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Sample records for addition x-ray photoelectron

  1. X-ray Photoelectron Spectroscopy Database (Version 4.1)

    National Institute of Standards and Technology Data Gateway

    SRD 20 X-ray Photoelectron Spectroscopy Database (Version 4.1) (Web, free access)   The NIST XPS Database gives access to energies of many photoelectron and Auger-electron spectral lines. The database contains over 22,000 line positions, chemical shifts, doublet splittings, and energy separations of photoelectron and Auger-electron lines.

  2. X-ray photoelectron spectroscopy analysis for the chemical impact of solvent addition rate on electromagnetic shielding effectiveness of HCl-doped polyaniline nanopowders

    SciTech Connect

    Tantawy, Hesham Ramzy; Aston, D. Eric; Kengne, Blaise-Alexis F.; McIlroy, David N.; Qiang, You; Nguyen, Tai; Heo, Deukhyoun

    2015-11-07

    An in-depth analysis of the chemical functionality in HCl-doped polyaniline (PANI) nanopowders is discussed through interpretations of x-ray photoelectron spectra. The distinctions between three PANI sample types, produced under varied synthesis conditions, are compared on the basis correlations between newly collected electron spectra for chemical analysis (or also x-ray photoelectron spectroscopy) and electromagnetic (EM) shielding effectiveness (SE) within two frequency bands (100–1500 MHz and ∼2–14 GHz). The findings are discussed with reference to previous data analysis of electrical conductivities and Raman and UV-vis spectra analyzed from replicates of the same PANI nanopowders, where only the 8–12 GHz range for SE was tested. They further corroborate previous results for limited-solvent conditions that enhance EM shielding. The three nanopowder types show distinctive differences in polaron, bipolaron, and polar lattice contributions. The collective findings describe the chemical connections between controlling and, most importantly, limiting the available solvent for polymerization with simultaneously doping and how it is that the newly developed solvent-limited approach for HCl-PANI nanopowders provides better shielding than traditionally solvent-rich methods by having more extended and perhaps even faster polaron delocalization than other PANI-based products. The maximum oxidation (50%) and doping (49%) levels obtained in the solvent-free nanopowders also produced the highest SE values of 37.3 ± 3.7 dB (MHz band) and 68.6 ± 4.6 dB (GHz band)

  3. X-ray photoelectron spectroscopy analysis for the chemical impact of solvent addition rate on electromagnetic shielding effectiveness of HCl-doped polyaniline nanopowders

    NASA Astrophysics Data System (ADS)

    Tantawy, Hesham Ramzy; Kengne, Blaise-Alexis F.; McIlroy, David N.; Nguyen, Tai; Heo, Deukhyoun; Qiang, You; Aston, D. Eric

    2015-11-01

    An in-depth analysis of the chemical functionality in HCl-doped polyaniline (PANI) nanopowders is discussed through interpretations of x-ray photoelectron spectra. The distinctions between three PANI sample types, produced under varied synthesis conditions, are compared on the basis correlations between newly collected electron spectra for chemical analysis (or also x-ray photoelectron spectroscopy) and electromagnetic (EM) shielding effectiveness (SE) within two frequency bands (100-1500 MHz and ˜2-14 GHz). The findings are discussed with reference to previous data analysis of electrical conductivities and Raman and UV-vis spectra analyzed from replicates of the same PANI nanopowders, where only the 8-12 GHz range for SE was tested. They further corroborate previous results for limited-solvent conditions that enhance EM shielding. The three nanopowder types show distinctive differences in polaron, bipolaron, and polar lattice contributions. The collective findings describe the chemical connections between controlling and, most importantly, limiting the available solvent for polymerization with simultaneously doping and how it is that the newly developed solvent-limited approach for HCl-PANI nanopowders provides better shielding than traditionally solvent-rich methods by having more extended and perhaps even faster polaron delocalization than other PANI-based products. The maximum oxidation (50%) and doping (49%) levels obtained in the solvent-free nanopowders also produced the highest SE values of 37.3 ± 3.7 dB (MHz band) and 68.6 ± 4.6 dB (GHz band).

  4. Beyond hard x-ray photoelectron spectroscopy: Simultaneous combination with x-ray diffraction

    SciTech Connect

    Rubio-Zuazo, Juan; Castro, German R.

    2013-05-15

    Hard x-ray photoelectron spectroscopy (HAXPES) is a powerful and novel emerging technique for the nondestructive determination of electronic properties and chemical composition of bulk, buried interfaces and surfaces. It benefits from the exceptionally large escape depth of high kinetic energy photoelectrons, increasing the information depth up to several tens of nanometers. Complementing HAXPES with an atomic structure sensitive technique (such as x-ray diffraction) opens a new research field with major applications for materials science. At SpLine, the Spanish CRG beamline at the European Synchrotron Radiation Facility, we have developed a novel experimental set-up that combines HAXPES and x-ray diffraction (x-ray reflectivity, surface x-ray diffraction, grazing incidence x-ray diffraction, and reciprocal space maps). Both techniques can be operated simultaneously on the same sample and using the same excitation source. The set-up includes a robust 2S + 3D diffractometer hosting a ultrahigh vacuum chamber equipped with a unique photoelectron spectrometer (few eV < electron kinetic energy < 15 keV), x-ray tube (Mg/Ti), 15 keV electron gun, and auxiliary standard surface facilities (molecular beam epitaxy evaporator, ion gun, low energy electron diffraction, sample heating/cooling system, leak valves, load-lock sample transfer, etc.). This end-station offers the unique possibility of performing simultaneous HAXPES + x-ray diffraction studies. In the present work, we describe the experimental set-up together with two experimental examples that emphasize its outstanding capabilities: (i) nondestructive characterization of the Si/Ge and HfO{sub 2}/SiO{sub 2} interfaces on Ge-based CMOS devices, and (ii) strain study on La{sub 0.7}Ca{sub 0.3}MnO{sub 3} ultrathin films grown on SrTiO{sub 3}(001) substrate.

  5. Photoelectron and X-ray Absorption Spectroscopy Of Pu

    SciTech Connect

    Tobin, J; Chung, B; Schulze, R; Farr, J; Shuh, D

    2003-11-12

    We have performed Photoelectron Spectroscopy and X-Ray Absorption Spectroscopy upon highly radioactive samples of Plutonium at the Advanced Light Source in Berkeley, CA, USA. First results from alpha and delta Plutonium are reported as well as plans for future studies of actinide studies.

  6. Interpretation of nanoparticle X-ray photoelectron intensities

    SciTech Connect

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

    2014-06-16

    X-ray photoelectron (XPS) intensities have been simulated for spherical core-shell nanoparticles (NPs) in different geometrical arrangements in order to investigate the validity of commonly made assumptions for the interpretation of XPS NP intensities. The single-sphere approximation is valid for a powder sample when all spatial coordinates of the NP positions are uncorrelated. Correlations along either the depth coordinate or the lateral coordinates lead to features in the angular distribution that provide information on these correlations. The XPS intensity is proportional to the surface-to-volume ratio of nanoparticles but only for NP sizes exceeding the inelastic mean free path of the photoelectrons.

  7. Probing deeper by hard x-ray photoelectron spectroscopy

    SciTech Connect

    Risterucci, P.; Renault, O. Martinez, E.; Delaye, V.; Detlefs, B.; Zegenhagen, J.; Gaumer, C.; Grenet, G.; Tougaard, S.

    2014-02-03

    We report an hard x-ray photoelectron spectroscopy method combining high excitation energy (15 keV) and improved modelling of the core-level energy loss features. It provides depth distribution of deeply buried layers with very high sensitivity. We show that a conventional approach relying on intensities of the core-level peaks is unreliable due to intense plasmon losses. We reliably determine the depth distribution of 1 ML La in a high-κ/metal gate stack capped with 50 nm a-Si. The method extends the sensitivity of photoelectron spectroscopy to depths beyond 50 nm.

  8. X-ray induced damage in DNA monitored by X-ray photoelectron spectroscopy

    SciTech Connect

    Ptasinska, Sylwia; Stypczynska, Agnieszka; Nixon, Tony; Mason, Nigel J.; Klyachko, Dimitri V.; Sanche, Leon

    2008-08-14

    In this work, the chemical changes in calf thymus DNA samples were analyzed by X-ray photoelectron spectroscopy (XPS). The DNA samples were irradiated for over 5 h and spectra were taken repeatedly every 30 min. In this approach the X-ray beam both damages and probes the samples. In most cases, XPS spectra have complex shapes due to contributions of C, N, and O atoms bonded at several different sites. We show that from a comparative analysis of the modification in XPS line shapes of the C 1s, O 1s, N 1s, and P 2p peaks, one can gain insight into a number of reaction pathways leading to radiation damage to DNA.

  9. Effect of X-ray flux on polytetrafluoroethylene in X-ray photoelectron spectroscopy

    NASA Technical Reports Server (NTRS)

    Wheeler, D. R.; Pepper, S. V.

    1982-01-01

    The effect of the X-ray flux in X-ray photoelectron spectroscopy (STAT) on the constitution of the polytetrafluoroethylene (PTFE) surface has been examined. The radiation dose rate for our specimen was about 10 to the 7th rad/s. The structure, magnitude and binding energy of the C(1s) and F(1s) features of the XPS spectrum and the mass spectrum of gaseous species evolved during irradiation are observed. The strong time dependence of these signals over a period of several hours indicated that the surface constitution of PTFE is greatly affected by this level of radiation dose. The results are consistent with the development of a heavily cross-linked or branched structure in the PTFE surface region and the evolution of short chain fragments into the gas phase.

  10. A new endstation at the Swiss Light Source for ultraviolet photoelectron spectroscopy, X-ray photoelectron spectroscopy, and X-ray absorption spectroscopy measurements of liquid solutions

    SciTech Connect

    Brown, Matthew A.; Redondo, Amaia Beloqui; Duyckaerts, Nicolas; Mächler, Jean-Pierre; Jordan, Inga; Wörner, Hans Jakob; Lee, Ming-Tao; Ammann, Markus; Nolting, Frithjof; Kleibert, Armin; Huthwelker, Thomas; Birrer, Mario; Honegger, Juri; Wetter, Reto; Bokhoven, Jeroen A. van

    2013-07-15

    A new liquid microjet endstation designed for ultraviolet (UPS) and X-ray (XPS) photoelectron, and partial electron yield X-ray absorption (XAS) spectroscopies at the Swiss Light Source is presented. The new endstation, which is based on a Scienta HiPP-2 R4000 electron spectrometer, is the first liquid microjet endstation capable of operating in vacuum and in ambient pressures up to the equilibrium vapor pressure of liquid water at room temperature. In addition, the Scienta HiPP-2 R4000 energy analyzer of this new endstation allows for XPS measurements up to 7000 eV electron kinetic energy that will enable electronic structure measurements of bulk solutions and buried interfaces from liquid microjet samples. The endstation is designed to operate at the soft X-ray SIM beamline and at the tender X-ray Phoenix beamline. The endstation can also be operated using a Scienta 5 K ultraviolet helium lamp for dedicated UPS measurements at the vapor-liquid interface using either He I or He II α lines. The design concept, first results from UPS, soft X-ray XPS, and partial electron yield XAS measurements, and an outlook to the potential of this endstation are presented.

