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.

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

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

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.

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

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)

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

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

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.

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.

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

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

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.)

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.

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.

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.

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...

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...

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

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...

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.

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.

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)

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)

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)

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...

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}.

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.

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...

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.

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.

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

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

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.

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.

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.

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.

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)

Spin-Polarization-Induced Preedge Transitions in the Sulfur K-Edge XAS Spectra of Open-Shell Transition-Metal Sulfates: Spectroscopic Validation of σ-Bond Electron Transfer.

Science.gov (United States)

Frank, Patrick; Szilagyi, Robert K; Gramlich, Volker; Hsu, Hua-Fen; Hedman, Britt; Hodgson, Keith O

2017-02-06

Sulfur K-edge X-ray absorption spectroscopy (XAS) spectra of the monodentate sulfate complexes [M II (itao)(SO 4 )(H 2 O) 0,1 ] (M = Co, Ni, Cu) and [Cu(Me 6 tren)(SO 4 )] exhibit well-defined preedge transitions at 2479.4, 2479.9, 2478.4, and 2477.7 eV, respectively, despite having no direct metal-sulfur bond, while the XAS preedge of [Zn(itao)(SO 4 )] is featureless. The sulfur K-edge XAS of [Cu(itao)(SO 4 )] but not of [Cu(Me 6 tren)(SO 4 )] uniquely exhibits a weak transition at 2472.1 eV, an extraordinary 8.7 eV below the first inflection of the rising K-edge. Preedge transitions also appear in the sulfur K-edge XAS of crystalline [M II (SO 4 )(H 2 O)] (M = Fe, Co, Ni, and Cu, but not Zn) and in sulfates of higher-valent early transition metals. Ground-state density functional theory (DFT) and time-dependent DFT (TDDFT) calculations show that charge transfer from coordinated sulfate to paramagnetic late transition metals produces spin polarization that differentially mixes the spin-up (α) and spin-down (β) spin orbitals of the sulfate ligand, inducing negative spin density at the sulfate sulfur. Ground-state DFT calculations show that sulfur 3p character then mixes into metal 4s and 4p valence orbitals and various combinations of ligand antibonding orbitals, producing measurable sulfur XAS transitions. TDDFT calculations confirm the presence of XAS preedge features 0.5-2 eV below the rising sulfur K-edge energy. The 2472.1 eV feature arises when orbitals at lower energy than the frontier occupied orbitals with S 3p character mix with the copper(II) electron hole. Transmission of spin polarization and thus of radical character through several bonds between the sulfur and electron hole provides a new mechanism for the counterintuitive appearance of preedge transitions in the XAS spectra of transition-metal oxoanion ligands in the absence of any direct metal-absorber bond. The 2472.1 eV transition is evidence for further radicalization from copper(II), which

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)

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.

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.

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

In Situ Spectroscopy and Mechanistic Insights into CO Oxidation on Transition-Metal-Substituted Ceria Nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Elias, Joseph S.; Stoerzinger, Kelsey A.; Hong, Wesley T.; Risch, Marcel; Giordano, Livia [Dipartimento; Mansour, Azzam N. [Naval; Shao-Horn, Yang

2017-09-12

Herein we investigate the reaction intermediates formed during CO oxidation on copper-substituted ceria nanoparticles (Cu0.1Ce0.9O2–x) by means of in situ spectroscopic techniques and identify an activity descriptor that rationalizes a trend with other metal substitutes (M0.1Ce0.9O2–x, M = Mn, Fe, Co, Ni). In situ X-ray absorption spectroscopy (XAS) performed under catalytic conditions demonstrates that O2– transfer occurs at dispersed copper centers, which are redox active during catalysis. In situ XAS reveals a dramatic reduction at the copper centers that is fully reversible under catalytic conditions, which rationalizes the high catalytic activity of Cu0.1Ce0.9O2–x. Ambient pressure X-ray photoelectron spectroscopy (AP-XPS) and in situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) show that CO can be oxidized to CO32– in the absence of O2. We find that CO32– desorbs as CO2 only under oxygen-rich conditions when the oxygen vacancy is filled by the dissociative adsorption of O2. These data, along with kinetic analyses, lend support to a mechanism in which the breaking of copper–oxygen bonds is rate-determining under oxygen-rich conditions, while refilling the resulting oxygen vacancy is rate-determining under oxygen-lean conditions. On the basis of these observations and density functional calculations, we introduce the computed oxygen vacancy formation energy (Evac) as an activity descriptor for substituted ceria materials and demonstrate that Evac successfully rationalizes the trend in the activities of M0.1Ce0.9O2–x catalysts that spans three orders of magnitude. The applicability of Evac as a useful design descriptor is demonstrated by the catalytic performance of the ternary oxide Cu0.1La0.1Ce0.8O2–x, which has an apparent activation energy rivaling those of state-of-the-art Au/TiO2 materials. Thus, we suggest that cost-effective catalysts for CO oxidation can be rationally designed by judicious choice of substituting

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

Room temperature redox reaction by oxide ion migration at carbon/Gd-doped CeO2 heterointerface probed by an in situ hard x-ray photoemission and soft x-ray absorption spectroscopies

Directory of Open Access Journals (Sweden)

Takashi Tsuchiya, Shogo Miyoshi, Yoshiyuki Yamashita, Hideki Yoshikawa, Kazuya Terabe, Keisuke Kobayashi and Shu Yamaguchi

2013-01-01

Full Text Available In situ hard x-ray photoemission spectroscopy (HX-PES and soft x-ray absorption spectroscopy (SX-XAS have been employed to investigate a local redox reaction at the carbon/Gd-doped CeO2 (GDC thin film heterointerface under applied dc bias. In HX-PES, Ce3d and O1s core levels show a parallel chemical shift as large as 3.2 eV, corresponding to the redox window where ionic conductivity is predominant. The window width is equal to the energy gap between donor and acceptor levels of the GDC electrolyte. The Ce M-edge SX-XAS spectra also show a considerable increase of Ce3+ satellite peak intensity, corresponding to electrochemical reduction by oxide ion migration. In addition to the reversible redox reaction, two distinct phenomena by the electrochemical transport of oxide ions are observed as an irreversible reduction of the entire oxide film by O2 evolution from the GDC film to the gas phase, as well as a vigorous precipitation of oxygen gas at the bottom electrode to lift off the GDC film. These in situ spectroscopic observations describe well the electrochemical polarization behavior of a metal/GDC/metal capacitor-like two-electrode cell at room temperature.

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.

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...

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

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...

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.

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.)

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.

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.

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.

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.

Hydrostatic-pressure-induced GAMMA-X mixing in delta-doped Al{sub x}Ga{sub 1-x}As

Energy Technology Data Exchange (ETDEWEB)

Mora-Ramos, M E [Facultad de Ciencias, Universidad Autonoma del Estado de Morelos, Av. Universidad 1001, Col. Chamilpa, CP 62209 Cuernavaca, MOR. (Mexico); Duque, C A, E-mail: memora@buzon.uaem.m [Instituto de Fisica, Universidad de Antioquia, AA 1226, Medellin (Colombia)

2009-05-01

The mixing between GAMMA and X points in the conduction band is known to manifest in GaAs/Al{sub x}Ga{sub 1-x}As heterostructures. Application of hydrostatic pressure leads to the variation of both the GAMMA- and X-energy gaps in such a way that around P = 39 kbar, the GaAs becomes an indirect gap one. Within a narrow interval of P around this value, both minima remain almost energetically aligned. Therefore, it can be expected that some kind of mixing between the states corresponding to the delta-quantum-wells formed at those points should manifest. In this work, we investigate the occurrence of GAMMA-X mixing induced by the application of hydrostatic pressure in n-type delta doped Al{sub x}Ga{sub 1-x}As, by means of a variational scheme that uses a 2x2 Hamiltonian with the off-diagonal element being a variational potential energy. Diagonal Schroedinger-like effective mass elements are written with potential functions given by the Thomas-Fermi approximation. The effect of the hydrostatic pressure is incorporated via the dependence on P of the different input parameters in the system: energy gaps, effective masses and dielectric constant. We report the variation of the ground state of the system as a function of P.

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.

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 ...

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

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.

Operando and in situ X-ray spectroscopies of degradation in La0.6Sr0.4Co0.2Fe0.8O(3-δ) thin film cathodes in fuel cells.

Science.gov (United States)

Lai, Samson Y; Ding, Dong; Liu, Mingfei; Liu, Meilin; Alamgir, Faisal M

2014-11-01

Information from ex situ characterization can fall short in describing complex materials systems simultaneously exposed to multiple external stimuli. Operando X-ray absorption spectroscopy (XAS) was used to probe the local atomistic and electronic structure of specific elements in a La0.6Sr0.4Co0.2Fe0.8O(3-δ) (LSCF) thin film cathode exposed to air contaminated with H2O and CO2 under operating conditions. While impedance spectroscopy showed that the polarization resistance of the LSCF cathode increased upon exposure to both contaminants at 750 °C, XAS near-edge and extended fine structure showed that the degree of oxidation for Fe and Co decreases with increasing temperature. Synchrotron-based X-ray photoelectron spectroscopy tracked the formation and removal of a carbonate species, a Co phase, and different oxygen moieties as functions of temperature and gas. The combined information provides insight into the fundamental mechanism by which H2O and CO2 cause degradation in the cathode of solid oxide fuel cells. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

Spectroscopic characterization of ion-irradiated multi-layer graphenes

Energy Technology Data Exchange (ETDEWEB)

Tsukagoshi, Akira [Graduate School of Engineering, University of Hyogo, Himeji, Hyogo 671-2280 (Japan); RIKEN SPring-8 Center, Sayo, Hyogo 679-5148 (Japan); Honda, Shin-ichi, E-mail: s-honda@eng.u-hyogo.ac.jp [Graduate School of Engineering, University of Hyogo, Himeji, Hyogo 671-2280 (Japan); RIKEN SPring-8 Center, Sayo, Hyogo 679-5148 (Japan); Osugi, Ryo [Graduate School of Engineering, University of Hyogo, Himeji, Hyogo 671-2280 (Japan); RIKEN SPring-8 Center, Sayo, Hyogo 679-5148 (Japan); Okada, Hiraku [Graduate School of Engineering, University of Hyogo, Himeji, Hyogo 671-2280 (Japan); Niibe, Masahito [Laboratory of Advanced Science and Technology for Industry, University of Hyogo, Kamigori, Hyogo 678-1205 (Japan); Terasawa, Mititaka [Laboratory of Advanced Science and Technology for Industry, University of Hyogo, Kamigori, Hyogo 678-1205 (Japan); RIKEN SPring-8 Center, Sayo, Hyogo 679-5148 (Japan); Hirase, Ryuji; Izumi, Hirokazu; Yoshioka, Hideki [Hyogo Prefectural Institute of Technology, Kobe 654-0037 (Japan); Niwase, Keisuke [Hyogo University of Teacher Education, Kato, Hyogo 673-1494 (Japan); Taguchi, Eiji [Research Center for Ultra-High Voltage Electron Microscopy, Osaka University, Ibaraki, Osaka 567-0047 (Japan); Lee, Kuei-Yi [Department of Electronic Engineering, National Taiwan University of Science and Technology, Taipei 106, Taiwan (China); Oura, Masaki [RIKEN SPring-8 Center, Sayo, Hyogo 679-5148 (Japan)

2013-11-15

Low-energy Ar ions (0.5–2 keV) were irradiated to multi-layer graphenes and the damage process, the local electronic states, and the degree of alignment of the basal plane, and the oxidation process upon ion irradiation were investigated by Raman spectroscopy, soft X-ray absorption spectroscopy (XAS) and in situ X-ray photoelectron spectroscopy (XPS). By Raman spectroscopy, we observed two stages similar to the case of irradiated graphite, which should relate to the accumulations of vacancies and turbulence of the basal plane, respectively. XAS analysis indicated that the number of sp{sup 2}-hybridized carbon (sp{sup 2}-C) atoms decreased after ion irradiation. Angle-resolved XAS revealed that the orientation parameter (OP) decreased with increasing ion energy and fluence, reflecting the turbulence of the basal plane under irradiation. In situ XPS shows the oxidation of the irradiated multi-layer graphenes after air exposure.

Arsenic speciation in solids using X-ray absorption spectroscopy

Science.gov (United States)

Foster, Andrea L.; Kim, Chris S.

2014-01-01

Synchrotron-based X-ray absorption spectroscopy (XAS) is an in situ, minimally-destructive, element-specific, molecular-scale structural probe that has been employed to study the chemical forms (species) of arsenic (As) in solid and aqueous phases (including rocks, soils, sediment, synthetic compounds, and numerous types of biota including humans) for more than 20 years. Although several excellent reviews of As geochemistry and As speciation in the environment have been published previously (including recent contributions in this volume), the explosion of As-XAS studies over the past decade (especially studies employing microfocused X-ray beams) warrants this new review of the literature and of data analysis methods.

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.

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

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

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.

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

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...

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

Characterization of Electrode Materials for Lithium Ion and Sodium Ion Batteries using Synchrotron Radiation Techniques

Energy Technology Data Exchange (ETDEWEB)

Mehta, Apurva; Stanford Synchrotron Radiation Lightsource; Doeff, Marca M.; Chen, Guoying; Cabana, Jordi; Richardson, Thomas J.; Mehta, Apurva; Shirpour, Mona; Duncan, Hugues; Kim, Chunjoong; Kam, Kinson C.; Conry, Thomas

2013-04-30

We describe the use of synchrotron X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) techniques to probe details of intercalation/deintercalation processes in electrode materials for Li ion and Na ion batteries. Both in situ and ex situ experiments are used to understand structural behavior relevant to the operation of devices.

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)

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.

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

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.)

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

Architecture of Pd-Au bimetallic nanoparticles in sodium bis(2-ethylhexyl)sulfosuccinate reverse micelles as investigated by X-ray absorption spectroscopy.

Science.gov (United States)

Chen, Ching-Hsiang; Sarma, Loka Subramanyam; Chen, Jium-Ming; Shih, Shou-Chu; Wang, Guo-Rung; Liu, Din-Goa; Tang, Mau-Tsu; Lee, Jyh-Fu; Hwang, Bing-Joe

2007-09-01

In this study, we demonstrate the unique application of X-ray absorption spectroscopy (XAS) as a fundamental characterization tool to help in designing and controlling the architecture of Pd-Au bimetallic nanoparticles within a water-in-oil microemulsion system of water/sodium bis(2-ethylhexyl)sulfosuccinate (AOT)/n-heptane. Structural insights obtained from the in situ XAS measurements recorded at each step during the formation process revealed that Pd-Au bimetallic clusters with various Pd-Au atomic stackings are formed by properly performing hydrazine reduction and redox transmetalation reactions sequentially within water-in-oil microemulsions. A structural model is provided to explain reasonably each reaction step and to give detailed insight into the nucleation and growth mechanism of Pd-Au bimetallic clusters. The combination of in situ XAS analysis at both the Pd K-edge and the Au L(III)-edge and UV-vis absorption spectral features confirms that the formation of Pd-Au bimetallic clusters follows a (Pd(nuclei)-Au(stack))-Pd(surf) stacking. This result further implies that the thickness of Au(stack) and Pd(surf) layers may be modulated by varying the dosage of the Au precursor and hydrazine, respectively. In addition, a bimetallic (Pd-Au)(alloy) nanocluster with a (Pd(nuclei)-Au(stack))-(Pd-Au(alloy))(surf) stacking was also designed and synthesized in order to check the feasibility of Pd(surf) layer modification. The result reveals that the Pd(surf) layer of the stacked (Pd(nuclei)-Au)(stack) bimetallic clusters can be successfully modified to form a (Au-Pd alloy)(surf) layer by a co-reduction of Pd and Au ions by hydrazine. Further, we demonstrate the alloying extent or atomic distribution of Pd and Au in Pd-Au bimetallic nanoparticles from the derived XAS structural parameters. The complete XAS-based methodology, demonstrated here on the Pd-Au bimetallic system, can easily be extended to design and control the alloying extent or atomic distribution, atomic

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

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...

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

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.

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.

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

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

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

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.

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.

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.

ENERGÍA DE ENLACE DE EXCITONES EN POZOS CUÁNTICOS DE GaAs/Ga1-xAl xAs

Directory of Open Access Journals (Sweden)

Parménides Aristizábal

2007-06-01

Full Text Available El uso de las estructuras de baja dimensionalidad es un elemento tecnológico clave en la creación de nuevos dispositivos cuánticos funcionales de la siguiente generación de circuitos integrados electrónicos, fotónicos y espintrónicos y muchos otros dispositivos nanotecnológicos que son necesarios para la sociedad de la información del siglo XXI. Una de las propiedades ópticas más importante es la fotoluminiscencia producida por agentes tales como impurezas y excitones en pozos, hilos y puntos cuánticos de arseniuro de galio GaAs con dimensiones nanométricas bajo la influencia de campos eléctricos y magnéticos y presiones externas. Se presenta la energía de enlace para los tres primeros estados excitónicos en pozos cuánticos de GaAs/Ga1-xAl xAs describiendo el sistema por medio de la teoría cuántica, en la aproximación de masa efectiva y usando el método variacional.The use of low dimensional structures is a key technological element in the creation of new quantum functional devices in the development of the next generation of the electronic, photonic, and spintronic integrated circuits and many other nanoscaled devices that are necessary for the information society of 21st century. One of the most important optical properties is the photoluminescence produced by agents as impurities and excitons in GaAs quantum wells, wires, and dots with nanometric dimensions under the influence of electric and magnetic fields and external pressures. The binding energy for the first three excitonic states in GaAs/Ga1-xA1xAs quantum wells describing the system through quantum theory in the effective mass approximation and using the variational method is presented.

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)

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...

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.

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.

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

Continuous room-temperature operation of GaAs-Al/sub x/Ga1/sub -//sub x/As double-heterostructure lasers prepared by molecular-beam epitaxy

International Nuclear Information System (INIS)

Cho, A.Y.; Dixon, R.W.; Casey, H.C. Jr.; Hartman, R.L.

1976-01-01

The continuous (cw) operation at temperatures as high as 100 0 C of stripe-geometry GaAs-Al/sub x/Ga/sub 1-x/As double-heterostructure lasers fabricated by molecular-beam epitaxial (MBE) techniques has been achieved. Improved MBE laser performance was the result of the extensive efforts to eliminate hydrocarbon and water vapor from the growth apparatus. For 12-μm-wide stripe-geometry lasers with 380-μm-long cavities, the cw threshold currents varied between 163 and 297 mA at room temperature

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.)

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

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)

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.

Hydrostatic-pressure effects on the correlated electron-hole transition energies in GaAs-Ga{sub 1-x}Al{sub x}As semiconductor quantum wells

Energy Technology Data Exchange (ETDEWEB)

Raigoza, N. [Instituto de Fisica, Universidad de Antioquia, AA 1226, Medellin (Colombia); Instituto de Fisica, Unicamp, CP 6165, Campinas, Sao Paulo, 13083-970 (Brazil); Duque, C.A. [Instituto de Fisica, Universidad de Antioquia, AA 1226, Medellin (Colombia); Reyes-Gomez, E. [Dept. of Theor. Physics, Univ. of Havana, San Lazaro y L, Vedado 10400, Havana (Cuba); Instituto de Fisica, Unicamp, CP 6165, Campinas, Sao Paulo, 13083-970 (Brazil); Oliveira, L.E. [Instituto de Fisica, Unicamp, CP 6165, Campinas, Sao Paulo, 13083-970 (Brazil)

2006-03-01

The effects of hydrostatic pressure on the correlated e-h transition energies in single GaAs-Ga{sub 1-x}Al{sub x}As quantum wells are calculated via a variational procedure, in the framework of the effective-mass and non-degenerate parabolic-band approximations. The valence-band anisotropy is included in our theoretical model by using different hole masses in different spatial directions. Both heavy- and light-hole exciton energies are obtained, and correlated e-h transition energies are found in good agreement with available experimental measurements. (copyright 2006 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

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...

Influence of H2O and H2S on the Composition, Activity, and Stability of Sulfided Mo, CoMo, and NiMo Supported on MgAl2O4 for Hydrodeoxygenation of Ethylene Glycol

DEFF Research Database (Denmark)

Dabros, Trine Marie Hartmann; Gaur, Abhijeet; Pintos, Delfina Garcia

2018-01-01

In this work, density functional theory (DFT), catalytic activity tests, and in-situ X-ray absorption spectroscopy (XAS) was performed to gain detailed insights into the activity and stability of MoS2, Ni-MoS2, and Co-MoS2 catalysts used for hydrodeoxygenation (HDO) of ethylene glycol upon...

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

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

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.

Atomic structure of machined semiconducting chips: An x-ray absorption spectroscopy study

Energy Technology Data Exchange (ETDEWEB)

Paesler, M.; Sayers, D.

1988-12-01

X-ray absorption spectroscopy (XAS) has been used to examine the atomic structure of chips of germanium that were produced by single point diamond machining. It is demonstrated that although the local (nearest neighbor) atomic structure is experimentally quite similar to that of single crystal specimens information from more distant atoms indicates the presence of considerable stress. An outline of the technique is given and the strength of XAS in studying the machining process is demonstrated.

Donor impurity-related optical absorption spectra in GaAs-Ga{sub 1-x}Al{sub x}As quantum wells: hydrostatic pressure and {gamma}-X conduction band mixing effects

Energy Technology Data Exchange (ETDEWEB)

Mora-Ramos, M.E. [Facultad de Ciencias, Universidad Autonoma del Estado de Morelos, Av. Universidad 1001, C.P. 62209, Cuernavaca, MOR (Mexico); Inst. de Ciencia de Materiales de Madrid, CSIC, Sor Juana Ines de la Cruz 3, 28049 Madrid (Spain); Lopez, S.Y. [Fac. de Educacion, Universidad de Antioquia, AA 1226, Medellin (Colombia); Duque, C.A. [Inst. de Fisica, Universidad de Antioquia, AA 1226, Medellin (Colombia); Velasco, V.R. [Inst. de Ciencia de Materiales de Madrid, CSIC, Sor Juana Ines de la Cruz 3, 28049 Madrid (Spain)

2007-07-01

Using a variational procedure within the effective mass approximation, the mixing between the {gamma} and X conduction band valleys in GaAs-Ga{sub 1-x}Al{sub x}As quantum wells is investigated by taking into account the effect of applied hydrostatic pressure. Some optical properties such as donor and/or acceptor binding energy and impurity-related transition energies are calculated and comparisons with available experimental data are presented. (copyright 2007 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

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

Morphology and chemical composition of cobalt germanide islands on Ge(001).

Science.gov (United States)

Ewert, M; Schmidt, Th; Flege, J I; Heidmann, I; Grzela, T; Klesse, W M; Foerster, M; Aballe, L; Schroeder, T; Falta, J

2016-08-12

The reactive growth of cobalt germanide on Ge(001) was investigated by means of in situ x-ray absorption spectroscopy photoemission electron microscopy (XAS-PEEM), micro-illumination low-energy electron diffraction (μ-LEED), and ex situ atomic force microscopy (AFM). At a Co deposition temperature of 670 °C, a rich morphology with different island shapes and dimensions is observed, and a correlation between island morphology and stoichiometry is found. By combining XAS-PEEM and μ-LEED, we were able to identify a large part of the islands to consist of CoGe2, with many of them having an unusual epitaxial relationship: CoGe2 [Formula: see text] [Formula: see text] Ge [Formula: see text]. Side facets with (112) and (113) orientation have been found for such islands. However, two additional phases were observed, most likely Co5Ge7 and CoGe. Comparing growth on Ge(001) single crystals and on Ge(001)/Si(001) epilayer substrates, the occurrence of these intermediate phases seems to be promoted by defects or residual strain.

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

Photoluminescence measurements of the 1,55 eV band of Ge doped Al sub(x)Ga sub(1-x)As

International Nuclear Information System (INIS)

Furtado, M.T.; Weid, J.P. von der.

1984-01-01

The photoluminescence of the 1,55 eV band of Ge doped Al sub(x)Ga sub(1-x)As, with x=0.30-0.33, grown by liquid phase epitaxy is presented. The broad shape was found to be due to a lattice relaxation upon optical transitions. Resonant modes with (h/2π)ω sub(q) approx. 35 + - 2 meV and (h/2π) ω sub(q) approx. 45 + - 2 meV are found for the optical band, yielding a zero phonon transition energy - 1.73 + - 0.02 eV and a Franck-Condon shift approx. 0.17-0.20 eV for the optical center. The activation energy of thermal quenching yields an associated donnor binding energy of 0.17 + - 0.04 eV. Possible mechanisms for the radiative transitions are discussed. (Author) [pt

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...

Four Models of In Situ Simulation

DEFF Research Database (Denmark)

Musaeus, Peter; Krogh, Kristian; Paltved, Charlotte

2014-01-01

Introduction In situ simulation is characterized by being situated in the clinical environment as opposed to the simulation laboratory. But in situ simulation bears a family resemblance to other types of on the job training. We explore a typology of in situ simulation and suggest that there are f......Introduction In situ simulation is characterized by being situated in the clinical environment as opposed to the simulation laboratory. But in situ simulation bears a family resemblance to other types of on the job training. We explore a typology of in situ simulation and suggest...... that there are four fruitful approaches to in situ simulation: (1) In situ simulation informed by reported critical incidents and adverse events from emergency departments (ED) in which team training is about to be conducted to write scenarios. (2) In situ simulation through ethnographic studies at the ED. (3) Using...... the following processes: Transition processes, Action processes and Interpersonal processes. Design and purpose This abstract suggests four approaches to in situ simulation. A pilot study will evaluate the different approaches in two emergency departments in the Central Region of Denmark. Methods The typology...

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.

[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.

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

Novel in-situ lamella fabrication technique for in-situ TEM.

Science.gov (United States)

Canavan, Megan; Daly, Dermot; Rummel, Andreas; McCarthy, Eoin K; McAuley, Cathal; Nicolosi, Valeria

2018-03-29

In-situ transmission electron microscopy is rapidly emerging as the premier technique for characterising materials in a dynamic state on the atomic scale. The most important aspect of in-situ studies is specimen preparation. Specimens must be electron transparent and representative of the material in its operational state, amongst others. Here, a novel fabrication technique for the facile preparation of lamellae for in-situ transmission electron microscopy experimentation using focused ion beam milling is developed. This method involves the use of rotating microgrippers during the lift-out procedure, as opposed to the traditional micromanipulator needle and platinum weld. Using rotating grippers, and a unique adhesive substance, lamellae are mounted onto a MEMS device for in-situ TEM annealing experiments. We demonstrate how this technique can be used to avoid platinum deposition as well as minimising damage to the MEMS device during the thinning process. Our technique is both a cost effective and readily implementable alternative to the current generation of preparation methods for in-situ liquid, electrical, mechanical and thermal experimentation within the TEM as well as traditional cross-sectional lamella preparation. Copyright © 2018 Elsevier B.V. All rights reserved.

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

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...

Uranium speciation and stability after reductive immobilization in aquifer sediments

Science.gov (United States)

Sharp, Jonathan O.; Lezama-Pacheco, Juan S.; Schofield, Eleanor J.; Junier, Pilar; Ulrich, Kai-Uwe; Chinni, Satya; Veeramani, Harish; Margot-Roquier, Camille; Webb, Samuel M.; Tebo, Bradley M.; Giammar, Daniel E.; Bargar, John R.; Bernier-Latmani, Rizlan

2011-11-01

It has generally been assumed that the bioreduction of hexavalent uranium in groundwater systems will result in the precipitation of immobile uraninite (UO 2). In order to explore the form and stability of uranium immobilized under these conditions, we introduced lactate (15 mM for 3 months) into flow-through columns containing sediments derived from a former uranium-processing site at Old Rifle, CO. This resulted in metal-reducing conditions as evidenced by concurrent uranium uptake and iron release. Despite initial augmentation with Shewanella oneidensis, bacteria belonging to the phylum Firmicutes dominated the biostimulated columns. The immobilization of uranium (˜1 mmol U per kg sediment) enabled analysis by X-ray absorption spectroscopy (XAS). Tetravalent uranium associated with these sediments did not have spectroscopic signatures representative of U-U shells or crystalline UO 2. Analysis by microfocused XAS revealed concentrated micrometer regions of solid U(IV) that had spectroscopic signatures consistent with bulk analyses and a poor proximal correlation (μm scale resolution) between U and Fe. A plausible explanation, supported by biogeochemical conditions and spectral interpretations, is uranium association with phosphoryl moieties found in biomass; hence implicating direct enzymatic uranium reduction. After the immobilization phase, two months of in situ exposure to oxic influent did not result in substantial uranium remobilization. Ex situ flow-through experiments demonstrated more rapid uranium mobilization than observed in column oxidation studies and indicated that sediment-associated U(IV) is more mobile than biogenic UO 2. This work suggests that in situ uranium bioimmobilization studies and subsurface modeling parameters should be expanded to account for non-uraninite U(IV) species associated with biomass.

