National Library of Energy BETA

Sample records for x-ray photoelectron spectroscopy

  1. Ambient Pressure Photoelectron Spectroscopy Using Soft X-ray...

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Ambient Pressure Photoelectron Spectroscopy Using Soft X-ray and Hard X-ray, and its applications in electrochemistry Friday, December 14, 2012 - 3:30pm SSRL, Bldg. 137, room 322...

  2. Ambient Pressure Photoelectron Spectroscopy Using Soft X-ray and Hard

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    X-ray, and its applications in electrochemistry | Stanford Synchrotron Radiation Lightsource Ambient Pressure Photoelectron Spectroscopy Using Soft X-ray and Hard X-ray, and its applications in electrochemistry Friday, December 14, 2012 - 3:30pm SSRL, Bldg. 137, room 322 Zhi Liu The synchrotron based ambient pressure x-ray photoelectron spectroscopy (AP-XPS) endstation[1] pioneered at ALS based on differentially pumped electron energy analyzer has been recognized by scientific communities as

  3. In Situ Ambient Pressure X-ray Photoelectron Spectroscopy Studies...

    Office of Scientific and Technical Information (OSTI)

    Journal Article: In Situ Ambient Pressure X-ray ... Citation Details In-Document Search Title: In Situ Ambient ... Resource Relation: Journal Name: Scientific Reports; Journal ...

  4. In-situ X-ray Photoelectron Spectroscopy of a Catalyst for Artificial

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Photosynthesis | Stanford Synchrotron Radiation Lightsource In-situ X-ray Photoelectron Spectroscopy of a Catalyst for Artificial Photosynthesis Monday, June 30, 2014 Plants and other organisms use a process called photosynthesis to produce carbohydrates and oxygen from water and carbon dioxide using sunlight. Artificial photosynthesis replicates this process to produce energy in the form of usable fuels for human needs. Researches have been developing devices for artificial photosynthesis,

  5. Hard x-ray photoelectron spectroscopy using an environmental cell with silicon nitride membrane windows

    SciTech Connect (OSTI)

    Tsunemi, Eika; Watanabe, Yoshio; Oji, Hiroshi; Cui, Yi-Tao; Son, Jin-Young

    2015-06-21

    We applied hard x-ray photoelectron spectroscopy (HAXPES) to a sample under ambient pressure conditions using an environmental cell with an approximately 24 nm-thick SiN{sub x} membrane window. As a model chemical substance, europium (II) iodide (EuI{sub 2}) sealed in the cell with argon gas was investigated with HAXPES to identify the chemical species present inside the cell. The optical and morphological properties of the sample within the cell were measured with optical and fluorescent microscopy, scanning electron microscopy, cathodoluminescence, and energy dispersive x-ray spectrometry. We confirmed the effectiveness of the gas barrier properties of the cell with the SiN{sub x} window and demonstrated its applicability to various other optical and electron measurements as well as HAXPES.

  6. In situ x-ray photoelectron spectroscopy for electrochemical reactions in ordinary solvents

    SciTech Connect (OSTI)

    Masuda, Takuya; PRESTO, Japan Science and Technology Agency , 4-1-8 Honcho, Kawaguchi, Saitama 333-0012 ; Yoshikawa, Hideki; Kobata, Masaaki; Kobayashi, Keisuke; Noguchi, Hidenori; PRESTO, Japan Science and Technology Agency , 4-1-8 Honcho, Kawaguchi, Saitama 333-0012; Graduate School of Chemical Sciences and Engineering, Hokkaido University, Sapporo, Hokkaido 060-0810; International Center for Materials Nanoarchitectonics , National Institute for Materials Science , Tsukuba, Ibaraki 305-0044 ; Kawasaki, Tadahiro; Uosaki, Kohei; Graduate School of Chemical Sciences and Engineering, Hokkaido University, Sapporo, Hokkaido 060-0810; International Center for Materials Nanoarchitectonics , National Institute for Materials Science , Tsukuba, Ibaraki 305-0044

    2013-09-09

    In situ electrochemical X-ray photoelectron spectroscopy (XPS) apparatus, which allows XPS at solid/liquid interfaces under potential control, was constructed utilizing a microcell with an ultra-thin Si membrane, which separates vacuum and a solution. Hard X-rays from a synchrotron source penetrate into the Si membrane surface exposed to the solution. Electrons emitted at the Si/solution interface can pass through the membrane and be analyzed by an analyzer placed in vacuum. Its operation was demonstrated for potential-induced Si oxide growth in water. Effect of potential and time on the thickness of Si and Si oxide layers was quantitatively determined at sub-nanometer resolution.

  7. Contact-free pyroelectric measurements using x-ray photoelectron spectroscopy

    SciTech Connect (OSTI)

    Ehre, D.; Cohen, H.

    2013-07-29

    Non-contact pyroelectricity measurements based on x-ray photoelectron spectroscopy (XPS) are presented. Applied to Lithium Tantalate crystals, we demonstrate how the XPS-derived surface potential provides a simple probe of the desired property, free of all top-contact related difficulties. In particular, the increase in Lithium Tantalate spontaneous polarization under cooling, an experimentally challenging feature, is evaluated. We further inspect the roll of surface contaminants and the control over trapped surface charge in the XPS vacuum environment. Our approach can be extended to other non-contact probes, as well as to measuring additional electrical properties, such as piezoelectricity and ferroelectricity.

  8. Probing hot-electron effects in wide area plasmonic surfaces using X-ray photoelectron spectroscopy

    SciTech Connect (OSTI)

    Ayas, Sencer; Cupallari, Andi; Dana, Aykutlu

    2014-12-01

    Plasmon enhanced hot carrier formation in metallic nanostructures increasingly attracts attention due to potential applications in photodetection, photocatalysis, and solar energy conversion. Here, hot-electron effects in nanoscale metal-insulator-metal (MIM) structures are investigated using a non-contact X-ray photoelectron spectroscopy based technique using continuous wave X-ray and laser excitations. The effects are observed through shifts of the binding energy of the top metal layer upon excitation with lasers of 445, 532, and 650?nm wavelength. The shifts are polarization dependent for plasmonic MIM grating structures fabricated by electron beam lithography. Wide area plasmonic MIM surfaces fabricated using a lithography free route by the dewetting of evaporated Ag on HfO{sub 2} exhibit polarization independent optical absorption and surface photovoltage. Using a simple model and making several assumptions about the magnitude of the photoemission current, the responsivity and external quantum efficiency of wide area plasmonic MIM surfaces are estimated as 500?nA/W and 11 10{sup ?6} for 445?nm illumination.

  9. Quantitative x-ray photoelectron spectroscopy: Quadrupole effects, shake-up, Shirley background, and relative sensitivity factors from a database of true x-ray photoelectron spectra

    SciTech Connect (OSTI)

    Seah, M. P.; Gilmore, I. S.

    2006-05-01

    An analysis is provided of the x-ray photoelectron spectroscopy (XPS) intensities measured in the National Physical Laboratory (NPL) XPS database for 46 solid elements. This present analysis does not change our previous conclusions concerning the excellent correlation between experimental intensities, following deconvolving the spectra with angle-averaged reflection electron energy loss data, and the theoretical intensities involving the dipole approximation using Scofield's cross sections. Here, more recent calculations for cross sections by Trzhaskovskaya et al. involving quadrupole terms are evaluated and it is shown that their cross sections diverge from the experimental database results by up to a factor of 5. The quadrupole angular terms lead to small corrections that are close to our measurement limit but do appear to be supported in the present analysis. Measurements of the extent of shake-up for the 46 elements broadly agree with the calculations of Yarzhemsky et al. but not in detail. The predicted constancy in the shake-up contribution by Yarzhemsky et al. implies that the use of the Shirley background will lead to a peak area that is a constant fraction of the true peak area including the shake-up intensities. However, the measured variability of the shake-up contribution makes the Shirley background invalid for quantification except for situations where the sensitivity factors are from reference samples similar to those being analyzed.

  10. Scanning electron microscopy and x-ray photoelectron spectroscopy evaluation of MHD channel electrodes

    SciTech Connect (OSTI)

    Martello, D.V.; Baltrus, J.P.; Diehl, J.R.; Makovsky, L.E.

    1994-12-31

    Anode elements from the coal-fired Magnetohydrodynamic (MHD) channel at the Component Development and Integration Facility (CDIF) in Butte, Montana have been selected for study of the effects of localized phase morphology and chemistry on anode degradation. The platinum/tungsten/copper anode elements from the 1A{sub 4} channel were examined with scanning electron microscopy and X-ray photoelectron spectroscopy following testing in the MHD channel, and the results compared to those for unexposed anodes. Evidence suggests that the surface of the tungsten anode is chemically attacked by a potassium-rich slag to form a fine-grained crystalline reaction product layer that is covered by a fused, glassy slag during channel operation. Examination of a mechanically separated, partially delaminated platinum cap and polished cross-sections of anode segments showed evidence of chemical attack along the braze used to join the two caps. Interface porosity may provide a path for slag penetration and diffusion of corrosive gases and liquids during channel operation, leading to delamination. The microstructure of the brazed joint cross-sections were similar, independent of exposure severity in the MHD channel. The primary mechanism of tungsten degradation appears to be grain exfoliation due to severe grain boundary attack.

  11. Adsorption of 2-propanol on ice probed by ambient pressure X-ray photoelectron spectroscopy

    SciTech Connect (OSTI)

    Newberg, John T.; Bluhm, Hendrik

    2015-08-18

    The interaction of 2-propanol with ice was examined via ambient pressure X-ray photoelectron spectroscopy (APXPS), a surface sensitive technique that probes the adsorbed 2-propanol directly with submonolayer resolution. Isothermal uptake experiments were performed on vapor deposited ice at 227 K in the presence of the equilibrium water vapor pressure of 0.05 Torr and 2-propanol partial pressures ranging from 5 × 10-5 to 2 × 10-3 Torr. The C 1s APXPS spectra of adsorbed 2-propanol showed two characteristic peaks associated with the COH alcohol group and CMe methyl groups in a 1 : 2 ratio, respectively. Coverage increased with 2-propanol partial pressure and followed first order Langmuir kinetics with a Langmuir constant of K = 6.3 × 103 Torr-1. The 1 : 2 ratio of COH : CMe remained constant with increasing coverage, indicating there is no chemical reaction upon adsorption. The observed Langmuir kinetics using APXPS is consistent with previous observations of other small chain alcohols via indirect adsorption methods using, e.g., Knudsen cell and coated wall flow tube reactors.

  12. Adsorption of 2-propanol on ice probed by ambient pressure X-ray photoelectron spectroscopy

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Newberg, John T.; Bluhm, Hendrik

    2015-08-18

    The interaction of 2-propanol with ice was examined via ambient pressure X-ray photoelectron spectroscopy (APXPS), a surface sensitive technique that probes the adsorbed 2-propanol directly with submonolayer resolution. Isothermal uptake experiments were performed on vapor deposited ice at 227 K in the presence of the equilibrium water vapor pressure of 0.05 Torr and 2-propanol partial pressures ranging from 5 × 10-5 to 2 × 10-3 Torr. The C 1s APXPS spectra of adsorbed 2-propanol showed two characteristic peaks associated with the COH alcohol group and CMe methyl groups in a 1 : 2 ratio, respectively. Coverage increased with 2-propanol partialmore » pressure and followed first order Langmuir kinetics with a Langmuir constant of K = 6.3 × 103 Torr-1. The 1 : 2 ratio of COH : CMe remained constant with increasing coverage, indicating there is no chemical reaction upon adsorption. The observed Langmuir kinetics using APXPS is consistent with previous observations of other small chain alcohols via indirect adsorption methods using, e.g., Knudsen cell and coated wall flow tube reactors.« less

  13. Closing the pressure gap in x-ray photoelectron spectroscopy by membrane hydrogenation

    SciTech Connect (OSTI)

    Delmelle, Renaud; Borgschulte, Andreas; Probst, Benjamin; Alberto, Roger; Zttel, Andreas; Bleiner, Davide

    2015-05-15

    Comprehensive studies of gas-solid reactions require the in-situ interaction of the gas at a pressure beyond the operating pressure of ultrahigh vacuum (UHV) X-ray photoelectron spectroscopy (XPS). The recent progress of near ambient pressure XPS allows to dose gases to the sample up to a pressure of 20 mbar. The present work describes an alternative to this experimental challenge, with a focus on H{sub 2} as the interacting gas. Instead of exposing the sample under investigation to gaseous hydrogen, the sample is in contact with a hydrogen permeation membrane, through which hydrogen is transported from the outside to the sample as atomic hydrogen. Thereby, we can reach local hydrogen concentrations at the sample inside an UHV chamber, which is equipped with surface science tools, and this corresponds to a hydrogen pressure up to 1 bar without affecting the sensitivity or energy resolution of the spectrometer. This experimental approach is validated by two examples, that is, the reduction of a catalyst precursor for CO{sub 2} hydrogenation and the hydrogenation of a water reduction catalyst for photocatalytic H{sub 2} production, but it opens the possibility of the new in situ characterisation of energy materials and catalysts.

  14. Band bending at ferroelectric surfaces and interfaces investigated by x-ray photoelectron spectroscopy

    SciTech Connect (OSTI)

    Apostol, Nicoleta Georgiana

    2014-11-24

    This work reports on the use of X-ray photoelectron spectroscopy to quantify band bending at ferroelectric free surfaces and at their interfaces with metals. Surfaces exhibiting out-of-plane ferroelectric polarization are characterized by a band bending, due to the formation of a dipole layer at the surface, composed by the uncompensated polarization charges (due to ionic displacement) and to the depolarization charge sheet of opposite sign, composed by mobile charge carriers, which migrate near surface, owing to the depolarization electric field. To this surface band bending due to out-of-plane polarization states, metal-semiconductor Schottky barriers must be considered additionally when ferroelectrics are covered by metal layers. It is found that the net band bending is not always an algebraic sum of the two effects discussed above, since sometimes the metal is able to provide additional charge carriers, which are able to fully compensate the surface charge of the ferroelectric, up to the vanishing of the ferroelectric band bending. The two cases which will be discussed in more detail are Au and Cu deposited by molecular beam epitaxy on PbZr{sub 0.2}Ti{sub 0.8}O{sub 3}(001) single crystal thin layers, prepared by pulsed laser deposition. Gold forms unconnected nanoparticles, and their effect on the band bending is the apparition of a Schottky band bending additional to the band bending due to the out-of-plane polarization. Copper, starting with a given thickness, forms continuous metal layers connected to the ground of the system, and provide electrons in sufficient quantity to compensate the band bending due to the out-of-plane polarization.

  15. X-ray Photoelectron Spectroscopy study of the compatibility of the explosive PETN with candidate plastic bonding materials

    SciTech Connect (OSTI)

    Vannet, M.D.; Wang, P.S.; Moddeman, W.E.; Bowling, W.C.

    1985-01-01

    The compatibility of the explosive PETN with two plastic bonding materials, ethyl cellulose and a halogenated vinyl polymer (FPC 461), was determined by X-ray Photoelectron Spectroscopy (XPS). Both were found to coat the PETN crystals, and no change in chemical composition was found in the PETN or the plastic due to either the process or their mutual presence. 3 refs., 1 fig., 1 tab.

  16. An X-ray photoelectron spectroscopy study of the hydration of C{sub 2}S thin films

    SciTech Connect (OSTI)

    Rheinheimer, Vanessa; Casanova, Ignasi

    2014-06-01

    Electron-beam evaporation was used to produce thin films of ?-dicalcium silicate. Chemical and mineralogical compositions were characterized by X-ray photoelectron spectroscopy (XPS) and grazing-angle X-ray diffraction (GAXRD), respectively. Results show that no fractionation occurs during evaporation and isostructural condensation of the material as synthesized films have the same composition as the initial bulk material. Samples were gradually hydrated under saturated water spray conditions and analyzed with XPS. Polymerization of the silicate chains due to hydration, and subsequent formation of C-S-H, has been monitored through evaluation of energy shifts on characteristic silicon peaks. Quantitative analyses show changes on the surface by the reduction of the Ca/Si ratio and an increase on the difference between binding energies of bridging and non-bridging oxygen. Finally, SEM/FIB observation shows clear differences between the surface and cross section of the initial sample and the reacted sample.

  17. X-ray photoelectron spectroscopy and ultraviolet photoelectron spectroscopy investigation of Al-related dipole at the HfO{sub 2}/Si interface

    SciTech Connect (OSTI)

    Zhu, L. Q.; Barrett, N.; Jegou, P.

    2009-01-15

    The presence of an ultrathin oxide layer at the high-k/SiO{sub 2} interface may result in an interfacial dipole related to the specific high-k dielectric used for the gate stacks. 1 nm HfO{sub 2}/x nmAl{sub 2}O{sub 3}/SiO{sub 2}/Si stacks with different x values (x=0, 0.4, 0.8, 1.2) have been prepared by atomic layer deposition. Using photoelectron spectroscopy, an Al-related interfacial dipole in the HfO{sub 2}/Al{sub 2}O{sub 3}/SiO{sub 2} gate stack has been identified. X-ray photoelectron spectroscopy analysis shows that the dipole is correlated with the formation of an interfacial Al-silicate. The dipole is located at the Al-silicate interface between Al{sub 2}O{sub 3} and SiO{sub 2}, and its strength increases with the increase in Al{sub 2}O{sub 3} thickness because of Al silicate growth. Such Al-related interfacial dipole should have potential applications in future positive metal-oxide-semiconductor devices.

  18. Electronic structure of Al- and Ga-doped ZnO films studied by hard X-ray photoelectron spectroscopy

    SciTech Connect (OSTI)

    Gabás, M.; Ramos Barrado, José R.; Torelli, P.; Barrett, N. T.

    2014-01-01

    Al- and Ga-doped sputtered ZnO films (AZO, GZO) are semiconducting and metallic, respectively, despite the same electronic valence structure of the dopants. Using hard X-ray photoelectron spectroscopy we observe that both dopants induce a band in the electronic structure near the Fermi level, accompanied by a narrowing of the Zn 3d/O 2p gap in the valence band and, in the case of GZO, a substantial shift in the Zn 3d. Ga occupies substitutional sites, whereas Al dopants are in both substitutional and interstitial sites. The latter could induce O and Zn defects, which act as acceptors explaining the semiconducting character of AZO and the lack of variation in the optical gap. By contrast, mainly substitutional doping is consistent with the metallic-like behavior of GZO.

  19. X-ray photoelectron spectroscopy studies on Pd doped SnO{sub 2} liquid petroleum gas sensor

    SciTech Connect (OSTI)

    Phani, A.R.

    1997-10-01

    The present investigation deals with the electrical response of palladium doped tin oxide, as a means of improving the selectivity for liquid petroleum gas (LPG) in the presence of CO, CH{sub 4}. The sensor element with the composition of Pd(1.5 wt{percent}) in the base material SnO{sub 2} sintered at 800{degree}C, has shown a high sensitivity towards LPG with a negligible cross interference of CO and CH{sub 4} at an operating temperature of 350{degree}C. This greatly suggests the possibility of utilizing the sensor for the detection of LPG. X-ray photoelectron spectroscopy studies have been carried out to determine the possible chemical species involved in the gas-solid interaction and the enhancing mechanism of the Pd doped SnO{sub 2} sensor element, towards LPG sensitivity. {copyright} {ital 1997 American Institute of Physics.}

  20. Spectroscopic evidence for Ag(III) in highly oxidized silver films by x-ray photoelectron spectroscopy

    SciTech Connect (OSTI)

    Kaspar, Tiffany C.; Droubay, Timothy C.; Chambers, Scott A.; Bagus, Paul S.

    2010-12-16

    In situ x-ray photoelectron spectroscopy (XPS) was utilized to identify the chemical state of silver in a range of silver oxide thin films obtained by co-deposition of silver and atomic oxygen. A highly oxidized silver species was observed at an unexpectedly low Ag 3d5/2 binding energy (BE) of 366.8 eV with an associated broad satellite at 368.2 eV; this species was assigned as Ag(III). It was found to be highly unstable in vacuum, but could be regenerated by further exposure to atomic oxygen. Both BE shifts and intensity changes of the O 1s peak were found to correlate with changes in the silver oxidation state. Theoretical calculations of the expected XPS of high spin Ag(III) provide insight into the significance of satellite structure and shake features in the Ag 3d spectra.

  1. Annealing dependence of diamond-metal Schottky barrier heights probed by hard x-ray photoelectron spectroscopy

    SciTech Connect (OSTI)

    Gaowei, M.; Muller, E. M.; Rumaiz, A. K.; Weiland, C.; Cockayne, E.; Woicik, J. C.; Jordan-Sweet, J.; Smedley, J.

    2012-05-14

    Hard x-ray photoelectron spectroscopy was applied to investigate the diamond-metal Schottky barrier heights for several metals and diamond surface terminations. The position of the diamond valence-band maximum was determined by theoretically calculating the diamond density of states and applying cross section corrections. The diamond-platinum Schottky barrier height was lowered by 0.2 eV after thermal annealing, indicating annealing may increase carrier injection in diamond devices leading to photoconductive gain. The platinum contacts on oxygen-terminated diamond was found to provide a higher Schottky barrier and therefore a better blocking contact than that of the silver contact in diamond-based electronic devices.

  2. Surface study of stainless steel electrode deposition from soil electrokinetic (EK) treatment using X-ray photoelectron spectroscopy (XPS)

    SciTech Connect (OSTI)

    Embong, Zaidi; Johar, Saffuwan; Tajudin, Saiful Azhar Ahmad; Sahdan, Mohd Zainizan

    2015-04-29

    Electrokinetic (EK) remediation relies upon application of a low-intensity direct current through the soil between stainless steel electrodes that are divided into a cathode array and an anode array. This mobilizes charged species, causing ions and water to move toward the electrodes. Metal ions and positively charged organic compounds move toward the cathode. Anions such as chloride, fluoride, nitrate, and negatively charged organic compounds move toward the anode. Here, this remediation techniques lead to a formation of a deposition at the both cathode and anode surface that mainly contributed byanion and cation from the remediated soil. In this research, Renggam-Jerangau soil species (HaplicAcrisol + RhodicFerralsol) with a surveymeter reading of 38.0 ± 3.9 μR/hr has been investigation in order to study the mobility of the anion and cation under the influence electric field. Prior to the EK treatment, the elemental composition of the soil and the stainless steel electrode are measured using XRF analyses. Next, the soil sample is remediated at a constant electric potential of 30 V within an hour of treatment period. A surface study for the deposition layer of the cathode and anode using X-ray Photoelectron spectroscopy (XPS) revealed that a narrow photoelectron signal from oxygen O 1s, carbon, C 1s silica, Si 2p, aluminium, Al 2p and chromium, Cr 2p exhibited on the electrode surface and indicate that a different in photoelectron intensity for each element on both electrode surface. In this paper, the mechanism of Si{sup 2+} and Al{sup 2+} cation mobility under the influence of voltage potential between the cathode and anode will be discussed in detail.

  3. ANALYSIS OF PASSIVATED SURFACES FOR MASS SPECTROMETER INLET SYSTEMS BY AUGER ELECTRON AND X-RAY PHOTOELECTRON SPECTROSCOPY

    SciTech Connect (OSTI)

    Ajo, H.; Clark, E.

    2010-09-01

    Stainless steel coupons approximately 0.5' in diameter and 0.125' thick were passivated with five different surface treatments and an untreated coupon was left as a control. These surface treatments are being explored for use in tritium storage containers. These coupons were made to allow surface analysis of the surface treatments using well-know surface analysis techniques. Depth profiles using Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS) were performed on these coupons to characterize the surface and near surface regions. Scanning electron microscope (SEM) images were collected as well. All of the surface treatments studied here appear to change the surface morphology dramatically, as evidenced by lack of tool marks on the treated samples. In terms of the passivation treatment, Vendors A-D appeared to have oxide layers that were very similar in thickness to each other (0.7-0.9 nm thick) as well as the untreated samples (the untreated sample oxide layers appeared to be somewhat larger). Vendor E's silicon coating appears to be on the order of 200 nm thick.

  4. NREL: Measurements and Characterization - X-Ray and UV Photoelectron

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Spectroscopy X-Ray and UV Photoelectron Spectroscopy Example of graph made with cluster tool; plots counts (Y-axis) vs. binding energy (X-axis) for PET Carbon 1S. High-resolution XPS spectra of carbon 1s from polyethylene terephthalate backsheet material, showing excellent quantitative agreement between measured and predicted peak area ratios. Subtle differences in polymer functionality are assessed by deviations from stoichiometry. In photoemission techniques, we use either X-rays or

  5. Using “Tender” x-ray ambient pressure x-Ray photoelectron spectroscopy as a direct probe of solid-liquid interface

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Axnanda, Stephanus; Crumlin, Ethan J.; Mao, Baohua; Rani, Sana; Chang, Rui; Karlsson, Patrik G.; Edwards, Mårten O. M.; Lundqvist, Måns; Moberg, Robert; Ross, Phil; et al

    2015-05-07

    We report a new method to probe the solid-liquid interface through the use of a thin liquid layer on a solid surface. An ambient pressure XPS (AP-XPS) endstation that is capable of detecting high kinetic energy photoelectrons (7 keV) at a pressure up to 110 Torr has been constructed and commissioned. Additionally, we have deployed a “dip & pull” method to create a stable nanometers-thick aqueous electrolyte on platinum working electrode surface. Combining the newly constructed AP-XPS system, “dip & pull” approach, with a “tender” X-ray synchrotron source (2 keV–7 keV), we are able to access the interface between liquidmore » and solid dense phases with photoelectrons and directly probe important phenomena occurring at the narrow solid-liquid interface region in an electrochemical system. Using this approach, we have performed electrochemical oxidation of the Pt electrode at an oxygen evolution reaction (OER) potential. Under this potential, we observe the formation of both Pt²⁺ and Pt⁴⁺ interfacial species on the Pt working electrode in situ. We believe this thin-film approach and the use of “tender” AP-XPS highlighted in this study is an innovative new approach to probe this key solid-liquid interface region of electrochemistry.« less

  6. Elemental content of enamel and dentin after bleaching of teeth (a comparative study between laser-induced breakdown spectroscopy and x-ray photoelectron spectroscopy)

    SciTech Connect (OSTI)

    Imam, H.; Ahmed, Doaa; Eldakrouri, Ashraf; Department of Optometry and Vision Science, College of Applied Medical Science, King Saud University, Riyadh

    2013-06-21

    The elemental content of the superficial and inner enamel as well as that of dentin was analyzed using laser-induced breakdown spectroscopy (LIBS) and x-ray photoelectron spectroscopy (XPS) of bleached and unbleached tooth specimens. It is thus clear from the spectral analysis using both the LIBS and XPS technique that elemental changes (though insignificant within the scopes of this study) of variable intensities do occur on the surface of the enamel and extend deeper to reach dentin. The results of the LIBS revealed a slight reduction in the calcium levels in the bleached compared to the control specimens in all the different bleaching groups and in both enamel and dentin. The good correlation found between the LIBS and XPS results demonstrates the possibility of LIBS technique for detection of minor loss in calcium and phosphorus in enamel and dentin.

  7. SMB, X-ray Emission Spectroscopy

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    include X-ray Emission Spectroscopy (XES), Resonant Inelastic X-ray Scattering (RIXS), High Energy Resolution Fluorescence Detection (HERFD) and X-ray Raman Spectroscopy (XRS). ...

  8. Electronic structure of β-Ga{sub 2}O{sub 3} single crystals investigated by hard X-ray photoelectron spectroscopy

    SciTech Connect (OSTI)

    Li, Guo-Ling; Zhang, Fabi; Guo, Qixin; Cui, Yi-Tao; Oji, Hiroshi; Son, Jin-Young

    2015-07-13

    By combination of hard X-ray photoelectron spectroscopy (HAXPES) and first-principles band structure calculations, the electronic states of β-Ga{sub 2}O{sub 3} were investigated to deepen the understanding of bulk information for this compound. The valence band spectra of HAXPES presented the main contribution from Ga 4sp, which are well represented by photoionization cross section weighted partial density of states. The experimental data complemented with the theoretical study yield a realistic picture of the electronic structure for β-Ga{sub 2}O{sub 3}.

  9. SMB, X-ray Absorption Spectroscopy

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Absorption Spectroscopy X-ray Absorption Spectroscopy X-ray absorption spectroscopy (XAS) is a well-established technique for simultaneous local geometric and electronic structure...

  10. Conduction band offset at GeO{sub 2}/Ge interface determined by internal photoemission and charge-corrected x-ray photoelectron spectroscopies

    SciTech Connect (OSTI)

    Zhang, W. F.; Nishimula, T.; Nagashio, K.; Kita, K.; Toriumi, A.

    2013-03-11

    We report a consistent conduction band offset (CBO) at a GeO{sub 2}/Ge interface determined by internal photoemission spectroscopy (IPE) and charge-corrected X-ray photoelectron spectroscopy (XPS). IPE results showed that the CBO value was larger than 1.5 eV irrespective of metal electrode and substrate type variance, while an accurate determination of valence band offset (VBO) by XPS requires a careful correction of differential charging phenomena. The VBO value was determined to be 3.60 {+-} 0.2 eV by XPS after charge correction, thus yielding a CBO (1.60 {+-} 0.2 eV) in excellent agreement with the IPE results. Such a large CBO (>1.5 eV) confirmed here is promising in terms of using GeO{sub 2} as a potential passivation layer for future Ge-based scaled CMOS devices.

  11. Measurement of the valence band-offset in a PbSe/ZnO heterojunction by x-ray photoelectron spectroscopy

    SciTech Connect (OSTI)

    Li Lin; Qiu Jijun; Weng Binbin; Yuan Zijian; Shi Zhisheng; Li Xiaomin; Gan Xiaoyan; Sellers, Ian R.

    2012-12-24

    A heterojunction of PbSe/ZnO has been grown by molecular beam epitaxy. X-ray photoelectron spectroscopy was used to directly measure the valence-band offset (VBO) of the heterojunction. The VBO, {Delta}E{sub V}, was determined as 2.51 {+-} 0.05 eV using the Pb 4p{sup 3/2} and Zn 2p{sup 3/2} core levels as a reference. The conduction-band offset, {Delta}E{sub C}, was, therefore, determined to be 0.59 {+-} 0.05 eV based on the above {Delta}E{sub V} value. This analysis indicates that the PbSe/ZnO heterojunction forms a type I (Straddling Gap) heterostructure.

  12. Surface carbonation of synthetic C-S-H samples: A comparison between fresh and aged C-S-H using X-ray photoelectron spectroscopy

    SciTech Connect (OSTI)

    Black, Leon Garbev, Krassimir; Gee, Ian

    2008-06-15

    This paper presents a continuation of studies into silicate anion structure using X-ray photoelectron spectroscopy (XPS). A series of C-S-H samples have been prepared mechanochemically, and then stored under ambient conditions for six months. Storage led to surface carbonation, the extent of which was dependent upon the calcium/silicon ratio of the fresh sample. Carbonation arose through decalcification of the C-S-H, leading to increased silicate polymerisation. The surfaces of the most calcium-rich phases (C/S = 1.33 and 1.50) underwent complete decalcification to yield silica (possibly containing some silanol groups) and calcium carbonate. Carbonation, and hence changes in silicate anion structure, was minimal for the C-S-H phases with C/S = 0.67 and 0.75.

  13. Electronic structure of the polymer-cathode interface of an organic electroluminescent device investigated using operando hard x-ray photoelectron spectroscopy

    SciTech Connect (OSTI)

    Ikeuchi, J.; Hamamatsu, H.; Miyamoto, T.; Tanaka, S.; Yamashita, Y.; Yoshikawa, H.; Ueda, S.

    2015-08-28

    The electronic structure of a polymer-cathode interface of an operating organic light-emitting diode (OLED) was directly investigated using hard X-ray photoelectron spectroscopy (HAXPES). The potential distribution profile of the light-emitting copolymer layer as a function of the depth under the Al/Ba cathode layer in the OLED depended on the bias voltage. We found that band bending occurred in the copolymer of 9,9-dioctylfluorene (50%) and N-(4-(2-butyl)-phenyl)diphenylamine (F8-PFB) layer near the cathode at 0 V bias, while a linear potential distribution formed in the F8-PFB when a bias voltage was applied to the OLED. Direct observation of the built-in potential and that band bending formed in the F8-PFB layer in the operating OLED suggested that charges moved in the F8-PFB layer before electron injection from the cathode.

