

    2012-01-01

    Full Text Available Molybdenum thin films were deposited by rf and dc magnetron sputtering and their properties analyzed with regards to their potential application as a back contact for CIGS solar cells. It is shown that both types of films tend to transition from tensile to compressive strain when the deposition pressure increases, while the conductivity and the grain size decreas. The nucleation of the films characterized by in situ and real time spectroscopic ellipsometry shows that both films follow a Volmer-Weber growth, with a higher surface roughness and lower deposition rate for the rf deposited films. The electronic relaxation time was then extracted as a function of bulk layer thickness for rf and dc films by fitting each dielectric function to a Drude free-electron model combined with a broad Lorentz oscillator. The values were fitted to a conical growth mode and demonstrated that the rf-deposited films have already smaller grains than the dc films when the bulk layer thickness is 30 nm.

  4. In-situ Study of Dynamic Phenomena at Metal Nanosolder Interfaces Using Aberration Corrected Scanning Transmission Electron Microcopy.

    Energy Technology Data Exchange (ETDEWEB)

    Lu, Ping

    2014-10-01

    Controlling metallic nanoparticle (NP) interactions plays a vital role in the development of new joining techniques (nanosolder) that bond at lower processing temperatures but remain viable at higher temperatures. The pr imary objective of this project is t o develop a fundamental understanding of the actual reaction processes, associated atomic mechanisms, and the resulting microstructure that occur during thermally - driven bond formation concerning metal - metal nano - scale (%3C50nm) interfaces. In this LDRD pr oject, we have studied metallic NPs interaction at the elevated temperatures by combining in - situ transmission electron microscopy (TEM ) using an aberration - corrected scanning transmission electron microscope (AC - STEM) and atomic - scale modeling such as m olecular dynamic (MD) simulations. Various metallic NPs such as Ag, Cu and Au are synthesized by chemical routines. Numerous in - situ e xperiments were carried out with focus of the research on study of Ag - Cu system. For the first time, using in - situ STEM he ating experiments , we directly observed t he formation of a 3 - dimensional (3 - D) epitaxial Cu - Ag core - shell nanoparticle during the thermal interaction of Cu and Ag NPs at elevated temperatures (150 - 300 o C). The reaction takes place at temperatures as low as 150 o C and was only observed when care was taken to circumvent the effects of electron beam irradiation during STEM imaging. Atomic - scale modeling verified that the Cu - Ag core - shell structure is energetically favored, and indicated that this phenomenon is a nano - scale effect related to the large surface - to - volume ratio of the NPs. The observation potentially can be used for developing new nanosolder technology that uses Ag shell as the "glue" that stic ks the particles of Cu together. The LDRD has led to several journal publications and numerous conference presentations, and a TA. In addition, we have developed new TEM characterization techniques and phase

  5. Determination of HER2 amplification in primary breast cancer using dual-colour chromogenic in situ hybridization is comparable to fluorescence in situ hybridization: a European multicentre study involving 168 specimens

    Science.gov (United States)

    García-Caballero, Tomás; Grabau, Dorthe; Green, Andrew R; Gregory, John; Schad, Arno; Kohlwes, Elke; Ellis, Ian O; Watts, Sarah; Mollerup, Jens

    2010-01-01

    García-Caballero T, Grabau D, Green A R, Gregory J, Schad A, Kohlwes E, Ellis I O, Watts S & Mollerup J (2010) Histopathology56, 472–480 Determination of HER2 amplification in primary breast cancer using dual-colour chromogenic in situ hybridization is comparable to fluorescence in situ hybridization: a European multicentre study involving 168 specimens Aims: Fluorescence in situ hybridization (FISH) can be used to reveal several genomic imbalances relevant to proper cancer diagnosis and to the correct treatment regime. However, FISH requires expensive and advanced fluorescence microscopes in addition to expertise in fluorescence microscopy. To determine whether a newly developed dual-colour chromogenic in situ hybridization (CISH) method is a suitable alternative to FISH, we analysed the human epidermal growth factor receptor 2 gene (HER2) amplification level of 168 breast cancer specimens using dual-colour CISH and FISH and compared the results. Methods and results: We found 100% agreement between HER2 status determined by FISH and dual-colour CISH. Furthermore, we observed that the time used to score slides was significantly reduced by 28% in dual-colour CISH compared with the FISH protocol. Concordance between HER2 protein status and dual-colour CISH or FISH was equally good with an overall agreement of 96.8%. Correlation between the HER2/centromere 17 gene ratios obtained with dual-colour CISH and FISH was highly significant with an overall correlation coefficient (ρ) of 0.96. Conclusions: We conclude that dual-colour CISH and bright field microscopy are excellent alternatives to FISH when analysing the HER2 status of primary breast cancer. PMID:20459554

  6. Towards optimization of experimental parameters for studying Li-O2 battery discharge products in TEM using in situ EELS.

    Science.gov (United States)

    Basak, Shibabrata; Jansen, Jacob; Kabiri, Yoones; Zandbergen, Henny W

    2018-05-01

    The key to understanding the performance of Li-O 2 batteries is to study the chemical and structural properties of their discharge product(s) at the nanometer scale. Using TEM for this purpose poses challenges due to the sensitivity of samples to air and electron beams. This paper describes our use of in situ EELS to evaluate experimental procedures to reduce electron-beam degradation and presents methods to deal with air sensitivity. Our results show that Li 2 O 2 decomposition is dependent on the total dose and is approximately 4-5 times more pronounced at 80 than at 200 kV. We also demonstrate the benefits of using low-dose-rate STEM. We show further that a "graphene cell", which encapsulates the sample within graphene sheets, can protect the sample against air and e-beam damage. Copyright © 2018 Elsevier B.V. All rights reserved.