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.

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.

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.

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)

Incorporation of Trace Elements in Ancient and Modern Human Bone: An X-Ray Absorption Spectroscopy Study

Science.gov (United States)

Pingitore, N. E.; Cruz-Jimenez, G.; Price, T. D.

2001-12-01

X-ray absorption spectroscopy (XAS) affords the opportunity to probe the atomic environment of trace elements in human bone. We are using XAS to investigate the mode(s) of incorporation of Sr, Zn, Pb, and Ba in both modern and ancient (and thus possibly altered) human and animal bone. Because burial and diagenesis may add trace elements to bone, we performed XAS analysis on samples of pristine contemporary and ancient, buried human and animal bone. We assume that deposition of these elements during burial occurs by processes distinct from those in vivo, and this will be reflected in their atomic environments. Archaeologists measure strontium in human and animal bone as a guide to diet. Carnivores show lower Sr/Ca ratios than their herbivore prey due to discrimination against Sr relative to Ca up the food chain. In an initial sample suite no difference was observed between modern and buried bone. Analysis of additional buried samples, using a more sensitive detector, revealed significant differences in the distance to the second and third neighbors of the Sr in some of the buried samples. Distances to the first neighbor, oxygen, were similar in all samples. Zinc is also used in paleo-diet studies. Initial x-ray absorption spectroscopy of a limited suite of bones did not reveal any differences between modern and buried samples. This may reflect the limited number of samples examined or the low levels of Zn in typical aqueous solutions in soils. Signals from barium and lead were too low to record useful XAS spectra. Additional samples will be studied for Zn, Ba, and Pb. We conducted our XAS experiments on beam lines 4-1 and 4-3 at the Stanford Synchrotron Radiation Laboratory. Data were collected in the fluorescence mode, using a Lytle detector and appropriate filter, and a solid state, 13-element Ge-detector.

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...

Construction of Bending Magnet Beamline at the APS for Environmental Studies

International Nuclear Information System (INIS)

Stern, E.A.

1999-01-01

The objective of this research was to design and construct a bending magnet beamline at the Advanced Photon Source. The beamline is to be optimized for x-ray absorption spectroscopy (XAS) studies with a major focus on environmental issues. The beamline will share the experimental facilities under development at the neighboring undulator-based insertion device beamline. It will utilize these facilities for XAS of both bulk and surface samples, with spatial and elemental imaging, on toxic and radioactive samples. It will help meet the rapidly growing need for the application of these techniques to environmental problems

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.

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...

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

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

Techno-economic and uncertainty analysis of in situ and ex situ fast pyrolysis for biofuel production

Energy Technology Data Exchange (ETDEWEB)

Li, Boyan; Ou, Longwen; Dang, Qi; Meyer, Pimphan A.; Jones, Susanne B.; Brown, Robert C.; Wright, Mark

2015-11-01

This study evaluates the techno-economic uncertainty in cost estimates for two emerging biorefinery technologies for biofuel production: in situ and ex situ catalytic pyrolysis. Stochastic simulations based on process and economic parameter distributions are applied to calculate biorefinery performance and production costs. The probability distributions for the minimum fuel-selling price (MFSP) indicate that in situ catalytic pyrolysis has an expected MFSP of $4.20 per gallon with a standard deviation of 1.15, while the ex situ catalytic pyrolysis has a similar MFSP with a smaller deviation ($4.27 per gallon and 0.79 respectively). These results suggest that a biorefinery based on ex situ catalytic pyrolysis could have a lower techno-economic risk than in situ pyrolysis despite a slightly higher MFSP cost estimate. Analysis of how each parameter affects the NPV indicates that internal rate of return, feedstock price, total project investment, electricity price, biochar yield and bio-oil yield are significant parameters which have substantial impact on the MFSP for both in situ and ex situ catalytic pyrolysis.

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

Impurity-related optical properties in rectangular-transverse section GaAs-Ga{sub 1-x}Al{sub x}As quantum well wires: Hydrostatic pressure and electric field effects

Energy Technology Data Exchange (ETDEWEB)

Gonzalez, J.W.; Duque, C.A. [Instituto de Fisica, Universidad de Antioquia, AA 1226, Medellin (Colombia); Lopez, S.Y. [Facultad de Educacion, Universidad de Antioquia, AA 1226, Medellin (Colombia); Rodriguez, A.H. [Instituto de Fisica, Universidad Nacional Autonoma de Mexico (UNAM), Apdo. Postal 20-364, San Angel 01000, Mexico DF (Mexico); Porras-Montenegro, N. [Departamento de Fisica, Universidad del Valle, AA 25360, Cali (Colombia)

2007-01-15

Using a variational procedure within the effective mass approximation, we have calculated the influence of an applied electric field and hydrostatic pressure on the shallow-impurity-related optical properties in a rectangular-transverse section GaAs-Ga{sub 1-x}Al{sub x}As quantum well wire. The electric field is applied in the plane of the transverse section of the wire and different angular directions have been considered. The results presented are for the impurity binding energy, its corresponding density of impurity states, and impurity-related transition energy and polarizability. (copyright 2007 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

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.

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 UO_2.00 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

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.

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

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.

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

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

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

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.

Actinide, lanthanide and fission product speciation and electrochemistry in high and low temperature ionic melts

Energy Technology Data Exchange (ETDEWEB)

Bhatt, Anand I.; Kinoshita, Hajime; Koster, Anne L.; May, Iain; Sharrad, Clint A.; Volkovich, Vladimir A.; Fox, O. Danny; Jones, Chris J.; Lewin, Bob G.; Charnock, John M.; Hennig, Christoph

2004-07-01

There is currently a great deal of research interest in the development of molten salt technology, both classical high temperature melts and low temperature ionic liquids, for the electrochemical separation of the actinides from spent nuclear fuel. We are interested in gaining a better understanding of actinide and key fission product speciation and electrochemical properties in a range of melts. Our studies in high temperature alkali metal melts (including LiCl and LiCl-KCl and CsCl-NaCl eutectics) have focussed on in-situ species of U, Th, Tc and Ru using X-ray absorption spectroscopy (XAS, both EXAFS and XANES) and electronic absorption spectroscopy (EAS). We report unusual actinide speciation in high temperature melts and an evaluation of the likelihood of Ru or Tc volatilization during plant operation. Our studies in lower temperature melts (ionic liquids) have focussed on salts containing tertiary alkyl group 15 cations and the bis(tri-fluor-methyl)sulfonyl)imide anion, melts which we have shown to have exceptionally wide electrochemical windows. We report Ln, Th, U and Np speciation (XAS, EAS and vibrational spectroscopy) and electrochemistry in these melts and relate the solution studies to crystallographic characterised benchmark species. (authors)

Actinide, lanthanide and fission product speciation and electrochemistry in high and low temperature ionic melts

International Nuclear Information System (INIS)

Bhatt, Anand I.; Kinoshita, Hajime; Koster, Anne L.; May, Iain; Sharrad, Clint A.; Volkovich, Vladimir A.; Fox, O. Danny; Jones, Chris J.; Lewin, Bob G.; Charnock, John M.; Hennig, Christoph

2004-01-01

There is currently a great deal of research interest in the development of molten salt technology, both classical high temperature melts and low temperature ionic liquids, for the electrochemical separation of the actinides from spent nuclear fuel. We are interested in gaining a better understanding of actinide and key fission product speciation and electrochemical properties in a range of melts. Our studies in high temperature alkali metal melts (including LiCl and LiCl-KCl and CsCl-NaCl eutectics) have focussed on in-situ species of U, Th, Tc and Ru using X-ray absorption spectroscopy (XAS, both EXAFS and XANES) and electronic absorption spectroscopy (EAS). We report unusual actinide speciation in high temperature melts and an evaluation of the likelihood of Ru or Tc volatilization during plant operation. Our studies in lower temperature melts (ionic liquids) have focussed on salts containing tertiary alkyl group 15 cations and the bis(tri-fluor-methyl)sulfonyl)imide anion, melts which we have shown to have exceptionally wide electrochemical windows. We report Ln, Th, U and Np speciation (XAS, EAS and vibrational spectroscopy) and electrochemistry in these melts and relate the solution studies to crystallographic characterised benchmark species. (authors)

Polluted soils with heavy metals. Stabilization by magnesium oxide. Ex-situ and in-situ testings; Suelos contaminados con metales pesados. Estabilizacion con oxido de magnesio. Ensayos ex situ-in situ

Energy Technology Data Exchange (ETDEWEB)

Cenoz, S.; Hernandez, J.; Gangutia, N.

2004-07-01

This work describes the use of Low-Grade MgO as a stabiliser agent for polluted soil reclaim. Low-Grade MgO may be an economically feasible alternative in the stabilisation of heavy metals from heavily contaminated soils. The effectiveness of Low-Grade MgO has been studied in three ex-situ stabilisation of heavily polluted soils contaminated by the flue-dust of pyrite roasting. LG-MgO provides an alkali reservoir guaranteeing long-term stabilisation without varying the pH conditions. The success of the ex-situ stabilisation was corroborated with the analysis of heavy metals in the leachates collected from the landfill o ver a long period of time. The study also includes the results obtained in an in-situ pilot scale stabilisation of contaminated soil. (Author) 17 refs.

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.

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.

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.

GaAs, AlAs, and AlxGa1-xAs: Material parameters for use in research and device applications

Science.gov (United States)

Adachi, Sadao

1985-08-01

The AlxGa1-xAs/GaAs heterostructure system is potentially useful material for high-speed digital, high-frequency microwave, and electro-optic device applications. Even though the basic AlxGa1-xAs/GaAs heterostructure concepts are understood at this time, some practical device parameters in this system have been hampered by a lack of definite knowledge of many material parameters. Recently, Blakemore has presented numerical and graphical information about many of the physical and electronic properties of GaAs [J. S. Blakemore, J. Appl. Phys. 53, R123 (1982)]. The purpose of this review is (i) to obtain and clarify all the various material parameters of AlxGa1-xAs alloy from a systematic point of view, and (ii) to present key properties of the material parameters for a variety of research works and device applications. A complete set of material parameters are considered in this review for GaAs, AlAs, and AlxGa1-xAs alloys. The model used is based on an interpolation scheme and, therefore, necessitates known values of the parameters for the related binaries (GaAs and AlAs). The material parameters and properties considered in the present review can be classified into sixteen groups: (1) lattice constant and crystal density, (2) melting point, (3) thermal expansion coefficient, (4) lattice dynamic properties, (5) lattice thermal properties, (6) electronic-band structure, (7) external perturbation effects on the band-gap energy, (8) effective mass, (9) deformation potential, (10) static and high-frequency dielectric constants, (11) magnetic susceptibility, (12) piezoelectric constant, (13) Fröhlich coupling parameter, (14) electron transport properties, (15) optical properties, and (16) photoelastic properties. Of particular interest is the deviation of material parameters from linearity with respect to the AlAs mole fraction x. Some material parameters, such as lattice constant, crystal density, thermal expansion coefficient, dielectric constant, and elastic constant

Voltammetric, in-situ spectroelectrochemical and in-situ electrocolorimetric characterization of phthalocyanines

Energy Technology Data Exchange (ETDEWEB)

Koca, Atif [Department of Chemical Engineering, Faculty of Engineering, Marmara University, Goeztepe, 34722 Istanbul (Turkey)], E-mail: akoca@eng.marmara.edu.tr; Bayar, Serife; Dincer, Hatice A. [Department of Chemistry, Technical University of Istanbul, Maslak, 34469 Istanbul (Turkey); Gonca, Erguen [Department of Chemistry, Fatih University, TR34500 B.Cekmece, Istanbul (Turkey)

2009-04-01

In this work, electrochemical, and in-situ spectroelectrochemical characterization of the metallophthalocyanines bearing tetra-(1,1-(dicarbethoxy)-2-(2-methylbenzyl))-ethyl 3,10,17,24-tetra chloro groups were performed. Voltammetric and in-situ spectroelectrochemical measurements show that while cobalt phthalocyanine complex gives both metal-based and ring-based redox processes, zinc and copper phthalocyanines show only ring-based reduction and oxidation processes. The redox processes are generally diffusion-controlled, reversible and one-electron transfer processes. Differently lead phthalocyanine demetallized during second oxidation reaction while it was stable during reduction processes. An in-situ electrocolorimetric method, based on the 1931 CIE (Commission Internationale de l'Eclairage) system of colorimetry, has been applied to investigate the color of the electro-generated anionic and cationic forms of the complexes for the first time in this study.

High covalence in CuSO4 and the radicalization of sulfate: an X-ray absorption and density functional study.

Science.gov (United States)

Szilagyi, Robert K; Frank, Patrick; DeBeer George, Serena; Hedman, Britt; Hodgson, Keith O

2004-12-27

Sulfur K-edge X-ray absorption spectroscopy (XAS) of anhydrous CuSO(4) reveals a well-resolved preedge transition feature at 2478.8 eV that has no counterpart in the XAS spectra of anhydrous ZnSO(4) or copper sulfate pentahydrate. Similar but weaker preedge features occur in the sulfur K-edge XAS spectra of [Cu(itao)SO(4)] (2478.4 eV) and [Cu[(CH(3))(6)tren]SO(4)] (2477.7 eV). Preedge features in the XAS spectra of transition metal ligands are generally attributed to covalent delocalization of a metal d-orbital hole into a ligand-based orbital. Copper L-edge XAS of CuSO(4) revealed that 56% of the Cu(II) 3d hole is delocalized onto the sulfate ligand. Hybrid density functional calculations on the two most realistic models of the covalent delocalization pathways in CuSO(4) indicate about 50% electron delocalization onto the sulfate oxygen-based 2p orbitals; however, at most 14% of that can be found on sulfate sulfur. Both experimental and computational results indicated that the high covalence of anhydrous CuSO(4) has made sulfate more like the radical monoanion, inducing an extensive mixing and redistribution of sulfur 3p-based unoccupied orbitals to lower energy in comparison to sulfate in ZnSO(4). It is this redistribution, rather than a direct covalent interaction between Cu(II) and sulfur, that is the origin of the observed sulfur XAS preedge feature. From pseudo-Voigt fits to the CuSO(4) sulfur K-edge XAS spectrum, a ground-state 3p character of 6% was quantified for the orbital contributing to the preedge transition, in reasonable agreement with the DFT calculation. Similar XAS fits indicated 2% sulfur 3p character for the preedge transition orbitals in [Cu(itao)SO(4)] and [Cu[(CH(3))(6)tren]SO(4)]. The covalent radicalization of ligands similar to sulfate, with consequent energy redistribution of the virtual orbitals, represents a new mechanism for the induction of ligand preedge XAS features. The high covalence of the Cu sites in CuSO(4) was found to be

Ex situ formation of metal selenide quantum dots using bacterially derived selenide precursors

International Nuclear Information System (INIS)

Fellowes, J W; Pattrick, R A D; Lloyd, J R; Charnock, J M; Coker, V S; Mosselmans, J F W; Weng, T-C; Pearce, C I

2013-01-01

Luminescent quantum dots were synthesized using bacterially derived selenide (Se II− ) as the precursor. Biogenic Se II− was produced by the reduction of Se IV by Veillonella atypica and compared directly against borohydride-reduced Se IV for the production of glutathione-stabilized CdSe and β-mercaptoethanol-stabilized ZnSe nanoparticles by aqueous synthesis. Biological Se II− formed smaller, narrower size distributed QDs under the same conditions. The growth kinetics of biologically sourced CdSe phases were slower. The proteins isolated from filter sterilized biogenic Se II− included a methylmalonyl-CoA decarboxylase previously characterized in the closely related Veillonella parvula. XAS analysis of the glutathione-capped CdSe at the S K-edge suggested that sulfur from the glutathione was structurally incorporated within the CdSe. A novel synchrotron based XAS technique was also developed to follow the nucleation of biological and inorganic selenide phases, and showed that biogenic Se II− is more stable and more resistant to beam-induced oxidative damage than its inorganic counterpart. The bacterial production of quantum dot precursors offers an alternative, ‘green’ synthesis technique that negates the requirement of expensive, toxic chemicals and suggests a possible link to the exploitation of selenium contaminated waste streams. (paper)

Ex Situ Formation of Metal Selenide Quantum Dots Using Bacterially Derived Selenide Precursors

Energy Technology Data Exchange (ETDEWEB)

Fellowes, Jonathan W.; Pattrick, Richard; Lloyd, Jon; Charnock, John M.; Coker, Victoria S.; Mosselmans, JFW; Weng, Tsu-Chien; Pearce, Carolyn I.

2013-04-12

Luminescent quantum dots were synthesized using bacterially derived selenide (SeII-) as the precursor. Biogenic SeII- was produced by the reduction of Se-IV by Veillonella atypica and compared directly against borohydride-reduced Se-IV for the production of glutathione-stabilized CdSe and beta-mercaptoethanol-stabilized ZnSe nanoparticles by aqueous synthesis. Biological SeII- formed smaller, narrower size distributed QDs under the same conditions. The growth kinetics of biologically sourced CdSe phases were slower. The proteins isolated from filter sterilized biogenic SeII- included a methylmalonyl-CoA decarboxylase previously characterized in the closely related Veillonella parvula. XAS analysis of the glutathione-capped CdSe at the S K-edge suggested that sulfur from the glutathione was structurally incorporated within the CdSe. A novel synchrotron based XAS technique was also developed to follow the nucleation of biological and inorganic selenide phases, and showed that biogenic SeII- is more stable and more resistant to beam-induced oxidative damage than its inorganic counterpart. The bacterial production of quantum dot precursors offers an alternative, 'green' synthesis technique that negates the requirement of expensive, toxic chemicals and suggests a possible link to the exploitation of selenium contaminated waste streams.

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

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

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)

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

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.

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

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....

Photoluminescence energy transitions in GaAs-Ga{sub 1-x}Al{sub x}As double quantum wells: Electric and magnetic fields and hydrostatic pressure effects

Energy Technology Data Exchange (ETDEWEB)

Lopez, S.Y. [Grupo de Educacion en Ciencias Experimentales y Matematicas-GECEM, Facultad de Educacion, Universidad de Antioquia, AA 1226 Medellin (Colombia); Mora-Ramos, M.E. [Facultad de Ciencias, Universidad Autonoma del Estado de Morelos, Av. Universidad 1001, CP 62209, Cuernavaca, Morelos (Mexico); Duque, C.A., E-mail: cduque@fisica.udea.edu.c [Instituto de Fisica, Universidad de Antioquia, AA 1226 Medellin (Colombia)

2009-12-15

The photoluminescence energy transitions in GaAs-Ga{sub 1-x}Al{sub x}As coupled double quantum wells are presented by considering the simultaneous effects of applied electric and magnetic fields and hydrostatic pressure. Calculations have been made in the framework of the effective mass and parabolic band approximations and using a variational procedure. The electric field is taken to be oriented along the growth direction of the heterostructure whereas for the magnetic field both in-plane and in-growth directions have been considered. The results show that the hydrostatic pressure and the applied electric field are two useful tools to tune the direct and indirect exciton transitions in such heterostructures. Our results are in good agreement with previous experimental findings in double quantum wells under applied electric field and hydrostatic pressure.

In-situ X-ray absorption spectroscopy analysis of capacity fade in nanoscale-LiCoO2

International Nuclear Information System (INIS)

Patridge, Christopher J.; Love, Corey T.; Swider-Lyons, Karen E.; Twigg, Mark E.; Ramaker, David E.

2013-01-01

The local structure of nanoscale (∼10–40 nm) LiCoO 2 is monitored during electrochemical cycling utilizing in-situ X-ray absorption spectroscopy (XAS). The high surface area of the LiCoO 2 nanoparticles not only enhances capacity fade, but also provides a large signal from the particle surface relative to the bulk. Changes in the nanoscale LiCoO 2 metal-oxide bond lengths, structural disorder, and chemical state are tracked during cycling by adapting the delta mu (Δμ) technique in complement with comprehensive extended X-ray absorption fine structure (EXAFS) modeling. For the first time, we use a Δμ EXAFS method, and by comparison of the difference EXAFS spectra, extrapolate significant coordination changes and reduction of cobalt species with cycling. This combined approach suggests Li–Co site exchange at the surface of the nanoscale LiCoO 2 as a likely factor in the capacity fade and irreversible losses in practical, microscale LiCoO 2 . - Graphical abstract: Electrochemical cycling of Li-ion batteries has strong impact on the structure and integrity of the cathode active material particularly near the surface/electrolyte interface. In developing a new method, we have used in-situ X-ray absorption spectroscopy during electrochemical cycling of nanoscale LiCoO 2 to track changes during charge and discharge and between subsequent cycles. Using difference spectra, several small changes in Co-O bond length, Co-O and Co-Co coordination, and site exchange between Co and Li sites can be tracked. These methods show promise as a new technique to better understand processes which lead to capacity fade and loss in Li-ion batteries. - Highlights: • A new method is developed to understand capacity fade in Li-ion battery cathodes. • Structural changes are tracked during Li intercalation/deintercalation of LiCoO 2 . • Surface structural changes are emphasized using nanoscale-LiCoO 2 and difference spectra. • Full multiple scattering calculations are used to

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.

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...

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

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.

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.)

Progress in KNbO/sub 3/ crystal growth and its use in second harmonic generation with a cw-Ga/sub 1-x/Al/sub x/As laser

International Nuclear Information System (INIS)

Looser, H.; Gunter, P.; Wu, X.; Arend, H.

1987-01-01

KNbO/sub 3/ is especially well suited for second harmonic generation of dye and Ga/sub 1-x/Al/sub x/As lasers with wavelength λ ≅ 860 nm. Using its high nonlinear optical coefficient, d/sub 32/ = 20.3 pm/V, noncritical type l phase matching is possible for fundamental wavelengths of 840-990 nm with crystal temperatures between -40 and 210 0 C. With a pulsed laser diode the authors previously reported 0.35-mW second harmonic peak power from 0.8-W fundamental frequency distributed among eight modes. In this paper, this work is extended to high-power monomode cw laser diodes. Other device parameters such as temperature stability and influence of the crystal homogeneity on the efficiency are discussed

Condensation mechanisms of tetravalent technetium in chloride media

International Nuclear Information System (INIS)

Poineau, F.

2004-10-01

In deep storage technetium can exist in degree IV or III. Recent studies on Tc(IV) have shown that Tc n O y (4n-2y)+ , Tc IV (μ-O) 2 Tc IV structure, is a precursor for precipitation of TcO 2 . Few data are available on Tc n O y (4n-2y)+ Subject of this thesis is the mechanism of condensation of Tc(IV) leading to this form. Kinetic studies have shown that the condensation of Tc IV Cl 5 (H 2 O) - in chloride media leads to a dimer. XAS studies resulted in a linear structure Tc IV -O-Tc IV . This compound, formulated as Tc 2 OCl 10 4- , is stable at pH = 0.3, it undergoes cyclization to Tc n O y (4n-2y)+ at pH =1.5 and is oxidized to TcO 4 - under α radiation. In 3 M chloride media, TcO 2 lead to formation Tc 2 OCl 10 4- at pH = 0.3 and to Tc n O y (4n-2y)+ at pH = 1.5. An electrochemical cell permitting 'in situ' XAS measurement was developed. XANES studies have shown that the reduction of Tc(VII) lead to a Tc(IV)/Tc(III) mixture. (author)

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.

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.

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...

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

In situ and ex situ modifications of bacterial cellulose for applications in tissue engineering.

Science.gov (United States)

Stumpf, Taisa Regina; Yang, Xiuying; Zhang, Jingchang; Cao, Xudong

2018-01-01

Bacterial cellulose (BC) is secreted by a few strains of bacteria and consists of a cellulose nanofiber network with unique characteristics. Because of its excellent mechanical properties, outstanding biocompatibilities, and abilities to form porous structures, BC has been studied for a variety of applications in different fields, including the use as a biomaterial for scaffolds in tissue engineering. To extend its applications in tissue engineering, native BC is normally modified to enhance its properties. Generally, BC modifications can be made by either in situ modification during cell culture or ex situ modification of existing BC microfibers. In this review we will first provide a brief introduction of BC and its attributes; this will set the stage for in-depth and up-to-date discussions on modified BC. Finally, the review will focus on in situ and ex situ modifications of BC and its applications in tissue engineering, particularly in bone regeneration and wound dressing. Copyright © 2016. Published by Elsevier B.V.

Coherent-potential approximation for vibrations in Ga/sub 1-x/In/sub x/Sb and Ga/sub 1-x/In/sub x/As mixed crystals

International Nuclear Information System (INIS)

Kleinert, P.

1982-01-01

The vibrational properties of the mixed crystals Ga/sub 1-x/In/sub x/As and Ga/sub 1-x/In/sub x/Sb are investigated using the coherent-potential approximation (CPA). These III-V systems switch from one-mode to two-mode behaviour as the composition is changed. Results are obtained for a one-dimensional model including self-consistently mass defects and force constant changes. The calculated density of states and the dielectric susceptibility are compared with results of the mass CPA. In addition, a three-dimensional CPA Bethe lattice treatment is carried out to calculate the optical properties of these disordered systems showing mixed-mode behaviour. The force-constant change is included by a virtual-crystal interpolation. The theory explains the mode switching behaviour and agrees fairly well with experimental peak positions and line shapes of the response function. (author)

Surface Chemistry and Tribology of Copper Surfaces in Carbon Dioxide and Water Vapor Environments

Science.gov (United States)

2011-02-23

state that the copper brushes in the superconducting homopolar motor experience wear at rates greater than 3X10" wear /distance traveled when biased...positively. It has been found the motor operates best in an atmosphere of carbon dioxide and water vapor. The objective of our research therefore is...possible to prepare different chemical states of the Cu, as those produced in the motor electrodes under positive and negative bias. In situ XAS

Breeding of in-situ Petroleum Degrading Bacteria in Hangzhou Bay and evaluating for the In-situ repair effect

Science.gov (United States)

Lan, Ru; Lin, Hai; Qiao, Bing; Dong, Yingbo; Zhang, Wei; Chang, Wen

2018-02-01

In this paper, the restoration behaviour of the in-situ microorganisms in seawater and sediments to the marine accident oil spill was researched. The experimental study on the breeding of in-situ petroleum-degrading bacteria in the seawater and sediments of Hangzhou Bay and the restoration of oil spill were carried out. Making use of the reinforced microbial flora, combined with physical and chemical methods in field environment, petroleum degrading and restoration experiment were performed, the effect of the breeding of in-situ degrading bacteria was evaluated, and the standard process of in-situ bacteria sampling, laboratory screening, domestication and degradation efficiency testing were formed. This study laid a foundation for further evaluation of the advantages and disadvantages for the petroleum-degrading bacteria of Hangzhou Bay during the process of in-situ restoration. The results showed that in-situ microbes of Hangzhou Bay could reach the growth peak in 5 days with the suitable environmental factors and sufficient nutrient elements, and the degradation efficiency could reach 65.2% (or 74.8% after acclimation). And also the microbes could adapt to the local sea water and environmental conditions, with a certain degree of degradation. The research results could provide parameter support for causal judgment and quantitative assessment of oil spill damage.

Soft X-ray Absorption Spectroscopy of Liquids and Solutions.

Science.gov (United States)

Smith, Jacob W; Saykally, Richard J

2017-12-13

X-ray absorption spectroscopy (XAS) is an electronic absorption technique for which the initial state is a deeply buried core level. The photon energies corresponding to such transitions are governed primarily by the binding energies of the initial state. Because the binding energies of core electrons vary significantly among atomic species, this makes XAS an element-selective spectroscopy. Proper interpretation of XA spectra can provide detailed information on the local chemical and geometric environment of the target atom. The introduction of liquid microjet and flow cell technologies into XAS experiments has enabled the general study of liquid samples. Liquids studied to date include water, alcohols, and solutions with relevance to biology and energy technology. This Review summarizes the experimental techniques employed in XAS studies of liquid samples and computational methods used for interpretation of the resulting spectra and summarizes salient experiments and results obtained in the XAS investigations of liquids.