  14. Angle-resolved environmental X-ray photoelectron spectroscopy: A new laboratory setup for photoemission studies at pressures up to 0.4 Torr

    SciTech Connect (OSTI)

    Mangolini, F.; Wabiszewski, G. E.; Egberts, P.; Ahlund, J.; Backlund, K.; Karlsson, P. G.; Adiga, V. P.; Streller, F.; Wannberg, B.; Carpick, R. W.

    2012-09-15

    The paper presents the development and demonstrates the capabilities of a new laboratory-based environmental X-ray photoelectron spectroscopy system incorporating an electrostatic lens and able to acquire spectra up to 0.4 Torr. The incorporation of a two-dimensional detector provides imaging capabilities and allows the acquisition of angle-resolved data in parallel mode over an angular range of 14 Degree-Sign without tilting the sample. The sensitivity and energy resolution of the spectrometer have been investigated by analyzing a standard Ag foil both under high vacuum (10{sup -8} Torr) conditions and at elevated pressures of N{sub 2} (0.4 Torr). The possibility of acquiring angle-resolved data at different pressures has been demonstrated by analyzing a silicon/silicon dioxide (Si/SiO{sub 2}) sample. The collected angle-resolved spectra could be effectively used for the determination of the thickness of the native silicon oxide layer.

  15. Band structure of the epitaxial Fe/MgO/GaAs(001) tunnel junction studied by x-ray and ultraviolet photoelectron spectroscopies

    SciTech Connect (OSTI)

    Lu, Y.; Le Breton, J. C.; Turban, P.; Lepine, B.; Schieffer, P.; Jezequel, G.

    2006-10-09

    The electronic band structure in the epitaxial Fe/MgO/GaAs(001) tunnel junction has been studied by x-ray and ultraviolet photoelectron spectroscopy measurements. The Schottky barrier height (SBH) of Fe on MgO/GaAs heterostructure is determined to be 3.3{+-}0.1 eV, which sets the Fe Fermi level at about 0.3 eV above the GaAs valence band maximum. This SBH is also exactly the same as that measured from Fe on MgO monocrystal. After Fe deposition, no band bending change is observed in MgO and GaAs underlayers. On the contrary, Au and Al depositions led to clear variation of the band bending in both MgO and GaAs layers. This effect is analyzed as a fingerprint of defect states at the MgO/GaAs interface.

  16. Analysis of passivated A-286 stainless steel surfaces for mass spectrometer inlet systems by Auger electron and X-ray photoelectron spectroscopy and scanning electron microscopy

    SciTech Connect (OSTI)

    Ajo, Henry; Blankenship, Donnie; Clark, Elliot

    2014-07-25

    In this study, various commercially available surface treatments are being explored for use on stainless steel components in mass spectrometer inlet systems. Type A-286 stainless steel coupons, approximately 12.5 mm in diameter and 3 mm thick, were passivated with one of five different surface treatments; an untreated coupon served as a control. The surface and near-surface microstructure and chemistry of the coupons were investigated using sputter depth profiling using Auger electron spectroscopy, x-ray photoelectron spectroscopy, and scanning electron microscopy (SEM). All the surface treatments studied appeared to change the surface morphology dramatically, as evidenced by lack of tool marks on the treated samples in SEM images. In terms of the passivation treatment, Vendors A-D appeared to have oxide layers that were very similar in thickness to each other (0.7–0.9 nm thick), as well as to the untreated samples (the untreated sample oxide layers appeared to be somewhat larger). Vendor E’s silicon coating appears to be on the order of 200 nm thick.

  17. Analysis of passivated A-286 stainless steel surfaces for mass spectrometer inlet systems by Auger electron and X-ray photoelectron spectroscopy and scanning electron microscopy

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Ajo, Henry; Blankenship, Donnie; Clark, Elliot

    2014-07-25

    In this study, various commercially available surface treatments are being explored for use on stainless steel components in mass spectrometer inlet systems. Type A-286 stainless steel coupons, approximately 12.5 mm in diameter and 3 mm thick, were passivated with one of five different surface treatments; an untreated coupon served as a control. The surface and near-surface microstructure and chemistry of the coupons were investigated using sputter depth profiling using Auger electron spectroscopy, x-ray photoelectron spectroscopy, and scanning electron microscopy (SEM). All the surface treatments studied appeared to change the surface morphology dramatically, as evidenced by lack of tool marks onmore » the treated samples in SEM images. In terms of the passivation treatment, Vendors A-D appeared to have oxide layers that were very similar in thickness to each other (0.7–0.9 nm thick), as well as to the untreated samples (the untreated sample oxide layers appeared to be somewhat larger). Vendor E’s silicon coating appears to be on the order of 200 nm thick.« less

  18. Evaluating the solid electrolyte interphase formed on silicon electrodes: A comparison of ex situ X-ray photoelectron spectroscopy and in situ neutron reflectometry

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Doucet, Mathieu; Browning, Jim; Baldwin, J. K.; Winiarz, Jeffrey; Kaiser, Helmut; Taub, H.; Veith, Gabriel M.

    2016-04-15

    This work details the in situ characterization of the interface between a silicon electrode and an electrolyte using a linear fluorinated solvent molecule, 0.1 M lithium bis(trifluoromethanesulfonyl)imide (LiTFSI) in deuterated dimethyl perfluoroglutarate (d6-PF5M2) (1.87 x 10-2 mS/cm-1). The solid electrolyte interphase (SEI) composition and thickness determined via in situ neutron reflectometry (NR) and ex situ X-ray photoelectron spectroscopy (XPS) were compared. The data show that SEI expansion and contraction (breathing) during electrochemical cycling was observed via both techniques; however, ex situ XPS suggests that the SEI thickness increases during Si lithiation and decreases during delithiation, while in situ NR suggestsmore » the opposite. The most likely cause of this discrepancy is the selective removal of SEI components (top 20 nm of the SEI) during the electrode rinse process, required to remove electrolyte residue prior to ex situ analysis, demonstrating the necessity of performing SEI characterizations in situ.« less

  19. Water adsorption, solvation and deliquescence of alkali halide thin films on SiO2 studied by ambient pressure X-ray photoelectron spectroscopy

    SciTech Connect (OSTI)

    Arima, Kenta; Jiang, Peng; Deng, Xingyi; Bluhm, Henrik; Salmeron, Miquel

    2010-03-31

    The adsorption of water on KBr thin films evaporated onto SiO2 was investigated as a function of relative humidity (RH) by ambient pressure X-ray photoelectron spectroscopy. At 30percent RH adsorbed water reaches a coverage of approximately one monolayer. As the humidity continues to increase, the coverage of water remains constant or increases very slowly until 60percent RH, followed by a rapid increase up to 100percent RH. At low RH a significant number of the Br atoms are lost due to irradiation damage. With increasing humidity solvation increases ion mobility and gives rise to a partial recovery of the Br/K ratio. Above 60percent RH the increase of the Br/K ratio accelerates. Above the deliquescence point (85percent RH), the thickness of the water layer continues to increase and reaches more than three layers near saturation. The enhancement of the Br/K ratio at this stage is roughly a factor 2.3 on a 0.5 nm KBr film, indicating a strong preferential segregation of Br ions to the surface of the thin saline solution on SiO2.

  20. In Situ Observation of Water Dissociation with Lattice Incorporation at FeO Particle Edges Using Scanning Tunneling Microscopy and X-ray Photoelectron Spectroscopy

    SciTech Connect (OSTI)

    Deng, Xingyi; Lee, Junseok; Wang, Congjun; Matranga, Christopher; Aksoy, Funda; Liu, Zhi

    2011-03-15

    The dissociation of H2O and formation of adsorbed hydroxyl groups, on FeO particles grown on Au(111) were identified with in situ,: X:ray photoelectron spectroscopy (XPS) at water pressures ranging from 3 x 10-8 to 0.1 Torr. The facile dissociation of H2O takes place at FeO particle edges, and it was successfully observed in situ With atomically resolved scanning tunneling microscopy (STM). The in situ STM studies show that adsorbed hydroxyl groups were formed exclusively along the edges of the FeO particles with the 0 atom becoming directly incorporated into the oxide crystalline lattice The STM results are consistent with coordinatively unsaturated ferrous (CUF) sites along the FeO particle edge causing the observed reactivity with H2O. Our results also directly illustrate how structural defects and under.-coordinated sites participate in chemical reactions.

  1. Electrical conductivity anomaly and X-ray photoelectron spectroscopy investigation of YCr{sub 1?x}Mn{sub x}O{sub 3} negative temperature coefficient ceramics

    SciTech Connect (OSTI)

    Zhang, Bo; University of Chinese Academy of Sciences, Beijing 100049 ; Zhao, Qing; Chang, Aimin E-mail: wuy@alfred.edu; Li, Yiyu; Liu, Yin; Wu, Yiquan E-mail: wuy@alfred.edu

    2014-03-10

    Electrical conductivity anomaly of perovskite-type YCr{sub 1?x}Mn{sub x}O{sub 3} negative temperature coefficient (NTC) ceramics produced by spark plasma sintering (SPS) has been investigated by using defect chemistry theory combination with X-ray photoelectron spectroscopy (XPS) analysis. From the results of the ln?-1/T curves and the XPS analysis, it can be considered that YCr{sub 1?x}Mn{sub x}O{sub 3} ceramics exhibit the hopping conductivity. The major carriers in YCrO{sub 3} are holes, which are compensated by the oxygen vacancies produced due to the introduction of Mn ions. The Mn{sup 4+} ion contents increase monotonically in the range of 0.2???x???0.5. The resistivity increases at first and then decreases with increasing Mn contents, which has the same varying tendency with activation energy. The electrical conductivity anomaly appearing in these ceramics may be due to the variation of Cr{sup 4+} and Mn{sup 4+} ions concentration as Mn content changes.

  2. Effects of Pt and Zr on the oxidation behavior of FeTbCo magneto-optic films: X-ray photoelectron spectroscopy

    SciTech Connect (OSTI)

    Majumdar, D.; Hatwar, T. K.

    1989-07-01

    We report the effects of Pt and Zr on the oxidation behavior of FeTbCo magneto-optic films. The addition of 10 at. % Pt or Zr increased environmental stability without significantly affecting the magneto-optic properties. X-ray photoelectron spectroscopy was used to study /ital in/ /ital situ/ oxidation of clean FeTbCoPt and FeTbCoZr films under 5/times/10/sup /minus/7/ Torr of oxygen at room temperature. Pt and Zr played different roles in increasing the oxidation resistance of the alloy. In the FeTbCoPt alloy, Pt reduced the oxygen uptake and retarded the oxidation kinetics of Fe. No oxidation of Pt was observed. In the FeTbCoZr alloy, Zr oxidized readily and segregated to the surface to form a protective layer. The Tb/Fe ratio at the surface increased with oxygen exposure in both alloys but at a faster rate in the FeTbCoPt alloy than in the FeTbCoZr alloy.

  3. X-ray photoelectron spectroscopy of negative electrodes from high-power lithium-ion cells showing various levels of power fade

    SciTech Connect (OSTI)

    Herstedt, Marie; Abraham, Daniel P.; Kerr, John B.

    2004-02-28

    High-power lithium-ion cells for transportation applications are being developed and studied at Argonne National Laboratory. The current generation of cells containing LiNi{sub 0.8}Co{sub 0.15}Al{sub 0.05}O{sub 2}-based cathodes, graphite-based anodes, and LiPF6-based electrolytes show loss of capacity and power during accelerated testing at elevated temperatures. Negative electrode samples harvested from some cells that showed varying degrees of power and capacity fade were examined by X-ray photoelectron spectroscopy (XPS). The samples exhibited a surface film on the graphite, which was thicker on samples from cells that showed higher fade. Furthermore, solvent-based compounds were dominant on samples from low power fade cells, whereas LiPF{sub 6}-based products were dominant on samples from high power fade cells. The effect of sample rinsing and air exposure is discussed. Mechanisms are proposed to explain the formation of compounds suggested by the XPS data.

  4. SMB, X-Ray Spectroscopy & Imaging

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Home » X-Ray Spectroscopy & Imaging X-Ray Spectroscopy & Imaging SSRL has five hard X-ray Spectroscopy beamlines and three Microfocus Imaging beamlines dedicated to Biological and Biomedical research funded by the NIH and DOE-BER. The SMB group supports and develops technical instrumentation and theoretical methods for state-of-the-art tender and hard X-ray spectroscopy and EXAFS studies on metalloproteins, cofactors and metals in medicine. The SMB group has also contributed to the

  5. Hard x-ray delay line for x-ray photon correlation spectroscopy...

    Office of Scientific and Technical Information (OSTI)

    Hard x-ray delay line for x-ray photon correlation spectroscopy and jitter-free pump-probe experiments at LCLS Citation Details In-Document Search Title: Hard x-ray delay line for...

  6. Femtosecond X-ray Absorption Spectroscopy at a Hard X-ray Free...

    Office of Scientific and Technical Information (OSTI)

    Femtosecond X-ray Absorption Spectroscopy at a Hard X-ray Free Electron Laser: Application to Spin Crossover Dynamics Citation Details In-Document Search Title: Femtosecond X-ray...

  7. X-ray photoelectron spectroscopic studies on yttria, zirconia, and yttria-stabilized zirconia

    SciTech Connect (OSTI)

    Majumdar, D. ); Chatterjee, D. )

    1991-07-15

    Surfaces of yttria, zirconia, and yttria-stabilized zirconia were studied using x-ray photoelectron spectroscopy. An almost threefold increase in the surface yttrium concentration was observed in the yttria-stabilized zirconia samples. The core level binding energies of yttrium, zirconium, and oxygen ions in yttria-stabilized zirconia showed chemical shifts. Valence bands and Auger parameters were monitored for the monoclinic and the tetragonal phases of zirconia. Characteristic differences were observed for the two phases due to their different oxygen coordination. The results were used to identify surface phase transitions which were difficult to detect by x-ray diffraction.

  8. X-ray transient absorption and picosecond IR spectroscopy of...

    Office of Scientific and Technical Information (OSTI)

    X-ray transient absorption and picosecond IR spectroscopy of fulvalene(tetracarbonyl)diruthenium on photoexcitation Citation Details In-Document Search Title: X-ray transient ...

  9. Effect of Cl{sub 2}- and HBr-based inductively coupled plasma etching on InP surface composition analyzed using in situ x-ray photoelectron spectroscopy

    SciTech Connect (OSTI)

    Bouchoule, S.; Vallier, L.; Patriarche, G.; Chevolleau, T.; Cardinaud, C.

    2012-05-15

    A Cl{sub 2}-HBr-O{sub 2}/Ar inductively coupled plasma (ICP) etching process has been adapted for the processing of InP-based heterostructures in a 300-mm diameter CMOS etching tool. Smooth and anisotropic InP etching is obtained at moderate etch rate ({approx}600 nm/min). Ex situ x-ray energy dispersive analysis of the etched sidewalls shows that the etching anisotropy is obtained through a SiO{sub x} passivation mechanism. The stoichiometry of the etched surface is analyzed in situ using angle-resolved x-ray photoelectron spectroscopy. It is observed that Cl{sub 2}-based ICP etching results in a significantly P-rich surface. The phosphorous layer identified on the top surface is estimated to be {approx}1-1.3-nm thick. On the other hand InP etching in HBr/Ar plasma results in a more stoichiometric surface. In contrast to the etched sidewalls, the etched surface is free from oxides with negligible traces of silicon. Exposure to ambient air of the samples submitted to Cl{sub 2}-based chemistry results in the complete oxidation of the P-rich top layer. It is concluded that a post-etch treatment or a pure HBr plasma step may be necessary after Cl{sub 2}-based ICP etching for the recovery of the InP material.

  10. In-operando hard X-ray photoelectron spectroscopy study on the impact of current compliance and switching cycles on oxygen and carbon defects in resistive switching Ti/HfO{sub 2}/TiN cells

    SciTech Connect (OSTI)

    Sowinska, Malgorzata Bertaud, Thomas; Walczyk, Damian; Calka, Pauline; Walczyk, Christian; Thiess, Sebastian; Alff, Lambert; Schroeder, Thomas

    2014-05-28

    In this study, direct experimental materials science evidence of the important theoretical prediction for resistive random access memory (RRAM) technologies that a critical amount of oxygen vacancies is needed to establish stable resistive switching in metal-oxide-metal samples is presented. In detail, a novel in-operando hard X-ray photoelectron spectroscopy technique is applied to non-destructively investigates the influence of the current compliance and direct current voltage sweep cycles on the Ti/HfO{sub 2} interface chemistry and physics of resistive switching Ti/HfO{sub 2}/TiN cells. These studies indeed confirm that current compliance is a critical parameter to control the amount of oxygen vacancies in the conducting filaments in the oxide layer during the RRAM cell operation to achieve stable switching. Furthermore, clear carbon segregation towards the Ti/HfO{sub 2} interface under electrical stress is visible. Since carbon impurities impact the oxygen vacancy defect population under resistive switching, this dynamic carbon segregation to the Ti/HfO{sub 2} interface is suspected to negatively influence RRAM device endurance. Therefore, these results indicate that the RRAM materials engineering needs to include all impurities in the dielectric layer in order to achieve reliable device performance.

  11. A combined capacitance-voltage and hard x-ray photoelectron spectroscopy characterisation of metal/Al{sub 2}O{sub 3}/In{sub 0.53}Ga{sub 0.47}As capacitor structures

    SciTech Connect (OSTI)

    Lin, Jun; Povey, Ian M.; Hurley, Paul K.; Walsh, Lee; Hughes, Greg; Woicik, Joseph C.; O'Regan, Terrance P.

    2014-07-14

    Capacitance-Voltage (C-V) characterization and hard x-ray photoelectron spectroscopy (HAXPES) measurements have been used to study metal/Al{sub 2}O{sub 3}/In{sub 0.53}Ga{sub 0.47}As capacitor structures with high (Ni) and low (Al) work function metals. The HAXPES measurements observe a band bending occurring prior to metal deposition, which is attributed to a combination of fixed oxide charges and interface states of donor-type. Following metal deposition, the Fermi level positions at the Al{sub 2}O{sub 3}/In{sub 0.53}Ga{sub 0.47}As interface move towards the expected direction as observed from HAXPES measurements. The In{sub 0.53}Ga{sub 0.47}As surface Fermi level positions determined from both the C-V analysis at zero gate bias and HAXPES measurements are in reasonable agreement. The results are consistent with the presence of electrically active interface states at the Al{sub 2}O{sub 3}/In{sub 0.53}Ga{sub 0.47}As interface and suggest an interface state density increasing towards the In{sub 0.53}Ga{sub 0.47}As valence band edge.

  12. Band alignment of HfO{sub 2}/multilayer MoS{sub 2} interface determined by x-ray photoelectron spectroscopy: Effect of CHF{sub 3} treatment

    SciTech Connect (OSTI)

    Liu, Xinke; He, Jiazhu; Tang, Dan; Jia, Fang; Lu, Youming Zhu, Deliang; Liu, Wenjun; Cao, Peijiang; Han, Sun; Liu, Qiang; Wen, Jiao; Yu, Wenjie; Pan, Jisheng; He, Zhubing; Ang, Kah-Wee

    2015-09-07

    The energy band alignment between HfO{sub 2}/multilayer (ML)-MoS{sub 2} was characterized using high-resolution x-ray photoelectron spectroscopy. The HfO{sub 2} was deposited using an atomic layer deposition tool, and ML-MoS{sub 2} was grown by chemical vapor deposition. A valence band offset (VBO) of 1.98 eV and a conduction band offset (CBO) of 2.72 eV were obtained for the HfO{sub 2}/ML-MoS{sub 2} interface without any treatment. With CHF{sub 3} plasma treatment, a VBO and a CBO across the HfO{sub 2}/ML-MoS{sub 2} interface were found to be 2.47 eV and 2.23 eV, respectively. The band alignment difference is believed to be dominated by the down-shift in the core level of Hf 4d and up-shift in the core level of Mo 3d, or the interface dipoles, which caused by the interfacial layer in rich of F.

  13. Laser plasma x-ray source for ultrafast time-resolved x-ray absorption spectroscopy

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Miaja-Avila, L.; O'Neil, G. C.; Uhlig, J.; Cromer, C. L.; Dowell, M. L.; Jimenez, R.; Hoover, A. S.; Silverman, K. L.; Ullom, J. N.

    2015-03-02

    We describe a laser-driven x-ray plasma source designed for ultrafast x-ray absorption spectroscopy. The source is comprised of a 1 kHz, 20 W, femtosecond pulsed infrared laser and a water target. We present the x-ray spectra as a function of laser energy and pulse duration. Additionally, we investigate the plasma temperature and photon flux as we vary the laser energy. We obtain a 75 μm FWHM x-ray spot size, containing ~106 photons/s, by focusing the produced x-rays with a polycapillary optic. Since the acquisition of x-ray absorption spectra requires the averaging of measurements from >107 laser pulses, we also presentmore » data on the source stability, including single pulse measurements of the x-ray yield and the x-ray spectral shape. In single pulse measurements, the x-ray flux has a measured standard deviation of 8%, where the laser pointing is the main cause of variability. Further, we show that the variability in x-ray spectral shape from single pulses is low, thus justifying the combining of x-rays obtained from different laser pulses into a single spectrum. Finally, we show a static x-ray absorption spectrum of a ferrioxalate solution as detected by a microcalorimeter array. Altogether, our results demonstrate that this water-jet based plasma source is a suitable candidate for laboratory-based time-resolved x-ray absorption spectroscopy experiments.« less

  14. Laser plasma x-ray source for ultrafast time-resolved x-ray absorption spectroscopy

    SciTech Connect (OSTI)

    Miaja-Avila, L.; O'Neil, G. C.; Uhlig, J.; Cromer, C. L.; Dowell, M. L.; Jimenez, R.; Hoover, A. S.; Silverman, K. L.; Ullom, J. N.

    2015-03-02

    We describe a laser-driven x-ray plasma source designed for ultrafast x-ray absorption spectroscopy. The source is comprised of a 1 kHz, 20 W, femtosecond pulsed infrared laser and a water target. We present the x-ray spectra as a function of laser energy and pulse duration. Additionally, we investigate the plasma temperature and photon flux as we vary the laser energy. We obtain a 75 μm FWHM x-ray spot size, containing ~106 photons/s, by focusing the produced x-rays with a polycapillary optic. Since the acquisition of x-ray absorption spectra requires the averaging of measurements from >107 laser pulses, we also present data on the source stability, including single pulse measurements of the x-ray yield and the x-ray spectral shape. In single pulse measurements, the x-ray flux has a measured standard deviation of 8%, where the laser pointing is the main cause of variability. Further, we show that the variability in x-ray spectral shape from single pulses is low, thus justifying the combining of x-rays obtained from different laser pulses into a single spectrum. Finally, we show a static x-ray absorption spectrum of a ferrioxalate solution as detected by a microcalorimeter array. Altogether, our results demonstrate that this water-jet based plasma source is a suitable candidate for laboratory-based time-resolved x-ray absorption spectroscopy experiments.

  15. XRMS: X-Ray Spectroscopy of Magnetic Solids

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    XRMS: X-Ray Spectroscopy of Magnetic Solids October 22-23, 2011 SLAC National Accelerator Laboratory, Menlo Park, CA More information...

  16. Atomic force microscopy and x-ray photoelectron spectroscopy investigations of the morphology and chemistry of a PdCl{sub 2}/SnCl{sub 2} electroless plating catalysis system adsorbed onto shape memory alloy particles

    SciTech Connect (OSTI)

    Silvain, J.F.; Fouassier, O.; Lescaux, S.

    2004-11-01

    A study of the different stages of the electroless deposition of copper on micronic NiTi shape memory alloy particles activated by one-step and two-step methods has been conducted from both a chemical and a morphological point of view. The combination of x-ray photoelectron spectroscopy (XPS) measurements and atomic force microscopy (AFM) imaging has allowed detection of the distribution of the formed compounds and depth quantification and estimation of the surface topographic parameters. For the two-step method, at the sensitization of the early stages, it is observed by AFM that Sn is absorbed in form of clusters that tend to completely cover the surface and form a continuous film. XPS analysis have shown that Sn and Pd are first absorbed in form of oxide (SnO{sub 2} and PdO) and hydroxide [Sn(OH){sub 4}]. After the entire sensitization step, the NiTi substrate is covered with Sn-based compounds. After the sensitization and the activation steps the powder roughness increases. Behavior of the Sn and Pd growth for the one-step method does not follow the behavior found for the two-step method. Indeed, XPS analysis shows a three-dimensional (3D) growth of Pd clusters on top of a mixture of metallic tin, oxide (SnO) and hydroxide [Sn(OH){sub 2}]. These Pd clusters are covered with a thin layer of Pd-oxide contamination induced by the electroless process. The mean roughness for the one-step and two-step processes are equivalent. After copper deposition, the decrease of mean roughness is attributed to a filling of surface valleys, observed after the Sn-Pd coating step.

  17. X-ray spectroscopy of manganese clusters

    SciTech Connect (OSTI)

    Grush, M.M.

    1996-06-01

    Much of this thesis represents the groundwork necessary in order to probe Mn clusters more productively than with conventional Mn K-edge XAS and is presented in Part 1. Part 2 contains the application of x-ray techniques to Mn metalloproteins and includes a prognosis at the end of each chapter. Individual Mn oxidation states are more readily distinguishable in Mn L-edge spectra. An empirical mixed valence simulation routine for determining the average Mn oxidation state has been developed. The first Mn L-edge spectra of a metalloprotein were measured and interpreted. The energy of Mn K{beta} emission is strongly correlated with average Mn oxidation state. K{beta} results support oxidation states of Mn(III){sub 2}(IV){sub 2} for the S{sub 1} state of Photosystem II chemical chemically reduced preparations contain predominantly Mn(II). A strength and limitation of XAS is that it probes all of the species of a particular element in a sample. It would often be advantageous to selectively probe different forms of the same element. The first demonstration that chemical shifts in x-ray fluorescence energies can be used to obtain oxidation state-selective x-ray absorption spectra is presented. Spin-dependent spectra can also be used to obtain a more simplified picture of local structure. The first spin-polarized extended x-ray absorption fine structure using Mn K{beta} fluorescence detection is shown.

  18. Hard x-ray photoelectron spectroscopy study of Ge{sub 2}Sb{sub 2}Te{sub 5}; as-deposited amorphous, crystalline, and laser-reamorphized

    SciTech Connect (OSTI)

    Richter, Jan H. Tominaga, Junji; Fons, Paul; Kolobov, Alex V.; Ueda, Shigenori; Yoshikawa, Hideki; Yamashita, Yoshiyuki; Ishimaru, Satoshi; Kobayashi, Keisuke

    2014-02-10

    We have investigated the electronic structure of as-deposited, crystalline, and laser-reamorphized Ge{sub 2}Sb{sub 2}Te{sub 5} using high resolution, hard x-ray photoemission spectroscopy. A shift in the Fermi level as well as a broadening of the spectral features in the valence band and the Ge 3d level between the amorphous and crystalline state is observed. Upon amorphization, Ge 3d and Sb 4d spectra show a surprisingly small breaking of resonant bonds and changes in the bonding character as evidenced by the very similar density of states in all cases.

  19. Characterization of Gas Shales by X-ray Raman Spectroscopy |...

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Characterization of Gas Shales by X-ray Raman Spectroscopy Thursday, February 23, 2012 - 10:30am SSRL Third Floor Conference Room 137-322 Drew Pomerantz, Schlumberger ...

  20. Characterization of Gas Shales by X-ray Raman Spectroscopy |...

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Characterization of Gas Shales by X-ray Raman Spectroscopy Monday, May 14, 2012 - 3:30pm SSRL Conference Room 137-322 Drew Pomerantz, Schlumberger Unconventional hydrocarbon ...

  1. Soft-x-ray spectroscopy study of nanoscale materials

    SciTech Connect (OSTI)

    Guo, J.-H.

    2005-07-30

    The ability to control the particle size and morphology of nanoparticles is of crucial importance nowadays both from a fundamental and industrial point of view considering the tremendous amount of high-tech applications. Controlling the crystallographic structure and the arrangement of atoms along the surface of nanostructured material will determine most of its physical properties. In general, electronic structure ultimately determines the properties of matter. Soft X-ray spectroscopy has some basic features that are important to consider. X-ray is originating from an electronic transition between a localized core state and a valence state. As a core state is involved, elemental selectivity is obtained because the core levels of different elements are well separated in energy, meaning that the involvement of the inner level makes this probe localized to one specific atomic site around which the electronic structure is reflected as a partial density-of-states contribution. The participation of valence electrons gives the method chemical state sensitivity and further, the dipole nature of the transitions gives particular symmetry information. The new generation synchrotron radiation sources producing intensive tunable monochromatized soft X-ray beams have opened up new possibilities for soft X-ray spectroscopy. The introduction of selectively excited soft X-ray emission has opened a new field of study by disclosing many new possibilities of soft X-ray resonant inelastic scattering. In this paper, some recent findings regarding soft X-ray absorption and emission studies of various nanostructured systems are presented.

  2. New focusing multilayer structures for X-ray plasma spectroscopy

    SciTech Connect (OSTI)

    Bibishkin, M S; Luchin, V I; Salashchenko, N N; Chernov, V V; Chkhalo, N I; Kazakov, E D; Shevelko, A P

    2008-02-28

    New focusing short-period multilayer structures are developed which opens up wide possibilities for X-ray and VUV spectroscopy. Multilayer structures are deposited on a flat surface of a mica crystal which is then bent to a small-radius cylinder. The use of this structure in a von Hamos spectrometer for X-ray laser plasma diagnostics is demonstrated. (interaction of laser radiation with matter. laser plasma)

  3. X-ray photoelectron spectroscopic investigation of nanocrystalline calcium silicate hydrates synthesised by reactive milling

    SciTech Connect (OSTI)

    Black, Leon . E-mail: l.black@shu.ac.uk; Garbev, Krassimir; Beuchle, Guenter; Stemmermann, Peter; Schild, Dieter

    2006-06-15

    X-ray photoelectron spectroscopy (XPS) has been used to analyse a series of mechanochemically synthesised, nanocrystalline calcium silicate hydrates (C-S-H). The samples, with Ca/Si ratios of 0.2 to 1.5, showed structural features of C-S-H(I). XPS analysis revealed changes in the extent of silicate polymerisation. Si 2p, Ca 2p and O 1s spectra showed that, unlike for the crystalline calcium silicate hydrate phases studied previously, there was no evidence of silicate sheets (Q{sup 3}) at low Ca/Si ratios. Si 2p and O 1s spectra indicated silicate depolymerisation, expressed by decreasing silicate chain length, with increasing C/S. In all spectra, peak narrowing was observed with increasing Ca/Si, indicating increased structural ordering. The rapid changes of the slope of FWHM of Si 2p, {delta} {sub Ca-Si} and {delta} {sub NBO-BO} as function of C/S ratio indicated a possible miscibility gap in the C-S-H-solid solution series between C/S 5/6 and 1. The modified Auger parameter ({alpha}') of nanocrystalline C-S-H decreased with increasing silicate polymerisation, a trend already observed studying crystalline C-S-H. Absolute values of {alpha}' were shifted about - 0.7 eV with respect to crystalline phases of equal C/S ratio, due to reduced crystallinity.