  11. Combined x-ray photoelectron spectroscopy and scanning electron microscopy studies of the LiBH4-MgH2 reactive hydride composite with and without a Ti-based additive

    NASA Astrophysics Data System (ADS)

    Deprez, E.; Muñoz-Márquez, M. A.; Jimenez de Haro, M. C.; Palomares, F. J.; Soria, F.; Dornheim, M.; Bormann, R.; Fernández, A.

    2011-01-01

    A detailed electronic and microstructural characterization is reported for the LiBH4-MgH2 reactive hydride composite system with and without titanium isopropoxide as additive. Surface characterization by x-ray photoelectron spectroscopy combined to a morphological study by scanning electron microscopy as well as elemental map composition analysis by energy dispersive x-ray emission are presented in this paper for the first time for all sorption steps. Although sorption reactions are not complete at the surface due to the unavoidable superficial oxidation, it has been shown that the presence of the additive is favoring the heterogeneous nucleation of the MgB2 phase. Ti-based phases appear in all the samples for the three sorption steps well dispersed and uniformly distributed in the material. Li-based phases are highly dispersed at the surface while the Mg-based ones appear, either partially covered by the Li-based phases, or forming bigger grains. Ball milling is promoting mixing of phases and a good dispersion of the additive what favors grain refinement and heterogeneous reactions at the interfaces.

  12. FORTRAN program for x ray photoelectron spectroscopy data reformatting

    NASA Technical Reports Server (NTRS)

    Abel, Phillip B.

    1989-01-01

    A FORTRAN program has been written for use on an IBM PC/XT or AT or compatible microcomputer (personal computer, PC) that converts a column of ASCII-format numbers into a binary-format file suitable for interactive analysis on a Digital Equipment Corporation (DEC) computer running the VGS-5000 Enhanced Data Processing (EDP) software package. The incompatible floating-point number representations of the two computers were compared, and a subroutine was created to correctly store floating-point numbers on the IBM PC, which can be directly read by the DEC computer. Any file transfer protocol having provision for binary data can be used to transmit the resulting file from the PC to the DEC machine. The data file header required by the EDP programs for an x ray photoelectron spectrum is also written to the file. The user is prompted for the relevant experimental parameters, which are then properly coded into the format used internally by all of the VGS-5000 series EDP packages.

  13. Corrosion and degradation studies utilizing X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Hixson, Holly Gwyndolen

    1997-08-01

    This dissertation involves studies of corrosion behavior at the surface of various metal samples, as well as the degradation of wool fibers obtained from the Star-Spangled Banner. Molybdenum metal and iron-zinc alloys were examined under corrosive conditions, and the degradation of the wool fibers was studied. The behavior of a polished molybdenum metal surface upon exposure to both aerated and deaerated water and 1.0 M NaCl solution was studied by X-ray Photoelectron Spectroscopy (XPS). Exposure to deaerated water and NaCl failed to produce oxidation of the metal surfaces, but exposing the polished metal surface to aerated water produced significant oxidation. Metal surfaces cleaned by argon-ion etching were found to be inert to oxidation by aerated water. The etching process also appears to passivate the metal surface. The behavior of molybdenum metal in 0.5 M Hsb2SOsb4 treated at various potentials has been studied using core and valence band XPS. The study indicates that Mosp{IV} and Mosp{VI} (including possibly Mosp{V} in some cases) were formed as the potential of the system was increased within the active range of molybdenum. The corrosive behavior of iron-zinc alloys that have been electroplated on plain steel in both aerated and deaerated quadruply-distilled water has been studied using XPS. Several different iron-zinc alloys were electroplated for comparative purposes: an iron-rich alloy, a zinc-rich alloy, and an alloy of similar iron and zinc composition. Treatment in aerated water produces oxidation for the iron-rich and similar composition alloys, but the oxide is reduced for the zinc-rich alloy. Degradation of the fibers in the original Star-Spangled Banner has been monitored using XPS and Scanning Electron Microscopy (SEM). Comparison of white and red wool fibers and linen fibers from the flag with new, mechanically-abraded, and chemically-treated white, red, and linen fibers, respectively, was performed in an attempt to determine the fibers' levels

  14. X-ray Photoelectron Spectroscopy (XPS), Rutherford Back Scattering (RBS) studies

    NASA Technical Reports Server (NTRS)

    Neely, W. C.; Bozak, M. J.; Williams, J. R.

    1993-01-01

    X-ray photoelectron spectroscopy (XPS), Rutherford Back Scattering (RBS) studies of each of sample received were completed. Since low angle X-ray could not be performed because of instrumentation problems, Auger spectrometry was employed instead. The results of these measurements for each of the samples is discussed in turn.

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

    NASA Astrophysics Data System (ADS)

    Ehre, D.; Cohen, H.

    2013-07-01

    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.

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

    SciTech Connect

    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.

  17. X-Ray Photoelectron Spectroscopy (XPS) Applications Using Microfocused X-Rays

    NASA Astrophysics Data System (ADS)

    Chaney, Robert; Cormia, Robert; Siordia, Ruth

    1986-08-01

    A focusing quartz crystal monochromator system. has been developed that provides a bright X-ray spot at 1486.6ev. The X-ray spot size may he varied from one-hundred fifty (150) to one-thousand (1000) microns in four (4) steps. The X-ray system is combined with a high. performance electron lens that collects greater than five (5) percent of the photoemitted electrons and passes them into a hemispherical capacitor energy analyzer. The electrons are detected at the exit plane with a two (2) dimensional position sensitivity detector. Using this system, XPS has been carried out on a wide variety of practical samples. We will provide a brief review of the system, design followed by examples of the solution to unique problems. Samples which have been CLosen for discussion include: Crash Zone on a Winchester Disk An interocular Lens . Single 5 micron Carbon. Fiber Plasma Modified Polymeric Say The unique benefits of a focused. source with high energy resolution will also be discussed.

  18. X-ray photoelectron spectroscopy peak assignment for perfluoropolyether oils

    NASA Technical Reports Server (NTRS)

    Mori, Shigeyuki; Morales, Wilfredo

    1990-01-01

    Perfluoroalkylpolyether (PFPE) oils are increasingly being used as vacuum pump oils and as lubricants for magnetic recording media and instrumentation for satellites. In this paper, the relative binding energies of three PFPE oils are determined. When sample oils are continuously irradiated during X-ray spectroscopy (XPS) measurements, the relative peak intensity of the spectra is altered significantly, indicating that gaseous products form from the oils during XPS measurements. Thus, attention should be paid to chemical changes when XPE is used to characterize fluorinated carbons such as PFPE oils.

  19. X-ray photoelectron spectroscopy characterization of the {omega} phase in water quenched Ti-5553 alloy

    SciTech Connect

    Qin, Dongyang; Lu, Yafeng; Zhang, Kong; Liu, Qian; Zhou, Lian

    2012-11-15

    X-ray photoelectron spectroscopy was used to investigate the {omega} phase in water quenched Ti-5553 alloy with a nominal composition of Ti-5Al-5V-5Mo-3Cr (wt.%), and the {omega} and the {beta} phase were distinguished by deconvoluting the XPS spectra of Al2p, V2p and Cr2p core level regions. In addition, it is found that the binding energy of core level electron of alloying elements shifts comparing with that of pure metals, and the fact was interpreted by charge redistribution model. X-ray photoelectron spectroscopy technique could be used to characterize the nano-scale {omega} phase in {beta} alloys. - Highlights: Black-Right-Pointing-Pointer We characterize the {omega} phase in Ti-5553 alloy by XPS. Black-Right-Pointing-Pointer Binding energy of Al2p, V2p and Cr2p electron are different in the {omega} and {beta} phase. Black-Right-Pointing-Pointer Structural difference leads to the binding energy gap.

  20. Polytetrafluoroethylene transfer film studied with X-ray photoelectron spectroscopy

    NASA Technical Reports Server (NTRS)

    Wheeler, D. R.

    1980-01-01

    Polytetrafluoroethylene (PTFE) was rubbed against nickel in ultrahigh vacuum at loads up to 3.9 N and speeds up to 94 mm/sec. The transfer film formed on the nickel was analyzed using X-ray phototectron spectroscopy. The film was indistinguishable from bulk PTFE except for the possible presence of a small amount of NiF2. The transfer film was found to be about 1 molecule (0.5 nm) thick under all conditions; but at speeds above 10 mm/sec, there was evidence of bulk transfer in the form of fragments as well. The thickness measurements required a choice among conflicting published values of the inelastic mean free path for electrons in polymers. The values chosen gave internally consistent results.

  1. Development and Trial Measurements of Hard X-ray Photoelectron Emission Microscope

    SciTech Connect

    Taniuchi, T.; Oshima, M.; Wakita, T.; Takagaki, M.; Kawamura, N.; Suzuki, M.; Nakamura, T.; Kobayashi, K.; Akinaga, H.; Muraoka, H.; Ono, K.

    2007-01-19

    Photoelectron emission microscope (PEEM) study is performed using hard x-ray illumination. We have successfully obtained images with high spatial resolution of 40 nm with hard x-rays. Spectro-microscopy of Co micro-patterns on Si substrates, which can be applied to XAFS measurements on a minute scale by PEEM. Magnetic imaging has been demonstrated at the Pt L-edges on perpendicular magnetic recording pattern of CoCrPt alloy. These results are the first step toward a new spectroscopic microscopy and magnetic imaging in a hard x-ray region.

  2. Correlation between N 1s core level x-ray photoelectron and x-ray absorption spectra of amorphous carbon nitride films

    NASA Astrophysics Data System (ADS)

    Quirós, C.; Gómez-García, J.; Palomares, F. J.; Soriano, L.; Elizalde, E.; Sanz, J. M.

    2000-08-01

    This work presents a comparative analysis of the N 1s core level spectra, as measured by x-ray photoelectron spectroscopy (XPS) and x-ray absorption spectroscopy (XAS), of amorphous CNx films which gives evidence of the existing correlation between the different components that constitute the respective spectra. After annealing, the contribution of XPS at 399.3 eV and the components of XAS at 399.6 and 400.8 eV are clearly enhanced. They are assigned to sp2 with two neighbors and to sp states of nitrogen. In addition, the XPS component at 401.3 eV is related to the XAS feature at 402.0 eV and has been assigned to sp2 nitrogen bonded to three carbon neighbors.