In-situ X-ray absorption spectroscopy analysis of capacity fade in nanoscale-LiCoO{sub 2}

Energy Technology Data Exchange (ETDEWEB)

Patridge, Christopher J. [NRC/NRL Cooperative Research Associate, U.S. Naval Research Laboratory, Washington, DC 20375 (United States); Love, Corey T., E-mail: corey.love@nrl.navy.mil [Chemistry Division, Code 6113, U.S. Naval Research Laboratory, Washington, DC 20375 (United States); Swider-Lyons, Karen E. [Chemistry Division, Code 6113, U.S. Naval Research Laboratory, Washington, DC 20375 (United States); Twigg, Mark E. [Electronics Science and Technology Division, Code 6812, U.S. Naval Research Laboratory, Washington, DC 20375 (United States); Ramaker, David E. [Chemistry Division, Code 6189, U.S. Naval Research laboratory, Washington, DC 20375 (United States)

2013-07-15

The local structure of nanoscale (∼10–40 nm) LiCoO{sub 2} is monitored during electrochemical cycling utilizing in-situ X-ray absorption spectroscopy (XAS). The high surface area of the LiCoO{sub 2} nanoparticles not only enhances capacity fade, but also provides a large signal from the particle surface relative to the bulk. Changes in the nanoscale LiCoO{sub 2} metal-oxide bond lengths, structural disorder, and chemical state are tracked during cycling by adapting the delta mu (Δμ) technique in complement with comprehensive extended X-ray absorption fine structure (EXAFS) modeling. For the first time, we use a Δμ EXAFS method, and by comparison of the difference EXAFS spectra, extrapolate significant coordination changes and reduction of cobalt species with cycling. This combined approach suggests Li–Co site exchange at the surface of the nanoscale LiCoO{sub 2} as a likely factor in the capacity fade and irreversible losses in practical, microscale LiCoO{sub 2}. - Graphical abstract: Electrochemical cycling of Li-ion batteries has strong impact on the structure and integrity of the cathode active material particularly near the surface/electrolyte interface. In developing a new method, we have used in-situ X-ray absorption spectroscopy during electrochemical cycling of nanoscale LiCoO{sub 2} to track changes during charge and discharge and between subsequent cycles. Using difference spectra, several small changes in Co-O bond length, Co-O and Co-Co coordination, and site exchange between Co and Li sites can be tracked. These methods show promise as a new technique to better understand processes which lead to capacity fade and loss in Li-ion batteries. - Highlights: • A new method is developed to understand capacity fade in Li-ion battery cathodes. • Structural changes are tracked during Li intercalation/deintercalation of LiCoO{sub 2}. • Surface structural changes are emphasized using nanoscale-LiCoO{sub 2} and difference spectra. • Full multiple

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

X-ray absorption spectroscopy and EPR studies of oriented spinach thylakoid preparations

Energy Technology Data Exchange (ETDEWEB)

Andrews, J.C. [Univ. of California, Berkeley, CA (United States). Dept. of Chemistry]|[Lawrence Berkeley Lab., CA (United States). Structural Biology Div.

1995-08-01

In this study, oriented Photosystem II (PS II) particles from spinach chloroplasts are studied with electron paramagnetic resonance (EPR) and x-ray absorption spectroscopy (XAS) to determine more details of the structure of the oxygen evolving complex (OEC). The nature of halide binding to Mn is also studied with Cl K-edge and Mn EXAFS (extended x-ray absorption fine structure) of Mn-Cl model compounds, and with Mn EXAFS of oriented PS II in which Br has replaced Cl. Attention is focused on the following: photosynthesis and the oxygen evolving complex; determination of mosaic spread in oriented photosystem II particles from signal II EPR measurement; oriented EXAFS--studies of PS II in the S{sub 2} state; structural changes in PS II as a result of treatment with ammonia: EPR and XAS studies; studies of halide binding to Mn: Cl K-edge and Mn EXAFS of Mn-Cl model compounds and Mn EXAFS of oriented Br-treated photosystem II.

Structural and optical high-pressure study of spinel-type MnIn2S4

International Nuclear Information System (INIS)

Manjon, F.J.; Segura, A.; Pellicer-Porres, J.; Sanchez-Royo, J.F.; Amboage, M.; Itie, J.P.; Flank, A.M.; Lagarde, P.; Polian, A.; Ursaki, V.V.; Tiginyanu, I.M.

2007-01-01

We report a combined study of the structural and electronic properties of the spinel-type semiconductor MnIn 2 S 4 under high pressures by means of X-ray diffraction (ADXRD), X-ray absorption (XAS), and optical absorption measurements. The three techniques evidence a reversible structural phase transition near 7 GPa, that according to ADXRD measurements is to a double-NaCl structure. XAS measurements evidence predominant tetrahedral coordination for Mn in the spinel phase that does not noticeably change with increasing pressure up to the phase transition. XAS measurements indicate that the static disorder increases considerably when the sample reverts from the double-NaCl phase to the spinel phase. Optical absorption measurements show that the direct gap of MnIn 2 S 4 exhibits a nonlinear behaviour with a positive pressure coefficient at pressures below 2.5 GPa and a negative pressure coefficient between 2.5 and 7 GPa. The pressure behavior of the bandgap seems to be affected by the defect concentration. The double-NaCl phase also exhibits a bandgap with a negative pressure coefficient. (copyright 2007 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

Ex-situ and in-situ mineral carbonation as a means to sequester carbon dioxide

Energy Technology Data Exchange (ETDEWEB)

Gerdemann, Stephen J.; Dahlin, David C.; O' Connor, William K.; Penner, Larry R.; Rush, G.E.

2004-01-01

The U. S. Department of Energy's Albany Research Center is investigating mineral carbonation as a method of sequestering CO2 from coal-fired-power plants. Magnesium-silicate minerals such as serpentine [Mg3Si2O5(OH)4] and olivine (Mg2SiO4) react with CO2 to produce magnesite (MgCO3), and the calcium-silicate mineral, wollastonite (CaSiO3), reacts to form calcite (CaCO3). It is possible to carry out these reactions either ex situ (above ground in a traditional chemical processing plant) or in situ (storage underground and subsequent reaction with the host rock to trap CO2 as carbonate minerals). For ex situ mineral carbonation to be economically attractive, the reaction must proceed quickly to near completion. The reaction rate is accelerated by raising the activity of CO2 in solution, heat (but not too much), reducing the particle size, high-intensity grinding to disrupt the crystal structure, and, in the case of serpentine, heat-treatment to remove the chemically bound water. All of these carry energy/economic penalties. An economic study illustrates the impact of mineral availability and process parameters on the cost of ex situ carbon sequestration. In situ carbonation offers economic advantages over ex situ processes, because no chemical plant is required. Knowledge gained from the ex situ work was applied to long-term experiments designed to simulate in situ CO2 storage conditions. The Columbia River Basalt Group (CRBG), a multi-layered basaltic lava formation, has potentially favorable mineralogy (up to 25% combined concentration of Ca, Fe2+, and Mg cations) for storage of CO2. However, more information about the interaction of CO2 with aquifers and the host rock is needed. Core samples from the CRBG, as well as samples of olivine, serpentine, and sandstone, were reacted in an autoclave for up to 2000 hours at elevated temperatures and pressures. Changes in core porosity, secondary mineralizations, and both solution and solid chemistry were measured.

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...

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.

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

Improved Oxygen Reduction Activity and Durability of Dealloyed PtCox Catalysts for Proton Exchange Membrane Fuel Cells: Strain, Ligand, and Particle Size Effects

Science.gov (United States)

Jia, Qingying; Caldwell, Keegan; Strickland, Kara; Ziegelbauer, Joseph M.; Liu, Zhongyi; Yu, Zhiqiang; Ramaker, David E.; Mukerjee, Sanjeev

2015-01-01

The development of active and durable catalysts with reduced platinum content is essential for fuel cell commercialization. Herein we report that the dealloyed PtCo/HSC and PtCo3/HSC nanoparticle (NP) catalysts exhibit the same levels of enhancement in oxygen reduction activity (~4-fold) and durability over pure Pt/C NPs. Surprisingly, ex situ high-angle annular dark field scanning transmission electron microscopy (HAADF STEM) shows that the bulk morphologies of the two catalysts are distinctly different: D-PtCo/HSC catalyst is dominated by NPs with solid Pt shells surrounding a single ordered PtCo core; however, the D-PtCo3/HSC catalyst is dominated by NPs with porous Pt shells surrounding multiple disordered PtCo cores with local concentration of Co. In situ X-ray absorption spectroscopy (XAS) reveals that these two catalysts possess similar Pt–Pt and Pt–Co bond distances and Pt coordination numbers (CNs), despite their dissimilar morphologies. The similar activity of the two catalysts is thus ascribed to their comparable strain, ligand, and particle size effects. Ex situ XAS performed on D-PtCo3/HSC under different voltage cycling stage shows that the continuous dissolution of Co leaves behind the NPs with a Pt-like structure after 30k cycles. The attenuated strain and/or ligand effects caused by Co dissolution are presumably counterbalanced by the particle size effects with particle growth, which likely accounts for the constant specific activity of the catalysts along with voltage cycling. PMID:26413384

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.

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.

Characterization of VPO ammoxidation catalysts by in situ methods

Energy Technology Data Exchange (ETDEWEB)

Martin, A.; Luecke, B.; Brueckner, A.; Steinike, U. [Institut fuer Angewandte Chemie Berlin-Adlershof e.V., Berlin (Germany); Brzezinka, K.W. [Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin (Germany); Meisel, M. [Humboldt-Universitaet, Berlin (Germany). Inst. fuer Chemie

1998-12-31

In-situ methods are well known as powerful tools in studying catalyst formation processes, their solid state properties under working conditions and the interaction with the feed, intermediates and products to reveal reaction mechanisms. This paper gives a short overview on results of intense studies using in-situ techniques to reveal VPO catalyst generation processes, interaction of educts, intermediates and products with VPO catalyst surfaces and mechanistic insights. Catalytic data of the ammoxidation of toluene on different VPOs complete these findings. The precursor-catalyst transformation processes were preferently investigated by in-situ XRD, in-situ Raman and in-situ ESR spectroscopy. The interaction of aromatic molecules and intermediates, resp., and VPO solid surfaces was followed by in-situ ESR and in-situ FTIR spectroscopy. Mechanistic information was mainly obtained using in-situ FTIR spectroscopy and the temporal-analysis-of-products (TAP) technique. Catalytic studies were carried out in a fixed-bed microreactor on pure (NH{sub 4}){sub 2}(VO){sub 3}(P{sub 2}O{sub 7}){sub 2}, generated [(NH{sub 4}){sub 2}(VO{sub 3})(P{sub 2}O{sub 7}){sub 2}+V{sub x}O{sub y}] catalysts, having different V{sub x}O{sub y} proportions by use of VOHPO{sub 4} x 1/2H{sub 2}O (V/P=1) and recently studied (VO){sub 3}(PO{sub 4}){sub 2} x 7 H{sub 2}O (V/P=1.5) precursors; the well-known (VO){sub 2}P{sub 2}O{sub 7} was used for comparison. (orig.)

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.

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

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: �

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

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

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)

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...

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

In-Situ Burning of Crude Oil on Water

DEFF Research Database (Denmark)

van Gelderen, Laurens

in the small scale water basin. Boilovers were also observed during the burning of a heavy crude oil with a substantial light fraction without a water layer, however, which suggests that water is not essential for boilover occurrence. Further studies are required to determine the conditions under which......The fire dynamics and fire chemistry of in-situ burning of crude oil on water was studied in order to improve predictions on the suitability of this oil spill response method. For this purpose, several operational parameters were studied to determine the factors that control the burning efficiency...... of in-situ burning, i.e. the amount of oil (in wt%) removed from the water surface by the burning process. The burning efficiency is the main parameter for expressing the oil removal effectiveness of in-situ burning as response method and is thus relevant for suitability predictions of in-situ burning...

In Situ TEM Electrical Measurements

DEFF Research Database (Denmark)

Canepa, Silvia; Alam, Sardar Bilal; Ngo, Duc-The

2016-01-01

understanding of complex physical and chemical interactions in the pursuit to optimize nanostructure function and device performance. Recent developments of sample holder technology for TEM have enabled a new field of research in the study of functional nanomaterials and devices via electrical stimulation...... influence the sample by external stimuli, e.g. through electrical connections, the TEM becomes a powerful laboratory for performing quantitative real time in situ experiments. Such TEM setups enable the characterization of nanostructures and nanodevices under working conditions, thereby providing a deeper...... and measurement of the specimen. Recognizing the benefits of electrical measurements for in situ TEM, many research groups have focused their effort in this field and some of these methods have transferred to ETEM. This chapter will describe recent advances in the in situ TEM investigation of nanostructured...

Automatic reduction of large X-ray fluorescence data-sets applied to XAS and mapping experiments

International Nuclear Information System (INIS)

Martin Montoya, Ligia Andrea

2017-02-01

In this thesis two automatic methods for the reduction of large fluorescence data sets are presented. The first method is proposed in the framework of BioXAS experiments. The challenge of this experiment is to deal with samples in ultra dilute concentrations where the signal-to-background ratio is low. The experiment is performed in fluorescence mode X-ray absorption spectroscopy with a 100 pixel high-purity Ge detector. The first step consists on reducing 100 fluorescence spectra into one. In this step, outliers are identified by means of the shot noise. Furthermore, a fitting routine which model includes Gaussian functions for the fluorescence lines and exponentially modified Gaussian (EMG) functions for the scattering lines (with long tails at lower energies) is proposed to extract the line of interest from the fluorescence spectrum. Additionally, the fitting model has an EMG function for each scattering line (elastic and inelastic) at incident energies where they start to be discerned. At these energies, the data reduction is done per detector column to include the angular dependence of scattering. In the second part of this thesis, an automatic method for texts separation on palimpsests is presented. Scanning X-ray fluorescence is performed on the parchment, where a spectrum per scanned point is collected. Within this method, each spectrum is treated as a vector forming a basis which is to be transformed so that the basis vectors are the spectra of each ink. Principal Component Analysis is employed as an initial guess of the seek basis. This basis is further transformed by means of an optimization routine that maximizes the contrast and minimizes the non-negative entries in the spectra. The method is tested on original and self made palimpsests.

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.

Theoretical x-ray absorption investigation of high pressure ice and compressed graphite

International Nuclear Information System (INIS)

Shaw, Dawn M; Tse, John S

2007-01-01

The x-ray absorption spectra (XAS) of high pressure ices II, VIII, and IX have been computed with the Car-Parrinello plane wave pseudopotential method. XAS for the intermediate structures obtained from uniaxial compression of hexagonal graphite along the c-axis are also studied. Whenever possible, comparisons to available experimental results are made. The reliability of the computational methods for the XAS for these structures is discussed

X-ray absorption spectroscopy study on the thermal and hydrazine reduction of graphene oxide

International Nuclear Information System (INIS)

Liang, Xianqing; Wang, Yu; Zheng, Huiyuan; Wu, Ziyu

2014-01-01

Highlights: • XAS study of GO and reduced GO was performed. • Detailed evolution of the electronic structures and chemical bonding of GO was revealed. • A new efficient route for the reduction of GO is proposed. - Abstract: X-ray absorption spectroscopy (XAS) was applied to systemically investigate the deoxygenation of graphene oxide (GO) via annealing and hydrazine treatment. Detailed evolution of the electronic structures and chemical bonding of GO was presented. The enhanced intensity of π * resonance and the appearance of splitting σ * resonance in C K-edge XAS spectra suggest high extents of recoveries of π-conjugation upon reduction using thermal annealing or hydrazine. Experimental results revealed that the carboxyl as well as epoxide and hydroxyl groups on the surface of GO were thermally reduced first, followed by the more difficult removal of carbonyl and cyclic ether groups at higher temperatures. The hydrazine reduction could remove epoxide, hydroxyl and carboxyl groups effectively, whereas the carbonyl groups were partially reduced with the incorporation of nitrogen species simultaneously. The residual oxygen functional groups on hydrazine-reduced GO could be further removed after modest thermal annealing. It was proposed that a combination of both types of reductions would give the best deoxygenation efficiency for the production of graphene

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...

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

In situ vitrification program treatability investigation progress report

International Nuclear Information System (INIS)

Arrenholz, D.A.

1991-02-01

This document presents a summary of the efforts conducted under the in situ vitrification treatability study during the period from its initiation in FY-88 until FY-90. In situ vitrification is a thermal treatment process that uses electrical power to convert contaminated soils into a chemically inert and stable glass and crystalline product. Contaminants present in the soil are either incorporated into the product or are pyrolyzed during treatment. The treatability study being conducted at the Idaho National Engineering Laboratory by EG ampersand G Idaho is directed at examining the specific applicability of the in situ vitrification process to buried wastes contaminated with transuranic radionuclides and other contaminants found at the Subsurface Disposal Area of the Radioactive Waste Management Complex. This treatability study consists of a variety of tasks, including engineering tests, field tests, vitrified product evaluation, and analytical models of the in situ vitrification process. 6 refs., 4 figs., 3 tabs

An X-ray absorption spectroscopy study of the interactions of Ni2+ with yeast enolase.

Science.gov (United States)

Wang, S; Scott, R A; Lebioda, L; Zhou, Z H; Brewer, J M

1995-05-15

An x-ray absorption spectroscopy (XAS) study was carried out at pH 7.6 on solutions of Ni2+ and yeast enolase depleted of its physiological cofactor (Mg2+) in the presence or absence of substrate/product, the very strongly bound competitive inhibitor 2-phosphonoacetohydroxamate and Mg2+. Both "conformational" and "catalytic" Ni2+ are distorted octahedral in coordination, in agreement with several spectroscopic studies but in contrast to the coordination in the crystal at pH 6.0. The data are consistent with direct coordination of what must be the catalytic Ni2+ to the phosphate of the substrate, in agreement with some previous data but in disagreement with recent interpretations by other workers. The ligands around the metal ions obtained from the x-ray structure give simulated XAS spectra in good agreement with the observed spectra.

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

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.

Mechanisms of uranium interactions with hydroxyapatite: Implications for groundwater remediation

Science.gov (United States)

Fuller, C.C.; Bargar, J.R.; Davis, J.A.; Piana, M.J.

2002-01-01

The speciation of U(VI) sorbed to synthetic hydroxyapatite was investigated using a combination of U LIII-edge XAS, synchrotron XRD, batch uptake measurements, and SEM-EDS. The mechanisms of U(VI) removal by apatite were determined in order to evaluate the feasibility of apatitebased in-situ permeable reactive barriers (PRBs). In batch U(VI) uptake experiments with synthetic hydroxyapatite (HA), near complete removal of dissolved uranium (>99.5%) to use in development of PRBs for groundwater U(VI) remediation.

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.

Double-staining chromogenic in situ hybridization as a useful alternative to split-signal fluorescence in situ hybridization in lymphoma diagnostics

DEFF Research Database (Denmark)

van Rijk, A.; Svenstroup-Poulsen, T.; Jones, M.

2010-01-01

within the reach of every pathology laboratory. Design and Methods Our study was initiated to determine the consistency between chromogenic in situ hybridization and fluorescence in situ hybridization, both using split-signal probes developed for the detection of chromosomal breaks. Five hundred...... and actual signal were compared to the original fluorescence hybridization results. In addition, hematoxylin background staining intensity and signal intensity of the double-staining chromogenic in situ hybridization procedure were analyzed. Results With respect to the presence or absence of chromosomal...

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

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

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.

Investigation of Co nanoparticle formation using time-dependent and spatially-resolved X-ray absorption spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Zinoveva, S

2008-04-15

A crucial step towards controlled synthesis of nanoparticles is the detailed understanding of the various chemical processes that take place during the synthesis. X-ray Absorption Spectroscopy (XAS) is especially suitable for elucidating the type and structure of the intermediate metal species. It is applicable to materials that have no long range order and provides information on both electronic and geometric structures. Here a comparative study is reported of the formation of cobalt nanoparticles via thermolysis of two organometallic precursors dicobalt octacarbonyl (DCO) and alkyne-bridged dicobalt hexacarbonyl (ADH) in the presence of aluminum organics. Using time-dependent XAS a reaction pathway different from both the atom based La Mer model and the Watzky and Finsky autocatalytic surface growth model is observed. Where prior to the nucleation several intermediates are formed and the initial nucleus is composed of Co atoms coordinated with ligands Co{sub n}(CO){sub m} with n=2-3, m=3-5. The formation of Co nanoparticles was also investigated using a reaction different from thermolysis of cobalt carbonyls, namely reduction of Co (II) acetate by sodium borohydrate. Here the combination of microreactor system and spatially resolved XAS allowed ''in situ'' monitoring of the wet chemical synthesis. Several steps of the reaction were spatially resolved in the microreactor. The vertical size of the X-ray beam (50 {mu}m) focused with Kirkpatrick-Baez mirror system, determines the time resolution (better than 2 ms). The results provide direct insight into rapid process of nanoparticles formation and demonstrate the potential of this new technique for the fundamental studies of such type of processes where miniaturization and timeresolution are important. Like in the carbonyls thermolysis no evidence for the reduction of the starting complex to isolated Co{sup 0} atoms followed by nucleation of Co{sup 0} atoms was observed. (orig.)

Investigation of Co nanoparticle formation using time-dependent and spatially-resolved X-ray absorption spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Zinoveva, S.

2008-04-15

A crucial step towards controlled synthesis of nanoparticles is the detailed understanding of the various chemical processes that take place during the synthesis. X-ray Absorption Spectroscopy (XAS) is especially suitable for elucidating the type and structure of the intermediate metal species. It is applicable to materials that have no long range order and provides information on both electronic and geometric structures. Here a comparative study is reported of the formation of cobalt nanoparticles via thermolysis of two organometallic precursors dicobalt octacarbonyl (DCO) and alkyne-bridged dicobalt hexacarbonyl (ADH) in the presence of aluminum organics. Using time-dependent XAS a reaction pathway different from both the atom based La Mer model and the Watzky and Finsky autocatalytic surface growth model is observed. Where prior to the nucleation several intermediates are formed and the initial nucleus is composed of Co atoms coordinated with ligands Co{sub n}(CO){sub m} with n=2-3, m=3-5. The formation of Co nanoparticles was also investigated using a reaction different from thermolysis of cobalt carbonyls, namely reduction of Co (II) acetate by sodium borohydrate. Here the combination of microreactor system and spatially resolved XAS allowed ''in situ'' monitoring of the wet chemical synthesis. Several steps of the reaction were spatially resolved in the microreactor. The vertical size of the X-ray beam (50 {mu}m) focused with Kirkpatrick-Baez mirror system, determines the time resolution (better than 2 ms). The results provide direct insight into rapid process of nanoparticles formation and demonstrate the potential of this new technique for the fundamental studies of such type of processes where miniaturization and timeresolution are important. Like in the carbonyls thermolysis no evidence for the reduction of the starting complex to isolated Co{sup 0} atoms followed by nucleation of Co{sup 0} atoms was observed. (orig.)

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.

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

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.

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.

''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

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)

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)

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

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.

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.

Engineering feasibility analysis for in-situ stabilization of Canonsburg residues

International Nuclear Information System (INIS)

1982-01-01

The US Department of Energy is considering several methods for carrying out remedial actions in Canonsburg, Pennsylvania, at the site of an inactive uranium-processing mill. The main objective of this study is to determine the feasibility of in-situ stabilization as the remedial action. In-situ stabilization is an alternative to site decontamination and offsite disposal. The problems associated with offsite hauling of large quantities of contaminated material and with the location and development of a new disposal site could be avoided by the implementation of an in-situ stabilization concept. In addition, the in-situ approach would be more cost-effective than offsite disposal. This study will establish that a technically feasible and implementable in-situ stabilization concept can be developed that meets regulatory requirements and is cost effective. This study in no way commits the DOE to implement any specific actions described herein. 11 refs., 30 figs., 24 tabs

In situ macromolecular crystallography using microbeams

International Nuclear Information System (INIS)

Axford, Danny; Owen, Robin L.; Aishima, Jun; Foadi, James; Morgan, Ann W.; Robinson, James I.; Nettleship, Joanne E.; Owens, Raymond J.; Moraes, Isabel; Fry, Elizabeth E.; Grimes, Jonathan M.; Harlos, Karl; Kotecha, Abhay; Ren, Jingshan; Sutton, Geoff; Walter, Thomas S.; Stuart, David I.; Evans, Gwyndaf

2012-01-01

A sample environment for mounting crystallization trays has been developed on the microfocus beamline I24 at Diamond Light Source. The technical developments and several case studies are described. Despite significant progress in high-throughput methods in macromolecular crystallography, the production of diffraction-quality crystals remains a major bottleneck. By recording diffraction in situ from crystals in their crystallization plates at room temperature, a number of problems associated with crystal handling and cryoprotection can be side-stepped. Using a dedicated goniometer installed on the microfocus macromolecular crystallography beamline I24 at Diamond Light Source, crystals have been studied in situ with an intense and flexible microfocus beam, allowing weakly diffracting samples to be assessed without a manual crystal-handling step but with good signal to noise, despite the background scatter from the plate. A number of case studies are reported: the structure solution of bovine enterovirus 2, crystallization screening of membrane proteins and complexes, and structure solution from crystallization hits produced via a high-throughput pipeline. These demonstrate the potential for in situ data collection and structure solution with microbeams

In situ macromolecular crystallography using microbeams

Energy Technology Data Exchange (ETDEWEB)

Axford, Danny; Owen, Robin L.; Aishima, Jun [Diamond Light Source, Harwell Science and Innovation Campus, Didcot, Oxfordshire OX11 0DE (United Kingdom); Foadi, James [Diamond Light Source, Harwell Science and Innovation Campus, Didcot, Oxfordshire OX11 0DE (United Kingdom); Imperial College, London SW7 2AZ (United Kingdom); Morgan, Ann W.; Robinson, James I. [University of Leeds, Leeds LS9 7FT (United Kingdom); Nettleship, Joanne E.; Owens, Raymond J. [Research Complex at Harwell, Rutherford Appleton Laboratory R92, Didcot, Oxfordshire OX11 0DE (United Kingdom); Moraes, Isabel [Imperial College, London SW7 2AZ (United Kingdom); Fry, Elizabeth E.; Grimes, Jonathan M.; Harlos, Karl; Kotecha, Abhay; Ren, Jingshan; Sutton, Geoff; Walter, Thomas S. [University of Oxford, Roosevelt Drive, Oxford OX3 7BN (United Kingdom); Stuart, David I. [Diamond Light Source, Harwell Science and Innovation Campus, Didcot, Oxfordshire OX11 0DE (United Kingdom); University of Oxford, Roosevelt Drive, Oxford OX3 7BN (United Kingdom); Evans, Gwyndaf, E-mail: gwyndaf.evans@diamond.ac.uk [Diamond Light Source, Harwell Science and Innovation Campus, Didcot, Oxfordshire OX11 0DE (United Kingdom)

2012-04-17

A sample environment for mounting crystallization trays has been developed on the microfocus beamline I24 at Diamond Light Source. The technical developments and several case studies are described. Despite significant progress in high-throughput methods in macromolecular crystallography, the production of diffraction-quality crystals remains a major bottleneck. By recording diffraction in situ from crystals in their crystallization plates at room temperature, a number of problems associated with crystal handling and cryoprotection can be side-stepped. Using a dedicated goniometer installed on the microfocus macromolecular crystallography beamline I24 at Diamond Light Source, crystals have been studied in situ with an intense and flexible microfocus beam, allowing weakly diffracting samples to be assessed without a manual crystal-handling step but with good signal to noise, despite the background scatter from the plate. A number of case studies are reported: the structure solution of bovine enterovirus 2, crystallization screening of membrane proteins and complexes, and structure solution from crystallization hits produced via a high-throughput pipeline. These demonstrate the potential for in situ data collection and structure solution with microbeams.

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)

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.

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

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...

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)

In situ macromolecular crystallography using microbeams.

Science.gov (United States)

Axford, Danny; Owen, Robin L; Aishima, Jun; Foadi, James; Morgan, Ann W; Robinson, James I; Nettleship, Joanne E; Owens, Raymond J; Moraes, Isabel; Fry, Elizabeth E; Grimes, Jonathan M; Harlos, Karl; Kotecha, Abhay; Ren, Jingshan; Sutton, Geoff; Walter, Thomas S; Stuart, David I; Evans, Gwyndaf

2012-05-01

Despite significant progress in high-throughput methods in macromolecular crystallography, the production of diffraction-quality crystals remains a major bottleneck. By recording diffraction in situ from crystals in their crystallization plates at room temperature, a number of problems associated with crystal handling and cryoprotection can be side-stepped. Using a dedicated goniometer installed on the microfocus macromolecular crystallography beamline I24 at Diamond Light Source, crystals have been studied in situ with an intense and flexible microfocus beam, allowing weakly diffracting samples to be assessed without a manual crystal-handling step but with good signal to noise, despite the background scatter from the plate. A number of case studies are reported: the structure solution of bovine enterovirus 2, crystallization screening of membrane proteins and complexes, and structure solution from crystallization hits produced via a high-throughput pipeline. These demonstrate the potential for in situ data collection and structure solution with microbeams. © 2012 International Union of Crystallography

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.