  4. Femtosecond x-ray absorption spectroscopy with hard x-ray free electron laser

    SciTech Connect (OSTI)

    Katayama, Tetsuo; Togashi, Tadashi; Tono, Kensuke; Kameshima, Takashi; Inubushi, Yuichi; Sato, Takahiro; Hatsui, Takaki; Yabashi, Makina; Obara, Yuki; Misawa, Kazuhiko; Bhattacharya, Atanu; Kurahashi, Naoya; Ogi, Yoshihiro; Suzuki, Toshinori; Molecular Reaction Dynamics Research Team, RIKEN Center for Advanced Photonics, 2-1 Hirosawa, Wako 351-0198

    2013-09-23

    We have developed a method of dispersive x-ray absorption spectroscopy with a hard x-ray free electron laser (XFEL), generated by a self-amplified spontaneous emission (SASE) mechanism. A transmission grating was utilized for splitting SASE-XFEL light, which has a relatively large bandwidth (ΔE/E ∼ 5 × 10{sup −3}), into several branches. Two primary split beams were introduced into a dispersive spectrometer for measuring signal and reference spectra simultaneously. After normalization, we obtained a Zn K-edge absorption spectrum with a photon-energy range of 210 eV, which is in excellent agreement with that measured by a conventional wavelength-scanning method. From the analysis of the difference spectra, the noise ratio was evaluated to be ∼3 × 10{sup −3}, which is sufficiently small to trace minute changes in transient spectra induced by an ultrafast optical laser. This scheme enables us to perform single-shot, high-accuracy x-ray absorption spectroscopy with femtosecond time resolution.

  5. X-ray absorption spectroscopy study of Gd[superscript 3+]-loaded...

    Office of Scientific and Technical Information (OSTI)

    Journal Article: X-ray absorption spectroscopy study of Gdsuperscript 3+-loaded ultra-short carbon nanotubes Citation Details In-Document Search Title: X-ray absorption ...

  6. A laboratory-based hard x-ray monochromator for high-resolution x-ray emission spectroscopy and x-ray absorption near edge structure measurements

    SciTech Connect (OSTI)

    Seidler, G. T. Mortensen, D. R.; Remesnik, A. J.; Pacold, J. I.; Ball, N. A.; Barry, N.; Styczinski, M.; Hoidn, O. R.

    2014-11-15

    We report the development of a laboratory-based Rowland-circle monochromator that incorporates a low power x-ray (bremsstrahlung) tube source, a spherically bent crystal analyzer, and an energy-resolving solid-state detector. This relatively inexpensive, introductory level instrument achieves 1-eV energy resolution for photon energies of ∼5 keV to ∼10 keV while also demonstrating a net efficiency previously seen only in laboratory monochromators having much coarser energy resolution. Despite the use of only a compact, air-cooled 10 W x-ray tube, we find count rates for nonresonant x-ray emission spectroscopy comparable to those achieved at monochromatized spectroscopy beamlines at synchrotron light sources. For x-ray absorption near edge structure, the monochromatized flux is small (due to the use of a low-powered x-ray generator) but still useful for routine transmission-mode studies of concentrated samples. These results indicate that upgrading to a standard commercial high-power line-focused x-ray tube or rotating anode x-ray generator would result in monochromatized fluxes of order 10{sup 6}–10{sup 7} photons/s with no loss in energy resolution. This work establishes core technical capabilities for a rejuvenation of laboratory-based hard x-ray spectroscopies that could have special relevance for contemporary research on catalytic or electrical energy storage systems using transition-metal, lanthanide, or noble-metal active species.

  7. Silicon nanocrystals with high boron and phosphorus concentration hydrophilic shell—Raman scattering and X-ray photoelectron spectroscopic studies

    SciTech Connect (OSTI)

    Fujii, Minoru Sugimoto, Hiroshi; Hasegawa, Masataka; Imakita, Kenji

    2014-02-28

    Boron (B) and phosphorus (P) codoped silicon (Si) nanocrystals, which exhibit very wide range tunable luminescence due to the donor to acceptor transitions and can be dispersed in polar liquids without organic ligands, are studied by Raman scattering and X-ray photoelectron spectroscopies. Codoped Si nanocrystals exhibit a Raman spectrum significantly different from those of intrinsic ones. First, the Raman peak energy is almost insensitive to the size and is very close to that of bulk Si crystal in the diameter range of 2.7 to 14 nm. Second, the peak is much broader than that of intrinsic ones. Furthermore, an additional broad peak, the intensity of which is about 20% of the main peak, appears around 650 cm{sup −1}. The peak can be assigned to local vibrational modes of substitutional B and B-P pairs, B clusters, B-interstitial clusters, etc. in Si crystal. The Raman and X-ray photoelectron spectroscopic studies suggest that a crystalline shell heavily doped with these species is formed at the surface of a codoped Si nanocrystal and it induces the specific properties, i.e., hydrophilicity, high-stability in water, high resistance to hydrofluoric acid, etc.

  8. X-ray absorption fine-structure spectroscopy (Book) | SciTech...

    Office of Scientific and Technical Information (OSTI)

    X-ray absorption fine-structure spectroscopy Citation Details In-Document Search Title: X-ray absorption fine-structure spectroscopy Authors: Newville, M. 1 + Show Author ...

  9. X-ray imaging crystal spectroscopy for use in plasma transport...

    Office of Scientific and Technical Information (OSTI)

    X-ray imaging crystal spectroscopy for use in plasma transport research Citation Details In-Document Search Title: X-ray imaging crystal spectroscopy for use in plasma transport ...

  10. In Operando Soft X-ray Spectroscopy of 3D Graphene Supercapacitor...

    Office of Scientific and Technical Information (OSTI)

    In Operando Soft X-ray Spectroscopy of 3D Graphene Supercapacitor Electrodes Citation Details In-Document Search Title: In Operando Soft X-ray Spectroscopy of 3D Graphene ...

  11. X-ray line polarization spectroscopy of Li-like satellite line...

    Office of Scientific and Technical Information (OSTI)

    X-ray line polarization spectroscopy of Li-like satellite line spectra Citation Details In-Document Search Title: X-ray line polarization spectroscopy of Li-like satellite line ...

  12. Soft X-Ray and Vacuum Ultraviolet Based Spectroscopy of the Actinides...

    Office of Scientific and Technical Information (OSTI)

    Conference: Soft X-Ray and Vacuum Ultraviolet Based Spectroscopy of the Actinides Citation Details In-Document Search Title: Soft X-Ray and Vacuum Ultraviolet Based Spectroscopy of ...

  13. Soft X-Ray and Vacuum Ultraviolet Based Spectroscopy of the Actinides...

    Office of Scientific and Technical Information (OSTI)

    Conference: Soft X-Ray and Vacuum Ultraviolet Based Spectroscopy of the Actinides Citation Details In-Document Search Title: Soft X-Ray and Vacuum Ultraviolet Based Spectroscopy of...

  14. Hubbard model corrections in real-space x-ray spectroscopy theory...

    Office of Scientific and Technical Information (OSTI)

    Hubbard model corrections in real-space x-ray spectroscopy theory Citation Details In-Document Search Title: Hubbard model corrections in real-space x-ray spectroscopy theory ...

  15. Calibration of Spherically Bent Crystals used in X-Ray Spectroscopy...

    Office of Scientific and Technical Information (OSTI)

    Calibration of Spherically Bent Crystals used in X-Ray Spectroscopy. Citation Details In-Document Search Title: Calibration of Spherically Bent Crystals used in X-Ray Spectroscopy. ...

  16. A new spectrometer design for the x-ray spectroscopy of laser...

    Office of Scientific and Technical Information (OSTI)

    the x-ray spectroscopy of laser-produced plasmas with high (sub-ns) time resolution Citation Details In-Document Search Title: A new spectrometer design for the x-ray ...

  17. New developments in high pressure x-ray spectroscopy beamline at High Pressure Collaborative Access Team

    SciTech Connect (OSTI)

    Xiao, Y. M. Chow, P.; Boman, G.; Bai, L. G.; Rod, E.; Bommannavar, A.; Kenney-Benson, C.; Sinogeikin, S.; Shen, G. Y.

    2015-07-15

    The 16 ID-D (Insertion Device - D station) beamline of the High Pressure Collaborative Access Team at the Advanced Photon Source is dedicated to high pressure research using X-ray spectroscopy techniques typically integrated with diamond anvil cells. The beamline provides X-rays of 4.5-37 keV, and current available techniques include X-ray emission spectroscopy, inelastic X-ray scattering, and nuclear resonant scattering. The recent developments include a canted undulator upgrade, 17-element analyzer array for inelastic X-ray scattering, and an emission spectrometer using a polycapillary half-lens. Recent development projects and future prospects are also discussed.

  18. Gas cell for in situ soft X-ray transmission-absorption spectroscopy...

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    cell for in situ soft X-ray transmission-absorption spectroscopy of materials Previous ... Abstract: A simple gas cell design, constructed primarily from commercially available ...

  19. Development of Time Resolved X-ray Spectroscopy in High Intensity...

    Office of Scientific and Technical Information (OSTI)

    Title: Development of Time Resolved X-ray Spectroscopy in High Intensity Laser-Plasma Interactions Authors: Notley, M ; Weber, R ; Fell, B ; Jefferies, J ; Freeman, R ; Mackinnon, ...

  20. SSRL School on Synchrotron X-ray Spectroscopy Techniques in Environmen...

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Transportation Tourism & Dining SSRL School on Synchrotron X-ray Spectroscopy Techniques in Environmental and Materials Sciences: Theory and Application June 2-5, 2009 Group...

  1. Stimulated X-Ray Emission for Spectroscopy | Stanford Synchrotron...

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Room 108A Speaker: Clemens Weninger, Max Planck Institute for the Physics of Complex Systems Program Description The recent advance of x-ray free electron lasers (XFELs)...

  2. Staff Research Physicist (X-Ray Spectroscopy) | Princeton Plasma...

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    of X-ray spectrometers for high energy density plasma at the National Ignition Facility (NIF) at the Lawrence Livermore National Laboratory (LLNL, Livermore, California). In...

  3. Near-Edge X-Ray Absorption Fine Structure Spectroscopy of Diamondoid Thiol Monolayers on Gold

    SciTech Connect (OSTI)

    Willey, T.M.; Fabbri, J.D.; Lee, J.R.I.; Schreiner, P.R.; Fokin, A.A.; Tkachenko, B.A.; Fokina, N.A.; Dahl, J.E.P.; Carlson, R.M.K.; Vance, A.L.; Yang, W.; Terminello, L.J.; Buuren, T.van; Melosh, N.A.

    2009-05-26

    Diamondoids, hydrocarbon molecules with cubic-diamond-cage structures, have unique properties with potential value for nanotechnology. The availability and ability to selectively functionalize this special class of nanodiamond materials opens new possibilities for surface modification, for high-efficiency field emitters in molecular electronics, as seed crystals for diamond growth, or as robust mechanical coatings. The properties of self-assembled monolayers (SAMs) of diamondoids are thus of fundamental interest for a variety of emerging applications. This paper presents the effects of thiol substitution position and polymantane order on diamondoid SAMs on gold using near-edge X-ray absorption fine structure spectroscopy (NEXAFS) and X-ray photoelectron spectroscopy (XPS). A framework to determine both molecular tilt and twist through NEXAFS is presented and reveals highly ordered diamondoid SAMs, with the molecular orientation controlled by the thiol location. C 1s and S 2p binding energies are lower in adamantane thiol than alkane thiols on gold by 0.67 {+-} 0.05 and 0.16 {+-} 0.04 eV, respectively. These binding energies vary with diamondoid monolayer structure and thiol substitution position, consistent with different degrees of steric strain and electronic interaction with the substrate. This work demonstrates control over the assembly, in particular the orientational and electronic structure, providing a flexible design of surface properties with this exciting new class of diamond nanoparticles.

  4. Near-Edge X-ray Absorption Fine Structure Spectroscopy of Diamondoid Thiol Monolayers on Gold

    SciTech Connect (OSTI)

    Willey, T M; Fabbri, J; Lee, J I; Schreiner, P; Fokin, A A; Tkachenko, B A; Fokina, N A; Dahl, J; Carlson, B; Vance, A L; Yang, W; Terminello, L J; van Buuren, T; Melosh, N

    2007-11-27

    Diamondoids, hydrocarbon molecules with cubic-diamond-cage structures, have unique properties with potential value for nanotechnology. The availability and ability to selectively functionalize this special class of nanodiamond materials opens new possibilities for surface-modification, for high-efficiency field emitters in molecular electronics, as seed crystals for diamond growth, or as robust mechanical coatings. The properties of self-assembled monolayers (SAMs) of diamondoids are thus of fundamental interest for a variety of emerging applications. This paper presents the effects of thiol substitution position and polymantane order on diamondoid SAMs on gold using near-edge X-ray absorption fine structure spectroscopy (NEXAFS) and X-ray photoelectron spectroscopy (XPS). A framework to determine both molecular tilt and twist through NEXAFS is presented and reveals highly ordered diamondoid SAMs, with the molecular orientation controlled by the thiol location. C 1s and S 2p binding energies are lower in adamantane thiol than alkane thiols on gold by 0.67 {+-} 0.05 eV and 0.16 {+-} 0.04 eV respectively. These binding energies vary with diamondoid monolayer structure and thiol substitution position, consistent with different amounts of steric strain and electronic interaction with the substrate. This work demonstrates control over the assembly, in particular the orientational and electronic structure, providing a flexible design of surface properties with this exciting new class of diamond clusters.

  5. X-Ray Photoelectron Spectroscopy (XPS) Applied to Soot & What...

    Office of Energy Efficiency and Renewable Energy (EERE) Indexed Site

    Presentation given at DEER 2006, August 20-24, 2006, Detroit, Michigan. Sponsored by the U.S. DOE's EERE FreedomCar and Fuel Partnership and 21st Century Truck Programs. ...

  6. Johann Spectrometer for High Resolution X-ray Spectroscopy

    SciTech Connect (OSTI)

    Machek, Pavel; Froeba, Michael; Welter, Edmund; Caliebe, Wolfgang; Brueggmann, Ulf; Draeger, Guenter

    2007-01-19

    A newly designed vacuum Johann spectrometer with a large focusing analyzer crystal for inelastic x-ray scattering and high resolution fluorescence spectroscopy has been installed at the DORIS III storage ring. Spherically bent crystals with a maximum diameter of 125 mm, and cylindrically bent crystals are employed as dispersive optical elements. Standard radius of curvature of the crystals is 1000 mm, however, the design of the mechanical components also facilitates measurements with smaller and larger bending radii. Up to four crystals are mounted on a revolving crystal changer which enables crystal changes without breaking the vacuum. The spectrometer works at fixed Bragg angle. It is preferably designed for the measurements in non-scanning mode with a broad beam spot, and offers a large flexibility to set the sample to the optimum position inside the Rowland circle. A deep depletion CCD camera is employed as a position sensitive detector to collect the energy-analyzed photons on the circumference of the Rowland circle. The vacuum in the spectrometer tank is typically 10-6 mbar. The sample chamber is separated from the tank either by 25 {mu}m thick Kapton windows, which allows samples to be measured under ambient conditions, or by two gate valves. The spectrometer is currently installed at wiggler beamline W1 whose working range is 4-10.5 keV with typical flux at the sample of 5x1010photons/s/mm2. The capabilities of the spectrometer are illustrated by resonant inelastic experiments on 3d transition metals and rare earth compounds, and by chemical shift measurements on chromium compounds.

  7. X-Ray Spectroscopy of the Mn(4) Ca Cluster in the Water-Oxidation...

    Office of Scientific and Technical Information (OSTI)

    Ca Cluster in the Water-Oxidation Complex of Photosystem II Citation Details In-Document Search Title: X-Ray Spectroscopy of the Mn(4) Ca Cluster in the Water-Oxidation Complex ...

  8. Low-dimensional systems investigated by x-ray absorption spectroscopy...

    Office of Scientific and Technical Information (OSTI)

    Title: Low-dimensional systems investigated by x-ray absorption spectroscopy: a selection of 2D, 1D and 0D cases Authors: Mino, Lorenzo ; Agostini, Giovanni ; Borfecchia, Elisa ; ...

  9. Theoretical study of Raman chirped adiabatic passage by X-ray absorption spectroscopy: Highly excited electronic states and rotational effects

    SciTech Connect (OSTI)

    Engin, Selma; Sisourat, Nicolas Selles, Patricia; Taïeb, Richard; Carniato, Stéphane

    2014-06-21

    Raman Chirped Adiabatic Passage (RCAP) is an efficient method to climb the vibrational ladder of molecules. It was shown on the example of fixed-in-space HCl molecule that selective vibrational excitation can thus be achieved by RCAP and that population transfer can be followed by X-ray Photoelectron spectroscopy [S. Engin, N. Sisourat, P. Selles, R. Taïeb, and S. Carniato, Chem. Phys. Lett. 535, 192–195 (2012)]. Here, in a more detailed analysis of the process, we investigate the effects of highly excited electronic states and of molecular rotation on the efficiency of RCAP. Furthermore, we propose an alternative spectroscopic way to monitor the transfer by means of X-ray absorption spectra.

  10. X-ray Photoelectron Spectroscopic Analyses of Corrosion Products Formed on Rock Bolt Carbon Steel in Chloride Media with Bicarbonate and Silicate Ions

    SciTech Connect (OSTI)

    Deodeshmukh, Vinay; Venugopal, A; Chandra, Dhanesh; Yilmaz, Ahmet; Daemen, Jack; Jones, D A.; Lea, Alan S.; Engelhard, Mark H.

    2004-11-01

    The passivation behavior of Yucca Mountain Repository rock bolt carbon steel in deaerated 3.5% NaCl solution containing SiO{sub 3}{sup 2} and HCO{sub 3} ions was investigated by potentiodynamic polarization, electrochemical impedance spectroscopy, scanning electron microscopy, and X-ray photoelectron spectroscopic methods. Polarization results indicate that combinations of silicate and bicarbonate anions decrease the passive current density and raise the pitting potential. XPS results indicate the enrichment of silica at passive potentials and the formation of mixed FeCO{sub 3} and silica film at lower potentials. This change in film composition was responsible for the changes in corrosion rate at lower and higher potentials. XPS results also support the thermodynamic data with regard to the occurrence of second oxidation peak observed in the polarization curves to be due to the oxidation of FeCO{sub 3} to Fe{sub 2}O{sub 3}.

  11. X-ray Spectroscopy for Quality Control of Chemotherapy Drugs

    SciTech Connect (OSTI)

    Greaves, E. D.; Barros, H.; Bermudez, J.; Sajo-Bohus, L.; Angeli-Greaves, M.

    2007-10-26

    We develop a method, employing Compton peak standardization and the use of matrix-matched spiked samples with Total Reflection X-ray Fluorescence (TXRF), for the determination of platinum plasma concentrations of patients undergoing chemotherapy with Pt-bearing drugs. Direct blood plasma analysis attains Pt detection limits of 70 ng/ml. Measurement results of prescribed drug doses are compared to achieved blood Pt concentrations indicating a lack of expected correlations. Direct analysis of Pt-containing infused drugs from a variety of suppliers indicates cases of abnormal concentrations which raises quality control issues. We demonstrate the potential usefulness of the method for pharmacokinetic studies or for routine optimization and quality control of Pt chemotherapy treatments.

  12. Ultrafast conversions between hydrogen bonded structures in liquid water observed by femtosecond x-ray spectroscopy

    SciTech Connect (OSTI)

    Wen, Haidan; Huse, Nils; Schoenlein, Robert W.; Lindenberg, Aaron M.

    2010-05-01

    We present the first femtosecond soft x-ray spectroscopy in liquids, enabling the observation of changes in hydrogen bond structures in water via core-hole excitation. The oxygen K-edge of vibrationally excited water is probed with femtosecond soft x-ray pulses, exploiting the relation between different water structures and distinct x-ray spectral features. After excitation of the intramolecular OH stretching vibration, characteristic x-ray absorption changes monitor the conversion of strongly hydrogen-bonded water structures to more disordered structures with weaker hydrogen-bonding described by a single subpicosecond time constant. The latter describes the thermalization time of vibrational excitations and defines the characteristic maximum rate with which nonequilibrium populations of more strongly hydrogen-bonded water structures convert to less-bonded ones. On short time scales, the relaxation of vibrational excitations leads to a transient high-pressure state and a transient absorption spectrum different from that of statically heated water.

  13. The X-ray correlation spectroscopy instrument at the Linac Coherent Light Source

    SciTech Connect (OSTI)

    Alonso-Mori, Roberto; Caronna, Chiara; Chollet, Matthieu; Curtis, Robin; Damiani, Daniel S.; Defever, Jim; Feng, Yiping; Flath, Daniel L.; Glownia, James M.; Lee, Sooheyong; Lemke, Henrik T.; Nelson, Silke; Bong, Eric; Sikorski, Marcin; Song, Sanghoon; Srinivasan, Venkat; Stefanescu, Daniel; Zhu, Diling; Robert, Aymeric

    2015-03-03

    The X-ray Correlation Spectroscopy instrument is dedicated to the study of dynamics in condensed matter systems using the unique coherence properties of free-electron lasers. It covers a photon energy range of 4–25 keV. The intrinsic temporal characteristics of the Linac Coherent Light Source, in particular the 120 Hz repetition rate, allow for the investigation of slow dynamics (milliseconds) by means of X-ray photon correlation spectroscopy. Double-pulse schemes could probe dynamics on the picosecond timescale. In addition, a description of the instrument capabilities and recent achievements is presented.

  14. The X-ray correlation spectroscopy instrument at the Linac Coherent Light Source

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Alonso-Mori, Roberto; Caronna, Chiara; Chollet, Matthieu; Curtis, Robin; Damiani, Daniel S.; Defever, Jim; Feng, Yiping; Flath, Daniel L.; Glownia, James M.; Lee, Sooheyong; et al

    2015-03-03

    The X-ray Correlation Spectroscopy instrument is dedicated to the study of dynamics in condensed matter systems using the unique coherence properties of free-electron lasers. It covers a photon energy range of 4–25 keV. The intrinsic temporal characteristics of the Linac Coherent Light Source, in particular the 120 Hz repetition rate, allow for the investigation of slow dynamics (milliseconds) by means of X-ray photon correlation spectroscopy. Double-pulse schemes could probe dynamics on the picosecond timescale. In addition, a description of the instrument capabilities and recent achievements is presented.

  15. High-order multilayer coated blazed gratings for high resolution soft x-ray spectroscopy

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Voronov, Dmitriy L.; Goray, Leonid I.; Warwick, Tony; Yashchuk, Valeriy V.; Padmore, Howard A.

    2015-02-17

    A grand challenge in soft x-ray spectroscopy is to drive the resolving power of monochromators and spectrometers from the 104 achieved routinely today to well above 105. This need is driven mainly by the requirements of a new technique that is set to have enormous impact in condensed matter physics, Resonant Inelastic X-ray Scattering (RIXS). Unlike x-ray absorption spectroscopy, RIXS is not limited by an energy resolution dictated by the core-hole lifetime in the excitation process. Using much higher resolving power than used for normal x-ray absorption spectroscopy enables access to the energy scale of soft excitations in matter. Thesemoreexcitations such as magnons and phonons drive the collective phenomena seen in correlated electronic materials such as high temperature superconductors. RIXS opens a new path to study these excitations at a level of detail not formerly possible. However, as the process involves resonant excitation at an energy of around 1 keV, and the energy scale of the excitations one would like to see are at the meV level, to fully utilize the technique requires the development of monochromators and spectrometers with one to two orders of magnitude higher energy resolution than has been conventionally possible. Here we investigate the detailed diffraction characteristics of multilayer blazed gratings. These elements offer potentially revolutionary performance as the dispersive element in ultra-high resolution x-ray spectroscopy. In doing so, we have established a roadmap for the complete optimization of the grating design. Traditionally 1st order gratings are used in the soft x-ray region, but we show that as in the optical domain, one can work in very high spectral orders and thus dramatically improve resolution without significant loss in efficiency.less

  16. High-Resolution Structure of the Photosynthetic Mn4Ca Catalyst from X-ray Spectroscopy

    SciTech Connect (OSTI)

    Yachandra, Vittal; Yano, Junko; Kern, Jan; Pushkar, Yulia; Sauer, Kenneth; Glatzel, Pieter; Bergmann, Uwe; Messinger, Johannes; Zouni, Athina; Yachandra, Vittal K.

    2007-08-01

    The application of high-resolution X-ray spectroscopy methods to study the photosynthetic water oxidizing complex, which contains a unique hetero-nuclear catalytic Mn4Ca cluster, are described. Issues of X-ray damage especially at the metal sites in the Mn4Ca cluster are discussed. The structure of the Mn4Ca catalyst at high-resolution which has so far eluded attempts of determination by X-ray diffraction, EXAFS and other spectroscopic techniques has been addressed using polarized EXAFS techniques applied to oriented PS II membrane preparations and PS II single crystals. A review of how the resolution of traditional EXAFS techniques can be improved, using methods such as range-extended EXAFS is presented, and the changes that occur in the structure of the cluster as it advances through the catalytic cycle are described. X-ray absorption and emission techniques (XANES and K? emission) have been used earlier to determine the oxidation states of the Mn4Ca cluster, and in this report we review the use of X-ray resonant Raman spectroscopy to understand the electronic structure of the Mn4Ca cluster as it cycles through the intermediate S-states.

  17. Passive Spectroscopy Bolometers, Grating- And X-Ray Imaging Crystal Spectrometers

    SciTech Connect (OSTI)

    Bitter, M; Hill, K W; Scott, S; Paul, S; Ince-Cushmann, A; Reinke, M; Rice, J; Beiersdorfer, P; Gu, M F; Lee, S G; Broennimann, C; Eikenberry, E F

    2007-11-07

    This tutorial gives a brief introduction into passive spectroscopy and describes the working principles of bolometers, a high-resolution grating spectrometer, and a novel X-ray imaging crystal spectrometer, which is of particular interest for profile measurements of the ion temperature and plasma rotation velocity on ITER and future burning plasma experiments.

  18. In Situ Diffuse Reflectance IR Spectroscopy and X-ray Absorption Spectroscopy for Fast Catalytic Processes

    SciTech Connect (OSTI)

    N Marinkovic; Q Wang; A Frenkel

    2011-12-31

    A new instrument for synchronous in situ investigations of catalytic materials by IR and X-ray absorption spectroscopies was designed and built at the X18A beamline of the National Synchrotron Light Source of Brookhaven National Laboratory. It provides analytical tools for solving structural, electronic and kinetic problems in catalysis science by two complementary methods. Among the features attractive for catalysis research are the broad range of catalytically active elements that can be investigated (starting with Ni and beyond), the wide range of reaction conditions (temperatures up to 873 K, various reactive gases) and time scales (starting from tens of seconds). The results of several representative experiments that illustrate the attractive capabilities of the new set-up are discussed.

  19. Sequential single shot X-ray photon correlation spectroscopy at the SACLA free electron laser

    SciTech Connect (OSTI)

    Lehmkühler, Felix; Kwaśniewski, Paweł; Roseker, Wojciech; Fischer, Birgit; Schroer, Martin A.; Tono, Kensuke; Katayama, Tetsuo; Sprung, Michael; Sikorski, Marcin; Song, Sanghoon; Glownia, James; Chollet, Matthieu; Nelson, Silke; Robert, Aymeric; Gutt, Christian; Yabashi, Makina; Ishikawa, Tetsuya; Grübel, Gerhard

    2015-11-27

    In this study, hard X-ray free electron lasers allow for the first time to access dynamics of condensed matter samples ranging from femtoseconds to several hundred seconds. In particular, the exceptional large transverse coherence of the X-ray pulses and the high time-averaged flux promises to reach time and length scales that have not been accessible up to now with storage ring based sources. However, due to the fluctuations originating from the stochastic nature of the self-amplified spontaneous emission (SASE) process the application of well established techniques such as X-ray photon correlation spectroscopy (XPCS) is challenging. Here we demonstrate a single-shot based sequential XPCS study on a colloidal suspension with a relaxation time comparable to the SACLA free-electron laser pulse repetition rate. High quality correlation functions could be extracted without any indications for sample damage. This opens the way for systematic sequential XPCS experiments at FEL sources.

  20. Anion photoelectron spectroscopy of radicals and clusters

    SciTech Connect (OSTI)

    Travis, Taylor R.

    1999-12-16

    Anion photoelectron spectroscopy is used to study free radicals and clusters. The low-lying {sup 2}{Sigma} and {sup 2}{Pi} states of C{sub 2n}H (n = 1--4) have been studied. The anion photoelectron spectra yielded electron affinities, term values, and vibrational frequencies for these combustion and astrophysically relevant species. Photoelectron angular distributions allowed the author to correctly assign the electronic symmetry of the ground and first excited states and to assess the degree of vibronic coupling in C{sub 2}H and C{sub 4}H. Other radicals studied include NCN and I{sub 3}. The author was able to observe the low-lying singlet and triplet states of NCN for the first time. Measurement of the electron affinity of I{sub 3} revealed that it has a bound ground state and attachment of an argon atom to this moiety enabled him to resolve the symmetric stretching progression.

  1. High resolution x-ray fluorescence spectroscopy - a new technique for site- and spin-selectivity

    SciTech Connect (OSTI)

    Wang, Xin

    1996-12-01

    X-ray spectroscopy has long been used to elucidate electronic and structural information of molecules. One of the weaknesses of x-ray absorption is its sensitivity to all of the atoms of a particular element in a sample. Through out this thesis, a new technique for enhancing the site- and spin-selectivity of the x-ray absorption has been developed. By high resolution fluorescence detection, the chemical sensitivity of K emission spectra can be used to identify oxidation and spin states; it can also be used to facilitate site-selective X-ray Absorption Near Edge Structure (XANES) and site-selective Extended X-ray Absorption Fine Structure (EXAFS). The spin polarization in K fluorescence could be used to generate spin selective XANES or spin-polarized EXAFS, which provides a new measure of the spin density, or the nature of magnetic neighboring atoms. Finally, dramatic line-sharpening effects by the combination of absorption and emission processes allow observation of structure that is normally unobservable. All these unique characters can enormously simplify a complex x-ray spectrum. Applications of this novel technique have generated information from various transition-metal model compounds to metalloproteins. The absorption and emission spectra by high resolution fluorescence detection are interdependent. The ligand field multiplet model has been used for the analysis of K{alpha} and K{beta} emission spectra. First demonstration on different chemical states of Fe compounds has shown the applicability of site selectivity and spin polarization. Different interatomic distances of the same element in different chemical forms have been detected using site-selective EXAFS.

  2. ON RELATIVISTIC DISK SPECTROSCOPY IN COMPACT OBJECTS WITH X-RAY CCD CAMERAS

    SciTech Connect (OSTI)

    Miller, J. M.; Cackett, E. M. [Department of Astronomy, University of Michigan, 500 Church Street, Ann Arbor, MI 48109 (United States); D'Ai, A. [Dipartimento di Scienze Fisiche ed Astronomiche, Universita di Palermo, Palermo (Italy); Bautz, M. W.; Nowak, M. A. [Kavli Institute for Astrophysics and Space Research, MIT, 77 Massachusetts Avenue, Cambridge, MA 02139 (United States); Bhattacharyya, S. [Department of Astronomy and Astrophysics, Tata Institute of Fundamental Research, Mumbai 400005 (India); Burrows, D. N.; Kennea, J. [Department of Astronomy and Astrophysics, Pennsylvania State University, 525 Davey Lab, College Park, PA 16802 (United States); Fabian, A. C.; Reis, R. C. [Institute of Astronomy, University of Cambridge, Madingley Road, Cambridge, CB3 OHA (United Kingdom); Freyberg, M. J.; Haberl, F. [Max-Planck-Institut fuer extraterrestrische Physik, Giessenbachstrasse, 85748 Garching (Germany); Strohmayer, T. E. [Astrophysics Science Division, NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Tsujimoto, M., E-mail: jonmm@umich.ed [Japan Aerospace Exploration Agency, Institute of Space and Astronomical Sciences, 3-1-1 Yoshino-dai, Sagamihara, Kanagawa 229-8510 (Japan)

    2010-12-01

    X-ray charge-coupled devices (CCDs) are the workhorse detectors of modern X-ray astronomy. Typically covering the 0.3-10.0 keV energy range, CCDs are able to detect photoelectric absorption edges and K shell lines from most abundant metals. New CCDs also offer resolutions of 30-50 (E/{Delta}E), which is sufficient to detect lines in hot plasmas and to resolve many lines shaped by dynamical processes in accretion flows. The spectral capabilities of X-ray CCDs have been particularly important in detecting relativistic emission lines from the inner disks around accreting neutron stars and black holes. One drawback of X-ray CCDs is that spectra can be distorted by photon 'pile-up', wherein two or more photons may be registered as a single event during one frame time. We have conducted a large number of simulations using a statistical model of photon pile-up to assess its impacts on relativistic disk line and continuum spectra from stellar-mass black holes and neutron stars. The simulations cover the range of current X-ray CCD spectrometers and operational modes typically used to observe neutron stars and black holes in X-ray binaries. Our results suggest that severe photon pile-up acts to falsely narrow emission lines, leading to falsely large disk radii and falsely low spin values. In contrast, our simulations suggest that disk continua affected by severe pile-up are measured to have falsely low flux values, leading to falsely small radii and falsely high spin values. The results of these simulations and existing data appear to suggest that relativistic disk spectroscopy is generally robust against pile-up when this effect is modest.