  7. In situ Raman scattering study on a controllable plasmon-driven surface catalysis reaction on Ag nanoparticle arrays

    International Nuclear Information System (INIS)

    Dai, Z G; Xiao, X H; Zhang, Y P; Ren, F; Wu, W; Zhang, S F; Zhou, J; Jiang, C Z; Mei, F

    2012-01-01

    Control of the plasmon-driven chemical reaction for the transformation of 4-nitrobenzenethiol to p,p′-dimercaptoazobenzene by Ag nanoparticle arrays was studied. The Ag nanoparticle arrays were fabricated by means of nanosphere lithography. By changing the PS particle size, the localized surface plasmon resonance (LSPR) peaks of the Ag nanoparticle arrays can be tailored from 460 to 560 nm. The controlled reaction process was monitored by in situ surface-enhanced Raman scattering. The reaction can be dramatically influenced by varying the duration of laser exposure, Ag nanoparticle size, laser power and laser excitation wavelength. The maximum reaction speed was achieved when the LSPR wavelength of the Ag nanoparticle arrays matched the laser excitation wavelength. The experimental results reveal that the strong LSPR can effectively drive the transfer of the ‘hot’ electrons that decay from the plasmon to the reactants. The experimental results were confirmed by theoretical calculations. (paper)

  8. A study of the kinetics and mechanisms of electrocrystallization of indium oxide on an in situ prepared metallic indium electrode

    International Nuclear Information System (INIS)

    Omanovic, S.; Metikos-Hukovic, M.

    2004-01-01

    The mechanisms and kinetics of nucleation and growth of indium oxide film on an in situ prepared metallic indium electrode was studied in a borate buffer solution of pH 10.0 using cyclic voltammetry and chroanoamperometry techniques. It was shown that the initial stage of nucleation of the oxide film includes a three-dimensional progressive nucleation process, combined with a diffusion-controlled growth of the stable indium oxide crystals. The thermodynamic data obtained indicated a strong tendency of indium to form an indium oxide film on its surface in an aqueous solution. It was found that the rate-determining step in the nucleation and growth process is the surface diffusion of electroactive species. The nucleation rate constant, and the number of nucleation active sites were calculated independently. It was shown that between 2 and 15% of sites on the indium surface act as active nucleation centers, and that each active site represents a critical nucleus

  9. In-situ cosmogenic 10Be and 36Cl studies in the earth sciences at the ANTARES AMS facility

    International Nuclear Information System (INIS)

    Fink, D.; Elliott, G.; Child, D.; Misfud, C.

    1998-01-01

    In parallel with a successful 14 C AMS program, routine measurements of 10 Be (T 1/2 = 1.5 Ma), 26 Al (0.7Ma) and 36 Cl (0.3Ma) have been demonstrated at the ANTARES AMS facility. With this capability, ANSTO is coordinating and funding a comprehensive program in the application of in-situ cosmogenic radioisotopes for Southern Hemisphere Quaternary climate change. The sub-projects within the program are based on strong university collaboration in the Earth Sciences and with the Australian Antarctic Division. A fully equipped geochemistry laboratory for chemically processing rock samples for AMS studies has been completed and is fully operational. In addition a variety of analytical techniques such as NAA, ICP-MS, XRF, XRD, etc are available through the Environment Division at ANSTO. A brief description of the research projects in glacial chronology and those related to landscape geomorphology is given

  10. In-situ STM study of phosphate adsorption on Cu(111), Au(111) and Cu/Au(111) electrodes

    DEFF Research Database (Denmark)

    Schlaup, Christian; Horch, Sebastian

    2013-01-01

    The interaction of Cu(111), Au(111) and Cu-covered Au(111) electrodes with a neutral phosphate buffer solution has been studied by means of cyclic voltammetry (CV) and in situ electrochemical scanning tunneling microscopy (EC-STM). Under low potential conditions, both the Cu(111) and the Au(111......) surface appear apparently adsorbate free, indicated by the presence of a (4×4) structure and the herringbone surface reconstruction, respectively. Upon potential increase, phosphate anions adsorb on both surfaces and for Cu(111) the formation of a (√3×√3)R30° structure is found, whereas on Au(111) a "(√3......×√7)" structure is formed. For a Cu-submonolayer on Au(111), coadsorption of phosphate anions leads to the formation of a (2×2) vacancy structure within an assumed pseudomorphic structure of the Cu-submonolayer with the phosphate anions occupying the vacancies. When desorbing the phosphate anions at low...

  11. In-situ metallography for damage assessment and life extension in power plants- a few case studies

    International Nuclear Information System (INIS)

    Raghu, N.; Muralidharan, N.G.; Jayakumar, T.; Kasiviswanathan, K.V.