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).

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.

In-Situ Grouting Treatability Study for the Idaho National Engineering and Environmental Laboratory Subsurface Disposal Area-Transuranic Pits and Trenches

International Nuclear Information System (INIS)

Loomis, G. G.; Jessmore, J. J.; Sehn, A. L.; Miller, C. M.

2002-01-01

At the Idaho National Engineering and Environmental Laboratory (INEEL), a Comprehensive Environmental Response, Compensation, and Liability Act (CERCLA) treatability study is being performed to examine the technology of in situ grouting for final in situ disposal of buried mixed transuranic (TRU) waste. At the INEEL, there is over 56,000 cubic meters of waste commingled with a similar amount of soil in a shallow (3-5 m) land burial referred to as Waste Area Group 7-13/14. Since this buried waste has been declared on the National Priorities List under CERCLA, it is being managed as a superfund site. Under CERCLA, options for this waste include capping and continued monitoring, retrieval and ex situ management of the retrieved waste, in situ stabilization by vitrification or grouting, in situ thermal dissorption, or some combination of these options. In situ grouting involves injecting grout at high pressures (400 bars) directly into the waste to create a solid monolith. The in situ grouting process is expected to both stabilize the waste against subsidence and provide containment against migration of waste to the Snake River Plain Aquifer lying 150-200 m below the waste. The treatability study involves bench testing, implementability testing, and field testing. The bench testing was designed to pick three grouts from six candidate grouts for the implementability field testing in full scale which were designed to down-select from those three grouts to one grout for use in a full-scale field demonstration of the technology in a simulated test pit. During the bench testing, grouts were evaluated for durability using American Nuclear Society 16.1 Leach Protocol as well as evaluating the effect on physical parameters such as hydraulic conductivity and compressive strength due to the presence of interferences such as soil, organic sludge, and nitrate salts. During full-scale implementability testing, three grouts were evaluated for groutability and monolith formation

A sample holder for in-house X-ray powder diffraction studies of protein powders

DEFF Research Database (Denmark)

Frankær, Christian Grundahl; Harris, Pernille; Ståhl, Kenny

2011-01-01

A sample holder for handling samples of protein for in-house X-ray powder diffraction (XRPD) analysis has been made and tested on lysozyme. The use of an integrated pinhole reduced the background, and good signal-to-noise ratios were obtained from only 7 l of sample, corresponding to approximatel...... 2-3 mg of dry protein. The sample holder is further adaptable to X-ray absorption spectroscopy (XAS) measurements. Both XRPD and XAS at the Zn K-edge were tested with hexameric Zn insulin....

Anionic and cationic redox and interfaces in batteries: Advances from soft X-ray absorption spectroscopy to resonant inelastic scattering

Science.gov (United States)

Yang, Wanli; Devereaux, Thomas P.

2018-06-01

Recent advances in battery science and technology have triggered both the challenges and opportunities on studying the materials and interfaces in batteries. Here, we review the recent demonstrations of soft X-ray spectroscopy for studying the interfaces and electrode materials. The focus of this review is on the recently developed mapping of resonant inelastic X-ray scattering (mRIXS) as a powerful probe of battery chemistry with superior sensitivity. Six different channels of soft X-ray absorption spectroscopy (sXAS) are introduced for different experimental purposes. Although conventional sXAS channels remain effective tools for quantitative analysis of the transition-metal states and surface chemistry, we elaborate the limitations of sXAS in both cationic and anionic redox studies. Particularly, based on experimental findings in various electrodes, we show that sXAS is unreliable for studying oxygen redox. We then demonstrate the mRIXS as a reliable technique for fingerprinting oxygen redox and summarize several crucial observations. We conclude that mRIXS is the tool-of-choice to study both the practical issue on reversibility of oxygen redox and the fundamental nature of bulk oxygen states. We hope this review clarifies the popular misunderstanding on oxygen sXAS results of oxide electrodes, and establishes a reliable technique for detecting oxygen redox through mRIXS.

Characterization of Binary Ag-Cu Ion Mixtures in Zeolites: Their Reduction Products and Stability to Air Oxidation

International Nuclear Information System (INIS)

Fiddy, Steven; Petranovskii, Vitalii; Ogden, Steve; Iznaga, Inocente Rodriguez

2007-01-01

A series of Ag+-Cu2+ binary mixtures with different Ag/Cu ratios were supported on mordenite with different Si/Al ratios and were subsequently reduced under hydrogen in the temperature range 323K - 473K. Ag and Cu K-edge X-ray Absorption Spectroscopy (XAS) was conducted on these systems in-situ to monitor the reduction species formed and the kinetics of their reduction. In-situ XANES clearly demonstrates that the formation of silver particles is severely impeded by the addition of copper and that the copper is converted from Cu(II) to Cu(I) during reduction and completely reverts back to Cu(II) during cooling. There are no indications at any stage of the formation of bimetallic Ag-Cu clusters. Interestingly, the Ag/Cu ratio appears to have no influence of the reduction kinetics and reduction products formed with only the highest Si/Al ratio (MR = 128) investigated during this study having an influence on the reduction and stability to air oxidation

A combined wet chemistry and EXAFS study of U(VI) uptake by cementitious materials

International Nuclear Information System (INIS)

Wieland, E.; Harfouche, M.; Tits, J.; Kunz, D.; Daehn, R.; Fujita, T.; Tsukamoto, M.

2006-01-01

The sorption behaviour and speciation of U(VI) in cementitious systems was investigated by a combination of wet chemistry experiments and synchrotron-based X-ray absorption spectroscopy (XAS) measurements. Radiotracer studies using 233 U were carried out on hardened cement paste (HCP) and calcium silicate hydrates (C-S-H), which are the major constituents of HCP, to determine the uptake kinetics and sorption isotherms. C-S-H phases were synthesized using different methods for solid phase preparation, which enabled us to study the U(VI) uptake by different types of C-S-H phases and a wide range of Ca/Si compositions, and to distinguish U(VI) sorption on the surface of C-S-H from U(VI) incorporation into the structure. XAS measurements were performed using U(VI) loaded HCP and C-S-H materials (sorption and co-precipitation samples) to gain structural information on the U(VI) speciation in these systems, i.e., the type and number of neighbouring atoms, and bond distances. Examples of studies that have utilized XAS to characterize U(VI) speciation in cementitious systems are still rare, and to the best of our knowledge, detailed XAS investigations of the U(VI)/C-S-H system are lacking. The results obtained from the combined use of wet chemical and spectroscopic techniques allow mechanistic models of the immobilization process to be proposed for cementitious waste forms containing low and high U(VI) inventories. In the latter case U(VI) immobilization is controlled by a solubility-limiting process with the U(VI) mineral predominantly formed under the conditions prevailing in cementitious systems. At low U(VI) concentrations, however, U(VI) appears to be predominantly bound onto C-S-H phases. The coordination environment of U(VI) taken up by C-S-H was found to resemble that of U(VI) in uranophane. A mechanistic understanding of the U(VI) binding by cementitious materials will allow more detailed and scientifically well founded predictions of the retention of

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.

Rapid Mapping of Lithiation Dynamics in Transition Metal Oxide Particles with Operando X-ray Absorption Spectroscopy

Science.gov (United States)

Nowack, Lea; Grolimund, Daniel; Samson, Vallerie; Marone, Federica; Wood, Vanessa

2016-02-01

Since the commercialization of lithium ion batteries (LIBs), layered transition metal oxides (LiMO2, where M = Co, Mn, Ni, or mixtures thereof) have been materials of choice for LIB cathodes. During cycling, the transition metals change their oxidation states, an effect that can be tracked by detecting energy shifts in the X-ray absorption near edge structure (XANES) spectrum. X-ray absorption spectroscopy (XAS) can therefore be used to visualize and quantify lithiation kinetics in transition metal oxide cathodes; however, in-situ measurements are often constrained by temporal resolution and X-ray dose, necessitating compromises in the electrochemistry cycling conditions used or the materials examined. We report a combined approach to reduce measurement time and X-ray exposure for operando XAS studies of lithium ion batteries. A highly discretized energy resolution coupled with advanced post-processing enables rapid yet reliable identification of the oxidation state. A full-field microscopy setup provides sub-particle resolution over a large area of battery electrode, enabling the oxidation state within many transition metal oxide particles to be tracked simultaneously. Here, we apply this approach to gain insights into the lithiation kinetics of a commercial, mixed-metal oxide cathode material, nickel cobalt aluminium oxide (NCA), during (dis)charge and its degradation during overcharge.

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

Noise canceling in-situ detection

Science.gov (United States)

Walsh, David O.

2014-08-26

Technologies applicable to noise canceling in-situ NMR detection and imaging are disclosed. An example noise canceling in-situ NMR detection apparatus may comprise one or more of a static magnetic field generator, an alternating magnetic field generator, an in-situ NMR detection device, an auxiliary noise detection device, and a computer.

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

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.

Cross-check of ex-situ and in-situ metrology of a bendable temperature stabilized KB mirror

International Nuclear Information System (INIS)

Yuan Sheng; Goldberg, Kenneth A.; Yashchuk, Valeriy V.; Celestre, Richard; McKinney, Wayne R.; Morrison, Gregory; Macdougall, James; Mochi, Iacopo; Warwick, Tony

2011-01-01

At the Advanced Light Source (ALS), we are developing broadly applicable, high-accuracy, in-situ, at-wavelength wavefront slope measurement techniques for Kirkpatrick-Baez (KB) mirror nano-focusing. In this paper, we report an initial cross-check of ex-situ and in-situ metrology of a bendable temperature stabilized KB mirror. This cross-check provides a validation of the in-situ shearing interferometry, currently under development at the ALS.

In-situ characterization of heterogeneous catalysts

CERN Document Server

Rodriguez, Jose A; Chupas, Peter J

2013-01-01

Helps researchers develop new catalysts for sustainable fuel and chemical production Reviewing the latest developments in the field, this book explores the in-situ characterization of heterogeneous catalysts, enabling readers to take full advantage of the sophisticated techniques used to study heterogeneous catalysts and reaction mechanisms. In using these techniques, readers can learn to improve the selectivity and the performance of catalysts and how to prepare catalysts as efficiently as possible, with minimum waste. In-situ Characterization of Heterogeneous Catalysts feat

High-resolution molybdenum K-edge X-ray absorption spectroscopy analyzed with time-dependent density functional theory.

Science.gov (United States)

Lima, Frederico A; Bjornsson, Ragnar; Weyhermüller, Thomas; Chandrasekaran, Perumalreddy; Glatzel, Pieter; Neese, Frank; DeBeer, Serena

2013-12-28

X-ray absorption spectroscopy (XAS) is a widely used experimental technique capable of selectively probing the local structure around an absorbing atomic species in molecules and materials. When applied to heavy elements, however, the quantitative interpretation can be challenging due to the intrinsic spectral broadening arising from the decrease in the core-hole lifetime. In this work we have used high-energy resolution fluorescence detected XAS (HERFD-XAS) to investigate a series of molybdenum complexes. The sharper spectral features obtained by HERFD-XAS measurements enable a clear assignment of the features present in the pre-edge region. Time-dependent density functional theory (TDDFT) has been previously shown to predict K-pre-edge XAS spectra of first row transition metal compounds with a reasonable degree of accuracy. Here we extend this approach to molybdenum K-edge HERFD-XAS and present the necessary calibration. Modern pure and hybrid functionals are utilized and relativistic effects are accounted for using either the Zeroth Order Regular Approximation (ZORA) or the second order Douglas-Kroll-Hess (DKH2) scalar relativistic approximations. We have found that both the predicted energies and intensities are in excellent agreement with experiment, independent of the functional used. The model chosen to account for relativistic effects also has little impact on the calculated spectra. This study provides an important calibration set for future applications of molybdenum HERFD-XAS to complex catalytic systems.

Cost accounting method for in-situ leaching mines and its application

International Nuclear Information System (INIS)

Cheng Zongfang; Yang Yihan; Liu Zhanxiang; Lai Yongchun

2008-01-01

Cost structures and accounting method for in-situ leaching mines are studied according to the technical characteeristics of in-situ leaching. A method of cost forecast for in-situ leaching deposit or mine area is presented, and the application of this method is illustrated with examples. (authors)

Contemporary management of ductal carcinoma in situ and lobular carcinoma in situ.

Science.gov (United States)

Obeng-Gyasi, Samilia; Ong, Cecilia; Hwang, E Shelley

2016-06-01

The management of in situ lesions ductal carcinoma in situ (DCIS) and lobular carcinoma in situ (LCIS) continues to evolve. These diagnoses now comprise a large burden of mammographically diagnosed cancers, and with a global trend towards more population-based screening, the incidence of these lesions will continue to rise. Because outcomes following treatment for DCIS and LCIS are excellent, there is emerging controversy about what extent of treatment is optimal for both diseases. Here we review the current approaches to the diagnosis and treatment of both DCIS and LCIS. In addition, we will consider potential directions for future management of these lesions.

Influence of fracture extension on in-situ stress in tight reservoir

Science.gov (United States)

Zhang, Yongping; Wei, Xu; Zhang, Ye; Xing, Libo; Xu, Jianjun

2018-01-01

Currently, hydraulic fracturing is an important way to develop low permeability reservoirs. The fractures produced during the fracturing process are the main influencing factors of changing in-situ stress. In this paper, the influence of fracture extension on in-situ stress is studied by establishing a mathematical model to describe the relationship between fracture length and in-situ stress. The results show that the growth rate gradually decreases after the fracture reaches a certain length with the increase of fracturing time; the continuous extension of the fracture is the main factor to change the in-situ stress. In order to reduce the impact on the subsequent fracture extension due to the changing of in-situ stress, controlling fracturing time and fracture length without affecting the stimulated reservoir effect is an important way. The results presented in this study can effectively reduce the impact of changing of in-situ stress on subsequent fracturing construction.

In-situ Raman spectroscopy. A method to study and control the growth of microcrystalline silicon for thin-film solar cells

Energy Technology Data Exchange (ETDEWEB)

Muthmann, Stefan

2012-08-22

This work deals with the design and application of a novel experiment, which enables in-situ Raman measurements during the parallel plate plasma enhanced chemical vapor deposition (PECVD) of {mu}cSi:H. Measurements of the crystalline volume fraction (I{sub C}{sup RS}) and the temperature of a growing film are carried out using the novel setup. To enable in-situ Raman measurement of central regions of the coated substrate in a PECVD system, optical access under normal incidence is necessary. An experimental setup in which an optical feed-through was integrated into a PECVD electrode was developed. This setup introduces a disturbance to the electrical field which sustains the plasma. By designing metallic shields the impact of the feed through was reduced considerably at low optical losses. The homogeneity of films deposited with the novel setup in different growth regimes was studied. A correlation between the magnitude of the inhomogeneity caused by the feed-through and the characteristics of the deposition regimes is found. Raman spectroscopy demands the illumination of a sample with a laser and the collection of the scattered radiation. Due to absorption of the laser light the temperature of the illuminated film is increased. Since the temperature determines the properties of a growing film the laser-induced temperature increase was studied. By pulsing the laser radiation of minimal temperature increase at maximal signal intensity was obtained. The crystalline volume fraction of a growing {mu}cSi:H layer was determined in-situ with the novel setup. A minimal temporal resolution of less than 17.5 s at sufficient signal-to-noise-ratio was achieved, which corresponds to less than 9 nm of deposited material during one measurement interval at the industrial standard growth rate of 0.5 nm/s. The obtained results were compared to depth resolved measurements which were carried out after the deposition. An excellent agreement between both methods validates the reliability

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

In Situ Ptychography of Heterogeneous Catalysts using Hard X-Rays

DEFF Research Database (Denmark)

Baier, Sina; Damsgaard, Christian Danvad; Scholz, Maria

2016-01-01

A new closed cell is presented for in situ X-ray ptychography which allows studies under gas flow and at elevated temperature. In order to gain complementary information by transmission and scanning electron microscopy, the cell makes use of a Protochips E-chipTM which contains a small, thin...... the same sample holder for ex situ electron microscopy before and after the in situ study underlines the unique possibilities available with this combination of electron microscopy and X-ray microscopy on the same sample....

Alternatieve in situ bodemsaneringstechnieken; literatuuronderzoek bij het project "In Situ Biorestauratie" Asten

NARCIS (Netherlands)

Scheuter AJ; LBG

1997-01-01

In developing in situ remediation most of the focus used to be on techniques using infiltration water to supply oxygen to the location. Later, techniques were developed in which soil was flushed with air to enhance the oxygen availability to microorganisms. The aim of the study reported here was to

In-situ failure test in the research tunnel at Olkiluoto

Energy Technology Data Exchange (ETDEWEB)

Autio, J.; Johansson, E.; Kirkkomaeki, T. [Saanio and Riekkola Consulting Engineers, Helsinki (Finland); Hakala, M. [Gridpoint Finland Oy (Finland); Heikkilae, E. [Helsinki Univ. of Technology, Otaniemi (Finland). Lab. of Rock Engineering

2000-05-01

A failure test suitable for execution in the Research Tunnel at Olkiluoto has been planned to study the failure of rock in-situ. The objectives of the in-situ failure test is to assess the applicability of numerical modelling codes and methods to the study of rock failure and associated crack propagation and to develop a novel technique to be used to determine the strength of rock in-situ. The objective of this study was to make a preliminary design of the failure test, assess the technical feasibility of the test and to give input information for further numerical modelling of the test. The design of the failure test is reported and results of preliminary modelling are given. The input information for future modelling includes a study of rock properties, fracture propagation in rock, in-situ stresses and the development of techniques for using the expanding agent to produce artificial stress field. The study showed that mechanical properties such as strength of gneissic tonalite, the main rock type in the Research Tunnel, depends highly on the orientation of schistocity. The in-situ failure test was shown to be technically feasible and a state of stress high enough to cause failure can be created artificially by using a proper expansive agent and design. (orig.)

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

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

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

Novel iron oxyhydroxide lepidocrocite nanosheet as ultrahigh power density anode material for asymmetric supercapacitors.

Science.gov (United States)

Chen, Ying-Chu; Lin, Yan-Gu; Hsu, Yu-Kuei; Yen, Shi-Chern; Chen, Kuei-Hsien; Chen, Li-Chyong

2014-09-24

A simple one-step electroplating route is proposed for the synthesis of novel iron oxyhydroxide lepidocrocite (γ-FeOOH) nanosheet anodes with distinct layered channels, and the microstructural influence on the pseudocapacitive performance of the obtained γ-FeOOH nanosheets is investigated via in situ X-ray absorption spectroscopy (XAS) and electrochemical measurement. The in situ XAS results regarding charge storage mechanisms of electrodeposited γ-FeOOH nanosheets show that a Li(+) can reversibly insert/desert into/from the 2D channels between the [FeO6 ] octahedral subunits depending on the applied potential. This process charge compensates the Fe(2+) /Fe(3+) redox transition upon charging-discharging and thus contributes to an ideal pseudocapacitive behavior of the γ-FeOOH electrode. Electrochemical results indicate that the γ-FeOOH nanosheet shows the outstanding pseudocapacitive performance, which achieves the extraordinary power density of 9000 W kg(-1) with good rate performance. Most importantly, the asymmetric supercapacitors with excellent electrochemical performance are further realized by using 2D MnO2 and γ-FeOOH nanosheets as cathode and anode materials, respectively. The obtained device can be cycled reversibly at a maximum cell voltage of 1.85 V in a mild aqueous electrolyte, further delivering a maximum power density of 16 000 W kg(-1) at an energy density of 37.4 Wh kg(-1). © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

In-situ uranium leaching

International Nuclear Information System (INIS)

Dotson, B.J.

1986-01-01

This invention provides a method for improving the recovery of mineral values from ore bodies subjected to in-situ leaching by controlling the flow behaviour of the leaching solution. In particular, the invention relates to an in-situ leaching operation employing a foam for mobility control of the leaching solution. A foam bank is either introduced into the ore bed or developed in-situ in the ore bed. The foam then becomes a diverting agent forcing the leaching fluid through the previously non-contacted regions of the deposit

Effect of silica particles modified by in-situ and ex-situ methods on the reinforcement of silicone rubber

International Nuclear Information System (INIS)

Song, Yingze; Yu, Jinhong; Dai, Dan; Song, Lixian; Jiang, Nan

2014-01-01

Highlights: • In-situ and ex-situ methods were applied to modify silica particles. • In-situ method was more beneficial to preparing silica particles with high BET surface area. • Silicone rubber filled with in-situ modified silica exhibits excellent mechanical and thermal properties. - Abstract: In-situ and ex-situ methods were applied to modify silica particles in order to investigate their effects on the reinforcement of silicone rubber. Surface area and pore analyzer, laser particle size analyzer, Fourier-transform infrared spectroscopy (FTIR), contact-angle instrument, and transmission electron microscope (TEM) were utilized to investigate the structure and properties of the modified silica particles. Dynamic mechanical thermal analyzer (DMTA) was employed to characterize the vulcanizing behavior and mechanical properties of the composites. Thermogravimetric analysis (TGA) was performed to test the thermal stability of the composites. FTIR and contact angle analysis indicated that silica particles were successfully modified by these two methods. The BET surface area and TEM results reflected that in-situ modification was more beneficial to preparing silica particles with irregular shape and higher BET surface area in comparison with ex-situ modification. The DMTA and TGA data revealed that compared with ex-situ modification, the in-situ modification produced positive influence on the reinforcement of silicone rubber

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.)

Comparison of in situ nutrient degradabilities of alternative by ...

African Journals Online (AJOL)

level of inclusion in the concentrate portion of lactating dairy cattle diets, ... Two rumen fistulated multiparous lactating Holstein cows were used for the in situ study. ... vitamins. Feeds were offered twice daily at 09:00 and 18:00. The in situ bag ...

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)

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.

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.)

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...

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

Floristic diversity of the soil weed seed bank in a rice-growing area of Brazil: in situ and ex situ evaluation

Directory of Open Access Journals (Sweden)

Mário Luiz Ribeiro Mesquita

2013-09-01

Full Text Available The objective of this study was to compare the ex situ and in situ floristic diversity of the soil weed seed bank of a rice field in northeastern Brazil. In a rice field in the county of Bacabal, located in the state of Maranhão, thirty 25-m² plots were laid out. From 15 plots, soil samples (6/plot; n = 90 were taken with a soil probe (25 × 16 × 3 cm and placed in aluminum trays in the greenhouse. From the remaining 15 plots, weed samples (6/plot; n = 90 were taken with the same soil probe. The number of seeds was estimated by germination. We evaluated the numbers of species and individuals, as well as the density, frequency, abundance and importance value (IV for each species. Diversity was computed by the Shannon index (H'. We recorded 13,892 individuals (among 20 families, 40 genera and 60 species, of which 11,530 (among 50 species germinated ex situ and 2,362 (among 34 species germinated in situ. The family Cyperaceae had the highest number of species (16, followed by Poaceae (10. The dominant species, in situ and ex situ, were Schoenoplectus juncoides (IV=47.4% and Ludwigia octovalvis (IV=34.8%, respectively. Floristic diversity was higher ex situ (H'=2.66. The information obtained here could help determine the infestation potential of these species, which could lead to improved management strategies.

Scanning transmission X-ray microscopy probe for in situ mechanism study of graphene-oxide-based resistive random access memory.

Science.gov (United States)

Nho, Hyun Woo; Kim, Jong Yun; Wang, Jian; Shin, Hyun-Joon; Choi, Sung-Yool; Yoon, Tae Hyun

2014-01-01

Here, an in situ probe for scanning transmission X-ray microscopy (STXM) has been developed and applied to the study of the bipolar resistive switching (BRS) mechanism in an Al/graphene oxide (GO)/Al resistive random access memory (RRAM) device. To perform in situ STXM studies at the C K- and O K-edges, both the RRAM junctions and the I0 junction were fabricated on a single Si3N4 membrane to obtain local XANES spectra at these absorption edges with more delicate I0 normalization. Using this probe combined with the synchrotron-based STXM technique, it was possible to observe unique chemical changes involved in the BRS process of the Al/GO/Al RRAM device. Reversible oxidation and reduction of GO induced by the externally applied bias voltages were observed at the O K-edge XANES feature located at 538.2 eV, which strongly supported the oxygen ion drift model that was recently proposed from ex situ transmission electron microscope studies.

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

Spectroscopic studies of U(VI) sorption at the kaolinite-water interface. Final report

International Nuclear Information System (INIS)

Thompson, H.A.; Parks, G.A.; Brown, G.E. Jr.

1994-01-01

Efficient use of U as a resource and safe handling, recycling and disposal of U-containing wastes require an understanding of the factors controlling the fate of U, where fate refers to the destination of U, typically expressed as an environmental medium or a process phase. The sorption process constitutes a change in elemental fate. Partitioning of an element from solution to a solid phase, or sorption, can be divided into three broad categories: adsorption, surface precipitation, and absorption. Extended X-ray absorption fine structure (EXAFS), a type of X-ray absorption spectroscopy (XAS), offers the possibility for distinguishing among different modes of sorption by characterizing the atomic environment of the sorbing element. In this study, the authors use EXAFS to determine the structure of U(VI) sorption complexes at the kaolinite-water interface. In Chapter One, they present an overview of selected aspects of U structural chemistry as a basis for considering the structural environment of U at the solid-water interface. To evaluate the utility of XAS for characterization of the structural environment of U(VI) at the solid-water interface, they have carried out an in-depth analysis of XAS data from U(VI)-containing solid and solution model compounds, which they describe in Chapter Two. In Chapter three, they consider sorption of U by kaolinite as a means of effecting the removal of U from surface collection pond waters on the Rocky Flats Plant site in northern Colorado

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)

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

Theoretical studies on core-level spectra of solids

International Nuclear Information System (INIS)

Kotani, Akio

1995-01-01

I present a review on theoretical studies of core-level spectra (CLS) in solids. In CLS, the dynamical response of outer electrons to a core hole is reflected through the screening of core hole potential. Impurity Anderson model (IAM) or cluster model is successfully applied to the analysis of X-ray photoemission spectra (XPS) and X-ray absorption spectra (XAS) in f and d electron systems, where the f and d electron states are hybridized with the other valence or conduction electron states. The effect of the core-hole potential in the final state of XPS and XAS plays an important role, as well as the solid state hybridization and intra-atomic multiplet coupling effects. As typical examples, the calculated results for XPS of rare-earth compounds and transition metal compounds are shown, and some discussions are given. As a subject of remarkable progress with high brightness synchrotron radiation sources, I discuss some theoretical aspects of X-ray emission spectra (XES) and their resonant enhancement at the X-ray absorption threshold. Some experimental data and their theoretical analysis are also given. (author)

ADVANTAGES/DISADVANTAGES FOR ISCO METHODS IN-SITU FENTON OXIDATION IN-SITU PERMANGANATE OXIDATION

Science.gov (United States)

The advantages and disadvantages of in-situ Fenton oxidation and in-situ permanganate oxidation will be presented. This presentation will provide a brief overview of each technology and a detailed analysis of the advantages and disadvantages of each technology. Included in the ...

In-situ studies of the recrystallization process of CuInS2 thin films by energy dispersive X-ray diffraction

International Nuclear Information System (INIS)

Thomas, D.; Mainz, R.; Rodriguez-Alvarez, H.; Marsen, B.; Abou-Ras, D.; Klaus, M.; Genzel, Ch.; Schock, H.-W.

2011-01-01

Recrystallization processes during the sulfurization of CuInS 2 (CIS) thin films have been studied in-situ using energy dispersive X-ray diffraction (EDXRD) with synchrotron radiation. In order to observe the recrystallization isolated from other reactions occurring during film growth, Cu-poor, small grained CIS layers covered with CuS on top were heated in a vacuum chamber equipped with windows for synchrotron radiation in order to analyze the grain growth mechanism within the CIS layer. In-situ monitoring of the grain size based on diffraction line profile analysis of the CIS-112 reflection was utilized to interrupt the recrystallization process at different points. Ex-situ studies by electron backscatter diffraction (EBSD) and energy dispersive X-ray spectroscopy (EDX) performed on samples of intermediate recrystallization states reveal that during the heat treatment Cu and In interdiffuse inside the layer indicating the importance of the mobility of these two elements during CuInS 2 grain growth.