  3. Multilayer graphene stacks grown by different methods-thickness measurements by X-ray diffraction, Raman spectroscopy and optical transmission

    SciTech Connect (OSTI)

    Tokarczyk, M. Kowalski, G.; Kępa, H.; Grodecki, K.; Drabińska, A.; Strupiński, W.

    2013-12-15

    X-ray diffraction, Raman spectroscopy and Optical absorption estimates of the thickness of graphene multi layer stacks (number of graphene layers) are presented for three different growth techniques. The objective of this work was focused on comparison and reconciliation of the two already widely used methods for thickness estimates (Raman and Absorption) with the calibration of the X-ray method as far as Scherer constant K is concerned and X-ray based Wagner-Aqua extrapolation method.

  4. 15.05.29 RH Operando X-ray - JCAP

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Direct Observation of a Semiconductor/Liquid Junction by Operando X-Ray Photoelectron Spectroscopy (XPS) Lichterman , M. F. et al. Direct Observation of the Energetics at a Semiconductor/Liquid Junction by Operando X-Ray Photoelectron Spectroscopy. Energy Environ. Sci ., 2015, DOI: 10.1039/C5EE01014D (2015). Scientific Achievement We demonstrated that the operando XPS technique, applied to a semiconductor/liquid junction, can directly measure the positions of the electronic states of the

  5. X ray photoelectron analysis of oxide-semiconductor interface after breakdown in Al{sub 2}O{sub 3}/InGaAs stacks

    SciTech Connect (OSTI)

    Shekhter, P.; Palumbo, F.; Cohen Weinfeld, K.; Eizenberg, M.

    2014-09-08

    In this work, the post-breakdown characteristics of metal gate/Al{sub 2}O{sub 3}/InGaAs structures were studied using surface analysis by x ray photoelectron spectroscopy. The results show that for dielectric breakdown under positive bias, localized filaments consisting of oxidized substrate atoms (In, Ga and As) were formed, while following breakdown under negative bias, a decrease of oxidized substrate atoms was observed. Such differences in the microstructure at the oxide-semiconductor interface after breakdown for positive and negative voltages are explained by atomic diffusion of the contact atoms into the gate dielectric in the region of the breakdown spot by the current induced electro-migration effect. These findings show a major difference between Al{sub 2}O{sub 3}/InGaAs and SiO{sub 2}/Si interfaces, opening the way to a better understanding of the breakdown characteristics of III-V complementary-metal-oxide-semiconductor technology.

  6. Applying Kβ Valence-to-Core X-ray Emission Spectroscopy to Cu(I) Binding

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Proteins with Relevance to Peptidylglycine Monooxygenase Reactivity | Stanford Synchrotron Radiation Lightsource Applying Kβ Valence-to-Core X-ray Emission Spectroscopy to Cu(I) Binding Proteins with Relevance to Peptidylglycine Monooxygenase Reactivity Thursday, June 30, 2016 Copper serves as a redox center in metalloproteins, often cycling between the +1 and +2 oxidation states. Oxidases, such as petidylglycine monooxygenase (PHM), bind oxygen at Cu(I) sites giving rise to "oxo"

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

    SciTech Connect (OSTI)

    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.

  8. Characterization of Gas Shales by X-ray Raman Spectroscopy | Stanford

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Synchrotron Radiation Lightsource Characterization of Gas Shales by X-ray Raman Spectroscopy Thursday, February 23, 2012 - 10:30am SSRL Third Floor Conference Room 137-322 Drew Pomerantz, Schlumberger Unconventional hydrocarbon resources such as gas shale and oil-bearing shale have emerged recently as economically viable sources of energy, dramatically altering America's energy landscape. Despite their importance, the basic chemistry and physics of shales are not understood as well as

  9. Characterization of Gas Shales by X-ray Raman Spectroscopy | Stanford

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Synchrotron Radiation Lightsource Characterization of Gas Shales by X-ray Raman Spectroscopy Monday, May 14, 2012 - 3:30pm SSRL Conference Room 137-322 Drew Pomerantz, Schlumberger Unconventional hydrocarbon resources such as gas shale and oil-bearing shale have emerged recently as economically viable sources of energy, dramatically altering America's energy landscape. Despite their importance, the basic chemistry and physics of shales are not understood as well as conventional reservoirs.

  10. Vertical dispersion methods in x-ray spectroscopy of high temperature plasmas

    SciTech Connect (OSTI)

    Renner, O.; Missalla, T.; Foerster, E.

    1995-12-31

    General formulae for the applying the vertical dispersion principle in x-ray spectroscopy of multiple charged ions are summarized, the characteristics of the experimental schemes based on flat and bent crystals are discussed. The unique properties of the novel spectroscopic methods, i.e., their extremely high dispersion, high spectral and 1-D spatial resolution and good collection efficiency, make them very attractive for ultrahigh-resolution spectroscopy. The examples of successful use of the vertical dispersion modifications of the double-crystal and the Johann spectrometer in diagnostics of several types of laser-generated plasma are presented.

  11. Note: Sample chamber for in situ x-ray absorption spectroscopy studies of battery materials

    SciTech Connect (OSTI)

    Pelliccione, CJ; Timofeeva, EV; Katsoudas, JP; Segre, CU

    2014-12-01

    In situ x-ray absorption spectroscopy (XAS) provides element-specific characterization of both crystalline and amorphous phases and enables direct correlations between electrochemical performance and structural characteristics of cathode and anode materials. In situ XAS measurements are very demanding to the design of the experimental setup. We have developed a sample chamber that provides electrical connectivity and inert atmosphere for operating electrochemical cells and also accounts for x-ray interactions with the chamber and cell materials. The design of the sample chamber for in situ measurements is presented along with example XAS spectra from anode materials in operating pouch cells at the Zn and Sn K-edges measured in fluorescence and transmission modes, respectively. (C) 2014 AIP Publishing LLC.

  12. Sequential single shot X-ray photon correlation spectroscopy at the SACLA free electron laser

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Lehmkühler, Felix; Kwaśniewski, Paweł; Roseker, Wojciech; Fischer, Birgit; Schroer, Martin A.; Tono, Kensuke; Katayama, Tetsuo; Sprung, Michael; Sikorski, Marcin; Song, Sanghoon; et al

    2015-11-27

    In this study, hard X-ray free electron lasers allow for the first time to access dynamics of condensed matter samples ranging from femtoseconds to several hundred seconds. In particular, the exceptional large transverse coherence of the X-ray pulses and the high time-averaged flux promises to reach time and length scales that have not been accessible up to now with storage ring based sources. However, due to the fluctuations originating from the stochastic nature of the self-amplified spontaneous emission (SASE) process the application of well established techniques such as X-ray photon correlation spectroscopy (XPCS) is challenging. Here we demonstrate a single-shotmore » based sequential XPCS study on a colloidal suspension with a relaxation time comparable to the SACLA free-electron laser pulse repetition rate. High quality correlation functions could be extracted without any indications for sample damage. This opens the way for systematic sequential XPCS experiments at FEL sources.« less

  13. New Homogeneous Standards by Atomic Layer Deposition for Synchrotron X-ray Fluorescence and Absorption Spectroscopies.

    SciTech Connect (OSTI)

    Butterworth, A.L.; Becker, N.; Gainsforth, Z.; Lanzirotti, A.; Newville, M.; Proslier, T.; Stodolna, J.; Sutton, S.; Tyliszczak, T.; Westphal, A.J.; Zasadzinski, J.

    2012-03-13

    Quantification of synchrotron XRF analyses is typically done through comparisons with measurements on the NIST SRM 1832/1833 thin film standards. Unfortunately, these standards are inhomogeneous on small scales at the tens of percent level. We are synthesizing new homogeneous multilayer standards using the Atomic Layer Deposition technique and characterizing them using multiple analytical methods, including ellipsometry, Rutherford Back Scattering at Evans Analytical, Synchrotron X-ray Fluorescence (SXRF) at Advanced Photon Source (APS) Beamline 13-ID, Synchrotron X-ray Absorption Spectroscopy (XAS) at Advanced Light Source (ALS) Beamlines 11.0.2 and 5.3.2.1 and by electron microscopy techniques. Our motivation for developing much-needed cross-calibration of synchrotron techniques is borne from coordinated analyses of particles captured in the aerogel of the NASA Stardust Interstellar Dust Collector (SIDC). The Stardust Interstellar Dust Preliminary Examination (ISPE) team have characterized three sub-nanogram, {approx}1{micro}m-sized fragments considered as candidates to be the first contemporary interstellar dust ever collected, based on their chemistries and trajectories. The candidates were analyzed in small wedges of aerogel in which they were extracted from the larger collector, using high sensitivity, high spatial resolution >3 keV synchrotron x-ray fluorescence spectroscopy (SXRF) and <2 keV synchrotron x-ray transmission microscopy (STXM) during Stardust ISPE. The ISPE synchrotron techniques have complementary capabilities. Hard X-ray SXRF is sensitive to sub-fg mass of elements Z {ge} 20 (calcium) and has a spatial resolution as low as 90nm. X-ray Diffraction data were collected simultaneously with SXRF data. Soft X-ray STXM at ALS beamline 11.0.2 can detect fg-mass of most elements, including cosmochemically important oxygen, magnesium, aluminum and silicon, which are invisible to SXRF in this application. ALS beamline 11.0.2 has spatial resolution

  14. X-ray Imaging Workshop

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    microscopy (PEEM), angle resolved photoemission spectroscopy (ARPES), coherent diffraction imaging, x-ray microscopy, micro-tomography, holographic imaging, and x-ray...

  15. High-Resolution Spectroscopy with the Chandra X-ray Observatory

    ScienceCinema (OSTI)

    Canizares, Claude R. [MIT, Cambridge, Massachusetts, United States

    2010-01-08

    The capabilities of the Chandra X-ray Observatory and XMM-Newton for high-resolution spectroscopy have brought tradition plasma diagnostic techniques to the study of cosmic plasma. Observations have probed nearly every class of astronomical object, from young proto-starts through massive O starts and black hole binaries, supernova remnants, active galactic nuclei, and the intergalactic medium. Many of these sources show remarkable rich spectra that reveal new physical information, such as emission measure distributions, elemental abundances, accretion disk and wind signatures, and time variability. This talk will present an overview of the Chandra instrumentaton and selected examples of spectral observations of astrophysical and cosmological importance.

  16. X-ray absorption spectroscopy studies of electrochemically deposited thin oxide films.

    SciTech Connect (OSTI)

    Balasubramanian, M.

    1998-06-02

    We have utilized ''in situ'' X-ray Absorption Fine Structure Spectroscopy to investigate the structure and composition of thin oxide films of nickel and iron that have been prepared by electrodeposition on a graphite substrate from aqueous solutions. The films are generally disordered. Structural information has been obtained from the analysis of the data. We also present initial findings on the local structure of heavy metal ions, e.g. Sr and Ce, incorporated into the electrodeposited nickel oxide films. Our results are of importance in a number of technological applications, among them, batteries, fuel cells, electrochromic and ferroelectric materials, corrosion protection, as well as environmental speciation and remediation.

  17. Slow dynamics of nanocomposite polymer aerogels as revealed by X-ray photocorrelation spectroscopy (XPCS)

    SciTech Connect (OSTI)

    Hernndez, Rebeca, E-mail: rhernandez@ictp.csic.es, E-mail: aurora.nogales@csic.es; Mijangos, Carmen [Instituto de Ciencia y Tecnologa de Polmeros, ICTP-CSIC, Juan de la Cierva, 3, 28006 Madrid (Spain)] [Instituto de Ciencia y Tecnologa de Polmeros, ICTP-CSIC, Juan de la Cierva, 3, 28006 Madrid (Spain); Nogales, Aurora, E-mail: rhernandez@ictp.csic.es, E-mail: aurora.nogales@csic.es; Ezquerra, Tiberio A. [Instituto de Estructura de la Materia, IEM-CSIC, Serrano 121, 28006 Madrid (Spain)] [Instituto de Estructura de la Materia, IEM-CSIC, Serrano 121, 28006 Madrid (Spain); Sprung, Michael [Petra III at DESY, Notkestr. 85, 22607 Hamburg (Germany)] [Petra III at DESY, Notkestr. 85, 22607 Hamburg (Germany)

    2014-01-14

    We report on a novel slow dynamics of polymer xerogels, aerogels, and nanocomposite aerogels with iron oxide nanoparticles, as revealed by X-ray photon correlation spectroscopy. The polymer aerogel and its nanocomposite aerogels, which are porous in nature, exhibit hyper-diffusive dynamics at room temperature. In contrast, non-porous polymer xerogels exhibit an absence of this peculiar dynamics. This slow dynamical process has been assigned to a relaxation of the characteristic porous structure of these materials and not to the presence of nanoparticles.

  18. Report on the Feasibility of Pu Photoelectron Spectroscopy with...

    Office of Scientific and Technical Information (OSTI)

    Report on the Feasibility of Pu Photoelectron Spectroscopy with Microscopic and Nanoscopic Samples at NSLSII Citation Details In-Document Search Title: Report on the Feasibility of ...

  19. Sample-morphology effects on x-ray photoelectron peak intensities. II. Estimation of detection limits for thin-film materials

    SciTech Connect (OSTI)

    Powell, Cedric J.; Werner, Wolfgang S. M.; Smekal, Werner

    2014-09-01

    The authors show that the National Institute of Standards and Technology database for the simulation of electron spectra for surface analysis (SESSA) can be used to determine detection limits for thin-film materials such as a thin film on a substrate or buried at varying depths in another material for common x-ray photoelectron spectroscopy (XPS) measurement conditions. Illustrative simulations were made for a W film on or in a Ru matrix and for a Ru film on or in a W matrix. In the former case, the thickness of a W film at a given depth in the Ru matrix was varied so that the intensity of the W 4d{sub 5/2} peak was essentially the same as that for a homogeneous RuW{sub 0.001} alloy. Similarly, the thickness of a Ru film at a selected depth in the W matrix was varied so that the intensity of the Ru 3p{sub 3/2} peak matched that from a homogeneous WRu{sub 0.01} alloy. These film thicknesses correspond to the detection limits of each minor component for measurement conditions where the detection limits for a homogeneous sample varied between 0.1 at.?% (for the RuW{sub 0.001} alloy) and 1 at.?% (for the WRu{sub 0.01} alloy). SESSA can be similarly used to convert estimates of XPS detection limits for a minor species in a homogeneous solid to the corresponding XPS detection limits for that species as a thin film on or buried in the chosen solid.

  20. Photoelectron spectroscopy of wet and gaseous samples through graphene membranes

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Kraus, Jürgen; Reichelt, Robert; Günther, Sebastian; Gregoratti, Luca; Amati, Matteo; Kiskinova, Maya; Yulaev, Alexander; Vlassiouk, Ivan V.; Kolmakov, Andrei

    2014-01-01

    Photoelectron spectroscopy (PES) and microscopy are highly important for exploring morphologically and chemically complex liquid–gas, solid–liquid and solid–gas interfaces under realistic conditions, but the very small electron mean free path inside dense media imposes serious experimental challenges. Currently, near ambient pressure PES is conducted using dexterously designed electron energy analyzers coupled with differentially pumped electron lenses which make it possible to conduct PES measurements at a few hPa. This report proposes an alternative ambient pressure approach that can be applied to a broad class of samples and be implemented in conventional PES instruments. It uses ultrathin electron transparent but molecularmore » impermeable membranes to isolate the high pressure sample environment from the high vacuum PES detection system. We show that the separating graphene membrane windows are both mechanically robust and sufficiently transparent for electrons in a wide energy range to allow soft X-ray PES of liquid and gaseous water. The performed proof-of-principle experiments confirm the possibility to probe vacuum-incompatible toxic or reactive samples placed inside such hermetic, gas flow or fluidic environmental cells.« less

  1. Americium characterization by X-ray fluorescence and absorption spectroscopy in plutonium uranium mixed oxide

    SciTech Connect (OSTI)

    Degueldre, Claude Cozzo, Cedric; Martin, Matthias; Grolimund, Daniel; Mieszczynski, Cyprian

    2013-06-01

    Plutonium uranium mixed oxide (MOX) fuels are currently used in nuclear reactors. The actinides in these fuels need to be analyzed after irradiation for assessing their behaviour with regard to their environment and the coolant. In this work the study of the atomic structure and next-neighbour environment of Am in the (Pu,U)O? lattice in an irradiated (60 MW d kg?) MOX sample was performed employing micro-X-ray fluorescence (-XRF) and micro-X-ray absorption fine structure (-XAFS) spectroscopy. The chemical bonds, valences and stoichiometry of Am (~0.66 wt%) are determined from the experimental data gained for the irradiated fuel material examined in its peripheral zone (rim) of the fuel. In the irradiated sample Am builds up as Am? species within an [AmO?]? coordination environment (e.g. >90%) and no (<10%) Am(IV) or (V) can be detected in the rim zone. The occurrence of americium dioxide is avoided by the redox buffering activity of the uranium dioxide matrix. - Graphical abstract: Americium LIII XAFS spectra recorded for the irradiated MOX sub-sample in the rim zone for a 300 ?m300 ?m beam size area investigated over six scans of 4 h. The records remain constant during multi-scan. The analysis of the XAFS signal shows that Am is found as trivalent in the UO? matrix. This analytical work shall open the door of very challenging analysis (speciation of fission product and actinides) in irradiated nuclear fuels. - Highlights: Americium was characterized by microX-ray absorption spectroscopy in irradiated MOX fuel. The americium redox state as determined from XAS data of irradiated fuel material was Am(III). In the sample, the Am? face an AmO??coordination environment in the (Pu,U)O? matrix. The americium dioxide is reduced by the uranium dioxide matrix.

  2. Core and Valence Excitations in Resonant X-ray Spectroscopy using Restricted Excitation Window Time-dependent Density Functional Theory

    SciTech Connect (OSTI)

    Zhang, Yu; Biggs, Jason D.; Healion, Daniel; Govind, Niranjan; Mukamel, Shaul

    2012-11-21

    We report simulations of X-ray absorption near edge structure (XANES), resonant inelastic X-ray scattering (RIXS) and 1D stimulated X-ray Raman spectroscopy (SXRS) signals of cysteine at the oxygen, nitrogen and sulfur K and L2,3 edges. The simulated XANES signals from the restricted window time-dependent density functional theory (REW-TDDFT) and the static exchange (STEX) method are compared with experiments, showing that REW-TDDFT is more accurate and computationally less expensive than STEX. Simulated RIXS and 1D SXRS signals from REW-TDDFT give some insights on the correlation of different excitations in the molecule.

  3. Correlated Single-Crystal Electronic Absorption Spectroscopy and X-ray Crystallography at NSLS Beamline X26-C

    SciTech Connect (OSTI)

    A Orville; R Buono; M Cowan; A Heroux; G Shea-McCarthy; D Schneider; J Skinner; M Skinner; D Stoner-Ma; R Sweet

    2011-12-31

    The research philosophy and new capabilities installed at NSLS beamline X26-C to support electronic absorption and Raman spectroscopies coupled with X-ray diffraction are reviewed. This beamline is dedicated full time to multidisciplinary studies with goals that include revealing the relationship between the electronic and atomic structures in macromolecules. The beamline instrumentation has been fully integrated such that optical absorption spectra and X-ray diffraction images are interlaced. Therefore, optical changes induced by X-ray exposure can be correlated with X-ray diffraction data collection. The installation of Raman spectroscopy into the beamline is also briefly reviewed. Data are now routinely generated almost simultaneously from three complementary types of experiments from the same sample. The beamline is available now to the NSLS general user population.

  4. Bimolecular reaction dynamics from photoelectron spectroscopy of negative ions

    SciTech Connect (OSTI)

    Bradforth, S.E.

    1992-11-01

    The transition state region of a neutral bimolecular reaction may be experimentally investigated by photoelectron spectroscopy of an appropriate negative ion. The photoelectron spectrum provides information on the spectroscopy and dynamics of the short lived transition state and may be used to develop model potential energy surfaces that are semi-quantitative in this important region. The principles of bound [yields] bound negative ion photoelectron spectroscopy are illustrated by way of an example: a full analysis of the photoelectron bands of CN[sup [minus

  5. Photon-in photon-out hard X-ray spectroscopy at the Linac Coherent...

    Office of Scientific and Technical Information (OSTI)

    different source characteristics and its resulting impact on sample delivery, X-ray optics, X-ray detection and data acquisition. Here it is described how photon-in photon-out...

  6. A multi-channel monolithic Ge detector system for fluorescence x-ray absorption spectroscopy

    SciTech Connect (OSTI)

    Bucher, J.J.; Allen, P.G.; Edelstein, N.M.; Shuh, D.K.; Madden, N.W.; Cork, C.; Luke, P.; Pehl, D.; Malone, D.

    1995-03-01

    Construction and performance of a monolithic quad-pixel Ge detector for fluorescence x-ray absorption spectroscopy (XAS) at synchrotron radiation sources are described. The detector semiconductor element has an active surface area of 4.0 cm{sup 2} which is electrically separated into four 1.0 cm{sup 2} pixels, with little interfacial dead volume. Spatial response of the array shows that cross-talk between adjacent pixels is < 10% for 5.9 keV photons that fall within 0.5 mm of the pixel boundaries. The detector electronics system uses pre-amplifiers built at LBNL with commercial Tennelec Model TC 244 amplifiers. Using an {sup 55}Fe test source (MnK{sub {alpha}}, 5.9 keV), energy resolution of better than 200 eV is achieved with a 4 {mu}sec peaking time. At 0.5 {mu}sec peaking time, pulse pileup results in a 75% throughput efficiency for an incoming count rate of 100 kHz. Initial XAS fluoresncece measurements at the beamline 4 wiggler end stations at SSRL show that the detector system has several advantages over commercial x-ray spectrometers for low-concentration counting.

  7. Millisecond Kinetics of Nanocrystal Cation Exchange UsingMicrofluidic X-ray Absorption Spectroscopy

    SciTech Connect (OSTI)

    Chan, Emory M.; Marcus, Matthew A.; Fakra, Sirine; Elnaggar,Mariam S.; Mathies, Richard A.; Alivisatos, A. Paul

    2007-05-07

    We describe the use of a flow-focusing microfluidic reactorto measure the kinetics of theCdSe-to-Ag2Se nanocrystal cation exchangereaction using micro-X-ray absorption spectroscopy (mu XAS). The smallmicroreactor dimensions facilitate the millisecond mixing of CdSenanocrystal and Ag+ reactant solutions, and the transposition of thereaction time onto spatial coordinates enables the in situ observation ofthe millisecond reaction with mu XAS. XAS spectra show the progression ofCdSe nanocrystals to Ag2Se over the course of 100 ms without the presenceof long-lived intermediates. These results, along with supporting stoppedflow absorption experiments, suggest that this nanocrystal cationexchange reaction is highly efficient and provide insight into how thereaction progresses in individual particles. This experiment illustratesthe value and potential of in situ microfluidic X-ray synchrotrontechniques for detailed studies of the millisecond structuraltransformations of nanoparticles and other solution-phase reactions inwhich diffusive mixing initiates changes in local bond structures oroxidation states.

  8. Design of Molecular Solar Cells via Feedback from Soft X-ray Spectroscopy

    SciTech Connect (OSTI)

    Himpsel, Franz J.

    2015-06-12

    Spectroscopy with soft X-rays was used to develop new materials and novel designs for solar cells and artificial photosynthesis. In order to go beyond the widely-used trial-and-error approach of gradually improving a particular design, we started from the most general layout of a solar cell (or a photo-electrochemical device) and asked which classes of materials are promising for best performance. For example, the most general design of a solar cell consists of a light absorber, an electron donor, and an electron acceptor. These are characterized by four energy levels, which were measured by a combination of spectroscopic X-ray techniques. Tuning synchrotron radiation to the absorption edges of specific elements provided element- and bond-selectivity. The spectroscopic results were complemented by state-of-the-art calculations of the electronic states. These helped explaining the observed energy levels and the orbitals associated with them. The calculations were extended to a large class of materials (for example thousands of porphyrin dye complexes) in order to survey trends in the energy level structure. A few highlights serve as examples: 1) Organic molecules combining absorber, donor, and acceptor with atomic precision. 2) Exploration of highly p-doped diamond films as inert, transparent electron donors. 3) Surface-sensitive characterization of nanorod arrays used as photoanodes in water splitting. 4) Computational design of molecular complexes for efficient solar cells using two photons.

  9. X-ray Absorption Spectroscopy Beamline at the Siam Photon Laboratory

    SciTech Connect (OSTI)

    Klysubun, Wantana; Tarawarakarn, Pongjakr; Sombunchoo, Panidtha; Klinkhieo, Supat; Chaiprapa, Jitrin; Songsiriritthigul, Prayoon

    2007-01-19

    A bending magnet beamline has been constructed and commissioned for x-ray absorption spectroscopy (XAS) at the Siam Photon Laboratory. The photon energy is tunable from 1830 eV to 8000 eV using a Lemmonier-type, fixed-exit double crystal monochromator equipped with InSb(111), Si(111), Ge(220) crystals. Elemental K-edges are then accessible from silicon to iron. A series of low conductance vacuum tubes has been designed and installed between the pumping chambers in the front end to obtain the proper pressure difference between the upstream and the downstream of the front end. Thus lower-energy photons, around K-edges of silicon, phosphorous, and sulfur, can be delivered to the experimental XAS station without being absorbed by a window. In this report, the design of the beamline is described. The commissioning results including the measured photon flux at sample and experimental XAS spectra are presented.

  10. Local electronic states of Fe{sub 4}N films revealed by x-ray absorption spectroscopy and x-ray magnetic circular dichroism

    SciTech Connect (OSTI)

    Ito, Keita; Toko, Kaoru; Suemasu, Takashi; Takeda, Yukiharu; Saitoh, Yuji; Oguchi, Tamio; Kimura, Akio

    2015-05-21

    We performed x-ray absorption spectroscopy (XAS) and x-ray magnetic circular dichroism (XMCD) measurements at Fe L{sub 2,3} and N K-edges for Fe{sub 4}N epitaxial films grown by molecular beam epitaxy. In order to clarify the element specific local electronic structure of Fe{sub 4}N, we compared experimentally obtained XAS and XMCD spectra with those simulated by a combination of a first-principles calculation and Fermi's golden rule. We revealed that the shoulders observed at Fe L{sub 2,3}-edges in the XAS and XMCD spectra were due to the electric dipole transition from the Fe 2p core-level to the hybridization state generated by ?* anti-bonding between the orbitals of N 2p at the body-centered site and Fe 3d on the face-centered (II) sites. Thus, the observed shoulders were attributed to the local electronic structure of Fe atoms at II sites. As to the N K-edge, the line shape of the obtained spectra was explained by the dipole transition from the N 1s core-level to the hybridization state formed by ?* and ?* anti-bondings between the Fe 3d and N 2p orbitals. This hybridization plays an important role in featuring the electronic structures and physical properties of Fe{sub 4}N.

  11. High Pressure Scanning Tunneling Microscopy and High PressureX-ray Photoemission Spectroscopy Studies of Adsorbate Structure,Composition and Mobility during Catalytic Reactions on A Model SingleCrystal

    SciTech Connect (OSTI)

    Montano, M.O.

    2006-05-12

    Our research focuses on taking advantage of the ability of scanning tunneling microscopy (STM) to operate at high-temperatures and high-pressures while still providing real-time atomic resolution images. We also utilize high-pressure x-ray photoelectron spectroscopy (HPXPS) to monitor systems under identical conditions thus giving us chemical information to compare and contrast with the structural and dynamic data provided by STM.

  12. Zero kinetic energy photoelectron spectroscopy of triphenylene

    SciTech Connect (OSTI)

    Harthcock, Colin; Zhang, Jie; Kong, Wei

    2014-06-28

    We report vibrational information of both the first electronically excited state and the ground cationic state of jet-cooled triphenylene via the techniques of resonantly enhanced multiphoton ionization (REMPI) and zero kinetic energy (ZEKE) photoelectron spectroscopy. The first excited electronic state S{sub 1} of the neutral molecule is of A{sub 1}? symmetry and is therefore electric dipole forbidden in the D{sub 3h} group. Consequently, there are no observable Franck-Condon allowed totally symmetric a{sub 1}? vibrational bands in the REMPI spectrum. All observed vibrational transitions are due to Herzberg-Teller vibronic coupling to the E? third electronically excited state S{sub 3}. The assignment of all vibrational bands as e? symmetry is based on comparisons with calculations using the time dependent density functional theory and spectroscopic simulations. When an electron is eliminated, the molecular frame undergoes Jahn-Teller distortion, lowering the point group to C{sub 2v} and resulting in two nearly degenerate electronic states of A{sub 2} and B{sub 1} symmetry. Here we follow a crude treatment by assuming that all e? vibrational modes resolve into b{sub 2} and a{sub 1} modes in the C{sub 2v} molecular frame. Some observed ZEKE transitions are tentatively assigned, and the adiabatic ionization threshold is determined to be 63?365 7 cm{sup ?1}. The observed ZEKE spectra contain a consistent pattern, with a cluster of transitions centered near the same vibrational level of the cation as that of the intermediate state, roughly consistent with the propensity rule. However, complete assignment of the detailed vibrational structure due to Jahn-Teller coupling requires much more extensive calculations, which will be performed in the future.

  13. THREE NEW GALACTIC CENTER X-RAY SOURCES IDENTIFIED WITH NEAR-INFRARED SPECTROSCOPY

    SciTech Connect (OSTI)

    DeWitt, Curtis; Bandyopadhyay, Reba M.; Eikenberry, Stephen S.; Sarajedini, Ata; Sellgren, Kris; Blum, Robert; Olsen, Knut; Bauer, Franz E.

    2013-11-01

    We have conducted a near-infrared spectroscopic survey of 47 candidate counterparts to X-ray sources discovered by the Chandra X-Ray Observatory near the Galactic center (GC). Though a significant number of these astrometric matches are likely to be spurious, we sought out spectral characteristics of active stars and interacting binaries, such as hot, massive spectral types or emission lines, in order to corroborate the X-ray activity and certify the authenticity of the match. We present three new spectroscopic identifications, including a Be high-mass X-ray binary (HMXB) or a ? Cassiopeiae (Cas) system, a symbiotic X-ray binary, and an O-type star of unknown luminosity class. The Be HMXB/? Cas system and the symbiotic X-ray binary are the first of their classes to be spectroscopically identified in the GC region.

  14. Simulating Cl K-edge X-ray absorption spectroscopy in MCl62-...

    Office of Scientific and Technical Information (OSTI)

    using time-dependent density functional theory Citation Details In-Document Search ... using time-dependent density functional theory We report simulations of the X-ray ...

  15. Core and Valence Excitations in Resonant X-ray Spectroscopy using...

    Office of Scientific and Technical Information (OSTI)

    Window Time-dependent Density Functional Theory Citation Details In-Document Search ... Window Time-dependent Density Functional Theory We report simulations of X-ray absorption ...