  3. Total reflection X-ray photoelectron spectroscopy as a semiconductor lubricant elemental analysis method

    NASA Astrophysics Data System (ADS)

    Alshehabi, Abbas; Sasaki, Nobuharu; Kawai, Jun

    2015-12-01

    Photoelectron spectra from a typical hard disk storage media device (HDD) were measured at total reflection and non-total reflection at unburnished, acetone-cleaned, and argon-sputtered conditions. F, O, N, and C usually making the upper layer of a typical hard disk medium were detected. Enhancement of the photoelectron emission of the fluorocarbon lubricant was observed at total reflection. Pt and Co were only found by non-total X-ray photoelectron spectroscopy (XPS) because they are constituents of a deeper region than the top and interface regions. Argon-sputtered, ultrasonic acetone-cleaned, and unburnished top layers were compared at total and non-total reflection conditions. Total reflection X-ray photoelectron spectroscopy (TRXPS) is demonstrated to be a powerful tool for storage media lubrication layer chemical state analysis, reliable for industrial quality control application , and reproducible.

  4. An x ray photoelectron spectroscopy study of Au(x)In(y) alloys

    NASA Technical Reports Server (NTRS)

    Jayne, Douglas T.; Fatemi, Navid S.; Weizer, Victor G.

    1990-01-01

    Four gold-indium alloys were studied by x ray photoelectron spectroscopy. The binding energies and intensity ratios of the Au 4f7/2 and In 3d5/2 core levels were determined for the bulk alloy compositions of Au(10 percent In), Au3In, AuIn, and AuIn2. These values were determined for the native oxides on the materials, for the surfaces prepared by ion bombardment to remove the oxide and for surfaces scraped in-situ with a ceramic tool to expose the bulk composition. These results furnish calibration values that allow determination of the composition of thin films of this alloy system. In addition the binding energies add to the data base for understanding the effect of alloying on core level binding energies. As an illustration, these results are used to determine the composition of a series of alloy films formed by incongruent evaporation of an alloy charge.

  5. X-Ray Photoelectron Spectroscopy Investigation of the Nitrogen Species in Photoactive Perfluorophenylazide-Modified Surfaces

    PubMed Central

    Zorn, Gilad; Liu, Li-Hong; Árnadóttir, Líney; Wang, Hui; Gamble, Lara J.; Castner, David G.; Yan, Mingdi

    2014-01-01

    X-ray Photoelectron Spectroscopy (XPS) was used to characterize the nitrogen species in perfluorophenylazide (PFPA) self-assembled monolayers. PFPA chemistry is a novel immobilization method for tailoring the surface properties of materials. It is a simple route for the efficient immobilization of graphene, proteins, carbohydrates and synthetic polymers onto a variety of surfaces. Upon light irradiation, the azido group in PFPA is converted to a highly reactive singlet nitrene species that readily undergoes CH insertion and C=C addition reactions. Here, the challenge of characterizing the PFPA modified surfaces was addressed by detailed XPS experimental analyses. The three nitrogen peaks detected in the XPS N1s spectra were assigned to amine/amide (400.5 eV) and azide (402.1 and 405.6 eV) species. The observed 2:1 ratio of the areas from the 402.1 eV to 405.6 eV peaks suggests the assignment of the peak at 402.1 eV to the two outer nitrogen atoms in the azido group and assignment of the peak at 405.6 eV to the central nitrogen atom in the azido group. The azide decomposition as the function of x-ray exposure was also determined. Finally, XPS analyses were conducted on patterned graphene to investigate the covalent bond formation between the PFPA and graphene. This study provides strong evidence for the formation of covalent bonds during the PFPA photocoupling process. PMID:24535931

  6. Structural and electronic characterization of self-assembled molecular nanoarchitectures by X-ray photoelectron spectroscopy.

    PubMed

    Gulino, Antonino

    2013-02-01

    Molecular monolayers and similar nanoarchitectures are indicative of the promising future of nanotechnology. Therefore, many scientists recently devoted their efforts to the synthesis, characterization, and properties of mono- and multilayer-based systems. In this context, X-ray photoelectron spectroscopy is an important technique for the in-depth chemical and structural characterization of nanoscopic systems. In fact, it is a surface technique suitable for probing thicknesses of the same order of the photoelectron inelastic mean free paths (a few tens of ångströms) and allows one to immediately obtain qualitative and quantitative data, film thickness, surface coverage, molecule footprint, oxidation states, and presence of functional groups. Nevertheless, other techniques are important in obtaining a complete spectroscopic characterization of the investigated systems. Therefore, in the present review we report on X-ray photoelectron spectroscopy of self-assembled molecular mono- and multilayer materials including some examples on which other characterization techniques produced important results. PMID:23014858

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

    SciTech Connect

    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. Photoelectron diffraction from laser-aligned molecules with X-ray free-electron laser pulses

    PubMed Central

    Nakajima, Kyo; Teramoto, Takahiro; Akagi, Hiroshi; Fujikawa, Takashi; Majima, Takuya; Minemoto, Shinichirou; Ogawa, Kanade; Sakai, Hirofumi; Togashi, Tadashi; Tono, Kensuke; Tsuru, Shota; Wada, Ken; Yabashi, Makina; Yagishita, Akira

    2015-01-01

    We report on the measurement of deep inner-shell 2p X-ray photoelectron diffraction (XPD) patterns from laser-aligned I2 molecules using X-ray free-electron laser (XFEL) pulses. The XPD patterns of the I2 molecules, aligned parallel to the polarization vector of the XFEL, were well matched with our theoretical calculations. Further, we propose a criterion for applying our molecular-structure-determination methodology to the experimental XPD data. In turn, we have demonstrated that this approach is a significant step toward the time-resolved imaging of molecular structures. PMID:26369428

  9. Optical and x-ray photoelectron spectroscopy studies of α-Al2O3

    NASA Astrophysics Data System (ADS)

    Prakash, Ram; Kumar, Sandeep; Kumar, Vinay; Choudhary, R. J.; Phase, D. M.

    2016-05-01

    α-Al2O3 powder sample was synthesized at 550 °C via solution combustion synthesis (SCS) method using urea as an organic fuel. The sample was characterized by X-ray diffraction (XRD), Optical spectroscopy and X-ray photoelectron spectroscopy (XPS) without any further thermal treatment. XRD study reveals that the powder crystallized directly in the hexagons α-Al2O3 phase. A band gap of 5.7 eV was estimated using diffuse reflectance spectra. For surface investigation X-ray photo electron spectroscopy (XPS) was carried out. The XPS survey scan study of α-Al2O3 powder reveals that the sample is free from impurity. The core levels of Al-2s and O-1s are also reported.

  10. Aqueous Cr(VI) reduction by pyrite: Speciation and characterisation of the solid phases by X-ray photoelectron, Raman and X-ray absorption spectroscopies

    NASA Astrophysics Data System (ADS)

    Mullet, Martine; Demoisson, Frédéric; Humbert, Bernard; Michot, Laurent J.; Vantelon, Delphine

    2007-07-01

    Optical microscopy, confocal Raman micro-spectrometry, X-ray photoelectron micro-spectroscopy (XPS) and synchrotron based micro-X-ray fluorescence (XRF), micro-X-ray absorption near edge spectroscopy (XANES) and micro-extended X-ray absorption fine structure (EXAFS) were used to investigate the reduction of aqueous Cr(VI) by pyrite. Special emphasis was placed on the characterisation of the solid phase formed during the reaction process. Cr(III) and Fe(III) species were identified by XPS analyses in addition to non-oxidised pyrite. Optical microscopy images and the corresponding Raman spectra reveal a strong heterogeneity of the samples with three different types of zones. (i) Reflective areas with Eg and Ag Raman wavenumbers relative to non-oxidised pyrite are the most frequently observed. (ii) Orange areas that display a drift of the Eg and Ag pyrite vibration modes of -3 and -6 cm -1, respectively. Such areas are only observed in the presence of Cr(VI) but are not specifically due to this oxidant. (iii) Bluish areas with vibration modes relative to a corundum-like structure that can be assigned to a solid solution Fe 2- xCr xO 3, x varying between 0.2 and 1.5. The heterogeneity in the spatial distribution of chromium observed by optical microscopy and associated Raman microspectroscopy is confirmed by μ-XRF. In agreement with both solution and XPS analyses, these spectroscopies clearly confirm that chromium is in the trivalent state. XANES spectra in the iron K-edge pre-edge region obtained in rich chromium areas reveal the presence of ferric ion thus revealing a systematic association between Cr(III) and Fe(III). In agreement with Raman analyses, Cr K-edge EXAFS can be interpreted as corresponding to Cr atoms involved in a substituted-type hematite structure Fe 2- xCr xO 3.

  11. Probing buried interfaces with standing-wave excited photoelectron spectroscopy and X-ray emission spectroscopy

    NASA Astrophysics Data System (ADS)

    Sell, Brian C.

    The experiments presented in this thesis are based on a few rather simple ideas that, when put together, can yield impressive amounts of information of relevance to nanoscience and nanotechnology. It is with this philosophy in mind that we will work our way through the generation of x-rays to their excitation of photoelectrons and x-rays to their final use to yield information about buried interfaces in a non-destructive manner. As a first idea, a strong soft x-ray standing wave can be created by irradiating a synthetic multilayer with a monochromatized synchrotron radiation beam at its first-order Bragg angle. The standing wave causes a strong modulation of the magnitude of the electric field inside and above the multilayer. This modulation in turn results in a modulation of the intensity of both photoelectrons and secondary x-rays emitted from the sample as a function of the depth of the emitting atoms below the surface. By growing one layer of the sample as a wedge on top of the multilayer and the other uniform-thickness layers of the sample on top of that, we can by translating the focused x-ray beam across the thickness of the wedge probe the stoichiometric and magnetic properties of the overlayers and their respective interfaces. These measured intensities can then be compared to theoretical calculations which include all x-ray optical effects. This standing wave/wedge approach, which we shall also term the "swedge" method, shows considerable promise for studying a variety of nanostructured materials and devices.

  12. A lab-based ambient pressure x-ray photoelectron spectrometer with exchangeable analysis chambers

    SciTech Connect

    Newberg, John T. Arble, Chris; Goodwin, Chris; Khalifa, Yehia; Broderick, Alicia; Åhlund, John

    2015-08-15

    Ambient pressure X-ray photoelectron spectroscopy (APXPS) is a powerful spectroscopy tool that is inherently surface sensitive, elemental, and chemical specific, with the ability to probe sample surfaces under Torr level pressures. Herein, we describe the design of a new lab-based APXPS system with the ability to swap small volume analysis chambers. Ag 3d(5/2) analyses of a silver foil were carried out at room temperature to determine the optimal sample-to-aperture distance, x-ray photoelectron spectroscopy analysis spot size, relative peak intensities, and peak full width at half maximum of three different electrostatic lens modes: acceleration, transmission, and angular. Ag 3d(5/2) peak areas, differential pumping pressures, and pump performance were assessed under varying N{sub 2}(g) analysis chamber pressures up to 20 Torr. The commissioning of this instrument allows for the investigation of molecular level interfacial processes under ambient vapor conditions in energy and environmental research.