Advances in high-resolution synchrotron micro-XANES for constraining the redox evolution of terrestrial and extraterrestrial magma

Science.gov (United States)

Lanzirotti, A.; Sutton, S. R.; Dyar, M. D.; McCanta, M. C.; Head, E.

2017-12-01

Quantifying the redox evolution of geological materials is of fundamental importance for understanding the evolution of the Earth and terrestrial planets. Microfocused, synchrotron X-ray Absorption Spectroscopy (XAS) provides direct, in-situ analyses of the valence state for elements that can be used as proxies for oxygen fugacity (Fe, V, Cr, Ti, S, Eu, and Ce). Such proxies span the entire fO2 range of solar system evolution, covering at least 16 log units. Recent technical improvements at the Advanced Photon Source 13-ID-E microspectroscopy beamline have improved the energy, spatial resolution and detection sensitivity for XAS. The application of multiple valence state oxybarometers to individual mineral grains is valuable as demonstrated in a study of Ti, V and Cr valence in olivine and pyroxene of the ungrouped achondrite NWA 7325 [1], results which yielded a very reduced fO2 estimate of IW-3 and suggested a likely origin of NWA 7325 in a parent body with similar redox conditions to the ureilite parent body. Simultaneously, we have made advances using multivariate prediction models to more precisely measure ever-smaller variations in elemental valence [2]. Applied to V XAS spectra in glasses, we have developed an MVA calibration model that directly relates the measured spectra to predicted fO2, improving the precision in calculating fO2 with more robust error analysis. These machine learning based algorithms also allow for XAS to be collected in an imaging modality to spatially map elemental redox states within samples. For example for imaging changes in Fe oxidation state in natural lunar picritic glasses [3] that may be related to magmatic degassing. This presentation highlights recent examples of this research at 13-ID-E, including application of Fe, S and V valence state oxybarometers in the analysis of terrestrial volcanic glasses and melt inclusions for looking at long term evolution of oxygen fugacity of magmas. [1] Sutton S. et al. (2017) GCA, 211, 115

An x-ray absorption spectroscopy study of Cd binding onto a halophilic archaeon

International Nuclear Information System (INIS)

Showalter, Allison R; Bunker, Bruce A; Szymanowski, Jennifer E S; Fein, Jeremy B

2016-01-01

X-ray absorption spectroscopy (XAS) and cadmium (Cd) isotherm experiments determine how Cd adsorbs to the surface of halophilic archaeon Halobacterium noricense . This archaeon, isolated from the Waste Isolation Pilot Plant (WIPP) near Carlsbad, New Mexico could be involved with the transport of toxic metals stored in the transuranic waste in the salt mine. The isotherm experiments show that adsorption is relatively constant across the tolerable pH range for H. noricense . The XAS results indicate that Cd adsorption occurs predominately via a sulfur site, most likely sulfhydryl, with the same site dominating all measured pH values. (paper)

An x-ray absorption spectroscopy study of Cd binding onto a halophilic archaeon

Science.gov (United States)

Showalter, Allison R.; Szymanowski, Jennifer E. S.; Fein, Jeremy B.; Bunker, Bruce A.

2016-05-01

X-ray absorption spectroscopy (XAS) and cadmium (Cd) isotherm experiments determine how Cd adsorbs to the surface of halophilic archaeon Halobacterium noricense. This archaeon, isolated from the Waste Isolation Pilot Plant (WIPP) near Carlsbad, New Mexico could be involved with the transport of toxic metals stored in the transuranic waste in the salt mine. The isotherm experiments show that adsorption is relatively constant across the tolerable pH range for H. noricense. The XAS results indicate that Cd adsorption occurs predominately via a sulfur site, most likely sulfhydryl, with the same site dominating all measured pH values.

Past In-Situ Burning Possibilities

National Research Council Canada - National Science Library

Yoshioka, Gary

1999-01-01

This study evaluated the feasibility of conducting in-situ burning (ISB) using current technology on post 1967 major oil spills over 10,00 barrels in North America and over 50,00 barrels in South America and Europe...

Integrating In-Situ and Ex-Situ Data Management Processes for Biodiversity Conservation

Directory of Open Access Journals (Sweden)

Karin R. Schwartz

2017-10-01

Full Text Available There is an increasing need for a “one plan approach” for conservation strategies that integrate in-situ and ex-situ management processes. Zoological institutions contribute directly to threatened species conservation through paradigms, such as reintroduction, head-starting, supplementation, or rescue/rehabilitation/release. This in-situ/ex-situ integration necessitates collaboration at all levels of conservation action including planning, implementation, monitoring and assessment to drive adaptive management processes. Each component is dependent on the availability and accuracy of data for evidence to facilitate evaluation and adaptive management processes. The Zoological Information Management System (ZIMS, managed by Species360, is a centralized web-based information system used in zoological institutions worldwide to pool life history, behavior and health data and facilitate animal husbandry, health, and breeding management processes. Currently used for few integrated conservation programs, ZIMS is an innovative tool that offers a new opportunity to link data management processes for animals that spend a part of their lives under human care and part in their natural environment and has great potential for use in managed wild populations.

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)

DOE In Situ Remediation Integrated Program

International Nuclear Information System (INIS)

Yow, J.L. Jr.

1993-01-01

The In Situ Remediation Integrated Program (ISRP) supports and manages a balanced portfolio of applied research and development activities in support of DOE environmental restoration and waste management needs. ISRP technologies are being developed in four areas: containment, chemical and physical treatment, in situ bioremediation, and in situ manipulation (including electrokinetics). the focus of containment is to provide mechanisms to stop contaminant migration through the subsurface. In situ bioremediation and chemical and physical treatment both aim to destroy or eliminate contaminants in groundwater and soils. In situ manipulation (ISM) provides mechanisms to access contaminants or introduce treatment agents into the soil, and includes other technologies necessary to support the implementation of ISR methods. Descriptions of each major program area are provided to set the technical context of the ISM subprogram. Typical ISM needs for major areas of in situ remediation research and development are identified

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

In situ microradioscopy and microtomography of fatigue-loaded dental two-piece implants

Energy Technology Data Exchange (ETDEWEB)

Wiest, Wolfram; Zabler, Simon, E-mail: simon.zabler@physik.uni-wuerzburg.de [University of Würzburg (Germany); Rack, Alexander [European Synchrotron Radiation Facility (France); Fella, Christian; Balles, Andreas [University of Würzburg (Germany); Nelson, Katja; Schmelzeisen, Rainer [Medical Centre – University of Freiburg (Germany); Hanke, Randolf [University of Würzburg (Germany); Fraunhofer EZRT, Fürth (Germany)

2015-10-09

Results of a novel in situ microradiography and microtomography setup for the study of fatigue processes are presented. This setup is optimized for the requirements of dental implants and use at synchrotron imaging beamlines. Synchrotron real-time radioscopy and in situ microtomography are the only techniques providing direct visible information on a micrometre scale of local deformation in the implant–abutment connection (IAC) during and after cyclic loading. The microgap formation at the IAC has been subject to a number of studies as it has been proposed to be associated with long-term implant success. The next step in this scientific development is to focus on the in situ fatigue procedure of two-component dental implants. Therefore, an apparatus has been developed which is optimized for the in situ fatigue analysis of dental implants. This report demonstrates both the capability of in situ radioscopy and microtomography at the ID19 beamline for the study of cyclic deformation in dental implants. The first results show that it is possible to visualize fatigue loading of dental implants in real-time radioscopy in addition to the in situ fatigue tomography. For the latter, in situ microtomography is applied during the cyclic loading cycles in order to visualize the opening of the IAC microgap. These results concur with previous ex situ studies on similar systems. The setup allows for easily increasing the bending force, to simulate different chewing situations, and is, therefore, a versatile tool for examining the fatigue processes of dental implants and possibly other specimens.

In situ microradioscopy and microtomography of fatigue-loaded dental two-piece implants

International Nuclear Information System (INIS)

Wiest, Wolfram; Zabler, Simon; Rack, Alexander; Fella, Christian; Balles, Andreas; Nelson, Katja; Schmelzeisen, Rainer; Hanke, Randolf

2015-01-01

Results of a novel in situ microradiography and microtomography setup for the study of fatigue processes are presented. This setup is optimized for the requirements of dental implants and use at synchrotron imaging beamlines. Synchrotron real-time radioscopy and in situ microtomography are the only techniques providing direct visible information on a micrometre scale of local deformation in the implant–abutment connection (IAC) during and after cyclic loading. The microgap formation at the IAC has been subject to a number of studies as it has been proposed to be associated with long-term implant success. The next step in this scientific development is to focus on the in situ fatigue procedure of two-component dental implants. Therefore, an apparatus has been developed which is optimized for the in situ fatigue analysis of dental implants. This report demonstrates both the capability of in situ radioscopy and microtomography at the ID19 beamline for the study of cyclic deformation in dental implants. The first results show that it is possible to visualize fatigue loading of dental implants in real-time radioscopy in addition to the in situ fatigue tomography. For the latter, in situ microtomography is applied during the cyclic loading cycles in order to visualize the opening of the IAC microgap. These results concur with previous ex situ studies on similar systems. The setup allows for easily increasing the bending force, to simulate different chewing situations, and is, therefore, a versatile tool for examining the fatigue processes of dental implants and possibly other specimens

Nitrogen removal from landfill leachate via ex situ nitrification and sequential in situ denitrification

International Nuclear Information System (INIS)

Zhong Qi; Li Daping; Tao Yong; Wang Xiaomei; He Xiaohong; Zhang Jie; Zhang Jinlian; Guo Weiqiang; Wang Lan

2009-01-01

Ex situ nitrification and sequential in situ denitrification represents a novel approach to nitrogen management at landfills. Simultaneous ammonia and organics removal was achieved in a continuous stirred tank reactor (CSTR). The results showed that the maximum nitrogen loading rate (NLR) and the maximum organic loading rate (OLR) was 0.65 g N l -1 d -1 and 3.84 g COD l -1 d -1 , respectively. The ammonia and chemical oxygen demand (COD) removal was over 99% and 57%, respectively. In the run of the CSTR, free ammonia (FA) inhibition and low dissolved oxygen (DO) were found to be key factors affecting nitrite accumulation. In situ denitrification was studied in a municipal solid waste (MSW) column by recalculating nitrified leachate from CSTR. The decomposition of MSW was accelerated by the recirculation of nitrified leachate. Complete reduction of total oxidized nitrogen (TON) was obtained with maximum TON loading of 28.6 g N t -1 TS d -1 and denitrification was the main reaction responsible. Additionally, methanogenesis inhibition was observed while TON loading was over 11.4 g N t -1 TS d -1 and the inhibition was enhanced with the increase of TON loading

Diagnosis of In Situ Metabolic State and Rates of Microbial Metabolism During In Situ Uranium Bioremediation with Molecular Techniques

Energy Technology Data Exchange (ETDEWEB)

Lovley, Derek R. [University of Massachusetts, Amherst

2012-11-28

The goal of these projects was to develop molecule tools to tract the metabolic activity and physiological status of microorganisms during in situ uranium bioremediation. Such information is important in able to design improved bioremediation strategies. As summarized below, the research was highly successful with new strategies developed for estimating in situ rates of metabolism and diagnosing the physiological status of the predominant subsurface microorganisms. This is a first not only for groundwater bioremediation studies, but also for subsurface microbiology in general. The tools and approaches developed in these studies should be applicable to the study of microbial communities in a diversity of soils and sediments.

Angstrom analysis with dynamic in-situ aberration corrected electron microscopy

International Nuclear Information System (INIS)

Gai, P L; Boyes, E D

2010-01-01

Following the pioneering development of atomic resolution in-situ environmental TEM (ETEM) for direct probing of gas-solid reactions, recent developments are presented of dynamic real time in-situ studies at the Angstrom level in an aberration corrected electron microscope. The in-situ data from Pt-Pd nanoparticles on carbon with the corresponding FFT/optical diffractogram (OD) illustrate an achieved resolution of 0 C and higher, in a double aberration corrected JEOL 2200 FS TEM/STEM employing a wider gap objective pole piece and gas tolerant TMP column pumping system. Direct observations of dynamic biofuel catalysts under controlled calcinations conditions and quantified with catalytic reactivity and physico-chemical studies show the benefits in-situ aberration correction in unveiling the evolution of surface active sites necessary for the development efficient heterogeneous catalysts. The new results open up opportunities for dynamic studies of materials in an aberration corrected environment and direct future development activities.

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

WIPP/SRL in-situ tests

International Nuclear Information System (INIS)

Mamsey, W.G.

1990-01-01

The Materials Interface Interactions Test (MIIT) is the only in-situ program involving the burial of simulated high-level waste forms operating in the United States. Fifteen glass and waste form compositions and their proposed package materials, supplied by 7 countries, are interred in salt at the Waste Isolation Pilot Plant (WIPP) in Carlsbad, New Mexico. A joint effort between Sandia National Laboratories and Savannah River Laboratory, MIIT is the largest international cooperative in-situ venture yet undertaken. The objective of the current study is to document the waste form compositions used in the MIIT program and then to examine compositional correlations based on structural considerations, bonding energies, and surface layer formation. These correlations show important similarities between the many different waste glass compositions studied world wide and suggest that these glasses would be expected to perform well and in a similar manner

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.

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....

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...

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.

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.

In situ vitrification laboratory-scale test work plan

International Nuclear Information System (INIS)

Nagata, P.K.; Smith, N.L.

1991-05-01

The Buried Waste Program was established in October 1987 to accelerate the studies needed to develop a long-term management plan for the buried mixed waste at the Radioactive Waste Management Complex at Idaho Engineering Laboratory. The In Situ Vitrification Project is being conducted in a Comprehensive Environmental Response, Compensation, and Liability Act feasibility study format to identify methods for the long-term management of mixed buried waste. To support the overall feasibility study, the situ vitrification treatability investigations are proceeding along the three parallel paths: laboratory-scale tests, intermediate field tests, and field tests. Laboratory-scale tests are being performed to provide data to mathematical modeling efforts, which, in turn, will support design of the field tests and to the health and safety risk assessment. This laboratory-scale test work plan provides overall testing program direction to meet the current goals and objectives of the in situ vitrification treatability investigation. 12 refs., 1 fig., 7 tabs

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...

X-ray absorption spectroscopy: EXAFS and XANES - A versatile tool to study the atomic and electronic structure of materials

International Nuclear Information System (INIS)

Alp, E.E.; Mini, S.M.; Ramanathan, M.

1990-01-01

X-ray absorption spectroscopy (XAS) had been an essential tool to gather spectroscopic information about atomic energy level structure in the early decades of this century. The correct interpretation of the oscillatory structure in the x-ray absorption cross-section above the absorption edge has transformed XAS from a spectroscopic tool to a structural technique. EXAFS (Extended X-ray Absorption Fine Structure) yields information about the interatomic distances, near neighbor coordination numbers, and lattice dynamics. XANES (X-ray Absorption Near Edge Structure), on the other hand, gives information about the valence state, energy bandwidth and bond angles. Today, there are about 50 experimental stations in various synchrotrons around the world dedicated to collecting x-ray absorption data from the bulk and surfaces of solids and liquids. In this chapter, they will give the basic principles of XAS, explain the information content of essentially two different aspects of the absorption process leading to EXAFS and XANES, and discuss the source and sample limitations

Estimation of the in situ degradation of the washout fraction of starch by using a modified in situ protocol and in vitro measurements

NARCIS (Netherlands)

Jonge, de L.H.; Laar, van H.; Dijkstra, J.

2015-01-01

The in situ degradation of the washout fraction of starch in six feed ingredients (i.e. barley, faba beans, maize, oats, peas and wheat) was studied by using a modified in situ protocol and in vitro measurements. In comparison with the washing machine method, the modified protocol comprises a milder

Electronic structures of B 2p and C 2p levels in boron-doped diamond films studied using soft x-ray absorption and emission spectroscopy

Science.gov (United States)

Nakamura, Jin; Kabasawa, Eiki; Yamada, Nobuyoshi; Einaga, Yasuaki; Saito, Daisuke; Isshiki, Hideo; Yugo, Shigemi; Perera, Rupert C. C.

2004-12-01

X-ray absorption (XAS) and emission (XES) spectroscopy near B K and C K edges have been performed on metallic ( ˜0.1at.% B, B-diamond) and semiconducting ( ˜0.03at.% B and N, BN-diamond) doped diamond films. Both B K XAS and XES spectra show a metallic partial density of states (PDOS) with the Fermi energy of 185.3eV , and there is no apparent boron-concentration dependence in contrast to the different electric property. In C K XAS spectrum of B-diamond, the impurity state ascribed to boron is clearly observed near the Fermi level. The Fermi energy is found to be almost same with the top of the valence band of nondoped diamond: EV=283.9eV . C K XAS of BN-diamond shows both the B-induced shallow level and N-induced deep and broad levels as the in-gap states, in which the shallow level is in good agreement with the activation energy (Ea=0.37eV) estimated from the temperature dependence of the conductivity; namely, the change in C2p PDOS of impurity-induced metallization is directly observed. The electric property of this diamond is ascribed mainly to the electronic structure of C2p near the Fermi level. The observed XES spectra are compared with the discrete variational Xα ( DVXα ) cluster calculation. The DVXα result supports the strong hybridization between B2p and C2p observed in XAS and XES spectra, and suggests that the small amount of boron (⩽0.1at.%) in diamond occupies the substitutional site rather than interstitial site.

Engineering feasibility analysis for in-situ stabilization of Canonsburg residues. [UMTRA project

Energy Technology Data Exchange (ETDEWEB)

1982-01-01

The US Department of Energy is considering several methods for carrying out remedial actions in Canonsburg, Pennsylvania, at the site of an inactive uranium-processing mill. The main objective of this study is to determine the feasibility of in-situ stabilization as the remedial action. In-situ stabilization is an alternative to site decontamination and offsite disposal. The problems associated with offsite hauling of large quantities of contaminated material and with the location and development of a new disposal site could be avoided by the implementation of an in-situ stabilization concept. In addition, the in-situ approach would be more cost-effective than offsite disposal. This study will establish that a technically feasible and implementable in-situ stabilization concept can be developed that meets regulatory requirements and is cost effective. This study in no way commits the DOE to implement any specific actions described herein. 11 refs., 30 figs., 24 tabs.

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.

Design and characterization of thick InxGa1-xAs metamorphic buffer layers grown by hydride vapor phase epitaxy

Science.gov (United States)

Schulte, K. L.; Zutter, B. T.; Wood, A. W.; Babcock, S. E.; Kuech, T. F.

2014-03-01

Thick InxGa1-xAs metamorphic buffer layers (MBLs) grown by hydride vapor phase epitaxy (HVPE) were studied. Relationships between MBL properties and growth parameters such as grading rate, cap layer thickness, final xInAs, and deposition temperature (TD) were explored. The MBLs were characterized by measurement of in-plane residual strain (ɛ¦¦), surface etch pit density (EPD), and surface roughness. Capping layer thickness had a strong effect on strain relaxation, with thickly capped samples exhibiting the lowest ɛ¦¦. EPD was higher in samples with thicker caps, reflecting their increased relaxation through dislocation generation. ɛ¦¦ and EPD were weakly affected by the grading rate, making capping layer thickness the primary structural parameter which controls these properties. MBLs graded in discrete steps had similar properties to MBLs with continuous grading. In samples with identical thickness and 10-step grading style, ɛ¦¦ increased almost linearly with final xInAs, while total relaxation stayed relatively constant. Relaxation as a function of xInAs could be described by an equilibrium model in which dislocation nucleation is impeded by the energy of the existing dislocation array. EPD was constant from xInAs = 0 to 0.24 then increased exponentially, which is related to the increased dislocation interaction and blocking seen at higher dislocation densities. RMS roughness increased with xInAs above a certain strain rate (0.15%/µm) samples grown below this level possessed large surface hillocks and high roughness values. The elimination of hillocks at higher values of xInAs is attributed to increased density of surface steps and is related to the out-of-plane component of the burgers vector of the dominant type of 60° dislocation. TD did not affect ɛ¦¦ for samples with a given xInAs. EPD tended to increase with TD, indicating dislocation glide likely is impeded at higher temperatures.

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.

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...

In situ microradioscopy and microtomography of fatigue-loaded dental two-piece implants.

Science.gov (United States)

Wiest, Wolfram; Zabler, Simon; Rack, Alexander; Fella, Christian; Balles, Andreas; Nelson, Katja; Schmelzeisen, Rainer; Hanke, Randolf

2015-11-01

Synchrotron real-time radioscopy and in situ microtomography are the only techniques providing direct visible information on a micrometre scale of local deformation in the implant-abutment connection (IAC) during and after cyclic loading. The microgap formation at the IAC has been subject to a number of studies as it has been proposed to be associated with long-term implant success. The next step in this scientific development is to focus on the in situ fatigue procedure of two-component dental implants. Therefore, an apparatus has been developed which is optimized for the in situ fatigue analysis of dental implants. This report demonstrates both the capability of in situ radioscopy and microtomography at the ID19 beamline for the study of cyclic deformation in dental implants. The first results show that it is possible to visualize fatigue loading of dental implants in real-time radioscopy in addition to the in situ fatigue tomography. For the latter, in situ microtomography is applied during the cyclic loading cycles in order to visualize the opening of the IAC microgap. These results concur with previous ex situ studies on similar systems. The setup allows for easily increasing the bending force, to simulate different chewing situations, and is, therefore, a versatile tool for examining the fatigue processes of dental implants and possibly other specimens.

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.

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.

Dynamics of oxide growth on Pt nanoparticles electrodes in the presence of competing halides by operando energy dispersive X-Ray absorption spectroscopy

KAUST Repository

Minguzzi, Alessandro

2018-03-17

In this work we studied the kinetics of oxide formation and reduction on Pt nanoparticles in HClO4 in the absence and in the presence of Br− and Cl− ions. The study combines potential step methods (i.e. chronoamperometry and choronocoulometry) with energy dispersive X-ray absorption spectroscopy (ED-XAS), which in principle allows to record a complete XAS spectrum in the timescale of milliseconds. Here, the information on the charge state and on the atomic surrounding of the considered element provided by XAS was exploited to monitor the degree of occupancy of 5d states of Pt in the course of oxide formation and growth, and to elucidate the competing halide adsorption/desorption phenomena. Electrochemical methods and XAS agree on the validity of a log(t) depending growth of Pt oxide, that is significantly delayed in the presence of Cl− and Br− anions. In the proximity of formation of one monolayer, the growth is further slowed down.

Dynamics of oxide growth on Pt nanoparticles electrodes in the presence of competing halides by operando energy dispersive X-Ray absorption spectroscopy

KAUST Repository

Minguzzi, Alessandro; Montagna, Linda; Falqui, Andrea; Vertova, Alberto; Rondinini, Sandra; Ghigna, Paolo

2018-01-01

In this work we studied the kinetics of oxide formation and reduction on Pt nanoparticles in HClO4 in the absence and in the presence of Br− and Cl− ions. The study combines potential step methods (i.e. chronoamperometry and choronocoulometry) with energy dispersive X-ray absorption spectroscopy (ED-XAS), which in principle allows to record a complete XAS spectrum in the timescale of milliseconds. Here, the information on the charge state and on the atomic surrounding of the considered element provided by XAS was exploited to monitor the degree of occupancy of 5d states of Pt in the course of oxide formation and growth, and to elucidate the competing halide adsorption/desorption phenomena. Electrochemical methods and XAS agree on the validity of a log(t) depending growth of Pt oxide, that is significantly delayed in the presence of Cl− and Br− anions. In the proximity of formation of one monolayer, the growth is further slowed down.

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.

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.

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.

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.)

In situ Measurements of Phytoplankton Fluorescence Using Low Cost Electronics

Directory of Open Access Journals (Sweden)

Dana L. Wright

2013-06-01

Full Text Available Chlorophyll a fluorometry has long been used as a method to study phytoplankton in the ocean. In situ fluorometry is used frequently in oceanography to provide depth-resolved estimates of phytoplankton biomass. However, the high price of commercially manufactured in situ fluorometers has made them unavailable to some individuals and institutions. Presented here is an investigation into building an in situ fluorometer using low cost electronics. The goal was to construct an easily reproducible in situ fluorometer from simple and widely available electronic components. The simplicity and modest cost of the sensor makes it valuable to students and professionals alike. Open source sharing of architecture and software will allow students to reconstruct and customize the sensor on a small budget. Research applications that require numerous in situ fluorometers or expendable fluorometers can also benefit from this study. The sensor costs US$150.00 and can be constructed with little to no previous experience. The sensor uses a blue LED to excite chlorophyll a and measures fluorescence using a silicon photodiode. The sensor is controlled by an Arduino microcontroller that also serves as a data logger.

Lifetime-broadening-suppressed X-ray absorption spectrum of β-YbAlB4 deduced from Yb 3d → 2p resonant X-ray emission spectroscopy

International Nuclear Information System (INIS)

Kawamura, Naomi; Mizumaki, Masaichiro; Kanai, Noriko; Hayashi, Hisashi; Matsuda, Yasuhiro H.; Kuga, Kentaro; Nakatsuji, Satoru; Watanabe, Shinji

2017-01-01

In this work, the Yb 3d → 2p (Yb Lα 1,2 ) resonant X-ray emission spectrum of β-YbAlB 4 was acquired using excitation energies around the Yb L 3 -edge, at 2 K. Subsequently, the lifetime-broadening-suppressed (LBS) X-ray absorption structure (XAS) spectrum was obtained using the SIM-RIXS program. This spectrum was found to exhibit clearly resolved pre-edge and shoulder structures. Resonant Lα 1 emission spectra were well reproduced from LBS-XAS profiles over wide ranges of excitation and emission energies. In contrast, noticeable discrepancies appeared between the experimental and simulated Lα 2 emission spectra, suggesting an effect resulting from M 4 M 5 O 1 Coster-Kronig transitions. LBS-XAS, in conjunction with partial fluorescence yield (PFY) XAS and transmission XAS, determined a value for the Yb valence (v) in β-YbAlB 4 of 2.76 ± 0.08 at 2 K. Despite this relatively large uncertainty in v, each method provided a consistent variation in valence (δv) as the temperature was raised from 2 to 280 K: 0.060 ± 0.004 (LBS-XAS), 0.061 ± 0.005 (PFY-XAS) and 0.058 ± 0.007 (transmission XAS). The smaller δv associated with LBS-XAS demonstrates the greater precision of this method. (author)

Use of bioreactor landfill for nitrogen removal to enhance methane production through ex situ simultaneous nitrification-denitrification and in situ denitrification.

Science.gov (United States)

Sun, Xiaojie; Zhang, Hongxia; Cheng, Zhaowen

2017-08-01

High concentrations of nitrate-nitrogen (NO 3 - -N) derived from ex situ nitrification phase can inhibit methane production during ex situ nitrification and in situ denitrification bioreactor landfill. A combined process comprised of ex situ simultaneous nitrification-denitrification (SND) in an aged refuse bioreactor (ARB) and in situ denitrification in a fresh refuse bioreactor (FRB) was conducted to reduce the negative effect of high concentrationsof NO 3 - -N. Ex situ SND can be achieved because NO 3 - -N concentration can be reduced and the removal rate of ammonium-nitrogen (NH 4 + -N) remains largely unchanged when the ventilation rate of ARB-A2 is controlled. The average NO 3 - -N concentrations of effluent were 470mg/L in ex situ nitrification ARB-A1 and 186mg/L in ex situ SND ARB-A2. The average NH 4 + -N removal rates of ARB-A1 and ARB-A2 were 98% and 94%, respectively. Based on the experimental data from week 4 to week 30, it is predicted that NH 4 + -N concentration in FRB-F1 of the ex situ nitrification and in situ denitrification process would reach 25mg/L after 63weeks, and about 40weeks for the FRB-F2 of ex situ SND and in situ denitrification process . Ex situ SND and in situ denitrification process can improve themethane production of FRB-F2. The lag phase time of methane production for the FRB-F2 was 11weeks. This phase was significantly shorter than the 15-week phases of FRB-F1 in ex situ nitrification and in situ denitrification process. A seven-week stabilizationphase was required to increase methane content from 5% to 50% for FRB-F2. Methane content in FRB-F1 did not reach 50% but reached the 45% peak after 20weeks. Copyright © 2017 Elsevier Ltd. All rights reserved.