    1996-01-01

    In-service inspection of components in power plants is necessary for damage assessment, life prediction and extension. The useful life of some of the components like pipelines are most crucial in case they are exposed to the conditions of high temperature and pressure. Periodic inservice inspection by means of non-destructive testing to obtain information on damage assessment is carried out as a routine and mandatory procedure. During these inspections, only reduction in localised and uniform wall thickness are measured. However, the microstructural degradation due to both normal and abnormal temperatures occurring conditions are not revealed by conventional non-destructive test methods during this routine inspection. For life prediction and extension programme, the information on microstructural degradation is essential and the same can be studies in an effective manner through in-situ metallography technique. (author)

  12. Flow-induced corrosion of absorbable magnesium alloy: In-situ and real-time electrochemical study

    Science.gov (United States)

    Wang, Juan; Jang, Yongseok; Wan, Guojiang; Giridharan, Venkataraman; Song, Guang-Ling; Xu, Zhigang; Koo, Youngmi; Qi, Pengkai; Sankar, Jagannathan; Huang, Nan; Yun, Yeoheung

    2016-01-01

    An in-situ and real-time electrochemical study in a vascular bioreactor was designed to analyze corrosion mechanism of magnesium alloy (MgZnCa) under mimetic hydrodynamic conditions. Effect of hydrodynamics on corrosion kinetics, types, rates and products was analyzed. Flow-induced shear stress (FISS) accelerated mass and electron transfer, leading to an increase in uniform and localized corrosions. FISS increased the thickness of uniform corrosion layer, but filiform corrosion decreased this layer resistance at high FISS conditions. FISS also increased the removal rate of localized corrosion products. Impedance-estimated and linear polarization-measured polarization resistances provided a consistent correlation to corrosion rate calculated by computed tomography. PMID:28626241

  13. Study of water masses variability in the Mediterranean Sea using in-situ data / NEMO-Med12 model.

    Science.gov (United States)

    Margirier, Félix; Testor, Pierre; Mortier, Laurent; Arsouze, Thomas; Bosse, Anthony; Houpert, Loic; Hayes, Dan

    2016-04-01

    In the past 10 years, numerous observation programs in the Mediterranean deployed autonomous platforms (moorings, argo floats, gliders) and thus considerably increased the number of in-situ observations and the data coverage. In this study, we analyse time series built with profile data on interannual scales. Sorting data in regional boxes, we follow the evolution of different water masses in the basin and generate indexes to characterize their evolution. We then put those indexes in relation with external (atmospheric) forcings and present an intercomparison with the NEMO-Med12 model to estimate both the skill of the model and the relevance of the data-sampling in reproducing the evolution of water masses properties.

  14. In-situ radiation grafting of polymer films and degradation studies of monomers for applications in fuel cell membranes

    Energy Technology Data Exchange (ETDEWEB)

    Mitov, S.

    2007-02-15

    The present work consists of three parts which deal with the optimization of the properties of polymers finding application as proton exchange membranes in PEMFCs. The focus is the oxidative and photochemical stability of non-fluorinated polymer membranes, as well as the radiation-induced grafting of commercially available fluoropolymer films. The use of the ESR technique is common for the first two parts of the dissertation. ESR spectroscopy is the major method of study, because of its sensitivity and specificity for the detection of radical intermediates. It is a suitable spectroscopic technique to identify the nature of radiation generated radicals in organic polymers, and to monitor their concentration in-situ during the grafting process. The third part comprises the results and discussions of DFT calculations for non-fluorinated and fluorinated fragments.

  15. Magnetotransport study of in situ magnetic field textured Dy1Ba2Cu3O7-δ superconductors

    International Nuclear Information System (INIS)

    Pekala, M.; Liege Univ.; Cloots, R.; Liege Univ.; Bougrine, H.; Liege Univ.; Maka, E.; Ausloos, M.

    1995-01-01

    The electrical resistivity, thermoelectric power and the Nernst effect have been studied as a function of temperature and magnetic field for a typical superconductor DyBa 2 Cu 3 O 7-δ magnetically textured in situ at 1035 C. The three transport coefficients show hybrid microscopic features. In particular, we show the anisotropy with respect to the field direction (H // a, H // c) in all transport coefficients. We verify that Tinkham's law is obeyed for the broadening of the resistive transition in a magnetic field. Similarly we obtain anisotropic broadening exponents for each integrated excess property. From Arrhenius plots we obtain orders of magnitude for the activation energies characterizing each property. They are markedly different from each other. (orig.)

  16. In situ XRD study of C60 polymerisation above pressures of 9 GPa and temperatures up to 830K

    International Nuclear Information System (INIS)

    Talyzin, A.V.; Jansson, U.; Dubrovinsky, L.S.; Oden, M.; Le Bihan, T.

    2002-01-01

    The C60 polymerization was studied by X-ray diffraction in situ in the pressure range 13-18 GPa and at temperatures up to 830 K. The results of the high pressure high temperature treatment are strongly dependent from the history of the sample and stress. At certain conditions no elliptical diffraction patterns were observed at 13 GPa and 830K. Samples with a relatively low internal stress showed a transformation to new phase. It is suggested that this phase is three-dimensional polymer with each C60 molecule bonded to eight neighbors. This phase showed an increased hardness (about 37 GPa) and a Raman spectrum distinctly different from previously known polymeric phases

  17. Morphological study and thermal analysis of surface modified α-FeOOH via in situ polymerization of methyl methacrylate

    International Nuclear Information System (INIS)

    Han Yaoxing; Ma Xinsheng; Cao Hongming; Zhang Haiying; Wu Qiufang

    2004-01-01

    Considering the interfacial characteristics of goethite (α-FeOOH, iron oxide yellow), the in situ polymerization of methyl methacrylate was employed to modify the surfaces of α-FeOOH pigments in aqueous slurry. The scanning electron micrographs indicated that the poly(methyl methacrylate) anchored on the surfaces of the particle homogeneously. From this study, it was found that one of the key requirements in the synthesis of the α-FeOOH-PMMA composite was to enhance interfacial compatibility between inorganic particles and organic monomer. Moreover, polymer-treated α-FeOOH particles were easily dispersed in organic medium to form a stable colloid and the heat resistance of α-FeOOH particles was improved

  18. In-situ PXRD Study on the Annealing of SrFe12O19 Nano Particles

    DEFF Research Database (Denmark)