  13. A lab-based ambient pressure x-ray photoelectron spectrometer with exchangeable analysis chambers

    NASA Astrophysics Data System (ADS)

    Newberg, John T.; Åhlund, John; Arble, Chris; Goodwin, Chris; Khalifa, Yehia; Broderick, Alicia

    2015-08-01

    Ambient pressure X-ray photoelectron spectroscopy (APXPS) is a powerful spectroscopy tool that is inherently surface sensitive, elemental, and chemical specific, with the ability to probe sample surfaces under Torr level pressures. Herein, we describe the design of a new lab-based APXPS system with the ability to swap small volume analysis chambers. Ag 3d(5/2) analyses of a silver foil were carried out at room temperature to determine the optimal sample-to-aperture distance, x-ray photoelectron spectroscopy analysis spot size, relative peak intensities, and peak full width at half maximum of three different electrostatic lens modes: acceleration, transmission, and angular. Ag 3d(5/2) peak areas, differential pumping pressures, and pump performance were assessed under varying N2(g) analysis chamber pressures up to 20 Torr. The commissioning of this instrument allows for the investigation of molecular level interfacial processes under ambient vapor conditions in energy and environmental research.

  14. X-ray photoelectron spectroscopy of copper(II), copper(I), and mixed valence systems.

    PubMed

    Rupp, H; Weser, U

    1976-01-01

    X-ray photoelectron spectroscopy using copper(II), copper(I) and the mixed valence Cu(II)/Cu(I) compounds was employed as a means of studying electron transfer reactions in copper proteins. The X-ray photoelectron spectra of copper(II) compounds display characteristic satellites of both variable size and resolution. Some of these satellites could be assigned to specific ligand interactions. Unlike electron paramagnetic resonance spectroscopy, the X-ray photoelectron spectroscopic measurements of copper(I) compounds allowed the unequivocal assignment of this oxidation state. No satellites at all could be detected in the Cu(I) spectra. Furthermore, established mixed valence Cu(II)/Cu(I) complexes including Cu2SO3-CuSO3-2H2O and Cu4Cl5 (ethylenediamine)2 proved essentially a mixture of distinct portions of Cu(I) and Cu(II). This indicates that both oxidation states of copper survive in such complexes. In contrast, all Cu X-ray photoelectron signals of the more tentatively described mixed valence complexes Na2Cu3S3 and the mineral covellite, CuI4CuII2(S2)2S2, could be attributed exclusively to Cu(I). In view of the known binding of copper with sulfur in many copper proteins, it was of utmost importance to study the copper-sulfur interactions. We have demonstrated the absence of Cu(II) in CuS. This indicates strong metal-induced polarization of sulfur resulting in electron transfer to copper to yield Cu(I). PMID:953045

  15. X-ray photoelectron spectroscopy of γ-ray-irradiated single-stranded DNA

    NASA Astrophysics Data System (ADS)

    Lee, Eunmo; Hong, W.; Han, J. H.; Choi, D. M.; Lee, Cheol Eui; Kim, H. D.; Kim, J.

    2015-07-01

    The effects of γ-ray irradiation on herring sperm single-stranded DNA have been studied by using X-ray photoelectron spectroscopy (XPS) in the view of the bonding configurations and the structural modifications. The significant changes in the hydrogen, carbon, nitrogen, and phosphorous bonding energies, as revealed by the XPS analysis, indicate that electron transfers result in the creation of radicals and in DNA strand breaks.

  16. Determination of protein orientation on surfaces with X-ray photoelectron spectroscopy.

    PubMed

    Margalit, R; Vasquez, R P

    1990-02-01

    The use of X-ray photoelectron spectroscopy (XPS) for determination of the preferred orientation of proteins on metal surfaces is demonstrated. A myoglobin derivative in which a pentaamineruthenium (III) group is attached to a specific histidine (residue 81) is used for this purpose, with the Ru and Fe acting as a double marker. The relative intensities of the XPS photoelectron spectra for these two markers are shown to be a sensitive measure of orientation of the protein film. On both aluminum and indium-tin-oxide surfaces, XPS indicates that the Ru-Fe axis of the myoglobin derivative is preferentially oriented with the Ru furthest from the substrate. PMID:2340069

  17. Characterization of plasma fluorinated zirconia for dental applications by X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Wolter, S. D.; Piascik, J. R.; Stoner, B. R.

    2011-09-01

    This paper discusses fluorination of biomedical-grade yttria-stabilized zirconia (YSZ) by sulfur hexafluoride plasma treatment and characterization of near-surface chemistry products by X-ray photoelectron spectroscopy (XPS). Deconvolution of the Zr 3d and Y 3d XPS core level spectra revealed formation of both ZrF4 and YF3. In addition, seven-coordinate ZrO2F5 and/or ZrO3F4 phases were deconvolved, retaining similar atomic coordination as the parent oxide and believed to have formed by substitutional displacement of oxygen by fluorine. No additional components attributed to yttria oxyfluoride were deconvolved. Argon ion sputter depth profiling determined the overlayer to be ∼4.0 nm in thickness, and angle resolved XPS showed no angle dependence on component percentages likely due to fluorination extending into the grain boundaries of the polycrystalline substrates. Importantly, the conversion layer did not induce any apparent change in zirconia crystallinity by inspection of Zr-O 3d5/2,3/2 peak positions and full-width-at-half-maximum values, important for retaining its desirable mechanical properties.

  18. X-ray photoelectron spectroscopic and Raman analysis of silk fibroin-Cu(II) films.

    PubMed

    Zhou, Li; Chen, Xin; Dai, Weilin; Shao, Zhengzhong

    2006-06-01

    There is evidence to suggest that Cu(II) is involved in the natural spinning process of a silkworm helping to convert the concentrated silk fibroin (SF) solution (or dope) into tough insoluble threads. To investigate the interaction between SF and Cu(II), a series of regenerated SF (RSF) films with different mass ratios of Cu(II) to SF were prepared. X-ray photoelectron spectroscopy (XPS) was employed to study the chemical interaction between Cu(II) and SF in these Cu(II)-RSF films. A significant change in the binding energy of Cu 2p(3/2) demonstrated that the chemical state of Cu(II) in the Cu(II)-RSF films was affected by the interaction between Cu(II) and SF. Moreover, chemical shifts of N 1s and O 1s of SF were also detected, implying that Cu(II) may coordinate with both N and O atoms in the SF. In addition, Raman spectra of the same series of Cu(II)-RSF films recorded the conformation transition of SF that may occur by the coordination of Cu(II) and SF macromolecular chains. PMID:16463361

  19. X-ray photoelectron spectroscopy as a probe of rhodium-ligand interaction in ionic liquids

    NASA Astrophysics Data System (ADS)

    Men, Shuang; Lovelock, Kevin R. J.; Licence, Peter

    2016-02-01

    We use X-ray photoelectron spectroscopy (XPS) to identify the interaction between the rhodium atom and phosphine ligands in six 1-octyl-3-methylimidazolium-based ionic liquids ([C8C1Im][X]). The formation of a mono-phosphine rhodium complex based upon addition of triphenylphosphine (PPh3) is confirmed by XPS in all ionic liquids studied herein. Due to the electron donation effect of the ligand, the rhodium atom becomes more negatively charged and thus exhibits a lower measured binding energy. The influence of the anion basicity on the formation of different types of rhodium complexes is also investigated. By introducing a biphosphine ligand, a chelated diphosphine rhodium complex is formed in ionic liquids with more basic anions and verified by both XPS and Infrared Spectroscopy (IR). The measured Rh 3d binding energies are correlated to the reaction selectivity of a hydroformylation reaction which inspires a method to design a metal catalyst to control the chemical reaction towards desired products in the future.

  20. X-ray photoelectron spectroscopy of select multi-layered transition metal carbides (MXenes)

    DOE PAGESBeta

    Halim, Joseph; Cook, Kevin M.; Naguib, Michael; Eklund, Per; Gogotsi, Yury; Rosen, Johanna; Barsoum, Michel W.

    2015-12-01

    A detailed high resolution X-ray photoelectron spectroscopy (XPS) analysis is presented in this work for select MXenes—a recently discovered family of two-dimensional (2D) carbides and carbonitrides. Given their 2D nature, understanding their surface chemistry is paramount. Thus we identify and quantify the surface groups present before, and after, sputter-cleaning as well as freshly prepared vs. aged multi-layered cold pressed discs. The nominal compositions of the MXenes studied here are Ti3C2Tx, Ti2CTx, Ti3CNTx, Nb2CTx and Nb4C3Tx, where T represents surface groups that this work attempts to quantify. In all the cases, the presence of three surface terminations, single bondO, single bondOHmore » and single bondF, in addition to OH-terminations relatively strongly bonded to H2O molecules, was confirmed. Moreover, from XPS peak fits, it was possible to establish the average sum of the negative charges of the terminations for the aforementioned MXenes. Based on this work, it is now possible to quantify the nature of the surface terminations. This information can, in turn, be used to better design and tailor these novel 2D materials for various applications.« less

  1. X-ray photoelectron spectroscopy of select multi-layered transition metal carbides (MXenes)

    SciTech Connect

    Halim, Joseph; Cook, Kevin M.; Naguib, Michael; Eklund, Per; Gogotsi, Yury; Rosen, Johanna; Barsoum, Michel W.

    2015-12-01

    A detailed high resolution X-ray photoelectron spectroscopy (XPS) analysis is presented in this work for select MXenes—a recently discovered family of two-dimensional (2D) carbides and carbonitrides. Given their 2D nature, understanding their surface chemistry is paramount. Thus we identify and quantify the surface groups present before, and after, sputter-cleaning as well as freshly prepared vs. aged multi-layered cold pressed discs. The nominal compositions of the MXenes studied here are Ti3C2Tx, Ti2CTx, Ti3CNTx, Nb2CTx and Nb4C3Tx, where T represents surface groups that this work attempts to quantify. In all the cases, the presence of three surface terminations, single bondO, single bondOH and single bondF, in addition to OH-terminations relatively strongly bonded to H2O molecules, was confirmed. Moreover, from XPS peak fits, it was possible to establish the average sum of the negative charges of the terminations for the aforementioned MXenes. Based on this work, it is now possible to quantify the nature of the surface terminations. This information can, in turn, be used to better design and tailor these novel 2D materials for various applications.

  2. Study of the oxidation of gold-tin preforms using x-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Taylor, J. Ashley; Merchant, Sailesh M.; Perry, D. L.