  16. X-ray absorption spectroscopy of Mn doped ZnO thin films prepared by rf sputtering technique

    SciTech Connect (OSTI)

    Yadav, Ashok Kumar; Jha, S. N.; Bhattacharyya, D.; Haque, Sk Maidul; Shukla, Dinesh; Choudhary, Ram Janay

    2015-11-15

    A set of r.f. sputter deposited ZnO thin films prepared with different Mn doping concentrations have been characterised by Extended X-ray Absorption Fine Structure (EXAFS) and X-ray Absorption Near Edge Spectroscopy (XANES) measurements at Zn, Mn and O K edges and at Mn L{sub 2,3} edges apart from long range structural characterisation by Grazing Incident X-ray Diffraction (GIXRD) technique. Magnetic measurements show room temperature ferromagnetism in samples with lower Mn doping which is however, gets destroyed at higher Mn doping concentration. The results of the magnetic measurements have been explained using the local structure information obtained from EXAFS and XANES measurements.

  17. Experimental station for laser-based picosecond time-resolved x-ray absorption near-edge spectroscopy

    SciTech Connect (OSTI)

    Dorchies, F. Fedorov, N.; Lecherbourg, L.

    2015-07-15

    We present an experimental station designed for time-resolved X-ray Absorption Near-Edge Spectroscopy (XANES). It is based on ultrashort laser-plasma x-ray pulses generated from a table-top 100 mJ-class laser at 10 Hz repetition rate. A high transmission (10%–20%) x-ray beam line transport using polycapillary optics allows us to set the sample in an independent vacuum chamber, providing high flexibility over a wide spectral range from 0.5 up to 4 keV. Some XANES spectra are presented, demonstrating 1% noise level in only ∼1 mn and ∼100 cumulated laser shots. Time-resolved measurements are reported, indicating that the time resolution of the entire experimental station is 3.3 ± 0.6 ps rms.

  18. Photon-in photon-out hard X-ray spectroscopy at the Linac Coherent Light Source

    SciTech Connect (OSTI)

    Alonso-Mori, Roberto; Sokaras, Dimosthenis; Zhu, Diling; Kroll, Thomas; Chollet, Mathieu; Feng, Yiping; Glownia, James M.; Kern, Jan; Lemke, Henrik T.; Nordlund, Dennis; Robert, Aymeric; Sikorski, Marcin; Song, Sanghoon; Weng, Tsu -Chien; Bergmann, Uwe

    2015-04-15

    X-ray free-electron lasers (FELs) have opened unprecedented possibilities to study the structure and dynamics of matter at an atomic level and ultra-fast timescale. Many of the techniques routinely used at storage ring facilities are being adapted for experiments conducted at FELs. In order to take full advantage of these new sources several challenges have to be overcome. They are related to the very different source characteristics and its resulting impact on sample delivery, X-ray optics, X-ray detection and data acquisition. Here it is described how photon-in photon-out hard X-ray spectroscopy techniques can be applied to study the electronic structure and its dynamics of transition metal systems with ultra-bright and ultra-short FEL X-ray pulses. In particular, some of the experimental details that are different compared with synchrotron-based setups are discussed and illustrated by recent measurements performed at the Linac Coherent Light Source.

  19. Photon-in photon-out hard X-ray spectroscopy at the Linac Coherent Light Source

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Alonso-Mori, Roberto; Sokaras, Dimosthenis; Zhu, Diling; Kroll, Thomas; Chollet, Mathieu; Feng, Yiping; Glownia, James M.; Kern, Jan; Lemke, Henrik T.; Nordlund, Dennis; et al

    2015-04-15

    X-ray free-electron lasers (FELs) have opened unprecedented possibilities to study the structure and dynamics of matter at an atomic level and ultra-fast timescale. Many of the techniques routinely used at storage ring facilities are being adapted for experiments conducted at FELs. In order to take full advantage of these new sources several challenges have to be overcome. They are related to the very different source characteristics and its resulting impact on sample delivery, X-ray optics, X-ray detection and data acquisition. Here it is described how photon-in photon-out hard X-ray spectroscopy techniques can be applied to study the electronic structure andmore » its dynamics of transition metal systems with ultra-bright and ultra-short FEL X-ray pulses. In particular, some of the experimental details that are different compared with synchrotron-based setups are discussed and illustrated by recent measurements performed at the Linac Coherent Light Source.« less

  20. Slow dynamics in an azopolymer molecular layer studied by x-ray photon correlation spectroscopy

    SciTech Connect (OSTI)

    Orsi, D.; Fluerasu, A.; Cristofolini, L.; Fontana, M.P.; Pontecorvo, E.; Caronna, C.; Zontone, F.; Madsen, A.

    2010-09-23

    We report the results of x-ray photon correlation spectroscopy (XPCS) experiments on multilayers of a photosensitive azo-polymer which can be softened by photoisomerization. Time correlation functions have been measured at different temperatures and momentum transfers (q) and under different illumination conditions (dark, UV or visible). The correlation functions are well described by the Kohlrausch-Williams-Watts (KWW) form with relaxation times that are proportional to q{sup -1}. The characteristic relaxation times follow the same Vogel-Fulcher-Tammann law describing the bulk viscosity of this polymer. The out-of-equilibrium relaxation dynamics following a UV photoperturbation are accelerated, which is in agreement with a fluidification effect previously measured by rheology. The transient dynamics are characterized by two times correlation function, and dynamical heterogeneity is evidenced by calculating the variance {chi} of the degree of correlation as a function of ageing time. A clear peak in {chi} appears at a well defined time {tau}{sub C} which scales with q{sup -1} and with the ageing time, in a similar fashion as previously reported in colloidal suspensions [O. Dauchot et al. Phys. Rev. Lett. 95 265701 (2005)]. From an accurate analysis of the correlation functions we could demonstrate a temperature and light dependent cross-over from compressed KWW to simple exponential behavior.

  1. Microscopic Dynamics in Nanocomposite Photosensitive Films Studies by X-ray Photon Correlation Spectroscopy

    SciTech Connect (OSTI)

    D Orsi; L Cristofolini; M Fontant; E Pontecorvo; C Caronna; A Fluerasu; F Zontone; A Madsen

    2011-12-31

    X-ray photon correlation spectroscopy measurements are reported of microscale dynamics in Langmuir-Schaeffer deposited multilayers of a photosensitive azopolymer with a low concentration of gold nanoparticles embedded. Correlation functions were measured as a function of exchanged momentum and illumination conditions (dark and UV light) and fitted with the Kohlrausch-Williams-Watts (KWW) exponential form. The microscopic dynamic of the nanoparticles was quantified, evidencing a non-Brownian superdiffusive behavior with relaxation times {tau} {approx} q{sup -1}, a result analogous to what previously had been observed in the pure azopolymer. Such behavior has been related to intermittent rearrangements or random dipolar interactions within an elastic medium. Photoperturbation with UV light makes the dynamics faster, in accordance with the reduction of the viscosity of the polymer found by shear rheology, but the KWW form of the correlation functions persists. At constant temperature, the dynamics of the nanoparticles embedded in the polymeric matrix is sensibly faster than the slow microscopic dynamic of the polymer. At the same time, the Vogel-Fulcher-Tammann law for the relaxation times indicates a less pronounced temperature dependence than for the pure polymer, resulting in a slightly lower activation temperature T{sub A}.

  2. X-ray Absorption Spectroscopy Characterization of a Li/S Cell

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Ye, Yifan; Kawase, Ayako; Song, Min-Kyu; Feng, Bingmei; Liu, Yi-Sheng; Marcus, Matthew A.; Feng, Jun; Cairns, Elton J.; Guo, Jinghua; Zhu, Junfa

    2016-01-11

    The X-ray absorption spectroscopy technique has been applied to study different stages of the lithium/sulfur (Li/S) cell life cycle. We investigated how speciation of S in Li/S cathodes changes upon the introduction of CTAB (cetyltrimethylammonium bromide, CH3(CH2)15N+(CH3)3Br₋) and with charge/discharge cycling. The introduction of CTAB changes the synthesis reaction pathway dramatically due to the interaction of CTAB with the terminal S atoms of the polysulfide ions in the Na2Sx solution. For the cycled Li/S cell, the loss of electrochemically active sulfur and the accumulation of a compact blocking insulating layer of unexpected sulfur reaction products on the cathode surface duringmore » the charge/discharge processes make the capacity decay. Lastly, a modified coin cell and a vacuum-compatible three-electrode electro-chemical cell have been introduced for further in-situ/in-operando studies.« less

  3. Bimolecular reaction dynamics from photoelectron spectroscopy of negative ions

    SciTech Connect (OSTI)

    Bradforth, S.E.

    1992-11-01

    The transition state region of a neutral bimolecular reaction may be experimentally investigated by photoelectron spectroscopy of an appropriate negative ion. The photoelectron spectrum provides information on the spectroscopy and dynamics of the short lived transition state and may be used to develop model potential energy surfaces that are semi-quantitative in this important region. The principles of bound {yields} bound negative ion photoelectron spectroscopy are illustrated by way of an example: a full analysis of the photoelectron bands of CN{sup {minus}}, NCO{sup {minus}} and NCS{sup {minus}}. Transition state photoelectron spectra are presented for the following systems Br + HI, Cl + HI, F + HI, F + CH{sub 3}0H,F + C{sub 2}H{sub 5}OH,F + OH and F + H{sub 2}. A time dependent framework for the simulation and interpretation of the bound {yields} free transition state photoelectron spectra is subsequently developed and applied to the hydrogen transfer reactions Br + HI, F + OH {yields} O({sup 3}P, {sup 1}D) + HF and F + H{sub 2}. The theoretical approach for the simulations is a fully quantum-mechanical wave packet propagation on a collinear model reaction potential surface. The connection between the wavepacket time evolution and the photoelectron spectrum is given by the time autocorrelation function. For the benchmark F + H{sub 2} system, comparisons with three-dimensional quantum calculations are made.

  4. Photoelectron spectrometer for attosecond spectroscopy of liquids and gases

    SciTech Connect (OSTI)

    Jordan, I.; Huppert, M.; Wörner, H. J.; Brown, M. A.; Bokhoven, J. A. van

    2015-12-15

    A new apparatus for attosecond time-resolved photoelectron spectroscopy of liquids and gases is described. It combines a liquid microjet source with a magnetic-bottle photoelectron spectrometer and an actively stabilized attosecond beamline. The photoelectron spectrometer permits venting and pumping of the interaction chamber without affecting the low pressure in the flight tube. This pressure separation has been realized through a sliding skimmer plate, which effectively seals the flight tube in its closed position and functions as a differential pumping stage in its open position. A high-harmonic photon spectrometer, attached to the photoelectron spectrometer, exit port is used to acquire photon spectra for calibration purposes. Attosecond pulse trains have been used to record photoelectron spectra of noble gases, water in the gas and liquid states as well as solvated species. RABBIT scans demonstrate the attosecond resolution of this setup.

  5. Soft X-ray Spectroscopy Study of the Electronic Structure of Oxidized and Partially Oxidized Magnetite Nanoparticles

    SciTech Connect (OSTI)

    Gilbert, Benjamin; Katz, Jordan E.; Denlinger, Jonathan D.; Yin, Yadong; Falcone, Roger; Waychunas, Glenn A.

    2010-10-24

    The crystal structure of magnetite nanoparticles may be transformed to maghemite by complete oxidation, but under many relevant conditions the oxidation is partial, creating a mixed-valence material with structural and electronic properties that are poorly characterized. We used X-ray diffraction, Fe K-edge extended X-ray absorption fine structure (EXAFS) spectroscopy, and soft X-ray absorption and emission spectroscopy to characterize the products of oxidizing uncoated and oleic acid-coated magnetite nanoparticles in air. The oxidization of uncoated magnetite nanoparticles creates a material that is structurally and electronically indistinguishable from maghemite. By contrast, while oxidized oleic acid-coated nanoparticles are also structurally indistinguishable from maghemite, Fe L-edge spectroscopy revealed the presence of interior reduced iron sites even after a 2-year period. We used X-ray emission spectroscopy at the O K-edge to study the valence bands (VB) of the iron oxide nanoparticles, using resonant excitation to remove the contributions from oxygen atoms in the ligands and from low-energy excitations that obscured the VB edge. The bonding in all nanoparticles was typical of maghemite, with no detectable VB states introduced by the long-lived, reduced-iron sites in the oleic acid-coated sample. However, O K-edge absorption spectroscopy observed a 0.2 eV shift in the position of the lowest unoccupied states in the coated sample, indicating an increase in the semiconductor band gap relative to bulk stoichiometric maghemite that was also observed by optical absorption spectroscopy. The results show that the ferrous iron sites within ferric iron oxide nanoparticles coated by an organic ligand can persist under ambient conditions with no evidence of a distinct interior phase and can exert an effect on the global electronic and optical properties of the material. This phenomenon resembles the band gap enlargement caused by electron accumulation in the

  6. The X-ray correlation spectroscopy instrument at the Linac Coherent...

    Office of Scientific and Technical Information (OSTI)

    characteristics of the Linac Coherent Light Source, in particular the 120 Hz repetition rate, allow for the investigation of slow dynamics (milliseconds) by means of X-ray photon...

  7. Low-level determination of plutonium by gamma and L x-ray spectroscopy

    SciTech Connect (OSTI)

    Nitsche, H.; Gatti, R.C.; Lee, S.C.

    1991-04-01

    we have developed an analytical method for detection of {sup 239}Pu in aqueous samples at concentrations as low as 10{sup {minus}10} M. This nuclear counting technique utilizes the uranium L X-rays, which follow the alpha decay of plutonium. Because L X-rays are specific for the element and not for the individual isotopes, the isotopic composition of the plutonium sample must be known. The counting efficiency in the 11--23 keV range is determined from a plutonium standard, and the concentration of the sample is then calculated from the L X-ray count and the isotopic composition. The total L X-ray count is corrected for possible contributions from other radionuclides present as impurities by measuring the low-energy gamma spectrum for each contaminant to establish specific photon/X-ray ratios. The ratios are important when {sup 241}Pu and {sup 242}Pu are measured, because the respective decay chain members produce non-U L X-rays. This new method can replace the use of labor-intensive radiochemical separation techniques and elaborate activation methods for analysis of {sup 239}Pu in aqueous samples. It is also applicable for assaying plutonium in liquid wastes that pose possible hazards to the environment.

  8. Sample-morphology effects on x-ray photoelectron peak intensities. III. Simulated spectra of model core–shell nanoparticles

    SciTech Connect (OSTI)

    Powell, Cedric J.; Chudzicki, Maksymilian; Werner, Wolfgang S. M.; Smekal, Werner

    2015-09-15

    The National Institute of Standards and Technology database for the simulation of electron spectra for surface analysis has been used to simulate Cu 2p photoelectron spectra for four types of spherical copper–gold nanoparticles (NPs). These simulations were made to extend the work of Tougaard [J. Vac. Sci. Technol. A 14, 1415 (1996)] and of Powell et al. [J. Vac. Sci. Technol. A 31, 021402 (2013)] who performed similar simulations for four types of planar copper–gold films. The Cu 2p spectra for the NPs were compared and contrasted with analogous results for the planar films and the effects of elastic scattering were investigated. The new simulations were made for a monolayer of three types of Cu/Au core–shell NPs on a Si substrate: (1) an Au shell of variable thickness on a Cu core with diameters of 0.5, 1.0, 2.0, 5.0, and 10.0 nm; (2) a Cu shell of variable thickness on an Au core with diameters of 0.5, 1.0, 2.0, 5.0, and 10.0 nm; and (3) an Au shell of variable thickness on a 1 nm Cu shell on an Au core with diameters of 0.5, 1.0, 2.0, 5.0, and 10.0 nm. For these three morphologies, the outer-shell thickness was varied until the Cu 2p{sub 3/2} peak intensity was the same (within 2%) as that found in our previous work with planar Cu/Au morphologies. The authors also performed similar simulations for a monolayer of spherical NPs consisting of a CuAu{sub x} alloy (also on a Si substrate) with diameters of 0.5, 1.0, 2.0, 5.0, and 10.0 nm. In the latter simulations, the relative Au concentration (x) was varied to give the same Cu 2p{sub 3/2} peak intensity (within 2%) as that found previously. For each morphology, the authors performed simulations with elastic scattering switched on and off. The authors found that elastic-scattering effects were generally strong for the Cu-core/Au-shell and weak for the Au-core/Cu-shell NPs; intermediate elastic-scattering effects were found for the Au-core/Cu-shell/Au-shell NPs. The shell thicknesses required to give

  9. Synchrotron x-ray spectroscopy studies of valence and magnetic state in europium metal to extreme pressures

    SciTech Connect (OSTI)

    Bi, W.; Souza-Neto, N.M.; Haskel, D.; Fabbris, G.; Alp, E.E.; Zhao, J.; Hennig, R.G.; Abd-Elmeguid, M.M.; Meng, Y.; McCallum, Ralph W.; Dennis, Kevin; Schilling, J.S.

    2012-05-22

    In order to probe the changes in the valence state and magnetic properties of Eu metal under extreme pressure, x-ray absorption near-edge spectroscopy, x-ray magnetic circular dichroism, and synchrotron Mössbauer spectroscopy experiments were carried out. The Mössbauer isomer shift exhibits anomalous pressure dependence, passing through a maximum near 20 GPa. Density functional theory has been applied to give insight into the pressure-induced changes in both Eu's electronic structure and Mössbauer isomer shift. Contrary to previous reports, Eu is found to remain nearly divalent to the highest pressures reached (87 GPa) with magnetic order persisting to at least 50 GPa. These results should lead to a better understanding of the nature of the superconducting state found above 75 GPa and of the sequence of structural phase transitions observed to 92 GPa.

  10. Voltage-controlled magnetic anisotropy in Fe|MgO tunnel junctions studied by x-ray absorption spectroscopy

    SciTech Connect (OSTI)

    Miwa, Shinji Matsuda, Kensho; Tanaka, Kazuhito; Goto, Minori; Suzuki, Yoshishige; Kotani, Yoshinori; Nakamura, Tetsuya

    2015-10-19

    In this study, voltage-controlled magnetic anisotropy (VCMA) in Fe|MgO tunnel junctions was investigated via the magneto-optical Kerr effect, soft x-ray absorption spectroscopy, and magnetic circular dichroism spectroscopy. The Fe|MgO tunnel junctions showed enhanced perpendicular magnetic anisotropy under external negative voltage, which induced charge depletion at the Fe|MgO interface. Despite the application of voltages of opposite polarity, no trace of chemical reaction such as a redox reaction attributed to O{sup 2−} migration was detected in the x-ray absorption spectra of the Fe. The VCMA reported in the Fe|MgO-based magnetic tunnel junctions must therefore originate from phenomena associated with the purely electric effect, that is, surface electron doping and/or redistribution induced by an external electric field.

  11. Runaway electron energy measurement using hard x-ray spectroscopy in 'Damavand' tokamak

    SciTech Connect (OSTI)

    Rasouli, C.; Farahbod, A. H.; Rasouli, H.; Lamehi, M.; Iraji, D.; Akhtari, K.; Modarresi, H.

    2009-01-15

    Set of experiments has been developed to study existing runaway electrons in ''Damavand'' tokamak plasma upon characteristics of hard x-ray emissions produced by collision of the runaway electrons with the plasma particles and limiters. As a first step, spatial distribution of hard x-ray emissions on the equatorial plane of the torus was considered. Obtained spectra of hard x-ray emissions for different alignments of shielded detector indicate isotropic emissivity in the equatorial plane. This is in agreement with wide angle cone of bremsstrahlung radiations, deduced from the mean value of energy of the runaway electrons. The mean energy was calculated from the slope of the energy spectrum of hard x-ray photons. In the second stage in order to investigate time evolution of energy of the runaway electrons, similar technique were applied to obtain hard x-ray energy in every 3 ms intervals, from the beginning to the end of plasma. The mean energy of the runaway electrons increases during the ramp up phase and reaches its maximum between 3 and 9 ms after plasma formation. Also considering the time dependence of the counted photons in each energy range shows that energetic photons are emitted during the ramp up phase of the plasma current in Damavand tokamak.

  12. X-Ray Photoelectron Spectroscopy (XPS) Applied to Soot & What It Can Do for You

    Office of Energy Efficiency and Renewable Energy (EERE)

    Presentation given at DEER 2006, August 20-24, 2006, Detroit, Michigan. Sponsored by the U.S. DOE's EERE FreedomCar and Fuel Partnership and 21st Century Truck Programs.

  13. In-situ X-ray Photoelectron Spectroscopy of a Catalyst for Artificial...

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Artificial photosynthesis replicates this process to produce energy in the form of usable ... JCAP, a multi-institute research program and the largest U.S. Department of Energy (DOE) ...

  14. Observing heme doming in myoglobin with femtosecond X-ray absorption spectroscopy

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Levantino, M.; Lemke, H. T.; Schirò, G.; Glownia, M.; Cupane, A.; Cammarata, M.

    2015-07-01

    We report time-resolved X-ray absorption measurements after photolysis of carbonmonoxy myoglobin performed at the LCLS X-ray free electron laser with nearly 100 fs (FWHM) time resolution. Data at the Fe K-edge reveal that the photoinduced structural changes at the heme occur in two steps, with a faster (~70 fs) relaxation preceding a slower (~400 fs) one. We tentatively attribute the first relaxation to a structural rearrangement induced by photolysis involving essentially only the heme chromophore and the second relaxation to a residual Fe motion out of the heme plane that is coupled to the displacement of myoglobin F-helix.

  15. Towards simultaneous measurements of electronic and structural properties in ultra-fast x-ray free electron laser absorption spectroscopy experiments

    SciTech Connect (OSTI)

    Gaudin, J.; Fourment, C.; Cho, B. I.; Engelhorn, K.; Galtier, E.; Harmand, M.; Leguay, P. M.; Lee, H. J.; Nagler, B.; Nakatsutsumi, M.; Ozkan, C.; Strmer, M.; Toleikis, S.; Tschentscher, Th.; Heimann, P. A.; Dorchies, F.

    2014-04-17

    The rapidly growing ultrafast science with X-ray lasers unveils atomic scale processes with unprecedented time resolution bringing the so called molecular movie within reach. X-ray absorption spectroscopy is one of the most powerful x-ray techniques providing both local atomic order and electronic structure when coupled with ad-hoc theory. Collecting absorption spectra within few x-ray pulses is possible only in a dispersive setup. We demonstrate ultrafast time-resolved measurements of the LIII-edge x-ray absorption near-edge spectra of irreversibly laser excited Molybdenum using an average of only few x-ray pulses with a signal to noise ratio limited only by the saturation level of the detector. The simplicity of the experimental set-up makes this technique versatile and applicable for a wide range of pump-probe experiments, particularly in the case of non-reversible processes.

  16. Towards simultaneous measurements of electronic and structural properties in ultra-fast x-ray free electron laser absorption spectroscopy experiments

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Gaudin, J.; Fourment, C.; Cho, B. I.; Engelhorn, K.; Galtier, E.; Harmand, M.; Leguay, P. M.; Lee, H. J.; Nagler, B.; Nakatsutsumi, M.; et al

    2014-04-17

    The rapidly growing ultrafast science with X-ray lasers unveils atomic scale processes with unprecedented time resolution bringing the so called “molecular movie” within reach. X-ray absorption spectroscopy is one of the most powerful x-ray techniques providing both local atomic order and electronic structure when coupled with ad-hoc theory. Collecting absorption spectra within few x-ray pulses is possible only in a dispersive setup. We demonstrate ultrafast time-resolved measurements of the LIII-edge x-ray absorption near-edge spectra of irreversibly laser excited Molybdenum using an average of only few x-ray pulses with a signal to noise ratio limited only by the saturation level ofmore » the detector. The simplicity of the experimental set-up makes this technique versatile and applicable for a wide range of pump-probe experiments, particularly in the case of non-reversible processes.« less

  17. Ligand-field symmetry effects in Fe(II) polypyridyl compounds probed by transient X-ray absorption spectroscopy

    SciTech Connect (OSTI)

    Cho, Hana; Strader, Matthew L.; Hong, Kiryong; Jamula, Lindsey; Kim, Tae Kyu; Groot, Frank M. F. de; McCusker, James K.; Schoenlein, Robert W.; Huse, Nils

    2012-02-28

    Ultrafast excited-state evolution in polypyridyl FeII complexes are of fundamental interest for understanding the origins of the sub-ps spin-state changes that occur upon photoexcitation of this class of compounds as well as for the potential impact such ultrafast dynamics have on incorporation of these compounds in solar energy conversion schemes or switchable optical storage technologies. We have demonstrated that ground-state and, more importantly, ultrafast time-resolved x-ray absorption methods can offer unique insights into the interplay between electronic and geometric structure that underpin the photo-induced dynamics of this class of compounds. The present contribution examines in greater detail how the symmetry of the ligand field surrounding the metal ion can be probed using these x-ray techniques. In particular, we show that steady-state K-edge spectroscopy of the nearest-neighbour nitrogen atoms reveals the characteristic chemical environment of the respective ligands and suggests an interesting target for future charge-transfer femtosecond and attosecond spectroscopy in the x-ray water window.

  18. Effects of Plant Cell Wall Matrix Polysaccharides on Bacterial Cellulose Structure Studied with Vibrational Sum Frequency Generation Spectroscopy and X-ray Diffraction

    SciTech Connect (OSTI)

    Park, Yong Bum; Lee, Christopher M; Kafle, Kabindra; Park, Sunkyu; Cosgrove, Daniel; Kim, Seong H

    2014-07-14

    The crystallinity, allomorph content, and mesoscale ordering of cellulose produced by Gluconacetobacter xylinus cultured with different plant cell wall matrix polysaccharides were studied with vibrational sum frequency generation (SFG) spectroscopy and X-ray diffraction (XRD).

  19. Investigating inertial confinement fusion target fuel conditions through x-ray spectroscopy

    SciTech Connect (OSTI)

    Hansen, Stephanie B.

    2012-05-15

    Inertial confinement fusion (ICF) targets are designed to produce hot, dense fuel in a neutron-producing core that is surrounded by a shell of compressing material. The x-rays emitted from ICF plasmas can be analyzed to reveal details of the temperatures, densities, gradients, velocities, and mix characteristics of ICF targets. Such diagnostics are critical to understand the target performance and to improve the predictive power of simulation codes.

  20. New developments in micro-X-ray diffraction and X-ray absorption spectroscopy for high-pressure research at 16-BM-D at the Advanced Photon Source

    SciTech Connect (OSTI)

    Park, Changyong Popov, Dmitry; Ikuta, Daijo; Lin, Chuanlong; Kenney-Benson, Curtis; Rod, Eric; Bommannavar, Arunkumar; Shen, Guoyin

    2015-07-15

    The monochromator and focusing mirrors of the 16-BM-D beamline, which is dedicated to high-pressure research with micro-X-ray diffraction (micro-XRD) and X-ray absorption near edge structure (XANES) (6-45 keV) spectroscopy, have been recently upgraded. Monochromatic X-rays are selected by a Si (111) double-crystal monochromator operated in an artificial channel-cut mode and focused to 5 μm × 5 μm (FWHM) by table-top Kirkpatrick-Baez type mirrors located near the sample stage. The typical X-ray flux is ∼5 × 10{sup 8} photons/s at 30 keV. The instrumental resolution, Δq/q{sub max}, reaches to 2 × 10{sup −3} and is tunable through adjustments of the detector distance and X-ray energy. The setup is stable and reproducible, which allows versatile application to various types of experiments including resistive heating and cryogenic cooling as well as ambient temperature compression. Transmission XANES is readily combined with micro-XRD utilizing the fixed-exit feature of the monochromator, which allows combined XRD-XANES measurements at a given sample condition.

  1. Probing Reaction Dynamics of Transition-Metal Complexes in Solution via Time-Resolved X-ray Spectroscopy

    SciTech Connect (OSTI)

    Huse, Nils; Khalil, Munira; Kim, Tae Kyu; Smeigh, Amanda L.; Jamula, Lindsey; McCusker, James K.; Schoenlein, Robert W.

    2009-05-24

    We report measurements of the photo-induced Fe(II) spin crossover reaction dynamics in solution via time-resolved x-ray absorption spectroscopy. EXAFS measurements reveal that the iron?nitrogen bond lengthens by 0.21+-0.03 Angstrom in the high-spin transient excited state relative to the ground state. XANES measurements at the Fe L-edge show directly the influence of the structural change on the ligand-field splitting of the Fe(II) 3d orbitals associated with the spin transition.

  2. Probing the hydrogen-bond network of water via time-resolved soft x-ray spectroscopy

    SciTech Connect (OSTI)

    Huse, Nils; Wen, Haidan; Nordlund, Dennis; Szilagyi, Erzsi; Daranciang, Dan; Miller, Timothy A.; Nilsson, Anders; Schoenlein, Robert W.; Lindenberg, Aaron M.

    2009-04-24

    We report time-resolved studies of hydrogen bonding in liquid H2O, in response to direct excitation of the O-H stretch mode at 3 mu m, probed via soft x-ray absorption spectroscopy at the oxygen K-edge. This approach employs a newly developed nanofluidic cell for transient soft x-ray spectroscopy in liquid phase. Distinct changes in the near-edge spectral region (XANES) are observed, and are indicative of a transient temperature rise of 10K following transient laser excitation and rapid thermalization of vibrational energy. The rapid heating occurs at constant volume and the associated increase in internal pressure, estimated to be 8MPa, is manifest by distinct spectral changes that differ from those induced by temperature alone. We conclude that the near-edge spectral shape of the oxygen K-edge is a sensitive probe of internal pressure, opening new possibilities for testing the validity of water models and providing new insight into the nature of hydrogen bonding in water.

  3. X-ray Spectroscopy with Elliptical Crystals and Face-On Framing Cameras

    SciTech Connect (OSTI)

    Heeter, R; Emig, J; Fournier, K; Hansen, S; May, M; Young, B

    2004-04-16

    X-ray spectrometers using elliptically bent crystals have desirable properties for applications requiring broad spectral coverage, good spectral resolution, and minimized source broadening. Previous work used custom-positioned film or microchannel plate detectors. They find it is also useful and cost-effective to field elliptical crystals in existing snouts on the face-on gated microchannel plate framing cameras commonly used at many facilities. they numerically explored the full design space (spectral range and resolution) of elliptical crystals compatible with the new MSPEC multipurpose spectrometer snout. They have tested at the Omega laser an elliptical RAP crystal with 174 mm focal length, 0.9885 eccentricity, and 4.6 degree inclination, viewing from 1.0 to at least 1.7 keV with E/dE of 300-500. A slit (2x mag) images 3 mm sources with 70 um spatial resolution.

  4. X-ray spectroscopy with elliptical crystals and face-on framing cameras

    SciTech Connect (OSTI)

    Heeter, R.F.; Emig, J.A.; Fournier, K.B.; Hansen, S.B.; May, M.J.; Young, B.K.F.

    2004-10-01

    X-ray spectrometers using elliptically bent crystals have desirable properties for applications requiring broad spectral coverage, good spectral resolution, and minimized source broadening. Previous work used custom-positioned film or microchannel plate detectors. We find it is also useful and cost-effective to field elliptical crystals in existing snouts on the face-on gated microchannel plate framing cameras commonly used at many facilities. We numerically explored the full design space (spectral range and resolution) of elliptical crystals compatible with the new multipurpose spectrometer snout. We have tested at the Omega laser an elliptical rubidium acid phthalate crystal with 174 mm focal length, 0.9885 eccentricity, and 4.6 deg. inclination, viewing from 1.0 to at least 1.7 keV with spectral resolution E/dE of 300-500. A slit (2xmagnification) images 3 mm sources with 70 {mu}m spatial resolution.

  5. Auto-oligomerization and hydration of pyrrole revealed by x-ray absorption spectroscopy

    SciTech Connect (OSTI)

    Advanced Light Source; Schwartz, Craig P.; Uejio, Janel S.; Duffin, Andrew M.; England, Alice H.; Prendergast, David; Saykally, Richard J

    2009-05-29

    Near edge x-ray absorption fine structure (NEXAFS) spectra have been measured at the carbon and nitrogen K-edges of the prototypical aromatic molecule, pyrrole, both in the gas phase and when solvated in water, and compared with spectra simulated using a combination of classical molecular dynamics and first principles density functional theory in the excited state core hole approximation. The excellent agreement enabled detailed assignments. Pyrrole is highly reactive, particularly in water, and reaction products formed by the auto-oligomerization of pyrrole are identified. The solvated spectra have been measured at two different temperatures, indicating that the final states remain largely unaffected by both hydration and temperature. This is somewhat unexpected, since the nitrogen in pyrrole can donate a hydrogen bond to water.