    Gjørup, Frederik; Saura-Múzquiz, Matilde; Christensen, Mogens

    Nano sized strontium hexaferrite is synthesized using a hydrothermal flow synthesis, at temperature and pressure above waters critical point. The nano particles are hexagonal platelets, with the easy axis of magnetization along the short c-axis of the platelet. The nano powders are normally pressed...... and annealed to form mechanically stable pellets. This study uses In-situ Powder X-Ray Diffraction (PXRD) to examine the particle growth during annealing of the powder, with emphasis on the ratio between the axes of the platelets (a/c-ratio). By applying an external magnetic field before annealing......, the particles will align along the field lines of the external magnet, and the contact surfaces along the c-axis should increase. It will be examined whether the external magnetic field increases the growth along the c-axis relative to the a/b-axis, compared to annealing without prior magnetization....

  19. Nitrogen budget of the northwestern Black Sea shelf inferred from modeling studies and in situ benthic measurements

    NARCIS (Netherlands)

    Grégoire, M.; Friedrich, J.

    2004-01-01

    A 3D eddy-resolving coupled biogeochemical-hydrodynamical model and in situ observations are used to investigate benthic processes on the Black Sea's NW shelf. Measurements of benthic fluxes (oxygen, nutrients, redox compounds) with in situ flux chambers are analyzed in regard to sediment dynamics

  20. Metal and ligand K-edge XAS of organotitanium complexes: metal 4p and 3d contributions to pre-edge intensity and their contributions to bonding.

    Science.gov (United States)

    George, Serena DeBeer; Brant, Patrick; Solomon, Edward I

    2005-01-19

    Titanium cyclopentadienyl (Cp) complexes play important roles as homogeneous polymerization catalysts and have recently received attention as potential anticancer agents. To systematically probe the contribution of the Cp to bonding in organotitanium complexes, Ti K-edge XAS has been applied to TiCl(4) and then to the mono- and bis-Cp complexes, TiCpCl(3) and TiCp(2)Cl(2). Ti K-edge XAS is used as a direct probe of metal 3d-4p mixing and provides insight into the contribution of the Cp to bonding. These data are complimented by Cl K-edge XAS data, which provide a direct probe of the effect of the Cp on the bonding to the spectator chloride ligand. The experimental results are correlated to DFT calculations. A model for metal 3d-4p mixing is proposed, which is based on covalent interactions with the ligands and demonstrates that metal K-pre-edge intensities may be used as a measure of ligand-metal covalency in molecular Ti(IV) systems in noncentrosymmetric environments.

  1. Improved Skin Penetration Using In Situ Nanoparticulate Diclofenac Diethylamine in Hydrogel Systems: In Vitro and In Vivo Studies.

    Science.gov (United States)

    Sengupta, Soma; Banerjee, Sarita; Sinha, Biswadip; Mukherjee, Biswajit

    2016-04-01

    Delivering diclofenac diethylamine transdermally by means of a hydrogel is an approach to reduce or avoid systemic toxicity of the drug while providing local action for a prolonged period. In the present investigation, a process was developed to produce nanosize particles (about 10 nm) of diclofenac diethylamine in situ during the development of hydrogel, using simple mixing technique. Hydrogel was developed with polyvinyl alcohol (PVA) (5.8% w/w) and carbopol 71G (1.5% w/w). The formulations were evaluated on the basis of field emission scanning electron microscopy, texture analysis, and the assessment of various physiochemical properties. Viscosity (163-165 cps for hydrogel containing microsize drug particles and 171-173 cps for hydrogel containing nanosize drug particles, respectively) and swelling index (varied between 0.62 and 0.68) data favor the hydrogels for satisfactory topical applications. The measured hardness of the different hydrogels was uniform indicating a uniform spreadability. Data of in vitro skin (cadaver) permeation for 10 h showed that the enhancement ratios of the flux of the formulation containing nanosize drug (without the permeation enhancer) were 9.72 and 1.30 compared to the formulation containing microsized drug and the marketed formulations, respectively. In vivo plasma level of the drug increased predominantly for the hydrogel containing nanosize drug-clusters. The study depicts a simple technique for preparing hydrogel containing nanosize diclofenac diethylamine particles in situ, which can be commercially viable. The study also shows the advantage of the experimental transdermal hydrogel with nanosize drug particles over the hydrogel with microsize drug particles.

  2. Combining a coupled FTIR-EGA system and in situ DRIFTS for studying soil organic matter in arable soils

    Directory of Open Access Journals (Sweden)

    M. S. Demyan

    2013-05-01

    Full Text Available An optimized spectroscopic method combining quantitative evolved gas analysis via Fourier transform infrared spectroscopy (FTIR-EGA in combination with a qualitative in situ thermal reaction monitoring via diffuse reflectance Fourier transform infrared spectroscopy (in situT DRIFTS is being proposed to rapidly characterize soil organic matter (SOM to study its dynamics and stability. A thermal reaction chamber coupled with an infrared gas cell was used to study the pattern of thermal evolution of carbon dioxide (CO2 in order to relate evolved gas (i.e., CO2 to different qualities of SOM. Soil samples were taken from three different arable sites in Germany: (i the Static Fertilization Experiment, Bad Lauchstädt (Chernozem, from treatments of farmyard manure (FYM, mineral fertilizer (NPK, their combination (FYM + NPK and control without fertilizer inputs; (ii Kraichgau; and (iii Swabian Alb (Cambisols areas, Southwest Germany. The two latter soils were further fractionated into particulate organic matter (POM, sand and stable aggregates (Sa + A, silt and clay (Si + C, and NaOCl oxidized Si + C (rSOC to gain OM of different inferred stabilities; respiration was measured from fresh soil samples incubated at 20 °C and 50% water holding capacity for 490 days. A variable long path length gas cell was used to record the mid-infrared absorbance intensity of CO2 (2400 to 2200 cm−1 being evolved during soil heating from 25 to 700 °C with a heating rate of 68 °C min−1 and holding time of 10 min at 700 °C. Separately, the heating chamber was placed in a diffuse reflectance chamber (DRIFTS for measuring the mid-infrared absorbance of the soil sample during heating. Thermal stability of the bulk soils and fractions was measured via the temperature of maximum CO2 evolution (CO2max. Results indicated that the FYM + NPK and FYM treatments of the Chernozem soils had a lower CO2max as compared to both NPK and CON treatments. On average, CO2max of the