    1995-11-01

    This study uses x-ray photoelectron spectroscopy (XPS) to investigate the nature of the oxide formed on clean Au-Sn binary alloys (ζ and δ phases) and on preforms with the eutectic composition (29 at % Sn) at low O2 pressures (<10-3 Torr) and at high O2 pressures (up to one atmosphere) at temperatures ranging from room temperature to 200 °C. Sn Auger parameters and XPS angular-resolved data were obtained in addition to the core binding energies to identify the oxide layer. The oxidation of the Au-Sn alloys is basically similar to the oxidation of metallic Sn. The Auger parameter indicates that with low-pressure oxidation a layered oxide structure is formed consisting of SnO and a slightly tin-rich oxide at the interface. Probably a thin skin of Sn(IV) oxide exists on the outer surface of the low-pressure oxide. High-temperature and low-pressure promotes the growth of SnO. As the pressure is increased the Sn(IV) oxide grows more noticeably and with high-pressure oxidation the Sn(IV) oxide grows thicker than the Sn(II) oxide at the interface. The Sn(II) oxide at the interface appears similar to the Sn(II) oxide structure formed at low pressure. The Auger parameter indicates that the Sn(IV) oxide possesses a structure different than that of Cassiterite.

  3. X-ray photoelectron spectroscopy of select multi-layered transition metal carbides (MXenes)

    NASA Astrophysics Data System (ADS)

    Halim, Joseph; Cook, Kevin M.; Naguib, Michael; Eklund, Per; Gogotsi, Yury; Rosen, Johanna; Barsoum, Michel W.

    2016-01-01

    In this work, a detailed high resolution X-ray photoelectron spectroscopy (XPS) analysis is presented for select MXenes-a recently discovered family of two-dimensional (2D) carbides and carbonitrides. Given their 2D nature, understanding their surface chemistry is paramount. Herein we identify and quantify the surface groups present before, and after, sputter-cleaning as well as freshly prepared vs. aged multi-layered cold pressed discs. The nominal compositions of the MXenes studied here are Ti3C2Tx, Ti2CTx, Ti3CNTx, Nb2CTx and Nb4C3Tx, where T represents surface groups that this work attempts to quantify. In all the cases, the presence of three surface terminations, sbnd O, sbnd OH and sbnd F, in addition to OH-terminations relatively strongly bonded to H2O molecules, was confirmed. From XPS peak fits, it was possible to establish the average sum of the negative charges of the terminations for the aforementioned MXenes. Based on this work, it is now possible to quantify the nature of the surface terminations. This information can, in turn, be used to better design and tailor these novel 2D materials for various applications.

  4. Characterization of an Yb:LuVO 4 single crystal using X-ray topography, high-resolution X-ray diffraction, and X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Paszkowicz, W.; Romanowski, P.; Bąk-Misiuk, J.; Wierzchowski, W.; Wieteska, K.; Graeff, W.; Iwanowski, R. J.; Heinonen, M. H.; Ermakova, O.; Dąbkowska, H.

    2011-10-01

    Knowledge on the defect and electronic structure allows for improved modeling of material properties. A short literature review has shown that the information on defect structure of rare earth orthovanadate single crystals is limited. In this paper, defect and electronic structure of a needle-shaped Yb:LuVO 4 single crystal grown by the slow cooling method have been studied by means of X-ray diffraction topography employing white synchrotron beam, high-resolution diffraction (HRD) and photoelectron spectroscopy (XPS) techniques. Topographic investigations show that the crystal is composed of two blocks disoriented by about 1.5° and separated by a narrow deformed region. Some contrasts observed within the crystal volume may be attributed to glide bands and sector boundaries. The contrasts appearing in the vicinity of the surface may be interpreted as due to the presence of small inclusions. The HRD study indicates, in particular, that among point defects, the vacancy type defects dominate and that the density of other defects is small in comparison. The XPS measurements enabled, despite highly insulating properties of the studied crystal, an analysis of its bulk electronic structure, including the main core-levels (O 1 s, V 2 p, Lu 4 f) as well as the valence band range.

  5. X-ray and photoelectron spectroscopy of the structure, reactivity, and electronic structure of semiconductor nanocrystals

    SciTech Connect

    Hamad, K.S.

    2000-05-01

    Semiconductor nanocrystals are a system which has been the focus of interest due to their size dependent properties and their possible use in technological applications. Many chemical and physical properties vary systematically with the size of the nanocrystal and thus their study enables the investigation of scaling laws. Due to the increasing surface to volume ratio as size is decreased, the surfaces of nanocrystals are expected to have a large influence on their electronic, thermodynamic, and chemical behavior. In spite of their importance, nanocrystal surfaces are still relatively uncharacterized in terms of their structure, electronic properties, bonding, and reactivity. Investigation of nanocrystal surfaces is currently limited by what techniques to use, and which methods are suitable for nanocrystals is still being determined. This work presents experiments using x-ray and electronic spectroscopies to explore the structure, reactivity, and electronic properties of semiconductor (CdSe, InAs) nanocrystals and how they vary with size. Specifically, x-ray absorption near edge spectroscopy (XANES) in conjunction with multiple scattering simulations affords information about the structural disorder present at the surface of the nanocrystal. X-ray photoelectron spectroscopy (XPS) and ultra-violet photoelectron spectroscopy (UPS) probe the electronic structure in terms of hole screening, and also give information about band lineups when the nanocrystal is placed in electric contact with a substrate. XPS of the core levels of the nanocrystal as a function of photo-oxidation time yields kinetic data on the oxidation reaction occurring at the surface of the nanocrystal.

  6. Effect of X-ray spot size on liquid jet photoelectron spectroscopy

    PubMed Central

    Olivieri, Giorgia; Goel, Alok; Kleibert, Armin; Brown, Matthew A.

    2015-01-01

    A 30 µm pinhole is introduced in the intermediate focus of the SIM beamline at the Swiss Light Source to improve the spot size at the second downstream focus, which is used here for liquid jet X-ray photoelectron spectroscopy experiments. The 30 µm pinhole reduces the beam dimensions from 250 (v) × 100 (h) µm to 75 × 45 µm for a vertical exit slit of 100 µm. The smaller X-ray spot results in a substantial decrease in the gas-phase contribution of the spectra from 40% down to 20% and will help to simplify the interpretation and peak assignments of future experiments. PMID:26524318

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

    SciTech Connect

    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.

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

    SciTech Connect

    Masuda, Takuya; Yoshikawa, Hideki; Kobata, Masaaki; Kobayashi, Keisuke; Noguchi, Hidenori; Kawasaki, Tadahiro; Uosaki, Kohei

    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.

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

    SciTech Connect

    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.

  10. Comparison of hard and soft x-ray photoelectron spectra of silicon

    NASA Astrophysics Data System (ADS)

    Offi, F.; Werner, W. S. M.; Sacchi, M.; Torelli, P.; Cautero, M.; Cautero, G.; Fondacaro, A.; Huotari, S.; Monaco, G.; Paolicelli, G.; Smekal, W.; Stefani, G.; Panaccione, G.

    2007-08-01

    A detailed comparison of the surface sensitivity of x-ray photoemission spectroscopy for hard and soft x rays is presented and discussed. Electron scattering parameters and their energy dependence are given for Si and two Si spectra are analyzed: a MgKα (hν=1253.6eV) excited spectrum of the Si2p and 2s lines and a hard x-ray excited spectrum (hν=5925eV) of the Si1s line. The differential inelastic scattering characteristics for Si are extracted from reflection electron energy loss spectra taken at energies of 1500 and 4000eV . Using these scattering characteristics and electron mean free paths from the literature, simulated spectra are compared with experiment. The experimental spectra are deconvoluted to give the true intrinsic line shape corresponding to the theoretical collision statistics when interference effects between intrinsic and extrinsic scattering are neglected. The magnitude of interference effects cannot be assessed by our analysis. Within the (unknown) uncertainty introduced by neglecting interference effects, it is possible to determine the relative intensity of intrinsic and extrinsic excitations. In this way, it is found that in the case of the soft x-ray excited photoelectron spectrum of the shallower electronic shells ( 2p and 2s ), intrinsic plasmon creation is rather weak, and the apparent asymmetric line shape of the spectrum might be interpreted as the fact that electron-hole pair creation dominates the intrinsic loss spectrum, while an alternative explanation in terms of surface core level shifted components is also proposed. For the deeper core electronic shell, probed with hard x rays, the opposite situation is observed: while intrinsic electron-hole pair creation was not observed, a strong contribution of intrinsic plasmon losses of about 30% was seen.

  11. Composition of RF-sputtered refractory compounds determined by X-ray photoelectron spectroscopy

    NASA Technical Reports Server (NTRS)

    Wheeler, D. R.; Brainard, W. A.

    1978-01-01

    RF-sputtered coatings of CrB2, MoSi2, Mo2C, TiC, and MoS2 were examined by X-ray photoelectron spectroscopy (XPS). Data on stoichiometry, impurity content, and chemical bonding were obtained. The influences of sputtering target history, deposition time, RF power level, and substrate bias were studied. Significant deviations from stoichiometry and high oxide levels were related to target outgassing. The effect of substrate bias depended on the particular coating material studied.

  12. A study of synthetic and natural uranium oxides by X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Teterin, Yu. A.; Kulakov, V. M.; Baev, A. S.; Nevzorov, N. B.; Melnikov, I. V.; Streltsov, V. A.; Mashirov, L. G.; Suglobov, D. N.; Zelenkov, A. G.

    1981-09-01

    Synthetic and natural uranium oxides UO x (2≦×≦3) have been studied with X-ray photoelectron spectroscopy (XPS) to determine the phase composition and content of uranium ions in uraninites with a varying degree of oxidation. A strong hybridization of U6 p and O2 s orbitals has been found which permits a quantitative assessment of the U-O bond lengths. The values of such bonds in some substances have been found to be smaller than those in synthetic U(VI) oxide. The oxides U2O5 and U3O8 contain two types of uranium ions with a varying degree of oxidation.

  13. X-ray-excited photoelectron detection using a scanning tunneling microscope

    SciTech Connect

    Rose, V.; Freeland, J. W.; Gray, K. E.; Streiffer, S. K.

    2008-05-12

    Detection of x-ray-enhanced electrons emitted by synchrotron radiation with the tip of a scanning tunneling microscope has the potential to open a path to high-resolution microscopy with chemical sensitivity. Nonresonant photoejected electrons typically yield a current background of a few hundred picoamperes at a bare tip. Coating the tip with an insulating boron nitride film can effectively reduce this background. In this configuration, we have quantitatively studied the bias dependent photoelectron collection for tip/sample separations of 400-1600 nm, where quantum mechanical tunneling does not contribute.

  14. Near-Edge X-Ray Absorption Fine Structures Revealed in Core Ionization Photoelectron Spectroscopy

    NASA Astrophysics Data System (ADS)

    Nakano, M.; Selles, P.; Lablanquie, P.; Hikosaka, Y.; Penent, F.; Shigemasa, E.; Ito, K.; Carniato, S.

    2013-09-01

    Simultaneous core ionization and core excitation have been observed in the C2H2n (n=1, 2, 3) molecular series using synchrotron radiation and a magnetic bottle time-of-flight electron spectrometer. Rich satellite patterns corresponding to (K-2V) core excited states of the K-1 molecular ions have been identified by detecting in coincidence the photoelectron with the two Auger electrons resulting from the double core hole relaxation. A theoretical model is proposed providing absolute photoionization cross sections and revealing clear signatures of direct (monopolar) and conjugate (dipolar near-edge x-ray absorption fine structure) shakeup lines of comparable magnitude.