The SENSEI Generic In Situ Interface

Energy Technology Data Exchange (ETDEWEB)

Ayachit, Utkarsh [Kitware, Inc., Clifton Park, NY (United States); Whitlock, Brad [Intelligent Light, Rutherford, NJ (United States); Wolf, Matthew [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Loring, Burlen [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Geveci, Berk [Kitware, Inc., Clifton Park, NY (United States); Lonie, David [Kitware, Inc., Clifton Park, NY (United States); Bethel, E. Wes [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)

2017-04-11

The SENSEI generic in situ interface is an API that promotes code portability and reusability. From the simulation view, a developer can instrument their code with the SENSEI API and then make make use of any number of in situ infrastructures. From the method view, a developer can write an in situ method using the SENSEI API, then expect it to run in any number of in situ infrastructures, or be invoked directly from a simulation code, with little or no modification. This paper presents the design principles underlying the SENSEI generic interface, along with some simplified coding examples.

A novel fabrication technology of in situ TiB2/6063Al composites: High energy ball milling and melt in situ reaction

International Nuclear Information System (INIS)

Zhang, S.-L.; Yang, J.; Zhang, B.-R.; Zhao, Y.-T.; Chen, G.; Shi, X.-X.; Liang, Z.-P.

2015-01-01

Highlights: • This paper presents a novel technology to fabricate the TiB 2 /6063Al composites. • The novel technology decreases in situ reaction temperature and shortens the time. • The reaction mechanism of in situ reaction at the low temperature is discussed. • Effect of ball milling time and in situ reaction time on the composites is studied. - Abstract: TiB 2 /6063Al matrix composites are fabricated from Al–TiO 2 –B 2 O 3 system by the technology combining high energy ball milling with melt in situ reaction. The microstructure and tensile properties of the composites are investigated by XRD, SEM, EDS, TEM and electronic tensile testing. The results indicate that high energy ball milling technology decreases the in situ reaction temperature and shortens the reaction time for Al–TiO 2 –B 2 O 3 system in contrast with the conventional melt in situ synthesis. The morphology of in situ TiB 2 particles is exhibited in irregular shape or nearly circular shape, and the average size of the particles is less than 700 nm, thereinto the minimum size is approximately 200 nm. In addition, the morphology and size of the reinforced particles are affected by the time of ball milling and in situ reaction. TEM images indicate that the interface between 6063Al matrix and TiB 2 particles is clear and no interfacial outgrowth is observed. Tensile testing results show that the as-cast TiB 2 /6063Al composites exhibit a much higher strength, reaching 191 MPa, which is 1.23 times as high as the as-cast 6063Al matrix. Besides, the tensile fracture surface of the composites displays the dimple-fracture character

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

Valence-to-core-detected X-ray absorption spectroscopy

DEFF Research Database (Denmark)

Hall, Eleanor R.; Pollock, Christopher J.; Bendix, Jesper

2014-01-01

X-ray absorption spectroscopy (XAS) can provide detailed insight into the electronic and geometric structures of transition-metal active sites in metalloproteins and chemical catalysts. However, standard XAS spectra inherently represent an average contribution from the entire coordination...... environment with limited ligand selectivity. To address this limitation, we have investigated the enhancement of XAS features using valence-to-core (VtC)-detected XAS, whereby XAS spectra are measured by monitoring fluorescence from valence-to-core X-ray emission (VtC XES) events. VtC emission corresponds...... to transitions from filled ligand orbitals to the metal 1s core hole, with distinct energetic shifts for ligands of differing ionization potentials. VtC-detected XAS data were obtained from multiple valence emission features for a series of well-characterized Mn model compounds; taken together, these data...

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

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

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.

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.

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.

Fracture of metal foams : In-situ testing and numerical modeling

NARCIS (Netherlands)

Onck, P.R.; van Merkerk, R.; de Hosson, J.T.M.; Schmidt, I

This paper is on a combined experimental/modeling study on the tensile fracture of open-cell foams. In-situ tensile tests show that individual struts can fail in a brittle or ductile mode, presumably depending on the presence of casting defects. In-situ single strut tests were performed, enabling

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

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.

Hydrostatic pressure effects on the {gamma}-X conduction band mixing and the binding energy of a donor impurity in GaAs-Ga{sub 1-x}Al{sub x}As quantum wells

Energy Technology Data Exchange (ETDEWEB)

Duque, C.A. [Instituto de Fisica, Universidad de Antioquia, AA 1226, Medellin (Colombia); Lopez, S.Y. [Facultad de Educacion, Universidad de Antioquia, AA 1226, Medellin (Colombia); Mora-Ramos, M.E. [Facultad de Ciencias, Universidad Autonoma del Estado de Morelos, Av. Universidad 1001, C.P. 62210, Cuernavaca (Mexico)

2007-06-15

Mixing between {gamma} and X valleys of the conduction band in GaAs-Ga{sub 1-x}Al{sub x}As quantum wells is investigated taken into account the effect of applied hydrostatic pressure. This effect is introduced via the pressure-dependent values of the corresponding energy gaps and the main band parameters. The mixing is considered along the lines of a phenomenological model. Variation of the confined ground state in the well as a function of the pressure is reported. The dependencies of the variationally calculated binding energy of a donor impurity with the hydrostatic pressure and well width are also presented. It is shown that the inclusion of the {gamma}-X mixing explains the non-linear behavior in the photoluminescence peak of confined exciton states that has been observed for pressures above 20 kbar. (copyright 2007 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

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.

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

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.

Thermal annealing dynamics of carbon-coated LiFePO{sub 4} nanoparticles studied by in-situ analysis

Energy Technology Data Exchange (ETDEWEB)

Krumeich, Frank, E-mail: krumeich@inorg.chem.ethz.ch [Department of Chemistry and Applied Biosciences, ETH Zurich, Vladimir-Prelog-Weg 1, 8093 Zurich (Switzerland); Waser, Oliver; Pratsinis, Sotiris E. [Department of Mechanical and Process Engineering, ETH Zurich, Sonneggstrasse 3, 8092 Zurich (Switzerland)

2016-10-15

The thermal behavior of core-shell carbon-coated lithium iron phosphate (LiFePO{sub 4}-C) nanoparticles made by flame spray pyrolysis (FSP) during annealing was investigated by in-situ transmission electron microscopy (TEM), in-situ X-ray powder diffraction (XRD) as well as ex-situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS). Crystallization of the initially glassy LiFePO{sub 4}-C nanoparticles starts at quite low temperatures (T=400 °C), forming single crystals inside the confinement of the carbon shell. Upon increasing the temperature to T≥700 °C, LiFePO{sub 4} starts to diffuse through the carbon shell resulting in cavities inside the mostly intact carbon shell. By increasing the temperature further to T≥800 °C, the initial core-shell morphology converts into open carbon shells (flakes and cenospheres) and bulky LiFePO{sub 4} particles (diameter in the range 300–400 nm), in agreement with ex-situ experiments. - Graphical abstract: TEM images of a typical sample area recorded at room temperature and after heating in-situ heating reveal the growth of particles and the formation of empty carbon cages. - Highlights: • LiFePO{sub 4} coated by a carbon shell is produced by flame spray pyrolysis. • The amorphous LiFePO{sub 4} starts to crystallize at 400 °C as revealed by in-situ XRD. • Crystal growth was visualized by TEM heating experiments. • The formation of empty carbon cages starts at 700 °C.

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

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.

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)

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

Revisiting the total ion yield x-ray absorption spectra of liquid water microjets

International Nuclear Information System (INIS)

Saykally, Richard J; Cappa, Chris D.; Smith, Jared D.; Wilson, Kevin R.; Saykally, Richard J.

2008-01-01

Measurements of the total ion yield (TIY) x-ray absorption spectrum (XAS) of liquid water by Wilson et al. (2002 J. Phys.: Condens. Matter 14 L221 and 2001 J. Phys. Chem. B 105 3346) have been revisited in light of new experimental and theoretical efforts by our group. Previously, the TIY spectrum was interpreted as a distinct measure of the electronic structure of the liquid water surface. However, our new results indicate that the previously obtained spectrum may have suffered from as yet unidentified experimental artifacts. Although computational results indicate that the liquid water surface should exhibit a TIY-XAS that is fundamentally distinguishable from the bulk liquid XAS, the new experimental results suggest that the observable TIY-XAS is actually nearly identical in appearance to the total electron yield (TEY-)XAS, which is a bulk probe. This surprising similarity between the observed TIY-XAS and TEY-XAS likely results from large contributions from x-ray induced electron stimulated desorption of ions, and does not necessarily indicate that the electronic structure of the bulk liquid and liquid surface are identical

An overview of in situ waste treatment technologies

International Nuclear Information System (INIS)

Walker, S.; Hyde, R.A.; Piper, R.B.; Roy, M.W.

1992-01-01

In situ technologies are becoming an attractive remedial alternative for eliminating environmental problems. In situ treatments typically reduce risks and costs associated with retrieving, packaging, and storing or disposing-waste and are generally preferred over ex situ treatments. Each in situ technology has specific applications, and, in order to provide the most economical and practical solution to a waste problem, these applications must be understood. This paper presents an overview of thirty different in situ remedial technologies for buried wastes or contaminated soil areas. The objective of this paper is to familiarize those involved in waste remediation activities with available and emerging in situ technologies so that they may consider these options in the remediation of hazardous and/or radioactive waste sites. Several types of in situ technologies are discussed, including biological treatments, containment technologies, physical/chemical treatments, solidification/stabilization technologies, and thermal treatments. Each category of in situ technology is briefly examined in this paper. Specific treatments belonging to these categories are also reviewed. Much of the information on in situ treatment technologies in this paper was obtained directly from vendors and universities and this information has not been verified

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

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

PROSCARA Inc. in-situ burning summary paper

International Nuclear Information System (INIS)

1994-06-01

In-situ burning as a viable response tactic in the event of an oil spill, was discussed. Key factors which influence a decision to use burning were enumerated, including a detailed analysis of the environmental effects of in-situ burning on soils. The critical parameters were time, soil heating and extent of oil penetration into the soil. It was noted that on water-saturated and frozen soil in-situ burning had no adverse effects. The advantages and disadvantages of in-situ burning vis-a-vis conventional mechanical recovery were discussed. Factors that do, and factors that do not support decisions in favour of in-situ burning were listed. 4 refs., 2 tabs

In Situ Hybridization Pada Kanker Payudara

OpenAIRE

Diah Witari, Ni Putu

2014-01-01

Kesulitan yang dijumpai pada penanganan kanker payudara adalah terjadinya kekambuhan atau relaps. Deteksi status HER2 pada pasien merupakan salah satu upaya untuk mendeteksi terjadinya relaps dan juga untuk menentukan jenis terapi yang ada diberikan. Ekspresi protein HER2 dapat dideteksi dengan immunohistochemistry (IHC), sedangkan mutasi gen HER2 dapat dideteksi dengan teknik in situ hybridization baik berupa fluorescence in situ hybridization (FISH) ataupun chromogenic in situ hy...

The influence of the roll diameter in flat rolling of of superconducting in situ and ex situ MgB2 tape

DEFF Research Database (Denmark)

Hancock, Michael Halloway; Bay, Niels

2007-01-01

, 150 and 210 mm in each step. The investigation has shown that the in situ powder is more readily compacted than the ex situ powder, with an average increase of relative density after mechanical processing of 37% for in situ powder and 19% for ex situ powder. Statistical analysis showed that the choice......Applying the powder in tube (PIT) method, single-filament MgB2/Fe wire and tape has been manufactured applying both the ex situ and the in situ approach. The influence of the roll diameter in three-step flat rolling on the powder density and critical temperature has been examined using rolls of 70...... roll in the first and second reductions followed by the 150 mm or 210 mm roll in the last reduction was the optimum strategy for both powder types. AC susceptibility testing showed that for the in situ tapes there was no correlation between the powder density and the critical temperature. For ex situ...

In-situ atomic layer deposition growth of Hf-oxide

International Nuclear Information System (INIS)

Karavaev, Konstantin

2010-01-01

We have grown HfO 2 on Si(001) by atomic layer deposition (ALD) using HfCl 4 , TEMAHf, TDMAHf and H 2 O as precursors. The early stages of the ALD were investigated with high-resolution photoelectron spectroscopy and X-ray absorption spectroscopy. We observed the changes occurring in the Si 2p, O 1s, Hf 4f, Hf 4d, and Cl 2p (for HfCl 4 experiment) core level lines after each ALD cycle up to the complete formation of two layers of HfO 2 . The investigation was carried out in situ giving the possibility to determine the properties of the grown film after every ALD cycle or even after a half cycle. This work focused on the advantages in-situ approach in comparison with ex-situ experiments. The study provides to follow the evolution of the important properties of HfO 2 : contamination level, density and stoichiometry, and influence of the experimental parameters to the interface layer formation during ALD. Our investigation shows that in-situ XPS approach for ALD gives much more information than ex-situ experiments. (orig.)

In-situ atomic layer deposition growth of Hf-oxide

Energy Technology Data Exchange (ETDEWEB)

Karavaev, Konstantin

2010-06-17

We have grown HfO{sub 2} on Si(001) by atomic layer deposition (ALD) using HfCl{sub 4}, TEMAHf, TDMAHf and H{sub 2}O as precursors. The early stages of the ALD were investigated with high-resolution photoelectron spectroscopy and X-ray absorption spectroscopy. We observed the changes occurring in the Si 2p, O 1s, Hf 4f, Hf 4d, and Cl 2p (for HfCl{sub 4} experiment) core level lines after each ALD cycle up to the complete formation of two layers of HfO{sub 2}. The investigation was carried out in situ giving the possibility to determine the properties of the grown film after every ALD cycle or even after a half cycle. This work focused on the advantages in-situ approach in comparison with ex-situ experiments. The study provides to follow the evolution of the important properties of HfO{sub 2}: contamination level, density and stoichiometry, and influence of the experimental parameters to the interface layer formation during ALD. Our investigation shows that in-situ XPS approach for ALD gives much more information than ex-situ experiments. (orig.)

A novel fabrication technology of in situ TiB{sub 2}/6063Al composites: High energy ball milling and melt in situ reaction

Energy Technology Data Exchange (ETDEWEB)

Zhang, S.-L.; Yang, J. [School of Materials Science and Engineering, Jiangsu University, Zhenjiang, Jiangsu 212013 (China); Zhang, B.-R. [School of Mechanical Engineering, Qilu University of Technology, Jinan, Shandong 250022 (China); Zhao, Y.-T., E-mail: 278075525@qq.com [School of Materials Science and Engineering, Jiangsu University, Zhenjiang, Jiangsu 212013 (China); Chen, G.; Shi, X.-X.; Liang, Z.-P. [School of Materials Science and Engineering, Jiangsu University, Zhenjiang, Jiangsu 212013 (China)

2015-08-05

Highlights: • This paper presents a novel technology to fabricate the TiB{sub 2}/6063Al composites. • The novel technology decreases in situ reaction temperature and shortens the time. • The reaction mechanism of in situ reaction at the low temperature is discussed. • Effect of ball milling time and in situ reaction time on the composites is studied. - Abstract: TiB{sub 2}/6063Al matrix composites are fabricated from Al–TiO{sub 2}–B{sub 2}O{sub 3} system by the technology combining high energy ball milling with melt in situ reaction. The microstructure and tensile properties of the composites are investigated by XRD, SEM, EDS, TEM and electronic tensile testing. The results indicate that high energy ball milling technology decreases the in situ reaction temperature and shortens the reaction time for Al–TiO{sub 2}–B{sub 2}O{sub 3} system in contrast with the conventional melt in situ synthesis. The morphology of in situ TiB{sub 2} particles is exhibited in irregular shape or nearly circular shape, and the average size of the particles is less than 700 nm, thereinto the minimum size is approximately 200 nm. In addition, the morphology and size of the reinforced particles are affected by the time of ball milling and in situ reaction. TEM images indicate that the interface between 6063Al matrix and TiB{sub 2} particles is clear and no interfacial outgrowth is observed. Tensile testing results show that the as-cast TiB{sub 2}/6063Al composites exhibit a much higher strength, reaching 191 MPa, which is 1.23 times as high as the as-cast 6063Al matrix. Besides, the tensile fracture surface of the composites displays the dimple-fracture character.

Comparing electrical characteristics of in situ and ex situ Al2O3/GaN interfaces formed by metalorganic chemical vapor deposition

Science.gov (United States)

Chan, Silvia H.; Bisi, Davide; Tahhan, Maher; Gupta, Chirag; DenBaars, Steven P.; Keller, Stacia; Zanoni, Enrico; Mishra, Umesh K.

2018-04-01

Al2O3/n-GaN MOS-capacitors grown by metalorganic chemical vapor deposition with in-situ- and ex-situ-formed Al2O3/GaN interfaces were characterized. Capacitors grown entirely in situ exhibited ˜4 × 1012 cm-2 fewer positive fixed charges and up to ˜1 × 1013 cm-2 eV-1 lower interface-state density near the band-edge than did capacitors with ex situ oxides. When in situ Al2O3/GaN interfaces were reformed via the insertion of a 10-nm-thick GaN layer, devices exhibited behavior between the in situ and ex situ limits. These results illustrate the extent to which an in-situ-formed dielectric/GaN gate stack improves the interface quality and breakdown performance.

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)

Hydrothermal conversion of cellulose to alkanes with in-situ hydrogen

Energy Technology Data Exchange (ETDEWEB)

Yin, Sudong; Tan, Zhongchao [Department of Mechanical and Mechatronics Engineering, University of Waterloo (Canada)], Email: tanz@uwaterloo.ca

2011-07-01

A recently study examined the probability of hydrothermal conversion of cellulose to alkanes with in-situ H2 instead of external H2. This paper discusses the results of that study. The study researched the effects of volumetric ratios of initial input water to the reactor (W/R) and of selected catalysts on the alkane yields and composition. It was found that with the proper W/R ratios, the reforming of steam in the steam gas phase would automatically produce in-situ H2 and the key was to maintain the right balance of steam phase and liquid phase in the reactor. All the study results conclude that direct hydrothermal conversion of cellulose to alkanes with in-situ H2 is technically feasible. In addition, the application of this technology would protect the alkane bio-oil production biomass from the impact of unstable external supply of H2.

Chemoselective Hydrogenation with Supported Organoplatinum(IV) Catalyst on Zn(II)-Modified Silica

Energy Technology Data Exchange (ETDEWEB)

Camacho-Bunquin, Jeffrey [Chemical Sciences and Engineering Division, Argonne National Laboratory, 9700 S Cass Avenue, Lemont, Illinois 60439, United States; Ferrandon, Magali [Chemical Sciences and Engineering Division, Argonne National Laboratory, 9700 S Cass Avenue, Lemont, Illinois 60439, United States; Sohn, Hyuntae [Chemical Sciences and Engineering Division, Argonne National Laboratory, 9700 S Cass Avenue, Lemont, Illinois 60439, United States; Yang, Dali [Chemical Sciences and Engineering Division, Argonne National Laboratory, 9700 S Cass Avenue, Lemont, Illinois 60439, United States; Liu, Cong [Chemical Sciences and Engineering Division, Argonne National Laboratory, 9700 S Cass Avenue, Lemont, Illinois 60439, United States; Ignacio-de Leon, Patricia Anne [Energy Sciences Division, Argonne National Laboratory, 9700 S Cass Avenue, Lemont, Illinois 60439, United States; Perras, Frédéric A. [Ames Laboratory, U.S. Department of Energy, Ames, Iowa 50010, United States; Pruski, Marek [Ames Laboratory, U.S. Department of Energy, Ames, Iowa 50010, United States; Department of Chemistry, Iowa State University, 2416 Pammel Drive, Ames, Iowa 50011, United States; Stair, Peter C. [Chemical Sciences and Engineering Division, Argonne National Laboratory, 9700 S Cass Avenue, Lemont, Illinois 60439, United States; Department of Chemistry, Northwestern University, 2145 Sheridan Road, Evanston, Illinois 60208, United States; Delferro, Massimiliano [Chemical Sciences and Engineering Division, Argonne National Laboratory, 9700 S Cass Avenue, Lemont, Illinois 60439, United States

2018-02-22

Well-defined organoplatinum(IV) sites were grafted on a Zn(II)-modified SiO2 support via surface organometallic chemistry in toluene at room temperature. Solid-state spectroscopies including XAS, DRIFTS, DRUV-Vis, and solid-state (SS)NMR enhanced by dynamic nuclear polarization (DNP), as well as TPR-H2 and TEM techniques revealed highly dispersed (methylcyclopentadi-enyl)methylplatinum(IV) sites on the surface ((MeCp)PtMe/Zn/SiO2, 1). In addition, computational modelling suggests that the surface reaction of (MeCp)PtMe3 with Zn(II)-modified SiO2 support is thermodynamically favorable (ΔG = -12.4 kcal/mol), likely due to the increased acidity of the hydroxyl group, as confirmed by NH3-TPD and DNP-enhanced 17O{1H} SSNMR. In situ DRIFTS and XAS hydrogenation experiments reveal the formation of a surface Pt(IV)-H upon hydrogenolysis of Pt-Me groups. The heterogenized organoplatinum(IV)-H sites catalyze the selective partial hydrogenation of 1,3-butadiene to butenes (up to 95%) and the reduction of nitrobenzene derivatives to anilines (up to 100%) with excellent tolerance of reduction-sensitive func-tional groups (olefin, carbonyl, nitrile, halogens) under mild reaction conditions.

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

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

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.

Assessment of in situ and ex situ phytorestoration with grass mixtures in soils polluted with nickel, copper, and arsenic

Science.gov (United States)

Zacarías Salinas, Montserrat; Beltrán Villavicencio, Margarita; Bustillos, Luis Gilberto Torres; González Aragón, Abelardo

This work shows a study of in situ and ex situ phytoextraction as a polishing step in the treatment of an industrial urban soil polluted with nickel, arsenic and copper. The soil was previously washed, and phytoextraction was performed by application of a mixture of grass (Festuca rubra, Cynodon dactylon, Lolium multiforum, Pennisetum). The soil had initial heavy metals concentrations of 131 ppm for Ni, 717 for As and 2734 for Cu (mg of metal/kg of dry soil). After seeding and emerging of grass, vegetal and soil samples were taken monthly during 4 months. Biomass generation, and concentration of Ni, As and Cu in vegetal tissue and soil were determined for every sample. Plants biomass growth in ex situ process was inhibited by 37% when compared with blank soil. Grass showed remarkable phytoextraction capability in situ, it produced 38 g of biomass every 15 days (wet weight) during a period of 3 months, but then declined in the fourth month. Concentrations of metals in grass biomass were up to 83 mg Ni/kg, 649 mg As/kg and 305 mg Cu/kg dry weight. Metal reduction of 49% for Ni, and 35% for Cu and As was observed at rhizospheric soil.

In situ vitrification: Application to buried waste

International Nuclear Information System (INIS)

Callow, R.A.; Thompson, L.E.

1991-01-01

Two in situ vitrification field tests were conducted in June and July 1990 at Idaho National Engineering Laboratory. In situ vitrification is a technology for in-place conversion of contaminated soils into a durable glass and crystalline waste form and is being investigated as a potential remediation technology for buried waste. The overall objective of the two tests was to assess the general suitability of the process to remediate buried waste structures found at Idaho National Engineering Laboratory. In particular, these tests were designed as part of a treatability study to provide essential information on field performance of the process under conditions of significant combustible and metal wastes, and to test a newly developed electrode feed technology. The tests were successfully completed, and the electrode feed technology provided valuable operational control for successfully processing the high metal content waste. The results indicate that in situ vitrification is a feasible technology for application to buried waste. 2 refs., 5 figs., 2 tabs

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.

Extreme Spectroscopy: In situ nuclear materials behavior from optical data

Energy Technology Data Exchange (ETDEWEB)

Guimbretiere, G.; Canizares, A.; Raimboux, N.; Omnee, R.; Duval, F.; Ammar, M.R.; Simon, P. [CNRS - UPR3079 CEMHTI, Universite d' Orleans, 45071Orleans cedex 2 (France); Desgranges, L.; Mohun, R. [CEA, DEN, DEC, F-13108 Saint-Paul-Lez-Durance (France); Jegou, C.; Magnin, M. [CEA/DTCD/SECM/LMPA, Marcoule 30207 Bagnols Sur Ceze (France); Clavier, N.; Dacheux, N. [ICSM-UMR5257 CEA/CNRS/UM2/ENSCM, Marcoule, BP17171, 30207 Bagnols sur Ceze (France)

2015-07-01

In the nuclear industry, materials are regularly exposed to high temperature or/and irradiation and a better knowledge and understanding of their behavior under such extreme conditions is a key-point for improvements and further developments. Nowadays, Raman spectroscopy begins to be well known as a promising technique in the post mortem and remote characterization of nuclear materials exposed to extreme conditions. On this topic, at ANIMMA 2013 conference, we have presented some results about its implementation in the study of model or real nuclear fuel. However, the strength of Raman spectroscopy as in situ characterization tool is mainly its ability to be implemented remotely through optical fibers. Aware of this, implementation of other optical techniques can be considered in order to gain information not only on the structural dynamics of materials but also on the electronic charge carrier populations. In this paper, we propose to present our last advances in Raman characterization of nuclear materials and enlarge to the in situ use of complementary optical spectroscopies. Emphasis will be made on the information that can be gained to the behavior of the model fuel depleted UO{sub 2} under extreme conditions of high temperature and ionic irradiation: - In Situ Raman identification of the radiolysis alteration products of UO{sub 2} in contact with water under ionic irradiation. - In Situ Raman recording of the damaged dynamic of UO{sub 2} under inert atmosphere. - In Situ Raman and photo-luminescence study of virgin and damaged UO2 at high temperature. - In Situ study of electronic charge carriers' behavior in U{sub x}Th{sub 1-x}O{sub 2} solid solutions by mean of Iono- and Thermo- luminescence under and post- ionic irradiation. (authors)

In-situ X-ray Nanocharacterization of Defect Kinetics in Chalcogenide Solar Cell Materials

Energy Technology Data Exchange (ETDEWEB)

Bertoni, Mariana [Arizona State Univ., Tempe, AZ (United States); Lai, Barry [Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source (APS); Masser, Jorg [Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source (APS); Buonassisi, Tonio [Massachusetts Inst. of Technology (MIT), Cambridge, MA (United States)

2016-09-21

For decades the optimization of polycrystalline absorbers has been done using an Edisonian approach, where trial and error and complex design of experiments in large parameter spaces have driven efficiencies to the record values we see today – CIGS at 22.5%, 22.1% for CdTe, 21.3% for high purity multi-crystalline silicon. Appropriate growth parameters are critical to ensure good quality crystals with low concentration of structural defects - low dislocation density and large grain sizes. However, to bridge the gap between the efficiencies today and the fundamental Shockley-Queisser limit for these materials a much more fundamental understanding of the role and interaction between composition, structure, defect density and electrical properties is required. In recent years multiple novel characterization techniques have shown the potential that nanoscale characterization can have in deciphering the composition of grain boundaries in materials like CIGS and CdTe. However, high resolution has come at the cost of small sampling areas and number of specimens, making it extremely difficult to draw conclusions based on the characteristic small sampling sizes. The missing links thus far have been: (1) the lack of statistical meaningfulness of the nanosclae studies and (2) the direct correlation of compositional variations to electrical performance with nanoscale resolution. In this work we present the use of synchrotron-based nano-X-ray fluorescence microscopy (nano-XRF), x-ray absorption nanospectroscopy (nano-XAS) coupled with nano-x-ray beam induced current (nano-XBIC) as ideal tools for investigating elemental, chemical and electrical properties of large areas of solar cell materials at the sub-micron scale with very high sensitivity. We show how the technique can provide statistical valuable information regarding the elemental segregation in CIGS and the direct correlation to current collection. For example, we demonstrate that Cu and Ga (and with that, CGI and GGI

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.

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...

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.

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.

Sperm cryopreservation in endangered felids: developing linkage of in situ-ex situ populations.