  3. Chromogenic in situ hybridisation for the assessment of HER2 status in breast cancer: an international validation ring study

    Science.gov (United States)

    van de Vijver, Marc; Bilous, Michael; Hanna, Wedad; Hofmann, Manfred; Kristel, Petra; Penault-Llorca, Frédérique; Rüschoff, Josef

    2007-01-01

    Introduction Before any new methodology can be introduced into the routine diagnostic setting it must be technically validated against the established standards. To this end, a ring study involving five international pathology laboratories was initiated to validate chromogenic in situ hybridisation (CISH) against fluorescence in situ hybridisation (FISH) and immunohistochemistry (IHC) as a test for assessing human epidermal growth factor receptor 2 (HER2) status in breast cancer. Methods Each laboratory performed CISH, FISH and IHC on its own samples. Unstained sections from each case were also sent to another participating laboratory for blinded retesting by CISH ('outside CISH'). Results A total of 211 invasive breast carcinoma cases were tested. In 76 cases with high amplification (HER2/CEP17 ratio >4.0) by FISH, 73 cases (96%) scored positive (scores ≥ 6) by 'outside CISH'. For FISH-negative cases (HER2/CEP17 ratio CISH scores indicating no amplification (score ≤ 5), and only three cases were positive by CISH; in the three remaining cases, no CISH result could be obtained. For cases with low-level amplification using FISH (HER2/CEP17 ratio 2.0–4.0), 20 of 35 had CISH scores indicating gene amplification. Inter-laboratory concordance was also very high: 95% for normal HER2 copy number (1–5 copies); and 92% for cases with HER2 copy numbers ≥ 6. CISH intra-laboratory concordance with IHC was 92% for IHC-negative cases (IHC 0/1+) and 91% for IHC 3+ cases. Among IHC 2+ cases, CISH was 100% concordant with samples showing high amplification by FISH, and 94% concordant with FISH-negative samples. Conclusion These results show that CISH inter- and intra-laboratory concordance to FISH and IHC is very high, even in equivocal IHC 2+ cases. Therefore, we conclude that CISH is a methodology that is a viable alternative to FISH in the HER2 testing algorithm. PMID:17922920

  4. In-situ XRD study of alloyed Cu2ZnSnSe4-CuInSe2 thin films for solar cells

    International Nuclear Information System (INIS)

    Hartnauer, Stefan; Wägele, Leonard A.; Jarzembowski, Enrico; Scheer, Roland

    2015-01-01

    We investigate the growth of Cu 2 ZnSnSe 4 -CuInSe 2 (CZTISe) thin films using a 2-stage (Cu-rich/Cu-free) co-evaporation process under simultaneous application of in-situ angle dispersive X-ray diffraction (XRD). In-situ XRD allows monitoring the phase formation during preparation. A variation of the content of indium in CZTISe leads to a change in the lattice constant. Single phase CZTISe is formed in a wide range, while at high In contents a phase separation is detected. Because of different thermal expansion coefficients, the X-ray diffraction peaks of ZnSe and CZTISe can be distinguished at elevated substrate temperatures. The formation of ZnSe appears to be inhibited even for low indium content. In-situ XRD shows no detectable sign for the formation of ZnSe. First solar cells of CZTISe have been prepared and show comparable performance to CZTSe. - Highlights: • In-situ XRD study of two-stage co-evaporated Cu 2 ZnSnSe 4 -CuInSe 2 alloyed thin films. • No detection of ZnSe with in-situ XRD due to Indium incorporation • Comparable efficiency of alloyed solar cells

  5. The treatment of an unstable slipped capital femoral epiphysis by either intracapsular cuneiform osteotomy or pinning in situ: a comparative study.

    Science.gov (United States)

    Walton, R D M; Martin, E; Wright, D; Garg, N K; Perry, D; Bass, A; Bruce, C

    2015-03-01

    We undertook a retrospective comparative study of all patients with an unstable slipped capital femoral epiphysis presenting to a single centre between 1998 and 2011. There were 45 patients (46 hips; mean age 12.6 years; 9 to 14); 16 hips underwent intracapsular cuneiform osteotomy and 30 underwent pinning in situ, with varying degrees of serendipitous reduction. No patient in the osteotomy group was lost to follow-up, which was undertaken at a mean of 28 months (11 to 48); four patients in the pinning in situ group were lost to follow-up, which occurred at a mean of 30 months (10 to 50). Avascular necrosis (AVN) occurred in four hips (25%) following osteotomy and in 11 (42%) following pinning in situ. AVN was not seen in five hips for which osteotomy was undertaken > 13 days after presentation. AVN occurred in four of ten (40%) hips undergoing emergency pinning in situ, compared with four of 15 (47%) undergoing non-emergency pinning. The rate of AVN was 67% (four of six) in those undergoing pinning on the second or third day after presentation. Pinning in situ following complete reduction led to AVN in four out of five cases (80%). In comparison, pinning in situ following incomplete reduction led to AVN in 7 of 21 cases (33%). The rate of development of AVN was significantly higher following pinning in situ with complete reduction than following intracapsular osteotomy (p = 0.048). Complete reduction was more frequent in those treated by emergency pinning and was strongly associated with AVN (p = 0.005). Non-emergency intracapsular osteotomy may have a protective effect on the epiphyseal vasculature and should be undertaken with a delay of at least two weeks. The place of emergency pinning in situ in these patients needs to be re-evaluated, possibly in favour of an emergency open procedure or delayed intracapsular osteotomy. Non-emergency pinning in situ should be undertaken after a delay of at least five days, with the greatest risk at two and three days after