  15. Near-edge x-ray absorption fine structures revealed in core ionization photoelectron spectroscopy.

    PubMed

    Nakano, M; Selles, P; Lablanquie, P; Hikosaka, Y; Penent, F; Shigemasa, E; Ito, K; Carniato, S

    2013-09-20

    Simultaneous core ionization and core excitation have been observed in the C(2)H(2n) (n=1, 2, 3) molecular series using synchrotron radiation and a magnetic bottle time-of-flight electron spectrometer. Rich satellite patterns corresponding to (K(-2)V) core excited states of the K(-1) molecular ions have been identified by detecting in coincidence the photoelectron with the two Auger electrons resulting from the double core hole relaxation. A theoretical model is proposed providing absolute photoionization cross sections and revealing clear signatures of direct (monopolar) and conjugate (dipolar near-edge x-ray absorption fine structure) shakeup lines of comparable magnitude. PMID:24093255

  16. Oxidation of stepped Pt(111) studied by x-ray photoelectron spectroscopy and density functional theory

    SciTech Connect

    Bandlow, Jochen; Kaghazchi, Payam; Jacob, Timo; Papp, C.; Traenkenschuh, B.; Streber, R.; Lorenz, M. P. A.; Fuhrmann, T.; Steinrueck, H.-P.; Denecke, R.

    2011-05-01

    In this comparative density functional theory and x-ray photoelectron spectroscopy study on the interaction of oxygen with stepped Pt(111) surfaces, we show that both the initial adsorption and oxidation occur at the steps rather than terraces. An equivalent behavior was observed for the oxide formation at higher chemical potentials, where, after the formation of a one-dimensional PtO{sub 2}-type oxide at the steps, similar oxide chains form on the (111) terraces, indicating the initial stages of bulk oxide formation.

  17. Calculation of Ar photoelectron satellites in the hard-x-ray region

    NASA Astrophysics Data System (ADS)

    Yarzhemsky, V. G.; Amusia, M. Ya.

    2016-06-01

    The intensities of photoelectron satellite lines, corresponding to the double core hole (DCH) states of Ar 1 s ionization by hard x rays, are calculated using the many-body perturbation theory. Calculations support the interpretation of the most intense lines as the shake-up excitations 2 p →4 p . It is demonstrated that the intensities of the spectrum lines corresponding to 4 s (and 3 d ) excited states in the DCH field can be explained only taking into account the knock-up process 2 p →3 d along with the shake-up process 1 s →4 s that accompanies 2 p photoionization.

  18. Ultrafast soft X-ray photoelectron spectroscopy at liquid water microjets.

    PubMed

    Faubel, M; Siefermann, K R; Liu, Y; Abel, B

    2012-01-17

    Since the pioneering work of Kai Siegbahn, electron spectroscopy for chemical analysis (ESCA) has been developed into an indispensable analytical technique for surface science. The value of this powerful method of photoelectron spectroscopy (PES, also termed photoemission spectroscopy) and Siegbahn's contributions were recognized in the 1981 Nobel Prize in Physics. The need for high vacuum, however, originally prohibited PES of volatile liquids, and only allowed for investigation of low-vapor-pressure molecules attached to a surface (or close to a surface) or liquid films of low volatility. Only with the invention of liquid beams of volatile liquids compatible with high-vacuum conditions was PES from liquid surfaces under vacuum made feasible. Because of the ubiquity of water interfaces in nature, the liquid water-vacuum interface became a most attractive research topic, particularly over the past 10 years. PES studies of these important aqueous interfaces remained significantly challenging because of the need to develop high-pressure PES methods. For decades, ESCA or PES (termed XPS, for X-ray photoelectron spectroscopy, in the case of soft X-ray photons) was restricted to conventional laboratory X-ray sources or beamlines in synchrotron facilities. This approach enabled frequency domain measurements, but with poor time resolution. Indirect access to time-resolved processes in the condensed phase was only achieved if line-widths could be analyzed or if processes could be related to a fast clock, that is, reference processes that are fast enough and are also well understood in the condensed phase. Just recently, the emergence of high harmonic light sources, providing short-wavelength radiation in ultrashort light pulses, added the dimension of time to the classical ESCA or XPS technique and opened the door to (soft) X-ray photoelectron spectroscopy with ultrahigh time resolution. The combination of high harmonic light sources (providing radiation with laserlike

  19. Depth-resolved soft x-ray photoelectron emission microscopy in nanostructures via standing-wave excited photoemission

    SciTech Connect

    Kronast, F.; Ovsyannikov, R.; Kaiser, A.; Wiemann, C.; Yang, S.-H.; Locatelli, A.; Burgler, D.E.; Schreiber, R.; Salmassi, F.; Fischer, P.; Durr, H.A.; Schneider, C.M.; Eberhardt, W.; Fadley, C.S.

    2008-11-24

    We present an extension of conventional laterally resolved soft x-ray photoelectron emission microscopy. A depth resolution along the surface normal down to a few {angstrom} can be achieved by setting up standing x-ray wave fields in a multilayer substrate. The sample is an Ag/Co/Au trilayer, whose first layer has a wedge profile, grown on a Si/MoSi2 multilayer mirror. Tuning the incident x-ray to the mirror Bragg angle we set up standing x-ray wave fields. We demonstrate the resulting depth resolution by imaging the standing wave fields as they move through the trilayer wedge structure.

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

    SciTech Connect

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

    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 liquid 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.

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

    DOE PAGESBeta

    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

  2. Using “Tender” X-ray Ambient Pressure X-Ray Photoelectron Spectroscopy as A Direct Probe of Solid-Liquid Interface

    PubMed Central

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

    2015-01-01

    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 liquid 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. PMID:25950241

  3. Using “Tender” X-ray Ambient Pressure X-Ray Photoelectron Spectroscopy as A Direct Probe of Solid-Liquid Interface

    NASA Astrophysics Data System (ADS)

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

    2015-05-01

    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 liquid 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.

  4. Repair and Utilization of the Kratos XSAM 800 X-Ray Photoelectron Spectrometer (XPS)

    NASA Technical Reports Server (NTRS)

    Hampton, Michael D.

    2002-01-01

    The objectives for this summer faculty fellowship were first to repair the Kratos XSAM 800 X-ray Photoelectron Spectrometer (XPS) and then to utilize the instrument to participate in ongoing research projects at KSC and in the researcher's own laboratory at UCF. The first 6 weeks were used in repairing the instrument. Working both alone and with the Kratos service engineer, a number of hardware problems, largely associated with the sample stage control system, were corrected. Defective parts were identified and fixed in the computer driver boards, the stage power supply, and the driver interface. The power supply was completely replaced. After four weeks of work, the instrument was functional. This occurred on a Wednesday. The following Friday the instrument had to be completely shut down because the power to the O & C Building was to be turned off. The instrument was properly secured. On Monday, the instrument was powered up and the original problems returned. After another 2 weeks of work, a software problem was identified. This problem caused the computer to use a defective port for the sample stage control. It was circumvented by rewriting the startup routine. The final 3 weeks of the fellowship were spent using the XPS to analyze samples being studied in the Langley materials project (Martha Williams) and a catalyst project (Dr. Orlando Melendez). During this time, several sample analysis requests from other groups at KSC also came in and those samples were run as well. The summer faculty fellowship also allowed many contacts to be made. After meeting with the sensors group, two projects were identified for collaboration and white papers are being prepared. One project aims to develop small, very sensitive hydrogen detectors and the other to develop a broad area, easily monitored, zero power consumption hydrogen detector. In addition to the work mentioned above, the XPS was utilized in a study underway in Dr. Hampton's laboratory at UCF.

  5. Repair and Utilization of the Kratos XSAM 800 X-Ray Photoelectron Spectrometer (XPS)

    NASA Astrophysics Data System (ADS)

    Hampton, Michael D.

    2002-06-01

    The objectives for this summer faculty fellowship were first to repair the Kratos XSAM 800 X-ray Photoelectron Spectrometer (XPS) and then to utilize the instrument to participate in ongoing research projects at KSC and in the researcher's own laboratory at UCF. The first 6 weeks were used in repairing the instrument. Working both alone and with the Kratos service engineer, a number of hardware problems, largely associated with the sample stage control system, were corrected. Defective parts were identified and fixed in the computer driver boards, the stage power supply, and the driver interface. The power supply was completely replaced. After four weeks of work, the instrument was functional. This occurred on a Wednesday. The following Friday the instrument had to be completely shut down because the power to the O & C Building was to be turned off. The instrument was properly secured. On Monday, the instrument was powered up and the original problems returned. After another 2 weeks of work, a software problem was identified. This problem caused the computer to use a defective port for the sample stage control. It was circumvented by rewriting the startup routine. The final 3 weeks of the fellowship were spent using the XPS to analyze samples being studied in the Langley materials project (Martha Williams) and a catalyst project (Dr. Orlando Melendez). During this time, several sample analysis requests from other groups at KSC also came in and those samples were run as well. The summer faculty fellowship also allowed many contacts to be made. After meeting with the sensors group, two projects were identified for collaboration and white papers are being prepared. One project aims to develop small, very sensitive hydrogen detectors and the other to develop a broad area, easily monitored, zero power consumption hydrogen detector. In addition to the work mentioned above, the XPS was utilized in a study underway in Dr. Hampton's laboratory at UCF.

  6. X-Ray Photoelectron Spectroscopic Analysis of the Oxide of GaAs

    NASA Astrophysics Data System (ADS)

    Ishikawa, Toshifumi; Ikoma, Hideaki

    1992-12-01

    Oxides of GaAs grown using various oxidation processes were analyzed with X-ray photoelectron spectroscopy (XPS). Oxides investigated were the native (naturally grown or exposed to air), the chemical (grown in boiling deionized water) and the thermal (at 350°C and 500°C in dry oxygen) ones. With the use of a spectral deconvolution technique, all types of suboxides of both As and Ga including elemental arsenic were observed in addition to well-known As2O3 and Ga2O3. Elemental arsenic is considered to be one of the oxidized forms of GaAs. As2O5 was observed in the thermal oxides. In the chemical oxide and the native oxide grown in short exposure to air, elemental arsenic is the main component of oxide, while As2O3 is the dominant species in more highly oxidized films such as the thermal oxide. XPS data suggest that oxidation of As bonded in GaAs proceeds as GaAs→elemental As (As0)→As2O (As1+)→AsO (As2+)→As2O3 (As3+)→As2O5 (As5+). Oxidation of Ga bonded in GaAs advances as GaAs→Ga2O (Ga1+)→GaO (Ga2+)→Ga2O3 (Ga3+). Angle-resolved XPS measurements and semiquantitative analyses of these data were performed and an effective thickness of each oxide was also derived with simplified assumptions. The native and the chemical oxides were nearly stoichiometric. However, the thermal oxide was substantially Ga-rich due to desorption and evaporation of As2O3 from the surface during oxidation.