Science.gov (United States)

Swanson, W F; Magarey, G M; Herrick, J R

2007-01-01

Many of the world's cat species face growing threats to their continued survival in nature. For some species, managed captive populations may provide a reservoir for future reintroduction or genetic augmentation. Because most zoo populations are derived from small founder sizes and are subject to loss of genetic variation over time, periodic infusion of founder alleles is necessary to avoid the dire consequences of inbreeding. Collection and freezing of semen from free-living nondomestic felids offers a viable option for introducing founder genes into captive populations without removal of animals from the wild. The effective application of this strategy requires established protocols for safely capturing and anaesthetising wild cats coupled with suitable methods of semen recovery, processing and cryopreservation under field conditions. In small-sized non-domestic felids, the general feasibility of this approach is being explored in two studies of black-footed cats and Pallas' cats. Two factors - relatively low sperm numbers per ejaculate and compromised status of frozen-thawed cat spermatozoa - suggest that in vitro fertilisation (IVF) and embryo transfer present the most efficient use of this limiting resource in small-sized cats. Our studies with captive felids have explored alternative methods of sperm cryopreservation that are adaptable to field situations and shown that frozen-thawed spermatozoa from Pallas' cats, ocelots, and fishing cats exhibit adequate function to fertilise heterologous and/or homologous oocytes in vitro. Most recently, we investigated the fertilising capacity of frozen-thawed spermatozoa obtained from wild Pallas' cats in Mongolia. Combined with improved methods for embryo culture and transfer in small cat species, sperm banking in situ will facilitate introduction of new founders into captive populations without causing further depletion of their wild counterparts. As one component of holistic conservation programs, including ongoing

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

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

IN SITU LEAD IMMOBILIZATION BY APATITE

Science.gov (United States)

Lead contamination is of environmental concern due to its effect on human health. The purpose of this study was to develop a technology to immobilize Pb in situ in contaminated soils and wastes using apatite. Hydroxyapatite [Ca10(PO4)6(O...

Unintended and in situ amorphisation of pharmaceuticals.

Science.gov (United States)

Priemel, P A; Grohganz, H; Rades, T

2016-05-01

Amorphisation of poorly water-soluble drugs is one approach that can be applied to improve their solubility and thus their bioavailability. Amorphisation is a process that usually requires deliberate external energy input. However, amorphisation can happen both unintentionally, as in process-induced amorphisation during manufacturing, or in situ during dissolution, vaporisation, or lipolysis. The systems in which unintended and in situ amorphisation has been observed normally contain a drug and a carrier. Common carriers include polymers and mesoporous silica particles. However, the precise mechanisms by which in situ amorphisation occurs are often not fully understood. In situ amorphisation can be exploited and performed before administration of the drug or possibly even within the gastrointestinal tract, as can be inferred from in situ amorphisation observed during in vitro lipolysis. The use of in situ amorphisation can thus confer the advantages of the amorphous form, such as higher apparent solubility and faster dissolution rate, without the disadvantage of its physical instability. Copyright © 2015 Elsevier B.V. All rights reserved.

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.

[Species diversity of ex-situ cultivated Chinese medicinal plants].

Science.gov (United States)

Que, Ling; Chi, Xiu-Lian; Zang, Chun-Xin; Zhang, Yu; Chen, Min; Yang, Guang; Jin, An-Qi

2018-03-01

Ex-situ conservation is an important means to protect biological genetic resources. Resource protection has received more and more attention with the continuous improvement of the comprehensive utilization of traditional Chinese medicine resources. In this paper, the research and compilation of the species list of ex-situ cultivated medicinal plants in 12 Chinese Academy of Sciences botanic gardens and 19 specialized medicinal botanic gardens in China were carried out. Based on the Species 2000(2017) and other classification databases, species diversity of medicinal plants ex-situ cultivated in these botanical gardens were analyzed. The study found that there were 16 351 higher plant species in our country, belonging to 276 families and 1 936 genera. Of these, 6 949 specieswere medicinal plants, accounting for 50.4% of the total medicinal plants. There were 1 280 medicinal plants were in threatened status, accounting for 19.6% of all threatened species in the Chinese Biodiversity Red List, with ex-situ cultivated proportion of 59.5%. And 3 988 medicinal plants were Chinese endemic species, accounting for 22.5% of all Chinese endemic species, with ex-situ cultivated proportion of 53.3%. This article has reference significance for the management and protection of medicinal plant resources. Copyright© by the Chinese Pharmaceutical Association.

In Situ Remediation Integrated Program. In situ physical/chemical treatment technologies for remediation of contaminated sites: Applicability, developing status, and research needs

International Nuclear Information System (INIS)

Siegrist, R.L.; Gates, D.D.; West, O.R.; Liang, L.; Donaldson, T.L.; Webb, O.F.; Corder, S.L.; Dickerson, K.S.

1994-06-01

The U.S. Department of Energy (DOE) In Situ Remediation Integrated Program (ISR IP) was established in June 1991 to facilitate the development and implementation of in situ remediation technologies for environmental restoration within the DOE complex. Within the ISR IP, four subareas of research have been identified: (1) in situ containment, (2) in situ physical/chemical treatment (ISPCT), (3) in situ bioremediation, and (4) subsurface manipulation/electrokinetics. Although set out as individual focus areas, these four are interrelated, and successful developments in one will often necessitate successful developments in another. In situ remediation technologies are increasingly being sought for environmental restoration due to the potential advantages that in situ technologies can offer as opposed to more traditional ex situ technologies. These advantages include limited site disruption, lower cost, reduced worker exposure, and treatment at depth under structures. While in situ remediation technologies can offer great advantages, many technology gaps exist in their application. This document presents an overview of ISPCT technologies and describes their applicability to DOE-complex needs, their development status, and relevant ongoing research. It also highlights research needs that the ISR IP should consider when making funding decisions

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

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.

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

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.

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.

In situ protocol for butterfly pupal wings using riboprobes.

Science.gov (United States)

Ramos, Diane; Monteiro, Antonia

2007-01-01

Here we present, in video format, a protocol for in situ hybridizations in pupal wings of the butterfly Bicyclus anynana using riboprobes. In situ hybridizations, a mainstay of developmental biology, are useful to study the spatial and temporal patterns of gene expression in developing tissues at the level of transcription. If antibodies that target the protein products of gene transcription have not yet been developed, and/or there are multiple gene copies of a particular protein in the genome that cannot be differentiated using available antibodies, in situs can be used instead. While an in situ technique for larval wing discs has been available to the butterfly community for several years, the current protocol has been optimized for the larger and more fragile pupal wings.

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) ...

In situ electric fields causing electro-stimulation from conductor contact of charged human

International Nuclear Information System (INIS)

Nagai, T.; Hirata, A.

2010-01-01

Contact currents flow from/into a human body when touching an object such as a metal structure with a different electric potential. These currents can stimulate muscle and peripheral nerves. In this context, computational analyses of in situ electric fields caused by the contact current have been performed, while their effectiveness for transient contact currents has not well been investigated. In the present study, using an anatomically based human model, a dispersive finite-difference time-domain model was utilised to computed transient contact current and in situ electric fields from a charged human. Computed in situ electric fields were highly localised in the hand. In order to obtain an insight into the relationship between in situ electric field and electro-stimulation, cell-maximum and 5-mm averaged in situ electric fields were computed and compared with strength-duration curves. The comparison suggests that both measures could be larger than thresholds derived from the strength- duration curves with parameters used in previous studies. (authors)

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.

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.)

Design and optimization of hybrid ex situ/in situ steam generation recovery processes for heavy oil and bitumen

Energy Technology Data Exchange (ETDEWEB)

Yang, X.; Gates, I.D. [Calgary Univ., AB (Canada). Dept. of Chemical and Petroleum Engineering; Larter, S.R. [Calgary Univ., AB (Canada). Dept. of Geoscience]|[Alberta Ingenuity Centre for In Situ Energy, Edmonton, AB (Canada)

2008-10-15

Hybrid steam-air based oil recovery techniques were investigated using advanced 3-D reactive thermal reservoir simulations. The hybrid techniques combined ex situ steam and in situ steam generation processes in order to raise efficiency, lower natural gas consumption, and reduce gas emissions. The steam-air based processes used 70 per cent of the energy of conventional steam assisted gravity drainage (SAGD) techniques to recover the same amount of oil. The process used an SAGD wellpair arrangement, where steam and air were injected through the top injection well. The kinetic parameters used in the study were developed by history matching a combustion tube experiments with Athabasca bitumen conducted to predict cumulative bitumen and gas production volumes and compositions. A total of 6 SAGD and 6 in situ combustion simulations were conducted with steam oxygen volume ratios set at 50 per cent steam and 50 per cent oxygen. Various case studies were considered over a 5 year period. Carbon dioxide (CO{sub 2}) emissions were also measured as well as cumulative water and methane consumption rates. Results of the study were used to develop an optimized hybrid operation that consisted of a SAGD well pair arrangement operating with cyclic steam-oxygen injection at high pressures. It was concluded that the high pressure operation increased the steam partial pressure within the reservoir and enhanced combustion performance. A 29 per cent improvement in the cumulative energy to oil ratio was obtained. 23 refs., 2 tabs., 9 figs.

[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

In situ vitrification: application analysis for stabilization of transuranic waste

International Nuclear Information System (INIS)

Oma, K.H.; Farnsworth, R.K.; Rusin, J.M.

1982-09-01

The in situ vitrification process builds upon the electric melter technology previously developed for high-level waste immobilization. In situ vitrification converts buried wastes and contaminated soil to an extremely durable glass and crystalline waste form by melting the materials, in place, using joule heating. Once the waste materials have been solidified, the high integrity waste form should not cause future ground subsidence. Environmental transport of the waste due to water or wind erosion, and plant or animal intrusion, is minimized. Environmental studies are currently being conducted to determine whether additional stabilization is required for certain in-ground transuranic waste sites. An applications analysis has been performed to identify several in situ vitrification process limitations which may exist at transuranic waste sites. Based on the process limit analysis, in situ vitrification is well suited for solidification of most in-ground transuranic wastes. The process is best suited for liquid disposal sites. A site-specific performance analysis, based on safety, health, environmental, and economic assessments, will be required to determine for which sites in situ vitrification is an acceptable disposal technique. Process economics of in situ vitrification compare favorably with other in-situ solidification processes and are an order of magnitude less than the costs for exhumation and disposal in a repository. Leachability of the vitrified product compares closely with that of Pyrex glass and is significantly better than granite, marble, or bottle glass. Total release to the environment from a vitrified waste site is estimated to be less than 10 -5 parts per year. 32 figures, 30 tables

In Situ Cleanable Alternative HEPA Filter Media

International Nuclear Information System (INIS)

Adamson, D. J.; Terry, M. T.

2002-01-01

The Westinghouse Savannah River Company, located at the Savannah River Site in Aiken, South Carolina, is currently testing two types of filter media for possible deployment as in situ regenerable/cleanable High Efficiency Particulate Air (HEPA) filters. The filters are being investigated to replace conventional, disposable, glass-fiber, HEPA filters that require frequent removal, replacement, and disposal. This is not only costly and subjects site personnel to radiation exposure, but adds to the ever-growing waste disposal problem. The types of filter media being tested, as part of a National Energy Technology Laboratory procurement, are sintered nickel metal and ceramic monolith membrane. These media were subjected to a hostile environment to simulate conditions that challenge the high-level waste tank ventilation systems. The environment promoted rapid filter plugging to maximize the number of filter loading/cleaning cycles that would occur in a specified period of time. The filters were challenged using nonradioactive simulated high-level waste materials and atmospheric dust; materials that cause filter pluggage in the field. The filters are cleaned in situ using an aqueous solution. The study found that both filter media were insensitive to high humidity or moisture conditions and were easily cleaned in situ. The filters regenerated to approximately clean filter status even after numerous plugging and in situ cleaning cycles. Air Techniques International is conducting particle retention testing on the filter media at the Oak Ridge Filter Test Facility. The filters are challenged using 0.3-mm di-octyl phthalate particles. Both the ceramic and sintered media have a particle retention efficiency > 99.97%. The sintered metal and ceramic filters not only can be cleaned in situ, but also hold great potential as a long life alternative to conventional HEPA filters. The Defense Nuclear Facility Safety Board Technical Report, ''HEPA Filters Used in the Department of

On iron radionuclide interactions and in situ measurement of iron corrosion products

International Nuclear Information System (INIS)

Puranen, A.; Jonsson, M.; Cui, D.; Scheidegger, A.M.; Wersin, P.; Spahiu, K.

2005-01-01

Full text of publication follows: In performance assessments of hard rock repositories, it is conservatively assumed that waste canisters are breached and that the spent fuel will get into contact with groundwater after 1000 years. When the canister eventually fails to protect HLW from groundwater, dissolved radionuclides from HLW will react with iron canister materials. The reactivity will depend on the conditions in solution and at the iron-water interface. To improve our understanding on the redox chemistry at near field conditions, batch experiments are conducted by contacting polished iron foils with a synthetic groundwater solution containing 10 mM NaCl, 2 mM NaHCO 3 and 5 ppm Se(IV), Se(VI), Tc(VII) and U(VI) in a glove box filled with Ar + 0.03% CO 2 gas mixture. The reaction rates are measured by analysing Se, Tc and U concentrations by ICP-MS. Iron corrosion products formed during the reaction(s) is monitored in-situ by a Layer Raman spectrometer through an optical window. The corrosion potential of the iron foil as well as the Eh and pH values of the bulk solution are recorded continuously during the experiment. The reacted iron foil is embedded with EPOXY resin, and the cross section will be analysed by SEM-EDS and XAS. The preliminary experimental results shows that with the formation of iron green rust FeII 4 FeIII 2 (OH) 12 CO 3 on iron foil, the rates of redox reactions between iron and the negatively charged radionuclides species are increased. The observation is explained by the fact that radionuclide anionic species can be first adsorbed then reduced on the positively charged outer surface of iron green rust. The positive charge is a result of the electrical balance of the negative charges of carbonate contained between the layered iron hydroxides in the green rust. Reduced forms of radionuclides are identified in the iron corrosion products. The results suggest that the formation of iron green rust as a corrosion product on the surface of iron

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

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.

In situ detrital zircon (U-Th)/He thermochronology

Science.gov (United States)

Tripathy, A.; Monteleone, B. D.; van Soest, M. C.; Hodges, K.; Hourigan, J. K.

2010-12-01

Detrital studies of both sand and rock are relevant to many problems, ranging from the climate and tectonics feedback debate to the long-term record of orogenic evolution. When applying the conventional (U-Th)/He technique to such studies, two important issues arise. Often, only euhedral grains are permissible for analysis in order to make simple geometric corrections for α-recoil. In detrital samples, this is problematic because euhedral grains can be scarce due to mechanical abrasion during transport, and potentially introduce bias in favour of more proximally sourced grains. Second, inherent to detrital studies is the need to date many grains (>100) per sample to ensure a representative sampling of the sediment source region, thus making robust conventional detrital studies both expensive and time-consuming. UV laser microprobes can improve this by permitting careful targeting of the grain interior away from the α-ejection zone, rendering the α-recoil correction unnecessary, thus eliminating bias toward euhedral grains. In the Noble Gas, Geochemistry, and Geochronology Laboratory at ASU, apatite and zircon have been successfully dated using in situ methods. For this study, the conventional and in situ techniques are compared by dating zircons from a modern river sand that drains a small catchment in the Mesozoic-Cenozoic Ladakh Batholith in NW India. This sample has a simple provenance, which allows us to demonstrate the robustness of the in situ method. Moreover, different microbeam techniques will be explored to establish the most efficient approach to obtain accurate and precise U-Th concentrations using synrock, which is our powdered, homogenized, and reconstituted zircon-rock standard. Without this, such in situ U-Th data would be difficult to obtain. 117 zircons were dated using the conventional (U-Th)/He method, revealing dates ranging from 9.70±0.35 to 106.6±3.5 Ma (2σ) with the major mode at 26 Ma. For comparison, 44 grains were dated using the in

Triplex in-situ hybridization

Science.gov (United States)

Fresco, Jacques R.; Johnson, Marion D.

2002-01-01

Disclosed are methods for detecting in situ the presence of a target sequence in a substantially double-stranded nucleic acid segment, which comprises: a) contacting in situ under conditions suitable for hybridization a substantially double-stranded nucleic acid segment with a detectable third strand, said third strand being capable of hybridizing to at least a portion of the target sequence to form a triple-stranded structure, if said target sequence is present; and b) detecting whether hybridization between the third strand and the target sequence has occured.

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...

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).

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.

Pattern classification by memristive crossbar circuits using ex situ and in situ training

Science.gov (United States)

Alibart, Fabien; Zamanidoost, Elham; Strukov, Dmitri B.

2013-06-01

Memristors are memory resistors that promise the efficient implementation of synaptic weights in artificial neural networks. Whereas demonstrations of the synaptic operation of memristors already exist, the implementation of even simple networks is more challenging and has yet to be reported. Here we demonstrate pattern classification using a single-layer perceptron network implemented with a memrisitive crossbar circuit and trained using the perceptron learning rule by ex situ and in situ methods. In the first case, synaptic weights, which are realized as conductances of titanium dioxide memristors, are calculated on a precursor software-based network and then imported sequentially into the crossbar circuit. In the second case, training is implemented in situ, so the weights are adjusted in parallel. Both methods work satisfactorily despite significant variations in the switching behaviour of the memristors. These results give hope for the anticipated efficient implementation of artificial neuromorphic networks and pave the way for dense, high-performance information processing systems.

In situ vitrification program treatability investigation progress report

International Nuclear Information System (INIS)

Arrenholz, D.A.

1990-12-01

This document presents a summary of the efforts conducted under the in situ vitrification treatability study during the period from its initiation in FY-88 until FY-90. In situ vitrification is a thermal treatment process that uses electrical power to convert contaminated soils into a chemically inert and stable glass and crystalline product. Contaminants present in the soil are either incorporated into the product or are pyrolyzed during treatment. The treatability study being conducted at the Idaho National Engineering Laboratory by EG ampersand G Idaho is directed at examining the specific applicability of the in situ vitrification process to buried wastes contaminated with transuranic radionuclides and other contaminants found at the Subsurface Disposal Area of the Radioactive Waste Management Complex. This treatability study consists of a variety of tasks, including engineering tests, field tests, vitrified product evaluation, and analytical models of the ISV process. The data collected in the course of these efforts will address the nine criteria set forth in the Comprehensive Environmental Response, Compensation, and Liability Act, which will be used to identify and select specific technologies to be used in the remediation of the buried wastes at the Subsurface Disposal Area. 6 refs., 4 figs., 3 tabs

A Combined SAXS/SANS Study for the in Situ Characterization of Ligand Shells on Small Nanoparticles: The Case of ZnO.

Science.gov (United States)

Schindler, T; Schmiele, M; Schmutzler, T; Kassar, T; Segets, D; Peukert, W; Radulescu, A; Kriele, A; Gilles, R; Unruh, T

2015-09-22

ZnO nanoparticles (NPs) have great potential for their use in, e.g., thin film solar cells due to their electro-optical properties adjustable on the nanoscale. Therefore, the production of well-defined NPs is of major interest. For a targeted production process, the knowledge of the stabilization layer of the NPs during and after their formation is of particular importance. For the study of the stabilizer layer of ZnO NPs prepared in a wet chemical synthesis from zinc acetate, only ex situ studies have been performed so far. An acetate layer bound to the surface of the dried NPs was found; however, an in situ study which addresses the stabilizing layer surrounding the NPs in a native dispersion was missing. By the combination of small angle scattering with neutrons and X-rays (SANS and SAXS) for the same sample, we are now able to observe the acetate shell in situ for the first time. In addition, the changes of this shell could be followed during the ripening process for different temperatures. With increasing size of the ZnO core (d(core)) the surrounding shell (d(shell)) becomes larger, and the acetate concentration within the shell is reduced. For all samples, the shell thickness was found to be larger than the maximum extension of an acetate molecule with acetate concentrations within the shell below 50 vol %. Thus, there is not a monolayer of acetate molecules that covers the NPs but rather a swollen shell of acetate ions. This shell is assumed to hinder the growth of the NPs to larger macrostructures. In addition, we found that the partition coefficient μ between acetate in the shell surrounding the NPs and the total amount of acetate in the solution is about 10% which is in good agreement with ex situ data determined by thermogravimetric analysis.

In Situ Synchrotron XRD on a Capillary Li-O2 Battery Cell

DEFF Research Database (Denmark)

Storm, Mie Møller; Johnsen, Rune; Norby, Poul

2014-01-01

of a electrolyte filled capillary with anode and cathode in each end suspended on stainless steel wires, the oxygen in-let is placed on the cathode side of the capillary with a flushing system for oxygen in-let. In this study we present a flexible design of a capillary based Li-O2 battery with discharge and charge...... a stainless steel wire where the cathode is attached. The in situ XRD measurements show how the Li2O2 growth depend on current discharge rate and how the FWHM changes dependent on reflection and charge/discharge.Several cells were tested both ex situ and in situ, and in situ XRD for 1st discharge/charge and 2...

In-situ testing methods using radioactive tracers

International Nuclear Information System (INIS)

Sauzay, G.

1976-01-01

Some typical applications of tracer techniques in hydrology are presented: study of the extraction of sands and gravels in a estuary; in-situ study of the transport of sediments by the swell at a depth ranging from 8 to 22m; study of the transport of sands on the site Bonne Anse - Saint Palais [fr

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

Fathead minnow whole-mount in situ hybridization (WISH)

Data.gov (United States)

U.S. Environmental Protection Agency — This study demonstrates the potential of whole-mount in situ hybridization (WISH), in conjunction with quantitative real-time polymerase chain reaction (QPCR)...

Investigations into low pressure methanol synthesis

DEFF Research Database (Denmark)

Sharafutdinov, Irek

The central topic of this work has been synthesis, characterization and optimization of novel Ni-Ga based catalysts for hydrogenation of CO2 to methanol. The overall goal was to search for materials that could be used as a low temperature (and low pressure) methanol synthesis catalyst....... This is required for small scale delocalized methanol production sites, where installation of energy demanding compression units should be avoided. The work was triggered by DFT calculations, which showed that certain bimetallic systems are active towards methanol synthesis from CO2 and H2 at ambient pressure...... containing 5:3 molar ratio of Ni:Ga, the intrinsic activity (methanol production rate per active surface area) is comparable to that of highly optimised Cu/ZnO/Al2O3. Formation of the catalyst was investigated with the aid of in-situ XRD and in-situ XAS techniques. The mechanism of alloying was proposed...

In situ Transmission Electron Microscopy of catalyst sintering

DEFF Research Database (Denmark)

DeLaRiva, Andrew T.; Hansen, Thomas Willum; Challa, Sivakumar R.

2013-01-01

Recent advancements in the field of electron microscopy, such as aberration correctors, have now been integrated into Environmental Transmission Electron Microscopes (TEMs), making it possible to study the behavior of supported metal catalysts under operating conditions at atomic resolution. Here......, we focus on in situ electron microscopy studies of catalysts that shed light on the mechanistic aspects of catalyst sintering. Catalyst sintering is an important mechanism for activity loss, especially for catalysts that operate at elevated temperatures. Literature from the past decade is reviewed...... along with our recent in situ TEM studies on the sintering of Ni/MgAl2O4 catalysts. These results suggest that the rapid loss of catalyst activity in the earliest stages of catalyst sintering could result from Ostwald ripening rather than through particle migration and coalescence. The smallest...

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.

Detection of denitrification genes by in situ rolling circle amplification - fluorescence in situ hybridization (in situ RCA-FISH) to link metabolic potential with identity inside bacterial cells

DEFF Research Database (Denmark)

Hoshino, Tatsuhiko; Schramm, Andreas

2010-01-01

target site. Finally, the RCA product inside the cells was detected by standard fluorescence in situ hybridization (FISH). The optimized protocol showed high specificity and signal-to-noise ratio but low detection frequency (up to 15% for single-copy genes and up to 43% for the multi-copy 16S rRNA gene...... as Candidatus Accumulibacter phosphatis by combining in situ RCA-FISH with 16S rRNA-targeted FISH. While not suitable for quantification because of its low detection frequency, in situ RCA-FISH will allow to link metabolic potential with 16S rRNA (gene)-based identification of single microbial cells.......). Nevertheless, multiple genes (nirS and nosZ; nirS and the 16S rRNA gene) could be detected simultaneously in P. stutzeri. Environmental application of in situ RCA-FISH was demonstrated on activated sludge by the differential detection of two types of nirS-defined denitrifiers; one of them was identified...

A bio-inspired approach for in situ synthesis of tunable adhesive

International Nuclear Information System (INIS)

Sun, Leming; Yi, Sijia; Wang, Yongzhong; Pan, Kang; Zhong, Qixin; Zhang, Mingjun

2014-01-01

Inspired by the strong adhesive produced by English ivy, this paper proposes an in situ synthesis approach for fabricating tunable nanoparticle enhanced adhesives. Special attention was given to tunable features of the adhesive produced by the biological process. Parameters that may be used to tune properties of the adhesive will be proposed. To illustrate and validate the proposed approach, an experimental platform was presented for fabricating tunable chitosan adhesive enhanced by Au nanoparticles synthesized in situ. This study contributes to a bio-inspired approach for in situ synthesis of tunable nanocomposite adhesives by mimicking the natural biological processes of ivy adhesive synthesis. (paper)

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

In-situ bioremediation via horizontal wells

International Nuclear Information System (INIS)

Hazen, T.C.; Looney, B.B.; Enzien, M.; Franck, M.M.; Fliermans, C.B.; Eddy, C.A.

1993-01-01

This project is designed to demonstrate in situ bioremediation of groundwater and sediment contaminated with chlorinated solvents. Indigenous microorganisms were stimulated to degrade TCE, PCE and their daughter products in situ by addition of nutrients to the contaminated zone. In situ biodegradation is a highly attractive technology for remediation because contaminants are destroyed, not simply moved to another location or immobilized, thus decreasing costs, risks, and time, while increasing efficiency and public and regulatory acceptability. Bioremediation has been found to be among the least costly technologies in applications where it will work (Radian 1989). Subsurface soils and water adjacent to an abandoned process sewer line at the SRS have been found to have elevated levels of TCE (Marine and Bledsoe 1984). This area of subsurface and groundwater contamination is the focus of a current integrated demonstration of new remediation technologies utilizing horizontal wells. Bioremediation has the potential to enhance the performance of in situ air stripping as well as offering stand-alone remediation of this and other contaminated sites (Looney et al. 1991). Horizontal wells could also be used to enhance the recovery of groundwater contaminants for bioreactor conversions from deep or inaccessible areas (e.g., under buildings) and to enhance the distribution of nutrient or microbe additions in an in situ bioremediation

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

In-situ gelling polymers for biomedical applications

CERN Document Server

2015-01-01

This book presents the research involving in situ gelling polymers and can be used as a guidebook for academics, industrialists and postgraduates interested in this area. This work summaries the academic contributions from the top authorities in the field and explore the fundamental principles of in situ gelling polymeric networks, along with examples of their major applications. This book aims to provide an up-to-date resource of in situ gelling polymer research.

In situ gelling dorzolamide loaded chitosan nanoparticles for the treatment of glaucoma.

Science.gov (United States)

Katiyar, Shefali; Pandit, Jayamanti; Mondal, Rabi S; Mishra, Anil K; Chuttani, Krishna; Aqil, Mohd; Ali, Asgar; Sultana, Yasmin

2014-02-15

The most important risk associated with glaucoma is the onset and progression of intraocular pressure. The objective of this study was to formulate in situ gel of chitosan nanoparticles to enhance the bioavailability and efficacy of dorzolamide in the glaucoma treatment. Optimized nanoparticles were spherical in shape (particle size: 164 nm) with a loading efficiency of 98.1%. The ex vivo release of the optimized in situ gel nanoparticle formulation showed a sustained drug release as compared to marketed formulation. The gamma scintigraphic study of prepared in situ nanoparticle gel showed good corneal retention compared to marketed formulation. HET-CAM assay of the prepared formulation scored 0.33 in 5 min which indicates the non-irritant property of the formulation. Thus in situ gel of dorzolamide hydrochloride loaded nanoparticles offers a more intensive treatment of glaucoma and a better patient compliance as it requires fewer applications per day compared to conventional eye drops. Copyright © 2013 Elsevier Ltd. All rights reserved.

Feasibility testing of in situ vitrification of uranium-contaminated soils

International Nuclear Information System (INIS)

Ikuse, H.; Tsuchino, S.; Tasaka, H.; Timmerman, C.L.

1989-01-01

Process feasibility studies using in situ vitrification (ISV) were successfully performed on two different uranium-contaminated wastes. In situ vitrification is a thermal treatment process that converts contaminated soils into durable glass and crystalline form. Of the two different wastes, one waste was uranium mill tailings, while the other was uranium-contaminated soils which had high water contents. Analyses of the data from the two tests are presented

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.