  6. Pre-Service Teachers' Defensive Pessimism in Situ: Two Case Studies within a Mathematics Classroom

    Science.gov (United States)

    Merz, Alice H.; Swim, Terri Jo

    2008-01-01

    In this study, defensive pessimism is reviewed in relation to anxiety, self-esteem, expectations, self-regulation, and self-handicapping. Then, two case studies of American pre-service teachers in a mathematics classroom are provided that move the research beyond survey and correlational studies. In the case analyses, defensive pessimists'…

  7. In Situ X-Ray Diffraction Study on Surface Melting of Bi Nanoparticles Embedded in a SiO2 Matrix

    International Nuclear Information System (INIS)

    Chen Xiao-Ming; Huo Kai-Tuo; Liu Peng

    2014-01-01

    Bi nanoparticles embedded in a SiO 2 matrix were prepared via the high energy ball milling method. The melting behavior of Bi nanoparticles was studied by means of differential scanning calorimetry (DSC) and high-temperature in situ X-ray diffraction (XRD). DSC cannot distinguish the surface melting from ‘bulk’ melting of the Bi nanoparticles. The XRD intensity of the Bi nanoparticles decreases progressively during the in situ heating process. The variation in the normalized integrated XRD intensity versus temperature is related to the average grain size of Bi nanoparticles. Considering the effects of temperature on Debye—Waller factor and Lorentz-polarization factor, we discuss the XRD results in accordance with surface melting. Our results show that the in situ XRD technique is effective to explore the surface melting of nanoparticles

  8. Study of the thermal transformations of Co- and Fe-exchanged zeolites A and X by 'in situ' XRD under reducing atmosphere

    Energy Technology Data Exchange (ETDEWEB)

    Ronchetti, Silvia, E-mail: silvia.ronchetti@polito.it [Dipartimento di Scienza dei Materiali e Ingegneria Chimica, Politecnico di Torino, Corso Duca degli Abruzzi 24, 10129 Torino (Italy); Turcato, Elisa Aurelia; Delmastro, Alessandro [Dipartimento di Scienza dei Materiali e Ingegneria Chimica, Politecnico di Torino, Corso Duca degli Abruzzi 24, 10129 Torino (Italy); Esposito, Serena; Ferone, Claudio; Pansini, Michele [Laboratorio Materiali del Dipartimento di Meccanica, Strutture, Ambiente e Territorio, Facolta di Ingegneria dell' Universita di Cassino, Via G. Di Biasio 43, 03043 Cassino (Italy); Onida, Barbara; Mazza, Daniele [Dipartimento di Scienza dei Materiali e Ingegneria Chimica, Politecnico di Torino, Corso Duca degli Abruzzi 24, 10129 Torino (Italy)

    2010-06-15

    'In situ' high temperature X-ray diffraction under reducing atmosphere is used for the first time to study the thermal stability and transformations of Co- and Fe-exchanged A and X zeolites. TG-DTA and 'ex situ' XRD characterization were also carried out. The temperature of incipient crystallization of metallic phase was found to be 700 {sup o}C in Fe-zeolites and 800 {sup o}C in Co-zeolites. Moreover, ex situ X-ray experiments, after thermal treatment both under inert and reducing atmosphere, revealed the formation of ceramic phases upon the thermal collapse of the zeolitic framework. Metal nanoparticles were obtained by reduction and the size of metal clusters was found to range between 24 and 40 nm.

  9. In situ XAS monitoring the formation of Pd2Ga/SiO2 nanoparticles for CO2 hydrogenation to methanol

    DEFF Research Database (Denmark)

    Carvalho, H.W.P.; Fiordaliso, Elisabetta Maria; Sharafutdinov, Irek

    2015-01-01

    Methanol is a bulk chemical used as basis for many important downstream products such as formaldehyde, acetic acid and plastics. Furthermore it can be directly used as fuel. We have prepared Pd2Ga/SiO2 catalyst by impregnation of nitrates followedby calcination and reduction under H2 atmosphere...... are converted to highly dispersed and disordered oxide phases which are alloyed under heating in H2/Ar atmosphere giving rise to Pd2Ga nanoparticles....