  6. X-ray absorption spectroscopy on the calcium cofactor to the manganese cluster in photosynthetic oxygen evolution

    SciTech Connect (OSTI)

    Cinco, Roehl M.

    1999-12-16

    Along with Mn, calcium and chloride ions are necessary cofactors for oxygen evolution in Photosystem II (PS II). To further test and verify whether Ca is close to the Mn cluster, the authors substituted strontium for Ca and probed from the Sr point of view for any nearby Mn. The extended X-ray absorption fine structure (EXAFS) of Sr-reactivated PS II indicates major differences between the intact and NH{sub 2}OH-treated samples. In intact samples, the Fourier transform of the Sr EXAFS shows a Fourier peak that is missing in inactive samples. This peak II is best simulated by two Mn neighbors at a distance of 3.5 Angstrom, confirming the proximity of Ca (Sr) cofactor to the Mn cluster. In addition, polarized Sr EXAFS on oriented Sr-reactivated samples shows this peak II is dichroic: large magnitude at 10 degrees (angle between the PS II membrane normal and the x-ray electric field vector) and small at 80 degrees. Analysis of the dichroism yields the relative angle between the Sr-Mn vector and membrane normal (23 degrees {+-} 4 degrees), and the isotropic coordination number for these layered samples. X-ray absorption spectroscopy has also been employed to assess the degree of similarity between the manganese cluster in PS II and a family of synthetic manganese complexes containing the distorted cubane [Mn{sub 4}O{sub 3}X] core (X = benzoate, acetate, methoxide, hydroxide, azide, fluoride, chloride or bromide). In addition, Mn{sub 4}O{sub 3}Cl complexes containing three or six terminal Cl ligands at three of the Mn were included in this study. The EXAFS method detects the small changes in the core structures as X is varied in this series, and serves to exclude these distorted cubanes of C3v symmetry as a topological model for the Mn catalytic cluster. The sulfur K-edge x-ray absorption near-edge structure (XANES) spectra for the amino acids cysteine, methionine, their corresponding oxidized forms cystine and methionine sulfoxide, and glutathione show distinct

  7. In operando observation system for electrochemical reaction by soft X-ray absorption spectroscopy with potential modulation method

    SciTech Connect (OSTI)

    Nagasaka, Masanari Kosugi, Nobuhiro; Yuzawa, Hayato; Horigome, Toshio

    2014-10-15

    In order to investigate local structures of electrolytes in electrochemical reactions under the same scan rate as a typical value 100 mV/s in cyclic voltammetry (CV), we have developed an in operando observation system for electrochemical reactions by soft X-ray absorption spectroscopy (XAS) with a potential modulation method. XAS spectra of electrolytes are measured by using a transmission-type liquid flow cell with built-in electrodes. The electrode potential is swept with a scan rate of 100 mV/s at a fixed photon energy, and soft X-ray absorption coefficients at different potentials are measured at the same time. By repeating the potential modulation at each fixed photon energy, it is possible to measure XAS of electrochemical reaction at the same scan rate as in CV. We have demonstrated successful measurement of the Fe L-edge XAS spectra of aqueous iron sulfate solutions and of the change in valence of Fe ions at different potentials in the Fe redox reaction. The mechanism of these Fe redox processes is discussed by correlating the XAS results with those at different scan rates.

  8. X-ray and vibrational spectroscopy of manganese complexes relevant to the oxygen-evolving complex of photosynthesis

    SciTech Connect (OSTI)

    Visser, Hendrik

    2001-05-16

    Manganese model complexes, relevant to the oxygen-evolving complex (OEC) in photosynthesis, were studied with Mn K-edge X-ray absorption near-edge spectroscopy (XANES), Mn Kb X-ray emission spectroscopy (XES), and vibrational spectroscopy. A more detailed understanding was obtained of the influence of nuclearity, overall structure, oxidation state, and ligand environment of the Mn atoms on the spectra from these methods. This refined understanding is necessary for improving the interpretation of spectra of the OEC. Mn XANES and Kb XES were used to study a di-(mu)-oxo and a mono-(mu)-oxo di-nuclear Mn compound in the (III,III), (III,IV), and (IV,IV) oxidation states. XANES spectra show energy shifts of 0.8 - 2.2 eV for 1-electron oxidation-state changes and 0.4 - 1.8 eV for ligand-environment changes. The shifts observed for Mn XES spectra were approximately 0.21 eV for oxidation state-changes and only approximately 0.04 eV for ligand-environment changes. This indicates that Mn Kb XES i s more sensitive to the oxidation state and less sensitive to the ligand environment of the Mn atoms than XANES. These complimentary methods provide information about the oxidation state and the ligand environment of Mn atoms in model compounds and biological systems. A versatile spectroelectrochemical apparatus was designed to aid the interpretation of IR spectra of Mn compounds in different oxidation states. The design, based on an attenuated total reflection device, permits the study of a wide spectral range: 16,700 (600 nm) - 225

  9. Trace elemental analysis of school chalk using energy dispersive X-ray florescence spectroscopy (ED-XRF)

    SciTech Connect (OSTI)

    Maruthi, Y. A.; Das, N. Lakshmana; Ramprasad, S.; Ram, S. S.; Sudarshan, M.

    2015-08-28

    The present studies focus the quantitative analysis of elements in school chalk to ensure the safety of its use. The elements like Calcium (Ca), Aluminum (Al), Iron (Fe), Silicon (Si) and Chromium (Cr) were analyzed from settled chalk dust samples collected from five classrooms (CD-1) and also from another set of unused chalk samples collected from local market (CD-2) using Energy Dispersive X-Ray florescence(ED-XRF) spectroscopy. Presence of these elements in significant concentrations in school chalk confirmed that, it is an irritant and occupational hazard. It is suggested to use protective equipments like filtered mask for mouth, nose and chalk holders. This study also suggested using the advanced mode of techniques like Digital boards, marker boards and power point presentations to mitigate the occupational hazard for classroom chalk.

  10. Proceedings of the eighth international colloquium on ultraviolet and x-ray spectroscopy of astrophysical and laboratory plasmas (IAU colloquium 86)

    SciTech Connect (OSTI)

    Not Available

    1984-01-01

    This volume represents the Proceedings of the Eighth International Colloquium on Ultraviolet and X-Ray Spectroscopy of Astrophysical and Laboratory Plasmas. The aim of this series of colloquia has been to bring together workers in the fields of astrophysical spectroscopy, laboratory spectroscopy and atomic physics in order to exchange ideas and results on problems which are common to these different disciplines. In addition to the presented papers there was a poster paper session. (WRF)

  11. Local structure of Fe in Fe-doped misfit-layered calcium cobaltite: An X-ray absorption spectroscopy study

    SciTech Connect (OSTI)

    Prasoetsopha, Natkrita; Pinitsoontorn, Supree; Bootchanont, Atipong; Kidkhunthod, Pinit; Srepusharawoot, Pornjuk; Kamwanna, Teerasak; Amornkitbamrung, Vittaya; Kurosaki, Ken; Yamanaka, Shinsuke

    2013-08-15

    Polycrystalline Ca{sub 3}Co{sub 4?x}Fe{sub x}O{sub 9+?} ceramics (x=0, 0.01, 0.03, 0.05) were fabricated using a simple thermal hydro-decomposition method and a spark plasma sintering technique. Thermoelectric property measurements showed that increasing Fe concentration resulted in a decrease in electrical resistivity, thermopower and thermal conductivity, leading to an improvement in the dimensionless figure-of-merit, >35% for x=0.05 at 1073 K. An X-ray absorption spectroscopy technique was used to investigate the local structure of Fe ions in the Ca{sub 3}Co{sub 4?x}Fe{sub x}O{sub 9+?} structure for the first time. By fitting data from the extended X-ray absorption fine structure (EXAFS) spectra and analyzing the X-ray absorption near-edge structure (XANES) spectra incorporated with first principle simulation, it was shown that Fe was substituted for Co in the the Ca{sub 2}CoO{sub 3} (rocksalt, RS) layer rather than in the CoO{sub 2} layer. Variation in the thermoelectric properties as a function of Fe concentration was attributed to charge transfer between the CoO{sub 2} and the RS layers. The origin of the preferential Fe substitution site was investigated considering the ionic radii of Co and Fe and the total energy of the system. - Graphical abstract: The Fe K-edge XANES spectra of: (a) experimental result in comparison to the simulated spectra when Fe atoms were substituted in the RS layer; (b) with magnetic moment; (c) without magnetic moment, and in the CoO{sub 2} layer; (d) with magnetic moment and (e) without magnetic moment. Highlights: Synthesis, structural studies, and thermoelectric properties of Ca{sub 3}Co{sub 4?x}Fe{sub x}O{sub 9+?}. Direct evidence for the local structure of the Fe ions in the Ca{sub 3}Co{sub 4?x}Fe{sub x}O{sub 9+?} using XAS analysis. EXAFS and XANES analysis showed that Fe was likely to be situated in the RS layer structure. Changes in TE property with Fe content was due to charge transfer between the CoO{sub 2} and

  12. Determining Orientational Structure of Diamondoid Thiols Attached to Silver Using Near Edge X-ray Absorption Fine Structure Spectroscopy

    SciTech Connect (OSTI)

    Willey, T M; Lee, J I; Fabbri, J D; Wang, D; Nielsen, M; Randel, J C; Schreiner, P R; Fokin, A A; Tkachenko, B A; Fokina, N A; Dahl, J P; Carlson, R K; Terminello, L J; Melosh, N A; van Buuren, T

    2008-10-07

    Near-edge x-ray absorption fine structure spectroscopy (NEXAFS) is a powerful tool for determination of molecular orientation in self-assembled monolayers and other surface-attached molecules. A general framework for using NEXAFS to simultaneously determine molecular tilt and twist of rigid molecules attached to surfaces is presented. This framework is applied to self-assembled monolayers of higher diamondoid, hydrocarbon molecules with cubic-diamond-cage structures. Diamondoid monolayers chemisorbed on metal substrates are known to exhibit interesting electronic and surface properties. This work compares molecular orientation in monolayers prepared on silver substrates using two different thiol positional isomers of [121]tetramantane, and thiols derived from two different pentamantane structural isomers, [1212]pentamantane and [1(2,3)4]pentamantane. The observed differences in monolayer structure demonstrate the utility and limitations of NEXAFS spectroscopy and the framework. The results also demonstrate the ability to control diamondoid assembly, in particular the molecular orientational structure, providing a flexible platform for the modification of surface properties with this exciting new class of nanodiamond materials.

  13. An instrument for the investigation of actinides with spin resolved photoelectron spectroscopy and bremsstrahlung isochromat spectroscopy

    SciTech Connect (OSTI)

    Yu, S.-W.; Tobin, J. G.; Chung, B. W.

    2011-01-01

    A new system for spin resolved photoelectron spectroscopy and bremsstrahlung isochromat spectroscopy has been built and commissioned at Lawrence Livermore National Laboratory for the investigation of the electronic structure of the actinides.Actinide materials are very toxic and radioactive and therefore cannot be brought to most general user facilities for spectroscopic studies. The technical details of the new system and preliminary data obtained therein will be presented and discussed.

  14. Spatially resolved high-resolution x-ray spectroscopy of high-current plasma-focus discharges

    SciTech Connect (OSTI)

    ZajaPc, S.; Rzadkiewicz, J.; Scholz, M.; Paduch, M.; Zielinska, E.; Rosmej, O.; Yongtao, Zhao; Gojska, A.

    2010-10-15

    Soft x-ray emission from a Mather-type plasma-focus device (PF-1000) operated at {approx}400 kJ was measured. The high density and temperature plasma were generated by the discharge in the deuterium-argon gas mixture in the modified (high-current) plasma-focus configuration. A spherically bent mica crystal spectrograph viewing the axial output of the pinch region was used to measure the x-ray spectra. Spatially resolved spectra including the characteristic x-ray lines of highly ionized Ar and continua were recorded by means of an x-ray film. The x-ray emission of PF-1000 device was studied at different areas of the pinch.

  15. Simulating Valence-to-Core X-ray Emission Spectroscopy of Transition Metal Complexes with Time-Dependent Density Functional Theory

    SciTech Connect (OSTI)

    Zhang, Yu; Mukamel, Shaul; Khalil, Munira; Govind, Niranjan

    2015-11-09

    Valence-to-core (VtC) X-ray emission spectroscopy (XES) has emerged as a power- ful technique for the structural characterization of complex organometallic compounds in realistic environments. Since the spectrum represents electronic transitions from the ligand molecular orbitals to the core holes of the metal centers, the approach is more chemically sensitive to the metal-ligand bonding character compared with con- ventional X-ray absorption techniques. In this paper we study how linear-response time-dependent density functional theory (LR-TDDFT) can be harnessed to simulate K-edge VtC X-ray emission spectra reliably. LR-TDDFT allows one to go beyond the single-particle picture that has been extensively used to simulate VtC-XES. We con- sider seven low- and high-spin model complexes involving chromium, manganese and iron transition metal centers. Our results are in good agreement with experiment.

  16. An in situ sample environment reaction cell for spatially resolved x-ray absorption spectroscopy studies of powders and small structured reactors

    SciTech Connect (OSTI)

    Zhang, Chu; Gustafson, Johan; Merte, Lindsay R.; Evertsson, Jonas; Norén, Katarina; Carlson, Stefan; Svensson, Håkan; Carlsson, Per-Anders

    2015-03-15

    An easy-to-use sample environment reaction cell for X-ray based in situ studies of powders and small structured samples, e.g., powder, pellet, and monolith catalysts, is described. The design of the cell allows for flexible use of appropriate X-ray transparent windows, shielding the sample from ambient conditions, such that incident X-ray energies as low as 3 keV can be used. Thus, in situ X-ray absorption spectroscopy (XAS) measurements in either transmission or fluorescence mode are facilitated. Total gas flows up to about 500 ml{sub n}/min can be fed while the sample temperature is accurately controlled (at least) in the range of 25–500 °C. The gas feed is composed by a versatile gas-mixing system and the effluent gas flow composition is monitored with mass spectrometry (MS). These systems are described briefly. Results from simultaneous XAS/MS measurements during oxidation of carbon monoxide over a 4% Pt/Al{sub 2}O{sub 3} powder catalyst are used to illustrate the system performance in terms of transmission XAS. Also, 2.2% Pd/Al{sub 2}O{sub 3} and 2% Ag − Al{sub 2}O{sub 3} powder catalysts have been used to demonstrate X-ray absorption near-edge structure (XANES) spectroscopy in fluorescence mode. Further, a 2% Pt/Al{sub 2}O{sub 3} monolith catalyst was used ex situ for transmission XANES. The reaction cell opens for facile studies of structure-function relationships for model as well as realistic catalysts both in the form of powders, small pellets, and coated or extruded monoliths at near realistic conditions. The applicability of the cell for X-ray diffraction measurements is discussed.

  17. Probing the Electronic Structure of a Photoexcited Solar Cell Dye with Transient X-ray Absorption Spectroscopy

    SciTech Connect (OSTI)

    Kuiken, Benjamin E. Van; Huse, Nils; Cho, Hana; Strader, Matthew L.; Lynch, Michael S.; Schoenlein, Robert W.; Khalil, Munira

    2012-05-01

    This study uses transient X-ray absorption (XA) spectroscopy and timedependent density functional theory (TD-DFT) to directly visualize the charge density around the metal atom and the surrounding ligands following an ultrafast metal-to-ligand charge-transfer (MLCT) process in the widely used RuII solar cell dye, Ru(dcbpy)2(NCS)2 (termed N3). We measure the Ru L-edge XA spectra of the singlet ground (1A1) and the transient triplet (3MLCT) excited state of N34 and perform TD-DFT calculations of 2p core-level excitations, which identify a unique spectral signature of the electron density on the NCS ligands. We find that the Ru 2p, Ru eg, and NCS orbitals are stabilized by 2.0, 1.0, and 0.6 eV, respectively, in the transient 3MLCT state of the dye. These results highlight the role of the NCS ligands in governing the oxidation state of the Ru center.

  18. Determining copper and lead binding in Larrea tridentata through chemical modification and X-ray absorption spectroscopy

    SciTech Connect (OSTI)

    Polette, L.; Gardea-Torresdey, J.L.; Chianelli, R.; Pickering, I.J.; George, G.N.

    1997-12-31

    Metal contamination in soils has become a widespread problem. Emerging technologies, such as phytoremediation, may offer low cost cleanup methods. The authors have identified a desert plant, Larrea tridentata (creosote bush), which naturally grows and uptakes copper and lead from a contaminated area near a smelting operation. They determined, through chemical modification of carboxyl groups with methanol, that these functional groups may be responsible for a portion of copper(II) binding. In contrast, lead binding was minimally affected by modification of carboxyl groups. X-ray absorption spectroscopy studies conducted at Stanford Synchrotron Radiation Laboratory (SSRL) further support copper binding to oxygen-coordinated ligands and also imply that the binding is not solely due to phytochelatins. The EXAFS data indicate the presence of both Cu-O and Cu-S back scatters, no short Cu-Cu interactions, but with significant Cu-Cu back scattering at 3.7 {angstrom} (unlike phytochelatins with predominantly Cu-S coordination and short Cu-Cu interactions at 2.7 {angstrom}). Cu EXAFS of roots and leaves also vary depending on the level of heavy metal contamination in the environment from which the various creosote samples were obtained. In contrast, Pb XANES data of roots and leaves of creosote collected from different contaminated sites indicate no difference in valence states or ligand coordination.

  19. X-ray absorption spectroscopy of LiBF 4 in propylene carbonate. A model lithium ion battery electrolyte

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Smith, Jacob W.; Lam, Royce K.; Sheardy, Alex T.; Shih, Orion; Rizzuto, Anthony M.; Borodin, Oleg; Harris, Stephen J.; Prendergast, David; Saykally, Richard J.

    2014-08-20

    Since their introduction into the commercial marketplace in 1991, lithium ion batteries have become increasingly ubiquitous in portable technology. Nevertheless, improvements to existing battery technology are necessary to expand their utility for larger-scale applications, such as electric vehicles. Advances may be realized from improvements to the liquid electrolyte; however, current understanding of the liquid structure and properties remains incomplete. X-ray absorption spectroscopy of solutions of LiBF4 in propylene carbonate (PC), interpreted using first-principles electronic structure calculations within the eXcited electron and Core Hole (XCH) approximation, yields new insight into the solvation structure of the Li+ ion in this model electrolyte.more » By generating linear combinations of the computed spectra of Li+-associating and free PC molecules and comparing to the experimental spectrum, we find a Li+–solvent interaction number of 4.5. This result suggests that computational models of lithium ion battery electrolytes should move beyond tetrahedral coordination structures.« less

  20. Some new schemes for producing high-accuracy elliptical X-ray mirrors by elastic bending

    SciTech Connect (OSTI)

    Padmore, H.A.; Howells, M.R.; Irick, S.; Renner, T.; Sandler, R.; Koo, Y.-M.

    1996-08-01

    Although x-ray micro-foci can be produced by a variety of diffractive methods, grazing incidence mirrors are the only route to an achromatic focus. In this paper we describe our efforts to produce elliptically shaped mirrors with the very high figure accuracy necessary for producing a micro-focus. The motivation for this work is provided by the need to produce achromatic foci for a range of applications ranging from tunable micro-focus x-ray photoelectron spectroscopy ({mu}-XPS) at soft x-ray energies to micro-focus white beam x-ray diffraction ({mu}-XRD) at hard x-ray energies. We describe the methodology of beam bending, a practical example of a system we have produced for {mu}-XRD, and results demonstrating the production of a surface with micro-radian figure accuracy.

  1. High energy resolution five-crystal spectrometer for high quality fluorescence and absorption measurements on an x-ray absorption spectroscopy beamline

    SciTech Connect (OSTI)

    Llorens, Isabelle; Lahera, Eric; Delnet, William; Proux, Olivier; Dermigny, Quentin; Gelebart, Frederic; Morand, Marc; Shukla, Abhay; Bardou, Nathalie; Ulrich, Olivier; and others

    2012-06-15

    Fluorescence detection is classically achieved with a solid state detector (SSD) on x-ray absorption spectroscopy (XAS) beamlines. This kind of detection however presents some limitations related to the limited energy resolution and saturation. Crystal analyzer spectrometers (CAS) based on a Johann-type geometry have been developed to overcome these limitations. We have tested and installed such a system on the BM30B/CRG-FAME XAS beamline at the ESRF dedicated to the structural investigation of very dilute systems in environmental, material and biological sciences. The spectrometer has been designed to be a mobile device for easy integration in multi-purpose hard x-ray synchrotron beamlines or even with a laboratory x-ray source. The CAS allows to collect x-ray photons from a large solid angle with five spherically bent crystals. It will cover a large energy range allowing to probe fluorescence lines characteristic of all the elements from Ca (Z = 20) to U (Z = 92). It provides an energy resolution of 1-2 eV. XAS spectroscopy is the main application of this device even if other spectroscopic techniques (RIXS, XES, XRS, etc.) can be also achieved with it. The performances of the CAS are illustrated by two experiments that are difficult or impossible to perform with SSD and the complementarity of the CAS vs SSD detectors is discussed.

  2. X-ray polarization spectroscopy to study anisotropic velocity distribution of hot electrons produced by an ultra-high-intensity laser

    SciTech Connect (OSTI)

    Inubushi, Y.; Okano, Y.; Nishimura, H.; Cai, H.; Nagatomo, H.; Kai, T.; Fujioka, S.; Nakamura, T.; Johzaki, T.; Mima, K.; Kawamura, T.; Batani, D.; Morace, A.; Redaelli, R.; Fourment, C.; Santos, J. J.; Malka, G.

    2010-03-15

    The anisotropy of the hot-electron velocity distribution in ultra-high-intensity laser produced plasma was studied with x-ray polarization spectroscopy using multilayer planar targets including x-ray emission tracer in the middle layer. This measurement serves as a diagnostic for hot-electron transport from the laser-plasma interaction region to the overdense region where drastic changes in the isotropy of the electron velocity distribution are observed. These polarization degrees are consistent with analysis of a three-dimensional polarization spectroscopy model coupled with particle-in-cell simulations. Electron velocity distribution in the underdense region is affected by the electric field of the laser and that in the overdense region becomes wider with increase in the tracer depth. A full-angular spread in the overdense region of 22.4 deg.{sub -2.4}{sup +5.4} was obtained from the measured polarization degree.

  3. The Electron-Phonon Interaction as Studied by Photoelectron Spectroscopy

    SciTech Connect (OSTI)

    D.W. Lynch

    2004-09-30

    With recent advances in energy and angle resolution, the effects of electron-phonon interactions are manifest in many valence-band photoelectron spectra (PES) for states near the Fermi level in metals.

  4. An analytic model for the response of a CZT detector in diagnostic energy dispersive x-ray spectroscopy

    SciTech Connect (OSTI)

    LeClair, Robert J.; Wang Yinkun; Zhao Peiying; Boileau, Michel; Wang, Lilie; Fleurot, Fabrice [Department of Physics and Astronomy, Laurentian University, 935 Ramsey Lake Road, Sudbury, Ontario P3E 2C6 (Canada) and Biomolecular Sciences Program, Laurentian University, 935 Ramsey Lake Road, Sudbury, Ontario P3E 2C6 (Canada); Department of Physics and Astronomy, Laurentian University, 935 Ramsey Lake Road, Sudbury, Ontario P3E 2C6 (Canada)

    2006-05-15

    A CdZnTe detector (CZTD) can be very useful for measuring diagnostic x-ray spectra. The semiconductor detector does, however, exhibit poor hole transport properties and fluorescence generation upon atomic de-excitations. This article describes an analytic model to characterize these two phenomena that occur when a CZTD is exposed to diagnostic x rays. The analytical detector response functions compare well with those obtained via Monte Carlo calculations. The response functions were applied to 50, 80, and 110 kV x-ray spectra. Two 50 kV spectra were measured; one with no filtration and the other with 1.35 mm Al filtration. The unfiltered spectrum was numerically filtered with 1.35 mm of Al in order to see whether the recovered spectrum resembled the filtered spectrum actually measured. A deviation curve was obtained by subtracting one curve from the other on an energy bin by bin basis. The deviation pattern fluctuated around the zero line when corrections were applied to both spectra. Significant deviations from zero towards the lower energies were observed when the uncorrected spectra were used. Beside visual observations, the exposure obtained using the numerically attenuated unfiltered beam was compared to the exposure calculated with the actual filtered beam. The percent differences were 0.8% when corrections were applied and 25% for no corrections. The model can be used to correct diagnostic x-ray spectra measured with a CdZnTe detector.

  5. Single-Crystal Raman Spectroscopy and X-ray Crystallography at Beamline X26-C of the NSLS

    SciTech Connect (OSTI)

    D Stoner-Ma; J Skinner; D Schneider; M Cowan; R Sweet; A Orville

    2011-12-31

    Three-dimensional structures derived from X-ray diffraction of protein crystals provide a wealth of information. Features and interactions important for the function of macromolecules can be deduced and catalytic mechanisms postulated. Still, many questions can remain, for example regarding metal oxidation states and the interpretation of 'mystery density', i.e. ambiguous or unknown features within the electron density maps, especially at {approx}2 {angstrom} resolutions typical of most macromolecular structures. Beamline X26-C at the National Synchrotron Light Source (NSLS), Brookhaven National Laboratory (BNL), provides researchers with the opportunity to not only determine the atomic structure of their samples but also to explore the electronic and vibrational characteristics of the sample before, during and after X-ray diffraction data collection. When samples are maintained under cryo-conditions, an opportunity to promote and follow photochemical reactions in situ as a function of X-ray exposure is also provided. Plans are in place to further expand the capabilities at beamline X26-C and to develop beamlines at NSLS-II, currently under construction at BNL, which will provide users access to a wide array of complementary spectroscopic methods in addition to high-quality X-ray diffraction data.

  6. NuSTAR study of hard X-ray morphology and spectroscopy of PWN G21.50.9

    SciTech Connect (OSTI)

    Nynka, Melania; Hailey, Charles J.; Gotthelf, Eric V.; Mori, Kaya; Perez, Kerstin [Columbia Astrophysics Laboratory, Columbia University, New York, NY 10027 (United States); Reynolds, Stephen P. [Physics Department, NC State University, Raleigh, NC 27695 (United States); An, Hongjun [Department of Physics, McGill University, Rutherford Physics Building, 3600 University Street, Montreal, Quebec H3A 2T8 (Canada); Baganoff, Frederick K. [Center for Space Research, Massachusetts Institute of Technology, Cambridge, MA 02139-4307 (United States); Boggs, Steven E.; Krivonos, Roman; Zoglauer, Andreas [Space Sciences Laboratory, University of California, Berkeley, CA 94720 (United States); Christensen, Finn E. [DTU Space, National Space Institute, Technical University of Denmark, Elektrovej 327, DK-2800 Lyngby (Denmark); Craig, William W. [Lawrence Livermore National Laboratory, Livermore, CA 94550 (United States); Grefenstette, Brian W.; Harrison, Fiona A.; Madsen, Kristin K. [Cahill Center for Astronomy and Astrophysics, California Institute of Technology, Pasadena, CA 91125 (United States); Stern, Daniel [Jet Propulsion Laboratory, California Institute of Technology, Pasadena, CA 91109 (United States); Wik, Daniel R.; Zhang, William W. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States)

    2014-07-01

    We present NuSTAR high-energy X-ray observations of the pulsar wind nebula (PWN)/supernova remnant G21.50.9. We detect integrated emission from the nebula up to ?40 keV, and resolve individual spatial features over a broad X-ray band for the first time. The morphology seen by NuSTAR agrees well with that seen by XMM-Newton and Chandra below 10 keV. At high energies, NuSTAR clearly detects non-thermal emission up to ?20 keV that extends along the eastern and northern rim of the supernova shell. The broadband images clearly demonstrate that X-ray emission from the North Spur and Eastern Limb results predominantly from non-thermal processes. We detect a break in the spatially integrated X-ray spectrum at ?9 keV that cannot be reproduced by current spectral energy distribution models, implying either a more complex electron injection spectrum or an additional process such as diffusion compared to what has been considered in previous work. We use spatially resolved maps to derive an energy-dependent cooling length scale, L(E)?E{sup m} with m = 0.21 0.01. We find this to be inconsistent with the model for the morphological evolution with energy described by Kennel and Coroniti. This value, along with the observed steepening in power-law index between radio and X-ray, can be quantitatively explained as an energy-loss spectral break in the simple scaling model of Reynolds, assuming particle advection dominates over diffusion. This interpretation requires a substantial departure from spherical magnetohydrodynamic, magnetic-flux-conserving outflow, most plausibly in the form of turbulent magnetic-field amplification.

  7. Microgap x-ray detector

    DOE Patents [OSTI]

    Wuest, Craig R.; Bionta, Richard M.; Ables, Elden

    1994-01-01

    An x-ray detector which provides for the conversion of x-ray photons into photoelectrons and subsequent amplification of these photoelectrons through the generation of electron avalanches in a thin gas-filled region subject to a high electric potential. The detector comprises a cathode (photocathode) and an anode separated by the thin, gas-filled region. The cathode may comprise a substrate, such a beryllium, coated with a layer of high atomic number material, such as gold, while the anode can be a single conducting plane of material, such as gold, or a plane of resistive material, such as chromium/silicon monoxide, or multiple areas of conductive or resistive material, mounted on a substrate composed of glass, plastic or ceramic. The charge collected from each electron avalanche by the anode is passed through processing electronics to a point of use, such as an oscilloscope.

  8. Microgap x-ray detector

    DOE Patents [OSTI]

    Wuest, C.R.; Bionta, R.M.; Ables, E.

    1994-05-03

    An x-ray detector is disclosed which provides for the conversion of x-ray photons into photoelectrons and subsequent amplification of these photoelectrons through the generation of electron avalanches in a thin gas-filled region subject to a high electric potential. The detector comprises a cathode (photocathode) and an anode separated by the thin, gas-filled region. The cathode may comprise a substrate, such a beryllium, coated with a layer of high atomic number material, such as gold, while the anode can be a single conducting plane of material, such as gold, or a plane of resistive material, such as chromium/silicon monoxide, or multiple areas of conductive or resistive material, mounted on a substrate composed of glass, plastic or ceramic. The charge collected from each electron avalanche by the anode is passed through processing electronics to a point of use, such as an oscilloscope. 3 figures.

  9. Room temperature reaction of oxygen with gold: an in situ ambient-pressure X-ray photoelectron spectroscopy investigation

    SciTech Connect (OSTI)

    Jiang, Peng; Porsgaard, Soeren; Borondics, Ferenc; Kober, Mariana; Caballero, Alfonso; Bluhm, Hendrik; Besenbacher, Flemming; Salmeron, Miquel

    2010-02-01

    Gold is commonly regarded as the most inert element.1 However, the discovery of the exceptional catalytic properties of gold nanoparticles (NPs) for low temperature CO oxidation2 initiated great interest due to its promising applications and spawned a large number of studies devoted to the understanding of the reaction mechanism.3-6 Nevertheless, no consistent and conclusive picture has arisen.7-13

  10. X-ray absorption spectroscopy of aluminum z-pinch plasma with tungsten backlighter planar wire array source

    SciTech Connect (OSTI)

    Osborne, G. C.; Kantsyrev, V. L.; Safronova, A. S.; Esaulov, A. A.; Weller, M. E.; Shrestha, I.; Shlyaptseva, V. V.; Ouart, N. D.