  7. The behavior of stainless steels in physiological solution containing complexing agent studied by X-ray photoelectron spectroscopy.

    PubMed

    Milosev, I; Strehblow, H H

    2000-11-01

    The passive film formed by electrochemical oxidation on two different stainless steels differing in molybdenum (Mo) content in physiological solution with and without the addition of complexing agent, i.e., citrate, was studied using X-ray photoelectron spectroscopy. The alloys were polarized at different oxidation potentials in the electrochemical chamber attached to the spectrometer. Thus, the composition of the film formed by oxidation was analyzed by X-ray photoelectron spectroscopy without prior exposure to air (quasi in situ). The passive film formed in physiological solution consists of two predominant oxides, i.e., chromium and iron oxides. Oxides of alloying elements nickel and Mo are also detected in the film. It seems that the strong enrichment of oxidized chromium and Mo in the passive layer, and strong enrichment of Mo and depletion of iron at the metal surface underneath the passive layer, are responsible for the outstanding corrosion resistance of orthopedic stainless steel in physiological solution. Commercial AISI 304 is not suitable for orthopedic applications. The addition of complexing agent affects significantly the passivation behavior of orthopedic stainless steel, because it changes the distribution of the elements within the passive layer and at the metal surface underneath. PMID:10951382

  8. Quantitative spectromicroscopy from inelastically scattered photoelectrons in the hard X-ray range

    NASA Astrophysics Data System (ADS)

    Renault, O.; Zborowski, C.; Risterucci, P.; Wiemann, C.; Grenet, G.; Schneider, C. M.; Tougaard, S.

    2016-07-01

    We demonstrate quantitative, highly bulk-sensitive x-ray photoelectron emission microscopy by analysis of inelastically scattered photoelectrons in the hard X-ray range, enabling elemental depth distribution analysis in deeply buried layers. We show results on patterned structures used in electrical testing of high electron mobility power transistor devices with an epitaxial Al0.25Ga0.75N channel and a Ti/Al metal contact. From the image series taken over an energy range of up to 120 eV in the Ti 1s loss feature region and over a typical 100 μm field of view, one can accurately retrieve, using background analysis together with an optimized scattering cross-section, the Ti depth distribution from 14 nm up to 25 nm below the surface. The method paves the way to multi-elemental, bulk-sensitive 3D imaging and investigation of phenomena at deeply buried interfaces and microscopic scales by photoemission.

  9. Evaluation of polymeric standard reference materials for monitoring the performance of X-ray photoelectron spectrometers

    NASA Astrophysics Data System (ADS)

    Strohmeier, Brian R.

    1991-04-01

    The use of standard reference materials is a common practice in X-ray photoelectron spectroscopy (XPS or ESCA). Recently, several polymeric standard reference materials have become available for monitoring various performance aspects of ESCA spectrometers. These reference materials include polyethylene (PE), polyethylene glycol (PEG), polytetrafluoroethylene (PTFE) and dimethyl silicon (DMS). The advantages and disadvantages encountered when using these materials as standards were investigated in this study. Results indicated that PEG, PTFE and DMS are useful standards for checking or determining relative elemental sensitivity factors for C, O, F and/or Si. These three materials can also be used for monitoring the linearity and stability of the instrumental binding energy scale. However, in general, metallic standards such as gold, silver and/or copper are superior to the polymeric standards for this purpose, because their photoelectron lines cover a wider binding energy range and their respective peak positions are much better known. Although PE exhibits a fairly narrow C1s line that can be used to monitor variations in the instrumental energy resolution, the FWHM observed for the C1s line is much broader that the FWHM values obtained from the appropriate lines of sputtered-cleaned metals. Results also indicated that the use of PTFE as a standard reference material must be done with caution, because PTFE readily degrades with time under X-ray exposure.

  10. X-ray photoelectron spectroscopy of graphitic carbon nanomaterials doped with heteroatoms

    PubMed Central

    Pichler, Thomas; Ayala, Paola

    2015-01-01

    Summary X-ray photoelectron spectroscopy (XPS) is one of the best tools for studying the chemical modification of surfaces, and in particular the distribution and bonding of heteroatom dopants in carbon nanomaterials such as graphene and carbon nanotubes. Although these materials have superb intrinsic properties, these often need to be modified in a controlled way for specific applications. Towards this aim, the most studied dopants are neighbors to carbon in the periodic table, nitrogen and boron, with phosphorus starting to emerge as an interesting new alternative. Hundreds of studies have used XPS for analyzing the concentration and bonding of dopants in various materials. Although the majority of works has concentrated on nitrogen, important work is still ongoing to identify its precise atomic bonding configurations. In general, care should be taken in the preparation of a suitable sample, consideration of the intrinsic photoemission response of the material in question, and the appropriate spectral analysis. If this is not the case, incorrect conclusions can easily be drawn, especially in the assignment of measured binding energies into specific atomic configurations. Starting from the characteristics of pristine materials, this review provides a practical guide for interpreting X-ray photoelectron spectra of doped graphitic carbon nanomaterials, and a reference for their binding energies that are vital for compositional analysis via XPS. PMID:25671162

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

    SciTech Connect

    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.

  12. Quantitative interpretation of molecular dynamics simulations for X-ray photoelectron spectroscopy of aqueous solutions.

    PubMed

    Olivieri, Giorgia; Parry, Krista M; Powell, Cedric J; Tobias, Douglas J; Brown, Matthew A

    2016-04-21

    Over the past decade, energy-dependent ambient pressure X-ray photoelectron spectroscopy(XPS) has emerged as a powerful analytical probe of the ion spatial distributions at the vapor (vacuum)-aqueous electrolyteinterface. These experiments are often paired with complementary molecular dynamics (MD) simulations in an attempt to provide a complete description of the liquidinterface. There is, however, no systematic protocol that permits a straightforward comparison of the two sets of results. XPS is an integrated technique that averages signals from multiple layers in a solution even at the lowest photoelectron kinetic energies routinely employed, whereas MD simulations provide a microscopic layer-by-layer description of the solution composition near the interface. Here, we use the National Institute of Standards and Technology database for the Simulation of Electron Spectra for Surface Analysis (SESSA) to quantitatively interpret atom-density profiles from MD simulations for XPS signal intensities using sodium and potassium iodide solutions as examples. We show that electron inelastic mean free paths calculated from a semi-empirical formula depend strongly on solution composition, varying by up to 30% between pure water and concentrated NaI. The XPS signal thus arises from different information depths in different solutions for a fixed photoelectron kinetic energy. XPS signal intensities are calculated using SESSA as a function of photoelectron kinetic energy (probe depth) and compared with a widely employed ad hoc method. SESSA simulations illustrate the importance of accounting for elastic-scattering events at low photoelectron kinetic energies (<300 eV) where the ad hoc method systematically underestimates the preferential enhancement of anions over cations. Finally, some technical aspects of applying SESSA to liquidinterfaces are discussed. PMID:27389231

  13. Quantitative interpretation of molecular dynamics simulations for X-ray photoelectron spectroscopy of aqueous solutions

    NASA Astrophysics Data System (ADS)

    Olivieri, Giorgia; Parry, Krista M.; Powell, Cedric J.; Tobias, Douglas J.; Brown, Matthew A.

    2016-04-01

    Over the past decade, energy-dependent ambient pressure X-ray photoelectron spectroscopy (XPS) has emerged as a powerful analytical probe of the ion spatial distributions at the vapor (vacuum)-aqueous electrolyte interface. These experiments are often paired with complementary molecular dynamics (MD) simulations in an attempt to provide a complete description of the liquid interface. There is, however, no systematic protocol that permits a straightforward comparison of the two sets of results. XPS is an integrated technique that averages signals from multiple layers in a solution even at the lowest photoelectron kinetic energies routinely employed, whereas MD simulations provide a microscopic layer-by-layer description of the solution composition near the interface. Here, we use the National Institute of Standards and Technology database for the Simulation of Electron Spectra for Surface Analysis (SESSA) to quantitatively interpret atom-density profiles from MD simulations for XPS signal intensities using sodium and potassium iodide solutions as examples. We show that electron inelastic mean free paths calculated from a semi-empirical formula depend strongly on solution composition, varying by up to 30% between pure water and concentrated NaI. The XPS signal thus arises from different information depths in different solutions for a fixed photoelectron kinetic energy. XPS signal intensities are calculated using SESSA as a function of photoelectron kinetic energy (probe depth) and compared with a widely employed ad hoc method. SESSA simulations illustrate the importance of accounting for elastic-scattering events at low photoelectron kinetic energies (<300 eV) where the ad hoc method systematically underestimates the preferential enhancement of anions over cations. Finally, some technical aspects of applying SESSA to liquid interfaces are discussed.

  14. Electronic Structures of Uranium Compounds Studied by Soft X-ray Photoelectron Spectroscopy

    NASA Astrophysics Data System (ADS)

    Fujimori, Shin-ichi; Takeda, Yukiharu; Okane, Tetsuo; Saitoh, Yuji; Fujimori, Atsushi; Yamagami, Hiroshi; Haga, Yoshinori; Yamamoto, Etsuji; Ōnuki, Yoshichika

    2016-06-01

    The electronic structures of uranium-based compounds have been studied by photoelectron spectroscopy with soft X-ray synchrotron radiation. Angle-resolved photoelectron spectroscopy with soft X-rays has made it possible to directly observe their bulk band structures and Fermi surfaces. It has been shown that the band structures and Fermi surfaces of itinerant compounds such as UB2, UN, and UFeGa5 are quantitatively described by a band-structure calculation treating all U 5f electrons as itinerant. Furthermore, the overall electronic structures of heavy-fermion compounds such as UPd2Al3, UNi2Al3, and URu2Si2 are also explained by a band-structure calculation, although some disagreements exist, which might originate from the electron correlation effect. This suggests that the itinerant description of U 5f states is an appropriate starting point for the description of their electronic structures. The situation is similar for ferromagnetic superconductors such as UGe2, URhGe, UCoGe, and UIr, although the complications from their low-symmetry crystal structures make it more difficult to describe their detailed electronic structures. The local electronic structures of the uranium site have been probed by core-level photoelectron spectroscopy with soft X-rays. The comparisons of core-level spectra of heavy-fermion compounds with typical itinerant and localized compounds suggest that the local electronic structures of most itinerant and heavy-fermion compounds are close to the U 5f3 configuration except for UPd2Al3 and UPt3. The core-level spectrum of UPd2Al3 has similarities to those of both itinerant and localized compounds, suggesting that it is located at the boundary between the itinerant and localized states. Moreover, the spectrum of UPt3 is very close to that of the localized compound UPd3, suggesting that it is nearly localized, although there are narrow quasi-particle bands in the vicinity of EF.