  10. Final Report DE-SC0006997; PI Sharp; Coupled Biological and Micro-XAS/XRF Analysis of In Situ Uranium Biogeochemical Processes

    Energy Technology Data Exchange (ETDEWEB)

    Sharp, Jonathan O. [Colorado School of Mines, Golden, CO (United States)

    2016-03-30

    Project Overview: The impact of the original seed award was substantially increased by leveraging a postdoctoral fellowship (Marie Curie Postdoctoral Fellowship) and parallel funds from (A) synergistic project supported by NSF and (B) with DOE collaborators (PI’s Ranville and Williams) as well as no-cost extension that greatly increased the impact and publications associated with the project. In aligning with SBR priorities, the project’s focus was extended more broadly to explore coupled biogeochemical analysis of metal (im)mobilization processes beyond uranium with a foundation in integrating microbial ecology with geochemical analyses. This included investigations of arsenic and zinc during sulfate reducing conditions in addition to direct microbial reduction of metals. Complimentary work with NSF funding and collaborative DOE interactions further increased the project scope to investigate metal (im)mobilization coupled to biogeochemical perturbations in forest ecosystems with an emphasis on coupled carbon and metal biogeochemistry. In total, the project was highly impactful and resulted in 9 publications and directly supported salary/tuition for 3 graduate students at various stages of their academic careers as well as my promotion to Associate Professor. In going forward, findings provided inspiration for a two subsequent proposals with collaborators at Lawrence Berkeley Laboratory and others that are currently in review (as of March 2016).

  11. Tinjauan Keanekaragaman Moluska Air Tawar Di Beberapa Situ Di DAS Ciliwung - Cisadane [Study on the Freshwater Mollusc Diversity of the Small Lakes Along Ciliwung and Cisadane Rivers

    OpenAIRE

    Marwoto, Ristiyanti M; Isnaningsih, Nur R

    2014-01-01

    The freshwater molluscs (snails and bivalves) can be found in many type of water course either flowing or stagnant water. Some of them have survived living in bad condition such as polluted water. There are 199 situ (small lakes) in Jabodetabek (Jakarta, Bogor, Depok, Tangerang, Bekasi) have been reported but only 20 % were in good condition, even 12% have dissapeared that caused by silting up of the situ. The aim of the study was to evaluate the diversity of the molluscs as well as to know t...

  12. In situ vitrification demonstration at Pit 1, Oak Ridge National Laboratory. Volume 1: Results of treatability study

    International Nuclear Information System (INIS)

    Spalding, B.P.; Naney, M.T.; Cline, S.R.; Bogle, M.A.

    1997-12-01

    A treatability study was initiated in October 1993 to apply in situ vitrification (ISV) to at least two segments of Oak Ridge National Laboratory (ORNL) seepage Pit 1 by the end of fiscal year (FY) 1995. This treatability study was later extended to include all of Pit 1 and was performed to support a possible Interim Record of Decision or removal action for closure of one or more of the seepage pits and trenches beginning as early as FY 1997. This treatability study was carried out to establish the field-scale technical performance of ISV for (1) attaining the required depth, nominally 15 ft, to incorporate source contamination within and beneath the pits; (2) demonstrating field capability for the overlap of melt settings which will be necessary to achieve fused, melted segments of the source contamination; (3) demonstrating off-gas handling technology for accommodating and minimizing the volatilization of 137 Cs; (4) demonstrating adequate site characterization techniques to predict ISV melting kinetics, processing temperatures, and product durability; and (5) promoting public acceptance of ISV technology by demonstrating its safety, implementability, site impacts, and air emissions and by coordinating the treatability study within the regulatory closure process. In April 1996 an expulsion of an estimated 10% of the 196 Mg (216 tons) melt body occurred resulting in significant damage to ISV equipment and, ultimately, led to an indefinite suspension of further ISV operations at Pit 1. This report summarizes the technical accomplishments and status of the project in fulfilling these objectives through September 1997

  13. In situ vitrification demonstration at Pit 1, Oak Ridge National Laboratory. Volume 1: Results of treatability study

    Energy Technology Data Exchange (ETDEWEB)

    Spalding, B.P.; Naney, M.T.; Cline, S.R.; Bogle, M.A. [Oak Ridge National Lab., TN (United States). Environmental Sciences Div.; Tixier, J.S. [Pacific Northwest National Lab., Richland, WA (United States)

    1997-12-01

    A treatability study was initiated in October 1993 to apply in situ vitrification (ISV) to at least two segments of Oak Ridge National Laboratory (ORNL) seepage Pit 1 by the end of fiscal year (FY) 1995. This treatability study was later extended to include all of Pit 1 and was performed to support a possible Interim Record of Decision or removal action for closure of one or more of the seepage pits and trenches beginning as early as FY 1997. This treatability study was carried out to establish the field-scale technical performance of ISV for (1) attaining the required depth, nominally 15 ft, to incorporate source contamination within and beneath the pits; (2) demonstrating field capability for the overlap of melt settings which will be necessary to achieve fused, melted segments of the source contamination; (3) demonstrating off-gas handling technology for accommodating and minimizing the volatilization of {sup 137}Cs; (4) demonstrating adequate site characterization techniques to predict ISV melting kinetics, processing temperatures, and product durability; and (5) promoting public acceptance of ISV technology by demonstrating its safety, implementability, site impacts, and air emissions and by coordinating the treatability study within the regulatory closure process. In April 1996 an expulsion of an estimated 10% of the 196 Mg (216 tons) melt body occurred resulting in significant damage to ISV equipment and, ultimately, led to an indefinite suspension of further ISV operations at Pit 1. This report summarizes the technical accomplishments and status of the project in fulfilling these objectives through September 1997.

  14. Approximal secondary caries lesion progression, a 20-week in situ study

    NARCIS (Netherlands)

    Thomas, R. Z.; Ruben, J. L.; ten Bosch, J. J.; Fidler, V.; Huysmans, M. C. D. N. J. M.