    2012-10-15

    Absorption features from K-shell aluminum z-pinch plasmas have recently been studied on Zebra, the 1.7 MA pulse power generator at the Nevada Terawatt Facility. In particular, tungsten plasma has been used as a semi-backlighter source in the generation of aluminum K-shell absorption spectra by placing a single Al wire at or near the end of a single planar W array. All spectroscopic experimental results were recorded using a time-integrated, spatially resolved convex potassium hydrogen phthalate (KAP) crystal spectrometer. Other diagnostics used to study these plasmas included x-ray detectors, optical imaging, laser shadowgraphy, and time-gated and time-integrated x-ray pinhole imagers. Through comparisons with previous publications, Al K-shell absorption lines are shown to be from much lower electron temperature ({approx}10-40 eV) plasmas than emission spectra ({approx}350-500 eV).

  11. An ultra-high vacuum electrochemical flow cell for in situ/operando soft X-ray spectroscopy study

    SciTech Connect (OSTI)

    Bora, Debajeet K. E-mail: jguo@lbl.gov; Glans, Per-Anders; Pepper, John; Liu, Yi-Sheng; Guo, J.-H. E-mail: jguo@lbl.gov; Du, Chun; Wang, Dunwei

    2014-04-15

    An in situ flow electrochemical cell has been designed and fabricated to allow better seal under UHV chamber thus to achieve a good signal to noise ratio in fluorescence yield detection of X-ray absorption spectra for spectroelectrochemical study. The cell also stabilizes the thin silicon nitride membrane window in an effective manner so that the liquid cell remains intact during X-ray absorption experiments. With the improved design of the liquid cell, electrochemical experiments such as cyclic voltammetry have been performed for 10 cycles with a good stability of sample window. Also an operando electrochemical experiment during photoelectrochemistry has been performed on n-type hematite electrode deposited on silicon nitride window. The experiment allows us to observe the formation of two extra electronic transitions before pre edge of O K-edge spectra.

  12. Magnetic properties of GdT2Zn20 (T = Fe, Co) investigated by x-ray diffraction and spectroscopy

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    J. R. L. Mardegan; Fabbris, G.; Francoual, S.; Veiga, L. S. I.; Strempfer, J.; Haskel, D.; Ribeiro, R. A.; Avila, M. A.; Giles, C.

    2016-01-26

    In this study, we investigate the magnetic and electronic properties of the GdT2Zn20 (T=Fe and Co) compounds using x-ray resonant magnetic scattering (XRMS), x-ray absorption near-edge structure (XANES), and x-ray magnetic circular dichroism (XMCD). The XRMS measurements reveal that GdCo2Zn20 has a commensurate antiferromagnetic spin structure with a magnetic propagation vector →/τ = (12,12,12) below the Néel temperature (TN ~ 5.7 K). Only the Gd ions carry a magnetic moment forming an antiferromagnetic structure with magnetic representation Γ6. For the ferromagnetic GdFe2Zn20 compound, an extensive investigation was performed at low temperature and under magnetic field using XANES and XMCD. Amore » strong XMCD signal of about 12.5% and 9.7% is observed below the Curie temperature (TC ~ 85K) at the Gd L2 and L3 edges, respectively. In addition, a small magnetic signal of about 0.06% of the jump is recorded at the Zn K edge, suggesting that the Zn 4p states are spin polarized by the Gd 5d extended orbitals.« less

  13. High resolution absorption spectroscopy of exploding wire plasmas using an x-pinch x-ray source and spherically bent crystal

    SciTech Connect (OSTI)

    Knapp, P. F.; Pikuz, S. A.; Shelkovenko, T. A.; Hammer, D. A.; Hansen, S. B.

    2011-06-15

    We present here the use of absorption spectroscopy of the continuum radiation from x-pinch-produced point x-ray sources as a diagnostic to investigate the properties of aluminum plasmas created by pulsed power machines. This technique is being developed to determine the charge state, temperature, and density as a function of time and space under conditions that are inaccessible to x-ray emission spectroscopic diagnostics. The apparatus and its characterization are described, and the spectrometer dispersion, magnification, and resolution are calculated and compared with experimental results. Spectral resolution of about 5000 and spatial resolution of about 20 {mu}m are demonstrated. This spectral resolution is the highest available to date in an absorption experiment. The beneficial properties of the x-pinch x-ray source as the backlighter for this diagnostic are the small source size (<5 {mu}m), smooth continuum radiation, and short pulse duration (<0.1 ns). Results from a closely spaced (1 mm) exploding wire pair are shown and the general features are discussed.

  14. High-Pressure Raman Spectroscopy and X-ray Diffraction Studies of a Terpolymer of Tetrafluoroethylene-Hexafluoropropylene-Vinylidene Fluoride: THV 500

    SciTech Connect (OSTI)

    Emmons, E.D.; Velisavljevic, N.; Schoonover, J.R.; Dattelbaum, D.M.

    2008-04-02

    High-pressure Raman spectroscopy and X-ray diffraction of THV 500, a terpolymer of tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride, were performed using diamond anvil cells (DAC). Changes in the interatomic spacing as well as shifts of several of the vibrational bands as a function of pressure were measured up to {approx}10 GPa. The changes in interatomic spacing and shifts of the vibrational bands are compared to those of polytetrafluoroethylene, showing the effects of copolymerization and reduced crystallinity. The high-pressure behavior of polymers is a relatively unexplored field but is becoming increasingly important due to applications where polymers experience extreme conditions.

  15. Bandpass x-ray diode and x-ray multiplier detector

    DOE Patents [OSTI]

    Wang, C.L.

    1982-09-27

    An absorption-edge of an x-ray absorption filter and a quantum jump of a photocathode determine the bandpass characteristics of an x-ray diode detector. An anode, which collects the photoelectrons emitted by the photocathode, has enhanced amplification provided by photoelectron-multiplying means which include dynodes or a microchannel-plate electron-multiplier. Suppression of undesired high frequency response for a bandpass x-ray diode is provided by subtracting a signal representative of energies above the passband from a signal representative of the overall response of the bandpass diode.

  16. NUSTAR and SUZAKU X-ray spectroscopy of NGC 4151: Evidence for reflection from the inner accretion disk

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Keck, M. L.; Brenneman, L. W.; Ballantyne, D. R.; Bauer, F.; Boggs, S. E.; Christensen, F. E.; Craig, W. W.; Dauser, T.; Elvis, M.; Fabian, A. C.; et al

    2015-06-15

    We present X-ray timing and spectral analyses of simultaneous 150 ks Nuclear Spectroscopic Telescope Array (NuSTAR) and Suzaku X-ray observations of the Seyfert 1.5 galaxy NGC 4151. We disentangle the continuum emission, absorption, and reflection properties of the active galactic nucleus (AGN) by applying inner accretion disk reflection and absorption-dominated models. With a time-averaged spectral analysis, we find strong evidence for relativistic reflection from the inner accretion disk. We find that relativistic emission arises from a highly ionized inner accretion disk with a steep emissivity profile, which suggests an intense, compact illuminating source. We find a preliminary, near-maximal black hole spinmore » $$a\\gt 0.9$$ accounting for statistical and systematic modeling errors. We find a relatively moderate reflection fraction with respect to predictions for the lamp post geometry, in which the illuminating corona is modeled as a point source. Through a time-resolved spectral analysis, we find that modest coronal and inner disk reflection (IDR) flux variation drives the spectral variability during the observations. As a result, we discuss various physical scenarios for the IDR model and we find that a compact corona is consistent with the observed features.« less

  17. X-Ray Diagnostics

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    including film developing and scanning, and image plate scanning. Related images X-ray framing camera being loaded into the TIM in the Trident North Target Area. X-ray framing...

  18. Quantitative Phase Composition of TiO2-Coated Nanoporous-Au Monoliths by X-ray Absorption Spectroscopy and Correlations to Catalytic

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Bagge-Hansen, Michael; Wichmann, Andre; Wittstock, Arne; Lee, Jonathan R. I.; Ye, Jianchao; Willey, Trevor M.; Kuntz, Joshua D.; van Buuren, Tony; Biener, Juergen; Baumer, Marcus; et al

    2014-02-03

    Porous titania/metal composite materials have many potential applications in the fields of green catalysis, energy harvesting, and storage in which both the overall morphology of the nanoporous host material and the crystallographic phase of the titania (TiO 2) guest determine the material’s performance. New insights into the structure–function relationships of these materials were obtained by near-edge X-ray absorption fine structure (NEXAFS) spectroscopy that, for example, provides quantitative crystallographic phase composition from ultrathin, nanostructured titania films, including sensitivity to amorphous components. We demonstrate that crystallographic phase, morphology, and catalytic activity of TiO 2-functionalized nanoporous gold (np-Au) can be controlled by amore » simple annealing procedure (T < 1300 K). The material was prepared by atomic layer deposition of ~2 nm thick TiO2 on millimeter-sized samples of np-Au (40–50 nm mean ligament size) and catalytically investigated with respect to aerobic CO oxidation. Moreover, the annealing-induced changes in catalytic activity are correlated with concurrent morphology and phase changes as provided by cross-sectional scanning electron microscopy, transmission electron microscopy, and near-edge X-ray absorption fine structure (NEXAFS) spectroscopy.« less

  19. Soft X-ray techniques to study mesoscale magnetism

    SciTech Connect (OSTI)

    Kortright, Jeffrey B.

    2003-06-26

    Heterogeneity in magnetization (M) is ubiquitous in modern systems. Even in nominally homogeneous materials, domains or pinning centers typically mediate magnetization reversal. Fundamental lengths determining M structure include the domain wall width and the exchange stiffness length, typically in the 4-400 nm range. Chemical heterogeneity (phase separation, polycrystalline microstructure, lithographic or other patterning, etc.) with length scales from nanometers to microns is often introduced to influence magnetic properties. With 1-2 nm wavelengths {lambda}, soft x-rays in principle can resolve structure down to {lambda}/2, and are well suited to study these mesoscopic length scales [1, 2]. This article highlights recent advances in resonant soft x-ray methods to resolve lateral magnetic structure [3], and discusses some of their relative merits and limitations. Only techniques detecting x-ray photons (rather than photo-electrons) are considered [4], since they are compatible with strong applied fields to probe relatively deeply into samples. The magneto-optical (MO) effects discovered by Faraday and Kerr were observed in the x-ray range over a century later, first at ''hard'' wavelengths in diffraction experiments probing interatomic magnetic structure [5]. In the soft x-ray range, magnetic linear [6] and circular [7] dichroism spectroscopies first developed that average over lateral magnetic structure. These large resonant MO effects enable different approaches to study magnetic structure or heterogeneity that can be categorized as microscopy or scattering [1]. Direct images of magnetic structure result from photo-emission electron microscopes [4, 8] and zone-plate microscopes [9, 10]. Scattering techniques extended into the soft x-ray include familiar specular reflection that laterally averages over structure but can provide depth-resolved information, and diffuse scattering and diffraction that provide direct information about lateral magnetic structure

  20. Upgraded high time-resolved x-ray imaging crystal spectroscopy system for J-TEXT ohmic plasmas

    SciTech Connect (OSTI)

    Jin, W.; Chen, Z. Y. Huang, D. W.; Li, Q. L.; Yan, W.; Luo, Y. H.; Huang, Y. H.; Tong, R. H.; Yang, Z. J.; Rao, B.; Ding, Y. H.; Zhuang, G.; Lee, S. G.; Shi, Y. J.

    2014-02-15

    This paper presents the upgraded x-ray imaging crystal spectrometer (XICS) system on Joint Texas Experimental Tokamak (J-TEXT) tokamak and the latest experimental results obtained in last campaign. With 500 Hz frame rate of the new Pilatus detector and 5 cm 10 cm spherically bent crystal, the XICS system can provide core electron temperature (T{sub e}), core ion temperature (T{sub i}), and plasma toroidal rotation (V{sub ?}) with a maximum temporal resolution of 2 ms for J-TEXT pure ohmic plasmas. These parameters with high temporal resolution are very useful in tokamak plasma research, especially for rapidly changed physical processes. The experimental results from the upgraded XICS system are presented.

  1. Direct speciation analysis of arsenic in sub-cellular compartments using micro-X-ray absorption spectroscopy

    SciTech Connect (OSTI)

    Bacquart, Thomas; Deves, Guillaume; Ortega, Richard

    2010-07-15

    Identification of arsenic chemical species at a sub-cellular level is a key to understanding the mechanisms involved in arsenic toxicology and antitumor pharmacology. When performed with a microbeam, X-ray absorption near-edge structure ({mu}-XANES) enables the direct speciation analysis of arsenic in sub-cellular compartments avoiding cell fractionation and other preparation steps that might modify the chemical species. This methodology couples tracking of cellular organelles in a single cell by confocal or epifluorescence microscopy with local analysis of chemical species by {mu}-XANES. Here we report the results obtained with a {mu}-XANES experimental setup based on Kirkpatrick-Baez X-ray focusing optics that maintains high flux of incoming radiation (>10{sup 11} ph/s) at micrometric spatial resolution (1.5x4.0 {mu}m{sup 2}). This original experimental setup enabled the direct speciation analysis of arsenic in sub-cellular organelles with a 10{sup -15} g detection limit. {mu}-XANES shows that inorganic arsenite, As(OH){sub 3}, is the main form of arsenic in the cytosol, nucleus, and mitochondrial network of cultured cancer cells exposed to As{sub 2}O{sub 3}. On the other hand, a predominance of As(III) species is observed in HepG2 cells exposed to As(OH){sub 3} with, in some cases, oxidation to a pentavalent form in nuclear structures of HepG2 cells. The observation of intra-nuclear mixed redox states suggests an inter-individual variability in a cell population that can only be evidenced with direct sub-cellular speciation analysis.

  2. X-Ray Diagnostics

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    X-Ray Diagnostics X-Ray Diagnostics Maintenance of existing devices and development of advanced concepts Contact John Oertel (505) 665-3246 Email Hot, dense matter produced by intense laser interaction with a solid target often produces x-rays with energies from 100 eV to those exceeding 100 keV. A suite of diagnostics and methods have been deployed at Trident to diagnose the x-ray emission from laser-matter interaction experiments, or to use the x-rays as a probe of dense matter. These

  3. Nitrogen termination of single crystal (100) diamond surface by radio frequency N{sub 2} plasma process: An in-situ x-ray photoemission spectroscopy and secondary electron emission studies

    SciTech Connect (OSTI)

    Chandran, Maneesh E-mail: choffman@tx.technion.ac.il; Shasha, Michal; Michaelson, Shaul; Hoffman, Alon E-mail: choffman@tx.technion.ac.il

    2015-09-14

    In this letter, we report the electronic and chemical properties of nitrogen terminated (N-terminated) single crystal (100) diamond surface, which is a promising candidate for shallow NV{sup −} centers. N-termination is realized by an indirect RF nitrogen plasma process without inducing a large density of surface defects. Thermal stability and electronic property of N-terminated diamond surface are systematically investigated under well-controlled conditions by in-situ x-ray photoelectron spectroscopy and secondary electron emission. An increase in the low energy cut-off of the secondary electron energy distribution curve (EDC), with respect to a bare diamond surface, indicates a positive electron affinity of the N-terminated diamond. Exposure to atomic hydrogen results in reorganization of N-terminated diamond to H-terminated diamond, which exhibited a negative electron affinity surface. The change in intensity and spectral features of the secondary electron EDC of the N-terminated diamond is discussed.

  4. A high resolution and large solid angle x-ray Raman spectroscopy end-station at the Stanford Synchrotron Radiation Lightsource

    SciTech Connect (OSTI)

    Sokaras, D.; Nordlund, D.; Weng, T.-C.; Velikov, P.; Wenger, D.; Garachtchenko, A.; George, M.; Borzenets, V.; Johnson, B.; Rabedeau, T.; Mori, R. Alonso; Bergmann, U.; Qian, Q.

    2012-04-15

    We present a new x-ray Raman spectroscopy end-station recently developed, installed, and operated at the Stanford Synchrotron Radiation Lightsource. The end-station is located at wiggler beamline 6-2 equipped with two monochromators-Si(111) and Si(311) as well as collimating and focusing optics. It consists of two multi-crystal Johann type spectrometers arranged on intersecting Rowland circles of 1 m diameter. The first one, positioned at the forward scattering angles (low-q), consists of 40 spherically bent and diced Si(110) crystals with 100 mm diameters providing about 1.9% of 4{pi} sr solid angle of detection. When operated in the (440) order in combination with the Si (311) monochromator, an overall energy resolution of 270 meV is obtained at 6462.20 eV. The second spectrometer, consisting of 14 spherically bent Si(110) crystal analyzers (not diced), is positioned at the backward scattering angles (high-q) enabling the study of non-dipole transitions. The solid angle of this spectrometer is about 0.9% of 4{pi} sr, with a combined energy resolution of 600 meV using the Si (311) monochromator. These features exceed the specifications of currently existing relevant instrumentation, opening new opportunities for the routine application of this photon-in/photon-out hard x-ray technique to emerging research in multidisciplinary scientific fields, such as energy-related sciences, material sciences, physical chemistry, etc.

  5. High-resolution elemental mapping of human placental chorionic villi using synchrotron X-ray fluorescence spectroscopy

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Punshon, Tracy; Chen, Si; Finney, Lydia; Howard, Louisa; Jackson, Brian P.; Karagas, Margaret R.; Ornvold, Kim

    2015-07-03

    The placenta is the organ that mediates transport of nutrients and waste materials between mother and fetus. Synchrotron X-ray fluorescence (SXRF) microanalysis is a tool for imaging the distribution and quantity of elements in biological tissue, which can be used to study metal transport across biological membranes. Our aims were to pilot placental biopsy specimen preparation techniques that could be integrated into an ongoing epidemiology birth cohort study without harming rates of sample acquisition. We studied the effects of fixative (formalin or glutaraldehyde) and storage duration (30 days or immediate processing) on metal distribution and abundance and investigated a thaw-fixationmore » protocol for archived specimens stored at -80° C. We measured fixative elemental composition with and without a placental biopsy via inductively coupled plasma mass spectrometry (ICP-MS) to quantify fixative-induced elemental changes. Formalin-fixed specimens showed hemolysis of erythrocytes. The glutaraldehyde-paraformaldehyde solution in HEPES buffer (GTA-HEPES) had superior anatomical preservation, avoided hemolysis, and minimized elemental loss, although some cross-linking of exogenous Zn was evident. Elemental loss from tissue stored in fixative for 1 month showed variable losses (≈ 40 % with GTA-HEPES), suggesting storage duration be controlled for. Lastly, thawing of tissue held at -80 °C in a GTA-HEPES solution provided high-quality visual images and elemental images« less

  6. High-resolution Elemental Mapping of Human Placental Chorionic Villi Using Synchrotron X-ray Fluorescence Spectroscopy

    SciTech Connect (OSTI)

    Punshon, Tracy; Chen, Si; Finney, Lydia; Howard, Louisa; Jackson, Brian P.; Karagas, Margaret R.; Ornvold, Kim

    2015-09-01

    The placenta is the organ that mediates transport of nutrients and waste materials between mother and fetus. Synchrotron X-ray fluorescence (SXRF) microanalysis is a tool for imaging the distribution and quantity of elements in biological tissue, which can be used to study metal transport across biological membranes. Our aims were to pilot placental biopsy specimen preparation techniques that could be integrated into an ongoing epidemiology birth cohort study without harming rates of sample acquisition. We studied the effects of fixative (formalin or glutaraldehyde) and storage duration (30 days or immediate processing) on metal distribution and abundance and investigated a thaw-fixation protocol for archived specimens stored at -80 A degrees C. We measured fixative elemental composition with and without a placental biopsy via inductively coupled plasma mass spectrometry (ICP-MS) to quantify fixative-induced elemental changes. Formalin-fixed specimens showed hemolysis of erythrocytes. The glutaraldehyde-paraformaldehyde solution in HEPES buffer (GTA-HEPES) had superior anatomical preservation, avoided hemolysis, and minimized elemental loss, although some cross-linking of exogenous Zn was evident. Elemental loss from tissue stored in fixative for 1 month showed variable losses (a parts per thousand 40 % with GTA-HEPES), suggesting storage duration be controlled for. Thawing of tissue held at -80 A degrees C in a GTA-HEPES solution provided high-quality visual images and elemental images

  7. Influence of structural disorder on soft x-ray optical behavior of NbC thin films

    SciTech Connect (OSTI)

    Singh, Amol E-mail: rrcat.amol@gmail.com; Modi, Mohammed H.; Sinha, A. K.; Lodha, G. S.; Rajput, Parasmani

    2015-05-07

    Structural and chemical properties of compound materials are modified, when thin films are formed from bulk materials. To understand these changes, a study was pursued on niobium carbide (NbC) thin films of different thicknesses deposited on Si (100) substrate using ion beam sputtering technique. Optical response of the film was measured in 4–36 nm wavelength region using Indus-1 reflectivity beamline. A discrepancy in soft x-ray performance of NbC film was observed which could not be explained with Henke's tabulated data (see http://henke.lbl.gov/optical{sub c}onstants/ ). In order to understand this, detailed structural and chemical investigations were carried out using x-ray reflectivity, grazing incidence x-ray diffraction, x-ray absorption near edge structure, extended x-ray absorption fine structure, and x-ray photoelectron spectroscopy techniques. It was found that the presence of unreacted carbon and Nb deficiency due to reduced Nb-Nb coordination are responsible for lower soft x-ray reflectivity performance. NbC is an important material for soft x-ray optical devices, hence the structural disorder need to be controlled to achieve the best performances.

  8. The Soft X-ray Research instrument at the Linac Coherent Light...

    Office of Scientific and Technical Information (OSTI)

    The Soft X-ray Research instrument at the Linac Coherent Light Source Georgi L. ... Fremont, CA 94539, USA. Keywords: FEL; X-ray; ultrafast; spectroscopy; materials science. ...

  9. X-Ray Diffraction > Analytical Resources > Research > The Energy Materials

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Center at Cornell Analytical Resources In This Section Differential Electrochemical Mass Spectroscopy (DEMS) Electron Microscopy X-Ray Diffraction X-Ray Diffraction

  10. Time-resolved soft-x-ray spectroscopy of a magnetic octupole transition in nickel-like xenon, cesium, and barium ions

    SciTech Connect (OSTI)

    Trabert, E; Beiersdorfer, P; Brown, G V; Boyce, K; Kelley, R L; Kilbourne, C A; Porter, F S; Szymkowiak, A

    2005-11-11

    A microcalorimeter with event mode capability for time-resolved soft-x-ray spectroscopy, and a high-resolution flat-field EUV spectrometer have been employed at the Livermore EBIT-I electron beam ion trap for observations and wavelength measurements of M1, E2, and M3 decays of long-lived levels in the Ni-like ions Xe{sup 26+}, Cs{sup 27+}, and Ba{sup 28+}. Of particular interest is the lowest excited level, 3d{sup 9}4s {sup 3}D{sub 3}, which can only decay via a magnetic octupole (M3) transition. For this level in Xe an excitation energy of (590.40 {+-} 0.03eV) and a level lifetime of (11.5 {+-} 0.5 ms) have been determined.

  11. Setup for in situ investigation of gases and gas/solid interfaces by soft x-ray emission and absorption spectroscopy

    SciTech Connect (OSTI)

    Benkert, A. E-mail: l.weinhardt@kit.edu; Blum, M.; Advanced Light Source, Lawrence Berkeley National Laboratory, 1 Cyclotron Road, Berkeley, California 94720 ; Meyer, F.; Wilks, R. G.; Yang, W.; Bär, M.; Solar Energy Research, Helmholtz-Zentrum Berlin für Materialien und Energie GmbH, Hahn-Meitner-Platz 1, 14109 Berlin; Insitut für Physik und Chemie, Brandenburgische Technische Universität Cottbus-Senftenberg, Konrad-Wachsmann-Allee 1, 03046 Cottbus ; and others

    2014-01-15

    We present a novel gas cell designed to study the electronic structure of gases and gas/solid interfaces using soft x-ray emission and absorption spectroscopies. In this cell, the sample gas is separated from the vacuum of the analysis chamber by a thin window membrane, allowing in situ measurements under atmospheric pressure. The temperature of the gas can be regulated from room temperature up to approximately 600 °C. To avoid beam damage, a constant mass flow can be maintained to continuously refresh the gaseous sample. Furthermore, the gas cell provides space for solid-state samples, allowing to study the gas/solid interface for surface catalytic reactions at elevated temperatures. To demonstrate the capabilities of the cell, we have investigated a TiO{sub 2} sample behind a mixture of N{sub 2} and He gas at atmospheric pressure.

  12. Particle size effect of hydride formation and surface hydrogen absorption of nanosized palladium catalysts : L{sub 3} edge vs K edge x-ray absorption spectroscopy.

    SciTech Connect (OSTI)

    Tew, M. W.; Miller, J. T.; van Bokhoven, J. A.

    2009-08-01

    The particle size effect on the formation of palladium hydride and on surface hydrogen adsorption was studied at room temperature using in situ X-ray absorption spectroscopy at the Pd K and L{sub 3} edges. Hydride formation was indirectly observed by lattice expansion in Pd K edge XANES spectra and by EXAFS analysis. Hydride formation was directly detected in the L{sub 3} edge spectra. A characteristic spectral feature caused by the formation of a Pd-H antibonding state showed strong particle size dependence. The L{sub 3} edge spectra were reproduced using full multiple scattering analysis and density of state calculations, and the contributions of bulk absorbed and surface hydrogen to the XANES spectra could be distinguished. The ratio of hydrogen on the surface versus that in the bulk increased with decreasing particle size, and smaller particles dissolved less hydrogen.

  13. Phase transitions in heated Sr{sub 2}MgTeO{sub 6} double perovskite oxide probed by X-ray diffraction and Raman spectroscopy

    SciTech Connect (OSTI)

    Manoun, Bouchaib Tamraoui, Y.; Lazor, P.; Yang, Wenge

    2013-12-23

    Double-perovskite oxide Sr{sub 2}MgTeO{sub 6} has been synthetized, and its crystal structure was probed by the technique of X-ray diffraction at room temperature. The structure is monoclinic, space group I2/m. Temperature-induced phase transitions in this compound were investigated by Raman spectroscopy up to 550 °C. Two low-wavenumber modes corresponding to external lattice vibrations merge at temperature of around 100 °C, indicating a phase transition from the monoclinic (I2/m) to the tetragonal (I4/m) structure. At 300 °C, changes in the slopes of temperature dependencies of external and O–Te–O bending modes are detected and interpreted as a second phase transition from the tetragonal (I4/m) to the cubic (Fm-3m) structure.

  14. Mapping the metal uptake in plants from Jasper Ridge Biological Preserve using synchrotron micro-focused X-ray fluorescence spectroscopy

    SciTech Connect (OSTI)

    Lo, Allison

    2015-08-20

    Serpentine soil originates in the Earth’s mantle and contains high concentrations of potentially toxic transition metals. Although serpentine soil limits plant growth, endemic and adapted plants at Jasper Ridge Biological Preserve, located behind SLAC National Accelerator Laboratory, can tolerate these conditions. Serpentine soil and seeds belonging to native California and invasive plants were collected at Jasper Ridge. The seeds were grown hydroponically and on serpentine and potting soil to examine the uptake and distribution of ions in the roots and shoots using synchrotron micro-focused X-ray fluorescence spectroscopy. The results were used to determine differences between serpentine-tolerant plants. Rye grown on potting soil was enriched in Ni, Fe, Mn, and Cr compared to purple needlegrass grown on serpentine soil. Serpentine vegetation equally suppressed the uptake of Mn, Ni, and Fe in the roots and shoots. The uptake of Ca and Mg affected the uptake of other elements such as K, S, and P.

  15. The apparent absence of chemical sensitivity in the 4d and 5d X-ray absorption spectroscopy of uranium compounds

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Tobin, J. G.

    2013-05-03

    X-ray absorption spectroscopy (XAS) and related derivative measurements have been used to demonstrate that the Pu 5f states are strongly relativistic and have a 5f occupation number near 5. Owing to the success in this regime, it has been argued that the XAS measurements should be a powerful tool to probe 5f occupation variation, both as a function of elemental nature (actinide atomic number) and as a function of physical and chemical perturbation, e.g., oxidation state. We show that XAS and its related measurements fail in this latter aspect for a wide variety of uranium compounds and materials. Possible causesmore » will be discussed.« less

  16. Correlation between Active Center Structure and Enhanced Dioxygen Binding in Co(salen) Nanoparticles: Characterization by In Situ Infrared, Raman, and X-ray Absorption Spectroscopies

    SciTech Connect (OSTI)

    Johnson,C.; Long, B.; Nguyen, J.; Day, V.; Borovik, A.; Subramaniam, B.; Guzman, J.

    2008-01-01

    The structure and ligand environment of Co(salen) nanoparticles and unprocessed Co(salen) have been determined by the combined application of infrared, Raman, X-ray absorption near edge structure (XANES), and extended X-ray absorption fine structure (EXAFS) spectroscopies, and X-ray diffraction (XRD) experiments before and during interaction with O2. The Co(salen) nanoparticles were prepared by the precipitation with compressed antisolvent (PCA) technique using commercially obtained Co(salen) [denoted as unprocessed Co(salen)] as the parent compound. The unprocessed Co(salen) particles exist as dimer species with a square-pyramidal coordination geometry that display no measurable O2 binding at room temperature. In sharp contrast, the Co(salen) nanoparticles show near-stoichiometric O2 adsorption, as demonstrated by microbalance gas binding experiments. The spectroscopy results indicate the presence of CoII centers with distorted tetrahedral geometry in the Co(salen) nanoparticles with no evidence of metallic Co clusters, confirmed by the lack of Co-Co contributions at bonding distances in the EXAFS spectra and the presence of characteristic features of CoII in the XANES spectra. The EXAFS data also indicate that there are on average two Co-N and two Co-O bonds with a distance of 1.81 {+-} 0.02 and 1.90 {+-} 0.02 Angstroms, respectively, consistent with typical metal salen structures. Upon O2 binding on the Co(salen) nanoparticles, the XANES results indicate oxidation of the CoII to CoIII, consistent with the vibrational data showing new bands associated with oxygen species bonded to Co centers and the increase in the oxygen coordination number from 1.8 to 2.9 in the EXAFS data. The results indicate that the enhanced O2 binding properties of Co(salen) nanoparticles are related to the unique distorted tetrahedral geometry, which is not observed in the unprocessed samples that contain mainly dimers with square planar geometry. The results presented here provide a

  17. Local X-ray magnetic circular dichroism study of Fe/Cu(111) using a tunneling smart tip

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    DiLullo, Andrew; Shirato, Nozomi; Cummings, Marvin; Kersell, Heath; Chang, Hao; Rosenmann, Daniel; Miller, Dean; Freeland, John W.; Hla, Saw -Wai; Rose, Volker

    2016-01-28

    Localized spectroscopy with simultaneous topographic, elemental and magnetic information is presented. A synchrotron X-ray scanning tunneling microscope has been employed for the local study of the X-ray magnetic circular dichroism at the FeL2,3-edges of a thin iron film grown on Cu(111). Polarization-dependent X-ray absorption spectra have been obtained through a tunneling smart tip that serves as a photoelectron detector. In contrast to conventional spin-polarized scanning tunneling microscopy, X-ray excitations provide magnetic contrast even with a non-magnetic tip. Intensity variations in the photoexcited tip current point to chemical variations within a single magnetic Fe domain.

  18. X-ray beamsplitter

    DOE Patents [OSTI]

    Ceglio, Natale M.; Stearns, Daniel S.; Hawryluk, Andrew M.; Barbee, Jr., Troy W.

    1989-01-01

    An x-ray beamsplitter which splits an x-ray beam into two coherent parts by reflecting and transmitting some fraction of an incident beam has applications for x-ray interferometry, x-ray holography, x-ray beam manipulation, and x-ray laser cavity output couplers. The beamsplitter is formed of a wavelength selective multilayer thin film supported by a very thin x-ray transparent membrane. The beamsplitter resonantly transmits and reflects x-rays through thin film interference effects. A thin film is formed of 5-50 pairs of alternate Mo/Si layers with a period of 20-250 A. The support membrane is 10-200 nm of silicon nitride or boron nitride. The multilayer/support membrane structure is formed across a window in a substrate by first forming the structure on a solid substrate and then forming a window in the substrate to leave a free-standing structure over the window.