In situ hydrogen loading on zirconium powder

Energy Technology Data Exchange (ETDEWEB)

Maimaitiyili, Tuerdi, E-mail: tuerdi.maimaitiyili@mah.se; Blomqvist, Jakob [Malmö University, Östra Varvsgatan 11 A, Malmö, Skane 20506 (Sweden); Steuwer, Axel [Lund University, Ole Römers väg, Lund, Skane 22100 (Sweden); Nelson Mandela Metropolitan University, Gardham Avenue, Port Elizabeth 6031 (South Africa); Bjerkén, Christina [Malmö University, Östra Varvsgatan 11 A, Malmö, Skane 20506 (Sweden); Zanellato, Olivier [Ensam - Cnam - CNRS, 151 Boulevard de l’Hôpital, Paris 75013 (France); Blackmur, Matthew S. [Materials Performance Centre, School of Materials, The University of Manchester, Manchester M1 7HS (United Kingdom); Andrieux, Jérôme [European Synchrotron Radiation Facility, 6 rue J Horowitz, Grenoble 38043 (France); Université de Lyon, 43 Bd du 11 novembre 1918, Lyon 69100 (France); Ribeiro, Fabienne [Institut de Radioprotection et Sûreté Nucléaire, IRSN, BP 3, 13115 Saint-Paul Lez Durance (France)

2015-06-26

Commercial-grade Zr powder loaded with hydrogen in situ and phase transformations between various Zr and ZrH{sub x} phases have been monitored in real time. For the first time, various hydride phases in a zirconium–hydrogen system have been prepared in a high-energy synchrotron X-ray radiation beamline and their transformation behaviour has been studied in situ. First, the formation and dissolution of hydrides in commercially pure zirconium powder were monitored in real time during hydrogenation and dehydrogenation, then whole pattern crystal structure analysis such as Rietveld and Pawley refinements were performed. All commonly reported low-pressure phases presented in the Zr–H phase diagram are obtained from a single experimental arrangement.

In situ hydrogen loading on zirconium powder

International Nuclear Information System (INIS)

Maimaitiyili, Tuerdi; Blomqvist, Jakob; Steuwer, Axel; Bjerkén, Christina; Zanellato, Olivier; Blackmur, Matthew S.; Andrieux, Jérôme; Ribeiro, Fabienne

2015-01-01

Commercial-grade Zr powder loaded with hydrogen in situ and phase transformations between various Zr and ZrH x phases have been monitored in real time. For the first time, various hydride phases in a zirconium–hydrogen system have been prepared in a high-energy synchrotron X-ray radiation beamline and their transformation behaviour has been studied in situ. First, the formation and dissolution of hydrides in commercially pure zirconium powder were monitored in real time during hydrogenation and dehydrogenation, then whole pattern crystal structure analysis such as Rietveld and Pawley refinements were performed. All commonly reported low-pressure phases presented in the Zr–H phase diagram are obtained from a single experimental arrangement

X-ray absorption studies of graphite intercalates and metal-ammonia solutions

International Nuclear Information System (INIS)

Robertson, A.S.

1979-09-01

X-ray absorption spectroscopy (XAS) was used to study the arsenic fluorocomplexes, including the AsF 5 and AsF 6 - intercalates of graphite, and rubidium metal-ammonia solutions. The As-F distances obtained for AsF 3 and AsF 5 gas are both in excellent agreement with electron diffraction data (within 0.004 A). A superior measurement which is significantly shorter than the accepted value of the bond distance in an undistorted AsF 6 - octahedra is reported. Both the XAES and EXAFS data presented support the hypothesis that the AsF 5 oxidizes graphite upon intercalation to produce AsF 6 - and AsF 3 intercalant species. Changes in the Rb K-edge features which are consistent with the known properties of Rb-NH 3 are correlated with conductivity and delocalization of the solvated electrons. In the XAES region, intensity and position changes of absorption transitions are explained. In the EXAFS region, the Rb-N bond distance and the relative number of nitrogen atoms in the first shell are measured. XAS has been shown to provide unique information about the nature of the metal-ammonia phase separation, phase transition, and density fluctuations

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.

Field Implementation Plan for the In-Situ Bioremediation Treatability Study at the Technical Area-V Groundwater Area of Concern

Energy Technology Data Exchange (ETDEWEB)

Li, Jun [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

2016-10-31

This Field Implementation Plan (FIP) was prepared by Sandia National Laboratories, New Mexico (SNL/NM) and provides instruction on conducting a series of in-situ bioremediation (ISB) tests as described in the Revised Treatability Study Work Plan for In-Situ Bioremediation at the Technical Area-V Groundwater Area of Concern, referred to as the Revised Work Plan in this FIP. The Treatability Study is designed to gravity inject an electron-donor substrate and bioaugmentation bacteria into groundwater via three injection wells to perform bioremediation of the constituents of concern (COCs), nitrate and trichloroethene (TCE), in the regions with the highest concentrations at the Technical Area-V Groundwater (TAVG) Area of Concern (AOC). The Treatability Study will evaluate the effectiveness of bioremediation solution delivery and COC treatment over time. This FIP is designed for SNL/NM work planning and management. It is not intended to be submitted for regulator’s approval. The technical details presented in this FIP are subject to change based on field conditions, availability of equipment and materials, feasibility, and inputs from Sandia personnel and Aboveground Injection System contractor.

Field Implementation Plan for the In-Situ Bioremediation Treatability Study at the Technical Area-V Groundwater Area of Concern

International Nuclear Information System (INIS)

Li, Jun

2016-01-01

This Field Implementation Plan (FIP) was prepared by Sandia National Laboratories, New Mexico (SNL/NM) and provides instruction on conducting a series of in-situ bioremediation (ISB) tests as described in the Revised Treatability Study Work Plan for In-Situ Bioremediation at the Technical Area-V Groundwater Area of Concern, referred to as the Revised Work Plan in this FIP. The Treatability Study is designed to gravity inject an electron-donor substrate and bioaugmentation bacteria into groundwater via three injection wells to perform bioremediation of the constituents of concern (COCs), nitrate and trichloroethene (TCE), in the regions with the highest concentrations at the Technical Area-V Groundwater (TAVG) Area of Concern (AOC). The Treatability Study will evaluate the effectiveness of bioremediation solution delivery and COC treatment over time. This FIP is designed for SNL/NM work planning and management. It is not intended to be submitted for regulator's approval. The technical details presented in this FIP are subject to change based on field conditions, availability of equipment and materials, feasibility, and inputs from Sandia personnel and Aboveground Injection System contractor.

Mars Oxygen In-Situ Resource Utilization Experiment

Data.gov (United States)

National Aeronautics and Space Administration — The Mars Oxygen In-Situ Resource Utilization Experiment (MOXIE) will be the first in-situ resource utilization (ISRU) technology demonstration on Mars. Competitively...

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

Soil weed seed bank in situ and ex situ at a smallholder field in Maranhão State, northeastern Brazil

Directory of Open Access Journals (Sweden)

Mário Luiz Ribeiro Mesquita

2014-11-01

Full Text Available The objective of this research was to assess the density, floristic composition,  phytosociology and diversity of a soil weed seed bank ex situ by germination in a greenhouse and in situ by weed sampling on a smallholder corn field located in Lago Verde County, Maranhão State. Fifteen pairs of 25 m2 plots were designated. In half of these plots, 90 soil samples were collected with an open metal template measuring 25 x 16 x 3 cm and placed in a greenhouse to germinate. In the other half, 90 weed samples were collected using the same metal template. We recorded a total of 1,998 individuals from 40 species, 31 genera and 16 families, from which 659 individuals germinated in situ and 1,339 exsitu. Density was higher ex situ, with 372 plants m-2. The Cyperaceae family had the highest floristic richness with nine species, followed by the Poaceae with six. The dominant species based on the Importance Value Index were Lindernia crustacea (IVI 27.7% in situ and Scleria lithosperma (IVI 37.0% ex situ. Floristic diversity was higher ex situ, with H’ = 2.66 nats ind-1. These results could help predict infestation potential and could lead to improved weed management strategies in corn-growing areas on smallholdings in Maranhão State, northeastern Brazil.

Clarifying the learning experiences of healthcare professionals with in situ and off-site simulation-based medical education: a qualitative study

NARCIS (Netherlands)

Sorensen, J.L.; Navne, L.E.; Martin, H.M.; Ottesen, B.; Albrecthsen, C.K.; Pedersen, B.W.; Kjaergaard, H.; Vleuten, C. van der

2015-01-01

OBJECTIVE: To examine how the setting in in situ simulation (ISS) and off-site simulation (OSS) in simulation-based medical education affects the perceptions and learning experience of healthcare professionals. DESIGN: Qualitative study using focus groups and content analysis. PARTICIPANTS:

In situ transmission electron microscopy studies of microstructure evolution in Ba(Zr0.2Ti0.8)O3-x(Ba0.7Ca0.3)TiO3 piezoceramic

International Nuclear Information System (INIS)

Zakhozheva, Marina

2016-01-01

The purpose of this work is to understand the microstructural features which contribute to the strong electromechanical properties of the lead-free Ba (Zr 0.2 Ti 0.8 )O 3 -x(Ba 0.7 Ca 0.3 )TiO 3 (BZT-xBCT) piezoelectric ceramic. Detailed conventional transmission electron microscopy (TEM) studies on a broad variety of BZT - xBCT were performed in order to demonstrate the composition dependent structural changes. Moreover, several in situ TEM techniques, including in situ hot- and cold-stage, in situ electric field and in situ electric field with simultaneous cooling, were successfully applied in order to monitor the domain morphology evolution in real time. By means of in situ temperature dependent TEM experiments it was shown that during rhombohedral → orthorhombic → tetragonal phase transition the domain morphology changed according to the crystal structure present. During in situ electric field investigations the displacement of the domain walls and changes in the domain configuration during electrical poling were observed, which indicates a high extrinsic contribution to the piezoelectric response in all BZT - xBCT compositions studied. From the results of in situ electric field TEM experiments with simultaneous cooling, we obtained experimental evidence that the further the composition deviates from the polymorphic phase boundary, the higher the electric field required to fully pole the material.

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.

In-situ bioremediation of TCE-contaminated groundwater

Energy Technology Data Exchange (ETDEWEB)

Travis, B.J. [Los Alamos National Lab., NM (United States); Rosenberg, N.D. [Lawrence Livermore National Lab., CA (United States)

1998-12-31

This is the final report of a two-year, Laboratory Directed Research and Development (LDRD) project at the Los Alamos National Laboratory (LANL). A barrier to wider use of in situ bioremediation technology is that results are often variable and difficult to predict. In situ bioremediation has shown some very notable and well publicized successes, but implementation of the technology is complex. An incomplete understanding of the effects of variable site characteristics and the lack of adequate tools to predict and measure success have made the design, control and validation of bioremediation more empirical than desired. The long-term objective of this project is to improve computational tools used to assess and optimize the expected performance of bioremediation at a site. An important component of the approach is the explicit inclusion of uncertainties and their effect on the end result. The authors have extended their biokinetics model to include microbial competition and predation processes. Predator species can feed on the microbial species that degrade contaminants, and the simulation studies show that species interactions must be considered when designing in situ bioremediation systems. In particular, the results for TCE indicate that protozoan grazing could reduce the amount of biodegradation by about 20%. These studies also indicate that the behavior of barrier systems can become complex due to predator grazing.

Immunohistochemical differentiation of atypical hyperplasia vs. carcinoma in situ of the breast.

Science.gov (United States)

Masood, S; Sim, S J; Lu, L

1992-01-01

The distinction between atypical hyperplasia and carcinoma in situ in breast lesions can be difficult. The identification of myoepithelial cell layers may be helpful in establishing a diagnosis of proliferative breast disease vs. intraepithelial neoplasia. We reviewed pathologic material on 20 cases of atypical hyperplasia and 29 cases of carcinoma in situ. Immunohistochemical stains were employed against muscle-specific actin, S-100 protein, and cytokeratin to identify myoepithelial cells and to recognize different staining patterns. In atypical hyperplasia, muscle-specific actin staining identified myoepithelial cells in fine branching fibrovascular layers or as scattered cells between other proliferating cells. This pattern was absent in carcinoma in situ. S-100 protein showed more positive staining in atypical hyperplasia than in carcinoma in situ with patterns distinct from muscle-specific actin. Immunostaining for cytokeratin demonstrated distinctly different patterns between the two lesions. This study suggests that muscle-specific actin, S-100 protein, and cytokeratin in combination may assist in distinguishing proliferative breast disease with atypia from carcinoma in situ.

Evaluation and analysis of geological condition of in-situ fragmentation leaching uranium

International Nuclear Information System (INIS)

Yang Jianming; Tan Kaixuan; Huang Xiaonai

2003-01-01

The ore geological condition, hydrogeological condition, engineering geological condition and technological mineralogical character of in-situ fragmentation leaching uranium are analyzed, and it is considered that the implementation of in-situ fragmentation leaching uranium technology is decided by different geological factor. Previously prospecting and geological condition evaluation of uranium ore is based on traditional mining method. If in-situ fragmentation leaching uranium method is adopted, one must re-evaluate previously prospected deposits before they are mined, or one must evaluate new prospecting deposits according to geological conditions of in-situ fragmentation leaching uranium method. The feasibility evaluation method of uranium deposit by in-situ fragmentation leaching uranium put forward by B. N. Mociniets is introducd, and it is considered that B. N. Mociniets method has guidable significance for geological condition evaluation before uranium deposits are mined. A feasibility study is done by applying B. N. Mociniets method to a uranium deposit. (authors)

Ex situ Flora of China

Directory of Open Access Journals (Sweden)

Hongwen Huang

2017-12-01

Full Text Available The role of living collections-based research and discovery has been a prominent feature throughout the history of evolution and advance of botanical science: such research is the core and soul of the botanical gardens. Currently, there are c. 162 Chinese botanical gardens, harboring c. 20,000 species in China. As an example of initiatives to utilize the garden cultivated flora to address plant diversity conservation and germplasm discovery for sustainable agriculture and the bio-industries, the Ex situ Flora of China project aims to catalog and document this mega-diversity of plants that are cultivated in the Chinese botanical gardens. The concept of Ex situ Flora of China is a complete new formulation of species, based on garden cultivated individuals and populations, to obtain better morphological descriptions, provide multi-purpose applicability and a fundamental data service that will support national bio-strategies and bio-industries. It emphasises integrative information, accurately collected from living collections across different Chinese botanical gardens, on biology, phenology, cultivation requirements and uses of plant resources, which are normally not available from traditional Floras based on herbarium specimens. The ex situ flora should provide better information coverage for taxonomy, biological and introduction and collection data and color photos of stems, leaves, flowers, fruits and seed, as well as useful information of cultivation key points and main use of each plant. In general, the Ex situ Flora of China provides more useful information than the traditional Flora Reipublicae Popularis Sinicae. The project of Ex situ Flora of China is planned to be one of the most important initiatives of the plant diversity research platform for sustainable economic and social development in China.

In situ monitoring of the electrochemical dissolution of tungsten

Energy Technology Data Exchange (ETDEWEB)

Krebsz, Melinda [Christian Doppler Laboratory for Combinatorial Oxide Chemistry at ICTAS, Johannes Kepler University Linz (Austria); Kollender, Jan Philipp [Institute for Chemical Technology of Inorganic Materials (ICTAS), Johannes Kepler University Linz (Austria); Hassel, Achim Walter [Christian Doppler Laboratory for Combinatorial Oxide Chemistry at ICTAS, Johannes Kepler University Linz (Austria); Institute for Chemical Technology of Inorganic Materials (ICTAS), Johannes Kepler University Linz (Austria)

2017-09-15

In the present work, which is aimed to monitor in situ the electrochemical dissolution of tungsten by using a Flow-Type Scanning Droplet Cell Microscope (FT-SDCM) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS), novel results are reported. The anodic oxide growth and its dissolution on the surface of W have been monitored in situ. The results of this current study show the importance of coupling electrochemical experiments to ICP-MS. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

In SITU Transmission Electron Microscopy on Operating Electrochemical CELLS

DEFF Research Database (Denmark)

Gualandris, Fabrizio; Simonsen, Søren Bredmose; Mogensen, Mogens Bjerg

2016-01-01

Solid oxide cells (SOC) have the potential of playing a significant role in the future efficient energy system scenario. In order to become widely commercially available, an improved performance and durability of the cells has to be achieved [1]. Conventional scanning and transmission SEM and TEM...... have been often used for ex-situ post mortem characterization of SOFCs and SOECs [2,3]. However, in order to get fundamental insight of the microstructural development of SOFC/SOEC during operation conditions in situ studies are necessary [4]....

Determination of the initial oxidation behavior of Zircaloy-4 by in-situ TEM

International Nuclear Information System (INIS)

Harlow, Wayne; Ghassemi, Hessam; Taheri, Mitra L.

2016-01-01

The corrosion behavior of Zircaloy-4 (Zry-4), specifically by oxidation, is a problem of great importance as this material is critical for current nuclear reactor cladding. The early formation behavior and structure of the oxide layer during oxidation was studied using in-situ TEM techniques that allowed for Zry-4 to be monitored during corrosion. These environmental exposure experiments were coupled with precession electron diffraction to identify and quantify the phases present in the samples before and after the oxidation. Following short-term, high temperature oxidation, the dominant phase was revealed to be monoclinic ZrO 2 in a columnar structure. These samples oxidized in-situ contained structures that correlated well with bulk Zry-4 subjected to autoclave treatment, which were used for comparison and validation of this technique. By using in-situ TEM the effect of microstructure features, such as grain boundaries, on oxidation behavior of an alloy can be studied. The technique presented herein holds the potential to be applied any alloy system to study these effects. - Highlights: • In-situ TEM was used to oxidize samples of Zircaloy-4. • Similar behavior was found in the in-situ oxidized and autoclave-oxidized samples. • Precession diffraction was used to characterize oxide phase and texture.

In situ groundwater bioremediation

Energy Technology Data Exchange (ETDEWEB)

Hazen, Terry C.

2009-02-01

In situ groundwater bioremediation of hydrocarbons has been used for more than 40 years. Most strategies involve biostimulation; however, recently bioaugmentation have been used for dehalorespiration. Aquifer and contaminant profiles are critical to determining the feasibility and strategy for in situ groundwater bioremediation. Hydraulic conductivity and redox conditions, including concentrations of terminal electron acceptors are critical to determine the feasibility and strategy for potential bioremediation applications. Conceptual models followed by characterization and subsequent numerical models are critical for efficient and cost effective bioremediation. Critical research needs in this area include better modeling and integration of remediation strategies with natural attenuation.

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...

Observatory Magnetometer In-Situ Calibration

Directory of Open Access Journals (Sweden)

A Marusenkov

2011-07-01

Full Text Available An experimental validation of the in-situ calibration procedure, which allows estimating parameters of observatory magnetometers (scale factors, sensor misalignment without its operation interruption, is presented. In order to control the validity of the procedure, the records provided by two magnetometers calibrated independently in a coil system have been processed. The in-situ estimations of the parameters are in very good agreement with the values provided by the coil system calibration.

Electrocatalytic oxygen reduction and hydrogen evolution reactions on phthalocyanine modified electrodes: Electrochemical, in situ spectroelectrochemical, and in situ electrocolorimetric monitoring

Energy Technology Data Exchange (ETDEWEB)

Koca, Atif, E-mail: akoca@eng.marmara.edu.tr [Department of Chemical Engineering, Faculty of Engineering, Marmara University, Goeztepe, 34722 Istanbul (Turkey); Kalkan, Ayfer; Bayir, Zehra Altuntas [Department of Chemistry, Technical University of Istanbul, Maslak, 34469 Istanbul (Turkey)

2011-06-30

Highlights: > Electrochemical and in situ spectroelectrochemical characterizations of the metallophthalocyanines were performed. > The presence of O{sub 2} influences both oxygen reduction reaction and the electrochemical behaviors of the complexes. > Homogeneous catalytic ORR process occurs via an 'inner sphere' chemical catalysis process. > CoPc and CuPc coated on a glassy carbon electrode decrease the overpotential of the working electrode for H{sup +} reduction. - Abstract: This study describes electrochemical, in situ spectroelectrochemical, and in situ electrocolorimetric monitoring of the electrocatalytic reduction of molecular oxygen and hydronium ion on the phthalocyanine-modified electrodes. For this purpose, electrochemical and in situ spectroelectrochemical characterizations of the metallophthalocyanines (MPc) bearing tetrakis-[4-((4'-trifluoromethyl)phenoxy)phenoxy] groups were performed. While CoPc gives both metal-based and ring-based redox processes, H{sub 2}Pc, ZnPc and CuPc show only ring-based electron transfer processes. In situ electrocolorimetric method was applied to investigate the color of the electrogenerated anionic and cationic forms of the complexes. The presence of O{sub 2} in the electrolyte system influences both oxygen reduction reaction and the electrochemical and spectral behaviors of the complexes, which indicate electrocatalytic activity of the complexes for the oxygen reduction reaction. Perchloric acid titrations monitored by voltammetry represent possible electrocatalytic activities of the complexes for hydrogen evolution reaction. CoPc and CuPc coated on a glassy carbon electrode decrease the overpotential of the working electrode for H{sup +} reduction. The nature of the metal center changes the electrocatalytic activities for hydrogen evolution reaction in aqueous solution. Although CuPc has an inactive metal center, its electrocatalytic activity is recorded more than CoPc for H{sup +} reduction in aqueous

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

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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

Training for teamwork through in situ simulations

Science.gov (United States)

Sorensen, Asta; Poehlman, Jon; Bollenbacher, John; Riggan, Scott; Davis, Stan; Miller, Kristi; Ivester, Thomas; Kahwati, Leila

2015-01-01

In situ simulations allow healthcare teams to practice teamwork and communication as well as clinical management skills in a team's usual work setting with typically available resources and equipment. The purpose of this video is to demonstrate how to plan and conduct in situ simulation training sessions, with particular emphasis on how such training can be used to improve communication and teamwork. The video features an in situ simulation conducted at a labour and delivery unit in response to postpartum hemorrhage. PMID:26294962

Kinematic analysis of in situ measurement during chemical mechanical planarization process

Energy Technology Data Exchange (ETDEWEB)

Li, Hongkai; Wang, Tongqing; Zhao, Qian; Meng, Yonggang; Lu, Xinchun, E-mail: xclu@tsinghua.edu.cn [State Key Laboratory of Tribology, Tsinghua University, Beijing 100084 (China)

2015-10-15

Chemical mechanical planarization (CMP) is the most widely used planarization technique in semiconductor manufacturing presently. With the aid of in situ measurement technology, CMP tools can achieve good performance and stable productivity. However, the in situ measurement has remained unexplored from a kinematic standpoint. The available related resources for the kinematic analysis are very limited due to the complexity and technical secret. In this paper, a comprehensive kinematic analysis of in situ measurement is provided, including the analysis model, the measurement trajectory, and the measurement time of each zone of wafer surface during the practical CMP process. In addition, a lot of numerical calculations are performed to study the influences of main parameters on the measurement trajectory and the measurement velocity variation of the probe during the measurement process. All the efforts are expected to improve the in situ measurement system and promote the advancement in CMP control system.

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.

In Situ/Remote Sensing Integration to Assess Forest Health—A Review

Directory of Open Access Journals (Sweden)

Marion Pause

2016-06-01

Full Text Available For mapping, quantifying and monitoring regional and global forest health, satellite remote sensing provides fundamental data for the observation of spatial and temporal forest patterns and processes. While new remote-sensing technologies are able to detect forest data in high quality and large quantity, operational applications are still limited by deficits of in situ verification. In situ sampling data as input is required in order to add value to physical imaging remote sensing observations and possibilities to interlink the forest health assessment with biotic and abiotic factors. Numerous methods on how to link remote sensing and in situ data have been presented in the scientific literature using e.g. empirical and physical-based models. In situ data differs in type, quality and quantity between case studies. The irregular subsets of in situ data availability limit the exploitation of available satellite remote sensing data. To achieve a broad implementation of satellite remote sensing data in forest monitoring and management, a standardization of in situ data, workflows and products is essential and necessary for user acceptance. The key focus of the review is a discussion of concept and is designed to bridge gaps of understanding between forestry and remote sensing science community. Methodological approaches for in situ/remote-sensing implementation are organized and evaluated with respect to qualifying for forest monitoring. Research gaps and recommendations for standardization of remote-sensing based products are discussed. Concluding the importance of outstanding organizational work to provide a legally accepted framework for new information products in forestry are highlighted.

X-ray absorption spectroscopic studies on novel microporous copper containing catalytic systems

International Nuclear Information System (INIS)

Bhargava, Suresh K.; Akolekar, Deepak B.; Foran, Garry

2006-01-01

Novel copper metal modified microporous aluminosilicate and aluminophosphate catalysts with the high phase purity were synthesized and characterized. CuK-edge XAS measurements were carried out over a series of copper containing SAPO-34 and ZSM-5 catalysts. EXAFS technique was used to obtain specific climacteric information related to the copper atomic distances, coordination and near neighbour environments. EXAFS studies indicated the presence of different of Cu species on ZSM-5/SAPO34 catalysts

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

Calcium in ancient glazes and glasses: a XAFS study

Energy Technology Data Exchange (ETDEWEB)

Veiga, J.P. [New University of Lisbon, CENIMAT, Materials Science Dept., Caparica (Portugal); Figueiredo, M.O. [New University of Lisbon, CENIMAT, Materials Science Dept., Caparica (Portugal); Crystallography and Mineralogy Centre, IICT, and INETI/IGM, Dept. Min. Resources, Alfragide (Portugal)

2008-07-15

Ceramic tiles used to manufacture artistic panels during the XVI to the XVIII centuries were decorated with high-lead soda-lime glazes, incorporating a diversity of chromophore cations, as ascertained by SRXRF (synchrotron radiation X-ray fluorescence). Previous X-ray absorption spectroscopy (XAS) studies have shown that sodium and lead are hosted by the glassy matrix in those glazes. However, the possible role of calcium as a modifier of the tetrahedral silica network is not fully clarified, despite being recognized that calcium cations alter some fundamental properties of glazes, namely transparency. An X-ray absorption fine structure (XAFS) study of glazes with varied colorings was therefore undertaken at Ca K- and L-edges. Well crystallized oxide minerals were used to model distinct coordination environments by oxygen atoms - close to octahedral geometry in calcite and dodecahedral in gypsum - while fluorite was chosen to mimic ideal cubic coordination. A first XAS approach suggested a minor variation in the energy separation between L{sub 2}-L{sub 3} absorption edges when comparing blue and yellow glazes, irrespective of the period of manufacture. A further study on the X-ray absorption near-edge structure (XANES) carried out at the K-edge corroborated this difference and, along with the theoretical spectra modeling performed with the FEFF code, allowed interpreting of the Ca 1s absorption spectra of glazes as arising from a non-regular high-coordination environment within the silica matrix. (orig.)

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

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.

Electron microscopy and EXAFS studies on oxide-supported gold-silver nanoparticles prepared by flame spray pyrolysis

Energy Technology Data Exchange (ETDEWEB)

Hannemann, Stefan [Institute of Chemical and Bioengineering, Swiss Federal Institute of Technology, ETH Hoenggerberg, CH-8093 Zurich (Switzerland); Grunwaldt, Jan-Dierk [Institute of Chemical and Bioengineering, Swiss Federal Institute of Technology, ETH Hoenggerberg, CH-8093 Zurich (Switzerland)]. E-mail: grunwaldt@chem.ethz.ch; Krumeich, Frank [Laboratory of Inorganic Chemistry, Swiss Federal Institute of Technology, ETH Hoenggerberg, CH-8093 Zurich (Switzerland); Kappen, Peter [Department of Physics, La Trobe University, Victoria 3086 (Australia); Baiker, Alfons [Institute of Chemical and Bioengineering, Swiss Federal Institute of Technology, ETH Hoenggerberg, CH-8093 Zurich (Switzerland)

2006-09-15

Gold and gold-silver nanoparticles prepared by flame spray pyrolysis (FSP) were characterized by electron microscopy, in situ X-ray absorption spectroscopy (XANES and EXAFS), X-ray diffraction (XRD) and their catalytic activity in CO oxidation. Within this one-step flame-synthesis procedure, precursor solutions of dimethyl gold(III) acetylacetonate and silver(I) benzoate together with the corresponding precursor of the silica, iron oxide or titania support, were sprayed and combusted. In order to prepare small metal particles, a low noble metal loading was required. A loading of 0.1-1 wt.% of Au and Ag resulted in 1-6 nm particles. The size of the noble metal particles increased with higher loadings of gold and particularly silver. Both scanning transmission electron microscopy (STEM) combined with energy dispersive X-ray spectroscopy (EDXS) and X-ray absorption spectroscopy (XAS) studies proved the formation of mixed Au-Ag particles. In case of 1% Au-1% Ag/SiO{sub 2}, TEM combined with electron spectroscopic imaging (ESI) using an imaging filter could be used in addition to prove the presence of silver and gold in the same noble metal particle. CO oxidation in the presence of hydrogen was chosen as a test reaction sensitive to small gold particles. Both the influence of the particle size and the alloying of gold and silver were reflected in the CO oxidation activity.