    2007-01-01

    There is no consensus about the definition and progression of outer and wall lesions in secondary caries. In this study we investigated whether lesion progression is influenced by an adjacent composite restoration and whether wall lesions develop at the composite-tooth interface. In order to study

  15. In-hospital resuscitation evaluated by in situ simulation: a prospective simulation study

    DEFF Research Database (Denmark)

    Mondrup, Frederik; Brabrand, Mikkel; Folkestad, Lars

    2011-01-01

    , and to examine differences in the resuscitation performance between the first responders and the cardiac arrest team. METHOD: S: A prospective observational study of 16 unannounced simulated cardiopulmonary arrest scenarios was conducted. The participants of the study involved all health care personel on duty...

  16. Provenance and composition study on Terengganu inscribed stone using in-situ nuclear technology

    International Nuclear Information System (INIS)

    Jaafar Abdullah; Roslan Yahya; Hearie Hassan; Engku Mohd Fahmi Engku Chik; Mohamad Rabaie Shari; Airwan Affendi Mahmood; Abdul Quddoss Abu Bakar; Ainul Mardhiah Terry

    2012-01-01

    This paper focused on the analysis of trace elements and provenance study of the Inscribed Stone of Terengganu (BBPT) using Neutron-induced Prompt Gamma-Ray Techniques (NIPGAT). In this study, portable NIPGAT system was designed and developed by using volume-based measurement. It is a nondestructive testing technique for the samples. This system uses low activity of isotopic neutron radioactive source from californium-252 (Cf-252) as an irradiation source. Gamma ray spectroscopy as well as specialized computer software has been utilized to conduct the research. The study has determined that the stone was a dolerite stone based on the composition of the stone elements. Although most of the scientific data for this study have been collected, this project is still running to complete the scope of provenance study. (author)

  17. In situ 119Sn Moessbauer spectroscopy used to study lithium insertion in c-Mg2Sn

    International Nuclear Information System (INIS)

    Aldon, L.; Ionica, C. M.; Lippens, P. E.; Larcher, D.; Tarascon, J.-M.; Olivier-Fourcade, J.; Jumas, J.-C.

    2006-01-01

    The electrochemical reactions of Li with c-Mg 2 Sn have been investigated by in situ Moessbauer spectroscopy of 119 Sn and X-ray diffraction. The lithiation transforms initially c-Mg 2 Sn part into Li x Mg 2 Sn alloy (x 2 MgSn ternary alloy. In situ Moessbauer spectroscopy provides valuable information on local environment of tin and swelling behavior and cracking of the particles during discharge and charge processes.

  18. In-Situ TEM Study of a Nanoporous Ni–Co Catalyst Used for the Dry Reforming of Methane

    Directory of Open Access Journals (Sweden)

    Takeshi Fujita

    2017-10-01

    Full Text Available We performed in-situ transmission electron microscopy (TEM on a dealloyed nanoporous NiCo catalyst used for the dry reforming of methane (DRM to investigate the origin of the catalytic activity and structural durability. The in-situ observations and local chemical analysis indicated that the DRM induced chemical demixing of Ni and Co accompanied by grain refinement, implying possible “synergic effects” in a general bimetallic NiCo catalyst when used for the DRM.

  19. Experimental and Thermodynamic Study of Selected in-Situ Composites from the Fe-Cr-Ni-Mo-C System

    Directory of Open Access Journals (Sweden)

    Wieczerzak K.

    2016-06-01

    Full Text Available The aim of the study was to synthesize and characterize the selected in-situ composites from the Fe-Cr-Ni-Mo-C system, additionally strengthened by intermetallic compounds. The project of the alloys was supported by thermodynamic simulations using Calculation of Phase Diagram approach via Thermo-Calc. Selected alloys were synthesized in an arc furnace in a high purity argon atmosphere using a suction casting unit. The studies involved a range of experimental techniques to characterize the alloys in the as-cast state, including optical emission spectrometry, light microscopy, scanning electron microscopy, electron microprobe analysis, X-ray diffraction and microhardness tests. These experimental studies were compared with the Thermo-Calc data and high resolution dilatometry. The results of investigations presented in this paper showed that there is a possibility to introduce intermetallic compounds, such as χ and σ, through modification of the chemical composition of the alloy with respect to Nieq and Creq. It was found that the place of intermetallic compounds precipitation strongly depends on matrix nature. Results presented in this paper may be successfully used to build a systematic knowledge about the group of alloys with a high volume fraction of complex carbides, and high physicochemical properties, additionally strengthened by intermetallic compounds.

  20. In situ transmission electron microscopy and scanning transmission electron microscopy studies of sintering of Ag and Pt nanoparticles

    International Nuclear Information System (INIS)

    Asoro, M.A.; Ferreira, P.J.; Kovar, D.

    2014-01-01

    Transmission electron microscopy and scanning transmission electron microscopy studies were conducted in situ on 2–5 nm Pt and 10–40 nm Ag nanoparticles to study mechanisms for sintering and to measure relevant sintering kinetics in nanoscale particles. Sintering between two separated particles was observed to initiate by either (1) diffusion of the particles on the sample support or (2) diffusion of atoms or small clusters of atoms to the neck region between the two particles. After particle contact, the rate of sintering was controlled by atomic surface diffusivity. The surface diffusivity was determined as a function of particle size and temperature from experimental measurements of the rate of neck growth of the particles. The surface diffusivities did not show a strong size effect for the range of particle sizes that were studied. The surface diffusivity for Pt nanoparticles exhibited the expected Arrhenius temperature dependence and did not appear to be sensitive to the presence of surface contaminants. In contrast, the surface diffusivity for Ag nanoparticles was affected by the presence of impurities such as carbon. The diffusivities for Ag nanoparticles were consistent with previous measurements of bulk surface diffusivities for Ag in the presence of C, but were significantly slower than those obtained from pristine Ag