  19. X-ray beamsplitter

    DOE Patents [OSTI]

    Ceglio, N.M.; Stearns, D.G.; Hawryluk, A.M.; Barbee, T.W. Jr.

    1987-08-07

    An x-ray beamsplitter which splits an x-ray beam into two coherent parts by reflecting and transmitting some fraction of an incident beam has applications for x-ray interferometry, x-ray holography, x-ray beam manipulation, and x-ray laser cavity output couplers. The beamsplitter is formed of a wavelength selective multilayer thin film supported by a very thin x-ray transparent membrane. The beamsplitter resonantly transmits and reflects x-rays through thin film interference effects. A thin film is formed of 5--50 pairs of alternate Mo/Si layers with a period of 20--250 A. The support membrane is 10--200 nm of silicon nitride or boron nitride. The multilayer/support membrane structure is formed across a window in a substrate by first forming the structure on a solid substrate and then forming a window in the substrate to leave a free-standing structure over the window. 6 figs.

  20. Chest x-Rays

    Broader source: Energy.gov [DOE]

    The B-reading is a special reading of a standard chest x-ray film performed by a physician certified by the National Institute for Occupational Safety and Health (NIOSH). The reading looks for changes on the chest x-ray that may indicate exposure and disease caused by agents such as asbestos or silica.

  1. Electronic structure of Al-doped ZnO transparent conductive thin films studied by x-ray absorption and emission spectroscopies

    SciTech Connect (OSTI)

    Huang, W. H.; Sun, S. J.; Chiou, J. W.; Chou, H.; Chan, T. S.; Lin, H.-J.; Kumar, Krishna; Guo, J.-H.

    2011-11-15

    This study used O K-, Zn L{sub 3}-, Zn K-, and Al K-edges x-ray absorption near-edge structure (XANES) and O K-edge x-ray emission spectroscopy (XES) measurements to investigate the electronic structure of transparent Al-doped ZnO (AZO) thin film conductors. The samples were prepared on glass substrates at a low temperature near 77 K by using a standard RF sputtering method. High-purity Ne (5N) was used as the sputtering gas. The crystallography of AZO thin films gradually transformed from the ZnO wurtize structure to an amorphous structure during sample deposition, which suggests the suitability to grow on flexible substrates, eliminating the severe degradation due to fragmentation by repeated bending. The O K- and Zn L{sub 3}-edges XANES spectra of AZO thin films revealed a decrease in the number of both O 2p and Zn 3d unoccupied states when the pressure of Ne was increased from 5 to 100 mTorr. In contrast, Al K-edges XANES spectra showed that the number of unoccupied states of Al 3p increased in conjunction with the pressure of Ne, indicating an electron transfer from Al to O atoms, and suggesting that Al doping increases the negative effective charge of oxygen ions. XES and XANES spectra of O 2p states at the O K-edge also revealed that Al doping not only raised the conduction-band-minimum, but also increased the valence-band-maximum and the band-gap. The results indicate that the reduction in conductivity of AZO thin films is due to the generation of ionic characters, the increase in band-gap, and the decrease in density of unoccupied states of oxygen.

  2. Simultaneous detection of electronic structure changes from two elements of a bifunctional catalyst using wavelength-dispersive X-ray emission spectroscopy and in situ electrochemistry

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Gul, Sheraz; Ng, Jia Wei Desmond; Alonso-Mori, Roberto; Kern, Jan; Sokaras, Dimosthenis; Anzenberg, Eitan; Lassalle-Kaiser, Benedikt; Gorlin, Yelena; Weng, Tsu-Chien; Zwart, Petrus H.; et al

    2015-02-25

    Multielectron catalytic reactions, such as water oxidation, nitrogen reduction, or hydrogen production in enzymes and inorganic catalysts often involve multimetallic clusters. In these systems, the reaction takes place between metals or metals and ligands to facilitate charge transfer, bond formation/breaking, substrate binding, and release of products. In this study, we present a method to detect X-ray emission signals from multiple elements simultaneously, which allows for the study of charge transfer and the sequential chemistry occurring between elements. Kβ X-ray emission spectroscopy (XES) probes charge and spin states of metals as well as their ligand environment. A wavelength-dispersive spectrometer based onmore » the von Hamos geometry was used to disperse Kβ signals of multiple elements onto a position detector, enabling an XES spectrum to be measured in a single-shot mode. This overcomes the scanning needs of the scanning spectrometers, providing data free from temporal and normalization errors and therefore ideal to follow sequential chemistry at multiple sites. We have applied this method to study MnOx-based bifunctional electrocatalysts for the oxygen evolution reaction (OER) and the oxygen reduction reaction (ORR). In particular, we investigated the effects of adding a secondary element, Ni, to form MnNiOx and its impact on the chemical states and catalytic activity, by tracking the redox characteristics of each element upon sweeping the electrode potential. In conclusion, the detection scheme we describe here is general and can be applied to time-resolved studies of materials consisting of multiple elements, to follow the dynamics of catalytic and electron transfer reactions.« less

  3. X-ray generator

    DOE Patents [OSTI]

    Dawson, John M.

    1976-01-01

    Apparatus and method for producing coherent secondary x-rays that are controlled as to direction by illuminating a mixture of high z and low z gases with an intense burst of primary x-rays. The primary x-rays are produced with a laser activated plasma, and these x-rays strip off the electrons of the high z atoms in the lasing medium, while the low z atoms retain their electrons. The neutral atoms transfer electrons to highly excited states of the highly striped high z ions giving an inverted population which produces the desired coherent x-rays. In one embodiment, a laser, light beam provides a laser spark that produces the intense burst of coherent x-rays that illuminates the mixture of high z and low z gases, whereby the high z atoms are stripped while the low z ones are not, giving the desired mixture of highly ionized and neutral atoms. To this end, the laser spark is produced by injecting a laser light beam, or a plurality of beams, into a first gas in a cylindrical container having an adjacent second gas layer co-axial therewith, the laser producing a plasma and the intense primary x-rays in the first gas, and the second gas containing the high and low atomic number elements for receiving the primary x-rays, whereupon the secondary x-rays are produced therein by stripping desired ions in a neutral gas and transfer of electrons to highly excited states of the stripped ions from the unionized atoms. Means for magnetically confining and stabilizing the plasma are disclosed for controlling the direction of the x-rays.

  4. X-ray laser

    DOE Patents [OSTI]

    Nilsen, Joseph

    1991-01-01

    An X-ray laser (10) that lases between the K edges of carbon and oxygen, i.e. between 44 and 23 Angstroms, is provided. The laser comprises a silicon (12) and dysprosium (14) foil combination (16) that is driven by two beams (18, 20) of intense line focused (22, 24) optical laser radiation. Ground state nickel-like dysprosium ions (34) are resonantly photo-pumped to their upper X-ray laser state by line emission from hydrogen-like silicon ions (32). The novel X-ray laser should prove especially useful for the microscopy of biological specimens.

  5. X-Ray Detection

    Office of Scientific and Technical Information (OSTI)

    ratio, I I on I off , recorded with plus (+, blue) and minus (-, red) x-ray helicities. This measurement was taken at -5 mA, which corresponds to a current...

  6. Simulating Ru L3-Edge X-ray Absorption Spectroscopy with Time-Dependent Density Functional Theory: Model Complexes and Electron Localization in Mixed-Valence Metal Dimers

    SciTech Connect (OSTI)

    Kuiken, Benjamin E. Van; Valiev, Marat; Daifuku, Stephanie L.; Bannan, Caitlin; Strader, Matthew L.; Cho, Hana; Huse, Nils; Schoenlein, Robert W.; Govind, Niranjan; Khalil, Munira

    2013-04-26

    Ruthenium L3-edge X-ray absorption (XA) spectroscopy probes unoccupied 4d orbitals of the metal atom and is increasingly being used to investigate the local electronic structure in ground and excited electronic states of Ru complexes. The simultaneous development of computational tools for simulating Ru L3-edge spectra is crucial for interpreting the spectral features at a molecular level. This study demonstrates that time-dependent density functional theory (TDDFT) is a viable and predictive tool for simulating ruthenium L3-edge XA spectroscopy. We systematically investigate the effects of exchange correlation functional and implicit and explicit solvent interactions on a series of RuII and RuIII complexes in their ground and electronic excited states. The TDDFT simulations reproduce all of the experimentally observed features in Ru L3-edge XA spectra within the experimental resolution (0.4 eV). Our simulations identify ligand-specific charge transfer features in complicated Ru L3-edge spectra of [Ru(CN)6]4- and RuII polypyridyl complexes illustrating the advantage of using TDDFT in complex systems. We conclude that the B3LYP functional most accurately predicts the transition energies of charge transfer features in these systems. We use our TDDFT approach to simulate experimental Ru L3-edge XA spectra of transition metal mixed-valence dimers of the form [(NC)5MII-CN-RuIII(NH3)5] (where M = Fe or Ru) dissolved in water. Our study determines the spectral signatures of electron delocalization in Ru L3-edge XA spectra. We find that the inclusion of explicit solvent molecules is necessary for reproducing the spectral features and the experimentally determined valencies in these mixed-valence complexes. This study validates the use of TDDFT for simulating Ru 2p excitations using popular quantum chemistry codes and providing a powerful interpretive tool for equilibrium and ultrafast Ru L3-edge XA spectroscopy.

  7. High resolution soft x-ray spectroscopy of low Z K-shell emission from laser-produced plasmas

    SciTech Connect (OSTI)

    Dunn, J; Magee, E W; Shepherd, R; Chen, H; Hansen, S B; Moon, S J; Brown, G V; Gu, M; Beiersdorfer, P; Purvis, M A

    2008-05-21

    A large radius, R = 44.3 m, High Resolution Grating Spectrometer (HRGS) with 2400 line/mm variable line spacing has been designed for laser-produced plasma experiments conducted at the Lawrence Livermore National Laboratory Jupiter Laser Facility. The instrument has been run with a low-noise, charge-coupled device detector to record high signal-to-noise spectra in the 10-50 {angstrom} wavelength range. The instrument can be run with a 10-20 {micro}m wide slit to achieve the best spectral resolving power, approaching 1000 and similar to crystal spectrometers at 12-20 {angstrom}, or in slitless operation with a small symmetrical emission source. We describe preliminary spectra emitted from various H-like and He-like low Z ion plasmas heated by 100-500 ps (FWHM), 527 nm wavelength laser pulses. This instrument can be developed as a useful spectroscopy platform relevant to laboratory-based astrophysics as well as high energy density plasma studies.

  8. ALS X-Rays Shine a New Light on Catalysis

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    were able to directly observe redox processes in thin-film iron and cobalt perovskite oxide electrocatalysts using surface-sensitive, x-ray absorption spectroscopy while...

  9. X-Ray Fluorescence (XRF) | Open Energy Information

    Open Energy Info (EERE)

    Dispersive Spectroscopy (WDS) typically performed using a SEM or EPMA, and X-Ray Diffraction (XRD) analyses. Rock Lab Analysis Core Analysis Cuttings Analysis Isotopic...

  10. Dissolution of thin iron oxide films used as models for iron passive films studied by in situ X-ray absorption near-edge spectroscopy

    SciTech Connect (OSTI)

    Virtanen, S; Schmuki, P.; Davenport, A.J.; Vitus, C.M.

    1997-01-01

    This paper reports results from X-ray absorption near-edge spectroscopy (XANES) studies during polarization of thin sputter-deposited iron oxide films in acidic solutions. The dissolution rate of iron oxides in acidic solutions was found to be strongly increased by the presence of Fe{sup 2+} in the oxide. During anodic polarization in acidic solutions, it is found that dissolution is accelerated by chloride anions in comparison with sulfates. In HCl solutions of increasing concentration, not only does the pH decrease, but also the increasing chloride concentration accelerates dissolution. On the other hand, the dissolution rate in sulfuric acid does not depend on the sulfate (bisulfate) concentration. During anodic polarization, the dissolution rate is fairly independent of the potential, except at very high anodic potentials, and the XANES spectra reveal no changes in the average oxide valence during anodic polarization. Thus the dissolution that takes place is mostly chemical rather than electrochemical. During cathodic polarization, the dissolution rate is independent of the anion in the electrolyte. The findings are interpreted in terms of the negative surface charge of n-type oxides at potentials lower than the flatband potential, retarding anion adsorption on the surface. Hence it is suggested that the detrimental role of chloride anions on the stability of iron oxide films is due to a surface complexation effect. The findings and their relevance to the stability of natural passive films on iron surfaces are discussed.

  11. X-ray absorption spectroscopy of LiBF 4 in propylene carbonate. A model lithium ion battery electrolyte

    SciTech Connect (OSTI)

    Smith, Jacob W.; Lam, Royce K.; Sheardy, Alex T.; Shih, Orion; Rizzuto, Anthony M.; Borodin, Oleg; Harris, Stephen J.; Prendergast, David; Saykally, Richard J.

    2014-08-20

    Since their introduction into the commercial marketplace in 1991, lithium ion batteries have become increasingly ubiquitous in portable technology. Nevertheless, improvements to existing battery technology are necessary to expand their utility for larger-scale applications, such as electric vehicles. Advances may be realized from improvements to the liquid electrolyte; however, current understanding of the liquid structure and properties remains incomplete. X-ray absorption spectroscopy of solutions of LiBF4 in propylene carbonate (PC), interpreted using first-principles electronic structure calculations within the eXcited electron and Core Hole (XCH) approximation, yields new insight into the solvation structure of the Li+ ion in this model electrolyte. By generating linear combinations of the computed spectra of Li+-associating and free PC molecules and comparing to the experimental spectrum, we find a Li+–solvent interaction number of 4.5. This result suggests that computational models of lithium ion battery electrolytes should move beyond tetrahedral coordination structures.

  12. Probing the f-state configuration of URu2Si2 with U LIII-edge resonant x-ray absorption spectroscopy

    SciTech Connect (OSTI)

    Medling, S. A.; Booth, C. H.; Tobin, J. G.; Baumbach, R. E.; Bauer, E. D.; Sokaras, D.; Nordlund, D.; Weng, T. C.

    2015-09-05

    It has often been said that the most interesting ph- syics occurs when competing interactions are of nearly the same magnitude. Such a situation is surely oc- curing at URu2Si2’s so-called “hidden-order transition”, which garners its name from the missing entropy at a 17.5 K phase transition relative to that expected for a conventional antiferromagnetic phase transition, de- spite the presence of only a very small ordered mag- netic moment.? Despite this discrepancy being identi- fied in 1985, the identification of the order parameter remains elusive, although progress toward understand- ing this transition has been steady since that time, and URu2Si2 remains an important research subject today.? The work described below provides measures of the 5f orbital occupancy and itinerancy using resonant x-ray emission spectroscopy (RXES) at the U LIII absorption edge and measuring U L 1 emission that potentially acts as a dividing line between different classes of “hidden- order” theories.

  13. X-ray fluorescence mapping

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    X-Ray Microscopy and Imaging: X-ray Fluorescence Mapping Of increasing scientific interest is the detection, quantification and mapping of elemental content of samples, often down...

  14. Electron mean free path from angle-dependent photoelectron spectroscopy of aerosol particles

    SciTech Connect (OSTI)

    Goldmann, Maximilian; Miguel-Sánchez, Javier; West, Adam H. C.; Yoder, Bruce L.; Signorell, Ruth

    2015-06-14

    We propose angle-resolved photoelectron spectroscopy of aerosol particles as an alternative way to determine the electron mean free path of low energy electrons in solid and liquid materials. The mean free path is obtained from fits of simulated photoemission images to experimental ones over a broad range of different aerosol particle sizes. The principal advantage of the aerosol approach is twofold. First, aerosol photoemission studies can be performed for many different materials, including liquids. Second, the size-dependent anisotropy of the photoelectrons can be exploited in addition to size-dependent changes in their kinetic energy. These finite size effects depend in different ways on the mean free path and thus provide more information on the mean free path than corresponding liquid jet, thin film, or bulk data. The present contribution is a proof of principle employing a simple model for the photoemission of electrons and preliminary experimental data for potassium chloride aerosol particles.

  15. X-ray microtomography

    SciTech Connect (OSTI)

    Landis, Eric N.; Keane, Denis T.

    2010-12-15

    In this tutorial, we describe X-ray microtomography as a technique to nondestructively characterize material microstructure in three dimensions at a micron level spatial resolution. While commercially available laboratory scale instrumentation is available, we focus our attention on synchrotron-based systems, where we can exploit a high flux, monochromatic X-ray beam to produce high fidelity three-dimensional images. A brief description of the physics and the mathematical analysis behind the technique is followed by example applications to specific materials characterization problems, with a particular focus on the utilization of three-dimensional image processing that can be used to extract a wide range of useful information.

  16. X-ray beam finder

    DOE Patents [OSTI]

    Gilbert, H.W.

    1983-06-16

    An X-ray beam finder for locating a focal spot of an X-ray tube includes a mass of X-ray opaque material having first and second axially-aligned, parallel-opposed faces connected by a plurality of substantially identical parallel holes perpendicular to the faces and a film holder for holding X-ray sensitive film tightly against one face while the other face is placed in contact with the window of an X-ray head.

  17. Evolution of titania nanotubes-supported WO{sub x} species by in situ thermo-Raman spectroscopy, X-ray diffraction and high resolution transmission electron microscopy

    SciTech Connect (OSTI)

    Cortes-Jacome, M.A.; Angeles-Chavez, C.; Morales, M.; Lopez-Salinas, E.; Toledo-Antonio, J.A.

    2007-10-15

    Structural evolution of WO{sub x} species on the surface of titania nanotubes was followed by in situ thermo-Raman spectroscopy. A total of 15 wt% of W atoms were loaded on the surface of a hydroxylated titania nanotubes by impregnation with ammonium metatungstate solution and then, the sample was thermally treated in a Linkam cell at different temperatures in nitrogen flow. The band characteristic of the W=O bond was observed at 962 cm{sup -1} in the dried sample, which vanished between 300 and 700 deg. C, and reappear again after annealing at 800 deg. C, along with a broad band centered at 935 cm{sup -1}, attributed to the v{sub 1} vibration of W=O in tetrahedral coordination. At 900 and 1000 deg. C, the broad band decomposed into four bands at 923, 934, 940 and 950 cm{sup -1}, corresponding to the symmetric and asymmetric vibration of W=O bonds in Na{sub 2}WO{sub 4} and Na{sub 2}W{sub 2}O{sub 7} phases as determined by X-ray diffraction and High resolution transmission electron microscopy (HRTEM). The structure of the nanotubular support was kept at temperatures below 450 deg. C, thereafter, it transformed into anatase being stabilized at temperatures as high as 900 deg. C. At 1000 deg. C, anatase phase partially converted into rutile. After annealing at 1000 deg. C, a core-shell model material was obtained, with a shell of ca. 5 nm thickness, composed of sodium tungstate nanoclusters, and a core composed mainly of rutile TiO{sub 2} phase. - Graphical abstract: Titania nanotubes loaded with 15 wt% W atoms were characterized from room temperature (rt) to 1000 deg. C by thermo-Raman spectroscopy in N{sub 2}. At 1000 deg. C, a core-shell model material was obtained, with a shell thickness of ca. 5 nm composed by nanoclusters of sodium tungstate, and a core composed mainly of rutile TiO{sub 2} phase.

  18. Silicon drift detector based X-ray spectroscopy diagnostic system for the study of non-thermal electrons at Aditya tokamak

    SciTech Connect (OSTI)

    Purohit, S., E-mail: pshishir@ipr.res.in; Joisa, Y. S.; Raval, J. V.; Ghosh, J.; Tanna, R.; Shukla, B. K.; Bhatt, S. B. [Institute for Plasma Research, Bhat, Gandhinagar 382 428 (India)

    2014-11-15

    Silicon drift detector based X-ray spectrometer diagnostic was developed to study the non-thermal electron for Aditya tokamak plasma. The diagnostic was mounted on a radial mid plane port at the Aditya. The objective of diagnostic includes the estimation of the non-thermal electron temperature for the ohmically heated plasma. Bi-Maxwellian plasma model was adopted for the temperature estimation. Along with that the study of high Z impurity line radiation from the ECR pre-ionization experiments was also aimed. The performance and first experimental results from the new X-ray spectrometer system are presented.

  19. Soft-x-ray

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Soft-x-ray emission, plasma equilibrium, and fluctuation studies on Madison Symmetric Torus C. Xiao Department of Physics, University of Wisconsin-Madison, Madison, Wisconsin and Department of Physics and Engineering Physics, University of Saskatchewan, Saskatoon, Canada P. Franz Consorzio RFX-Associazione EURATOM ENEA Sulla Fusione, Italy and Istituto Nazionale di Fisica della Materia, Unita' di Ricerca di Padova, Italy B. E. Chapman and D. Craig Department of Physics, University of

  20. Comparison of galaxy clusters selected by weak-lensing, optical spectroscopy, and X-rays in the deep lens survey F2 field

    SciTech Connect (OSTI)

    Starikova, Svetlana; Jones, Christine; Forman, William R.; Vikhlinin, Alexey; Kurtz, Michael J.; Fabricant, Daniel G.; Murray, Stephen S.; Geller, Margaret J.; Dell'Antonio, Ian P.

    2014-05-10

    We compare galaxy clusters selected in Chandra and XMM-Newton X-ray observations of the 4 deg{sup 2} Deep Lens Survey (DLS) F2 field to the cluster samples previously selected in the same field from a sensitive weak-lensing shear map derived from the DLS and from a detailed galaxy redshift surveythe Smithsonian Hectospec Lensing Survey (SHELS). Our Chandra and XMM-Newton observations cover 1.6 deg{sup 2} of the DLS F2 field, including all 12 weak-lensing peaks above a signal-to-noise ratio of 3.5, along with 16 of the 20 SHELS clusters with published velocity dispersions >500 km s{sup 1}. We detect 26 extended X-ray sources in this area and confirm 23 of them as galaxy clusters using the optical imaging. Approximately 75% of clusters detected in either X-ray or spectroscopic surveys are found in both; these follow the previously established scaling relations between velocity dispersion, L {sub X}, and T {sub X}. A lower percentage, 60%, of clusters are in common between X-ray and DLS samples. With the exception of a high false-positive rate in the DLS weak-lensing search (5 out of 12 DLS candidates appear to be false), differences between the three cluster detection methods can be attributed primarily to observational uncertainties and intrinsic scatter between different observables and cluster mass.

  1. Fluctuation X-Ray Scattering

    SciTech Connect (OSTI)

    Saldin, PI: D. K.; Co-I's: J. C. H. Spence and P. Fromme

    2013-01-25

    The work supported by the grant was aimed at developing novel methods of finding the structures of biomolecules using x-rays from novel sources such as the x-ray free electron laser and modern synchrotrons

  2. Spatiotemporal Monte Carlo transport methods in x-ray semiconductor detectors: Application to pulse-height spectroscopy in a-Se

    SciTech Connect (OSTI)

    Fang Yuan; Badal, Andreu; Allec, Nicholas; Karim, Karim S.; Badano, Aldo

    2012-01-15

    Purpose: The authors describe a detailed Monte Carlo (MC) method for the coupled transport of ionizing particles and charge carriers in amorphous selenium (a-Se) semiconductor x-ray detectors, and model the effect of statistical variations on the detected signal. Methods: A detailed transport code was developed for modeling the signal formation process in semiconductor x-ray detectors. The charge transport routines include three-dimensional spatial and temporal models of electron-hole pair transport taking into account recombination and trapping. Many electron-hole pairs are created simultaneously in bursts from energy deposition events. Carrier transport processes include drift due to external field and Coulombic interactions, and diffusion due to Brownian motion. Results: Pulse-height spectra (PHS) have been simulated with different transport conditions for a range of monoenergetic incident x-ray energies and mammography radiation beam qualities. Two methods for calculating Swank factors from simulated PHS are shown, one using the entire PHS distribution, and the other using the photopeak. The latter ignores contributions from Compton scattering and K-fluorescence. Comparisons differ by approximately 2% between experimental measurements and simulations. Conclusions: The a-Se x-ray detector PHS responses simulated in this work include three-dimensional spatial and temporal transport of electron-hole pairs. These PHS were used to calculate the Swank factor and compare it with experimental measurements. The Swank factor was shown to be a function of x-ray energy and applied electric field. Trapping and recombination models are all shown to affect the Swank factor.

  3. X-ray position detector and implementation in a mirror pointing servo system

    DOE Patents [OSTI]

    Rabedeau, Thomas A.; Van Campen, Douglas G.; Stefan, Peter M.

    2016-04-05

    An X-ray beam position and stability detector is provided having a first metal blade collinear with a second metal blade, where an edge of the first metal blade is opposite an edge of the second metal blade, where the first metal blade edge and the second metal blade edge are disposed along a centerline with respect to each other, where the metal blades are capable of photoelectron emission when exposed to an x-ray beam, a metal coating on the metal blades that is capable of enhancing the photoelectron emission, or suppressing energy-resonant contaminants, or enhancing the photoelectron emission and suppressing energy-resonant contaminants, a background shielding element having an electrode capable of suppressing photoelectron emission from spurious x-rays not contained in an x-ray beam of interest, and a photoelectron emission detector having an amplifier capable of detecting the photoelectron emission as a current signal.

  4. Tunable X-ray source

    DOE Patents [OSTI]

    Boyce, James R.

    2011-02-08

    A method for the production of X-ray bunches tunable in both time and energy level by generating multiple photon, X-ray, beams through the use of Thomson scattering. The method of the present invention simultaneously produces two X-ray pulses that are tunable in energy and/or time.

  5. Surface electronic structure of GaAs(110) studied by Auger photoelectron coincidence spectroscopy

    SciTech Connect (OSTI)

    Bartynski, R.A.; Garrison, K.; Jensen, E.; Hulbert, S.L.; Weinert, M.

    1990-12-31

    We have used Auger photoelectron coincidence spectroscopy to study the M{sub 4,5}VV Auger spectra of GaAs(110). Using this technique, the Ga and As spectra can be separated and studied independently. The lineshape of the As-M{sub 4,5}VV measured in coincidence with the As 3d photoemission line differs significantly from the conventional Auger spectrum. We attribute this to the surface electronic properties of the system. In addition, we have found that the ss-component of the As spectrum is more intense than expected based on calculations using atomic matrix elements. The Ga-M{sub 4,5}VV spectrum, of which only the pp-component is observed, agrees well with that expected from an independent electron model. A first principles electronic structure calculation of a 5-layer GaAs(110) slab has been performed to aid in the interpretation of the Auger spectra.

  6. Surface electronic structure of GaAs(110) studied by Auger photoelectron coincidence spectroscopy

    SciTech Connect (OSTI)

    Bartynski, R.A.; Garrison, K. ); Jensen, E. . Dept. of Physics); Hulbert, S.L.; Weinert, M. )

    1990-01-01

    We have used Auger photoelectron coincidence spectroscopy to study the M{sub 4,5}VV Auger spectra of GaAs(110). Using this technique, the Ga and As spectra can be separated and studied independently. The lineshape of the As-M{sub 4,5}VV measured in coincidence with the As 3d photoemission line differs significantly from the conventional Auger spectrum. We attribute this to the surface electronic properties of the system. In addition, we have found that the ss-component of the As spectrum is more intense than expected based on calculations using atomic matrix elements. The Ga-M{sub 4,5}VV spectrum, of which only the pp-component is observed, agrees well with that expected from an independent electron model. A first principles electronic structure calculation of a 5-layer GaAs(110) slab has been performed to aid in the interpretation of the Auger spectra.

  7. Photodissociation and charge transfer dynamics of negative ions studied with femtosecond photoelectron spectroscopy

    SciTech Connect (OSTI)

    Zanni, Martin T.

    1999-12-17

    This dissertation presents studies aimed at understanding the potential energy surfaces and dynamics of isolated negative ions, and the effects of solvent on each. Although negative ions play important roles in atmospheric and solution phase chemistry, to a large extent the ground and excited state potential energy surfaces of gas phase negative ions are poorly characterized, and solvent effects even less well understood. In an effort to fill this gap, the author's coworkers and the author have developed a new technique, anion femtosecond photoelectron spectroscopy, and applied it to gas phase photodissociation and charge transfer processes. Studies are presented that (1) characterize the ground and excited states of isolated and clustered anions, (2) monitor the photodissociation dynamics of isolated and clustered anions, and (3) explore the charge-transfer-to-solvent states of atomic iodide clustered with polar and non-polar solvents.

  8. Study of radicals, clusters and transition state species by anion photoelectron spectroscopy

    SciTech Connect (OSTI)

    Arnold, D.W.

    1994-08-01

    Free radicals, elemental and van der Waals clusters and transition state species for bimolecular chemical reactions are investigated using anion photoelectron spectroscopy. Several low-lying electronic states of ozone have been identified via photoelectron spectroscopy of O{sub 3}{sup {minus}}. A characterization of these states is important to models for atmospheric ozone reaction kinetics. The fluoroformyloxyl radical, FCO{sub 2}, has been investigated, providing vibrational frequencies and energies for two electronic states. The technique has also been employed to make the first direct observation and characterization of the NNO{sub 2} molecule. Several electronic states are observed for this species which is believed to play a role as a reactive intermediate in the N + NO{sub 2} reaction. The experimental results for all three of these radicals are supplemented by ab initio investigations of their molecular properties. The clusters investigations include studies of elemental carbon clusters (C{sub 2}{sup {minus}} {minus} C{sub 11}{sup {minus}}), and van der Waals clusters (X{sup {minus}}(CO{sub 2}){sub n}, X = I, Br, Cl; n {le} 13 and I{sup {minus}} (N{sub 2}O){sub n=1--11}). Primarily linear clusters are observed for the smaller carbon clusters, while the spectra of the larger clusters contain contribution from cyclic anion photodetachment. Very interesting ion-solvent interactions are observed in the X{sup {minus}}(CO{sub 2})n clusters. The transition state regions for several bimolecular chemical reactions have also been investigated by photodetachment of a negative ion precursor possessing a geometry similar to that of the transition state species. These spectra show features which are assigned to motions of the unstable neutral complex existing between reactants and products.

  9. A new spectrometer design for the x-ray spectroscopy of laser-produced plasmas with high (sub-ns) time resolution

    SciTech Connect (OSTI)

    Bitter, M. Hill, K. W.; Efthimion, P. C.; Delgado-Aparicio, L.; Pablant, N.; Lu, Jian; Beiersdorfer, P.; Chen, Hui

    2014-11-15

    This paper describes a new type of x-ray crystal spectrometer, which can be used in combination with gated x-ray detectors to obtain spectra from laser-produced plasmas with a high (sub-ns) time resolution. The spectrometer consists of a convex, spherically bent crystal, which images individual spectral lines as perfectly straight lines across multiple, sequentially gated, strip detectors. Since the Bragg-reflected rays are divergent, the distance between detector and crystal is arbitrary, so that this distance can be appropriately chosen to optimize the experimental arrangement with respect to the detector parameters. The spectrometer concept was verified in proof-of-principle experiments by imaging the L?{sub 1}- and L?{sub 2}-lines of tungsten, at 9.6735 and 9.96150 keV, from a micro-focus x-ray tube with a tungsten target onto a two-dimensional pixilated Pilatus detector, using a convex, spherically bent Si-422 crystal with a radius of curvature of 500 mm.

  10. X-ray lithography source

    DOE Patents [OSTI]

    Piestrup, M.A.; Boyers, D.G.; Pincus, C.

    1991-12-31

    A high-intensity, inexpensive X-ray source for X-ray lithography for the production of integrated circuits is disclosed. Foil stacks are bombarded with a high-energy electron beam of 25 to 250 MeV to produce a flux of soft X-rays of 500 eV to 3 keV. Methods of increasing the total X-ray power and making the cross section of the X-ray beam uniform are described. Methods of obtaining the desired X-ray-beam field size, optimum frequency spectrum and eliminating the neutron flux are all described. A method of obtaining a plurality of station operation is also described which makes the process more efficient and economical. The satisfying of these issues makes transition radiation an excellent moderate-priced X-ray source for lithography. 26 figures.