  15. Capturing interfacial photoelectrochemical dynamics with picosecond time-resolved X-ray photoelectron spectroscopy.

    PubMed

    Neppl, Stefan; Shavorskiy, Andrey; Zegkinoglou, Ioannis; Fraund, Matthew; Slaughter, Daniel S; Troy, Tyler; Ziemkiewicz, Michael P; Ahmed, Musahid; Gul, Sheraz; Rude, Bruce; Zhang, Jin Z; Tremsin, Anton S; Glans, Per-Anders; Liu, Yi-Sheng; Wu, Cheng Hao; Guo, Jinghua; Salmeron, Miquel; Bluhm, Hendrik; Gessner, Oliver

    2014-01-01

    Time-resolved core-level spectroscopy using laser pulses to initiate and short X-ray pulses to trace photoinduced processes has the unique potential to provide electronic state- and atomic site-specific insight into fundamental electron dynamics in complex systems. Time-domain studies using transient X-ray absorption and emission techniques have proven extremely valuable to investigate electronic and structural dynamics in isolated and solvated molecules. Here, we describe the implementation of a picosecond time-resolved X-ray photoelectron spectroscopy (TRXPS) technique at the Advanced Light Source (ALS) and its application to monitor photoinduced electron dynamics at the technologically pertinent interface formed by N3 dye molecules anchored to nanoporous ZnO. Indications for a dynamical chemical shift of the Ru3d photoemission line originating from the N3 metal centre are observed ∼30 ps after resonant HOMO-LUMO excitation with a visible laser pump pulse. The transient changes in the TRXPS spectra are accompanied by a characteristic surface photovoltage (SPV) response of the ZnO substrate on a pico- to nanosecond time scale. The interplay between the two phenomena is discussed in the context of possible electronic relaxation and recombination pathways that lead to the neutralisation of the transiently oxidised dye after ultrafast electron injection. A detailed account of the experimental technique is given including an analysis of the chemical modification of the nano-structured ZnO substrate during extended periods of solution-based dye sensitisation and its relevance for studies using surface-sensitive spectroscopy techniques. PMID:25415599

  16. X-ray photoelectron spectroscopic analysis of rice kernels and flours: Measurement of surface chemical composition.

    PubMed

    Nawaz, Malik A; Gaiani, Claire; Fukai, Shu; Bhandari, Bhesh

    2016-12-01

    The objectives of this study were to evaluate the ability of X-ray photoelectron spectroscopy (XPS) to differentiate rice macromolecules and to calculate the surface composition of rice kernels and flours. The uncooked kernels and flours surface composition of the two selected rice varieties, Thadokkham-11 (TDK11) and Doongara (DG) demonstrated an over-expression of lipids and proteins and an under-expression of starch compared to the bulk composition. The results of the study showed that XPS was able to differentiate rice polysaccharides (mainly starch), proteins and lipids in uncooked rice kernels and flours. Nevertheless, it was unable to distinguish components in cooked rice samples possibly due to complex interactions between gelatinized starch, denatured proteins and lipids. High resolution imaging methods (Scanning Electron Microscopy and Confocal Laser Scanning Microscopy) were employed to obtain complementary information about the properties and location of starch, proteins and lipids in rice kernels and flours. PMID:27374542

  17. X-ray photoelectron spectroscopy study of chemically-etched Nd-Ce-Cu-O surfaces

    NASA Technical Reports Server (NTRS)

    Vasquez, R. P.; Gupta, A.; Kussmaul, A.

    1991-01-01

    Acetic acid, Br2, and HCl solutions are investigated for removing insulating species from Nd(1.85)Ce(0.15)CuO(4-delta) (NCCO) thin film surfaces. X-ray photoelectron spectroscopy (XPS) shows that the HCl etch is most effective, yielding O 1s spectra comparable to those obtained from samples cleaned in vacuum and a clear Fermi edge in the valence band region. Reduction and oxidation reversibly induces and eliminates, respectively, Fermi level states for undoped samples, but has no clearly observable effect on the XPS spectra for doped samples. Reactivity to air is much less for NCCO compared to hole superconductors, which is attributed to the lack of reactive alkaline earth elements in NCCO.

  18. Probing DNA hybridization efficiency and single base mismatch by X-ray photoelectron spectroscopy.

    PubMed

    Liu, Zheng-Chun; Zhang, Xin; He, Nong-Yue; Lu, Zu-Hong; Chen, Zhen-Cheng

    2009-07-01

    We demonstrated the use of X-ray photoelectron spectroscopy (XPS) to study DNA hybridization. Target DNA labeled with hexachloro-fluorescein (HEX) was hybridized to DNA arrays with four different probes. Each probe dot of the hybridized arrays was detected with XPS. The XPS Cl2p peak areas were found to decrease with an increase in mismatched bases in DNA probes. The Cl2p core-level peak area ratio of a probe perfectly matched to one, two and three base-mismatched probes accorded well with the results of conventional fluorescent imaging, which shows that XPS is a potential tool for analyzing DNA arrays. The DNA arrays' hybridization efficiency was assessed by the molar ratio of chlorine to phosphorus in a DNA strand, which was determined from the relevant XPS Cl2p and P2p core-level peak areas after hybridization. This could provide a new method to detect DNA hybridization efficiency. PMID:19282155

  19. Uses of Auger and x ray photoelectron spectroscopy in the study of adhesion and friction

    NASA Technical Reports Server (NTRS)

    Miyoshi, Kazuhisa

    1990-01-01

    Three studies are described characterizing the possible contributions of surface science to tribology. These include surface contamination formed by the interaction of a surface with the environment, contaminants obtained with diffusion of compounds, and surface chemical changes resulting from selective thermal evaporation. Surface analytical tools such as Auger electron spectroscopy (AES) and x ray photoelectron spectroscopy (XPS) incorporated directly into adhesion and friction systems are primarily used to define the nature of tribological surfaces before and after tribological experimentation and to characterize the mechanism of solid-to-solid interaction. Emphasis is on fundamental studies involving the role of surfaces in controlling the adhesion and friction properties of materials emerging as a result of the surface analyses. The materials which were studied include metals and ceramics such as elemental metals, amorphous alloys (metallic glasses), and silicon-based ceramics.

  20. X-ray photoelectron spectroscopy study of radiofrequency-sputtered refractory compound steel interfaces

    NASA Technical Reports Server (NTRS)

    Wheeler, D. R.; Brainard, W. A.

    1978-01-01

    Radiofrequency sputtering was used to deposit Mo2C, Mo2B5, and MoSi2 coatings on 440C steel substrates. Both sputter etched and preoxidized substrates were used, and the films were deposited with and without a substrate bias of -300 V. The composition of the coatings was measured as a function of depth by X-ray photoelectron spectroscopy combined with argon ion etching. In the interfacial region there was evidence that bias produced a graded interface in Mo2B5 but not in Mo2C. Oxides of iron and of all film constituents except carbon were presented in all cases but the iron oxide concentration was higher and the layer thicker on the preoxidized substrates. The film and iron oxides were mixed in the MoSi2 and Mo2C films but layered in the Mo2B5 film. The presence of mixed oxides correlates with enhanced film adhesion.

  1. Measurement of barrier height of Pd on diamond (100) surface by X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Li, F. N.; Liu, J. W.; Zhang, J. W.; Wang, X. L.; Wang, W.; Liu, Z. C.; Wang, H. X.

    2016-05-01

    Barrier height (ФBH) values for Pd/hydrogen-terminated diamond (H-diamond) and Pd/oxygen-terminated diamond (O-diamond) have been investigated by X-ray photoelectron spectroscopy technique. H-diamond and O-diamond have been formed on the same diamond (100) layer grown by microwave plasma-enhanced chemical vapor deposition,on which Pd layers have been evaporated. The ФBH values for Pd/H-diamond and Pd/O-diamond are determined to be -0.27 eV and 1.73 eV, respectively. It indicates that Pd is a suitable metal for ohmic and Schottky contacts on H-diamond and O-diamond, respectively. The experimental ΦBH values are in good agreement with the theoretical calculation results.

  2. Relaxation of Cs atomic polarization at surface coatings characterized by X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Kushida, Kotaro; Niwano, Toshihiro; Moriya, Takemasa; Shimizu, Tomohito; Meguro, Kazuki; Nakazawa, Hideki; Hatakeyama, Atsushi

    2015-06-01

    Paraffin coatings on glass slides were investigated through both X-ray photoelectron spectroscopy (XPS) and spin relaxation measurement for cesium (Cs) vapor. The components of the glass substrate, such as silicon and oxygen, existed in the XPS spectra of the coated slides, indicating the imperfection of the prepared paraffin coatings. The substrate was not observed after the annealing of the coatings in Cs vapor, which is known as a “ripening” process for spin relaxation measurement. We found a general trend that effective anti-spin relaxation performance requires high paraffin and low Cs coverage on the surface. We also examined a type of diamond-like carbon film, anticipating the effect of anti-spin relaxation; our attempts have failed to date.

  3. X-ray photoelectron spectroscopy study of catalyzed aluminum carbide formation at aluminum-carbon interfaces

    NASA Technical Reports Server (NTRS)

    Rabenberg, L.; Maruyama, Benji

    1990-01-01

    Aluminum carbide may form at aluminum-graphite interfaces during the high-temperature processing of graphite fiber-reinforced aluminum metal matrix composites. The chemical interactions leading to the formation of the aluminum carbide in the solid state involve the breaking of the carbon-carbon bonds within the graphite, the transport of the carbon atoms across the interface, and the reaction with the aluminum to form Al4C3. The aluminum carbide formation process has been followed using X-ray photoelectron spectroscopy of model, thin-film, reaction couples. The overall reaction is shown to be catalyzed by the presence of water vapor. Water at the interface increases reaction kinetics by apparently weakening the bonds between the surface carbon atoms and their substrate. This result is in general agreement with what is known to occur during the oxidation of graphite in air.

  4. Hydrogenation and dehydrogenation of nitrogen-doped graphene investigated by X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Späth, F.; Zhao, W.; Gleichweit, C.; Gotterbarm, K.; Bauer, U.; Höfert, O.; Steinrück, H.-P.; Papp, C.

    2015-04-01

    We studied the hydrogenation and dehydrogenation of nitrogen-doped graphene (NDG) by in situ high-resolution X-ray photoelectron spectroscopy (XPS) and temperature-programmed XPS (TPXPS). Nitrogen-doped graphene was prepared by low energy nitrogen implantation in pristine graphene on Ni(111). Hydrogenation of NDG was performed by exposure to atomic hydrogen. Upon hydrogenation the XP spectra in the C 1s region reveal one new peak, shifted to lower binding energies as compared to graphene, which is associated with newly formed CH groups. In the N 1s region two new peaks, shifted to higher binding energies are observed; these are associated with hydrogenated pyridinic and graphitic nitrogen. TPXPS spectra reveal a different thermal stability of the two hydrogenated nitrogen species, while the C-H groups of graphene show no significant changes compared to undoped hydrogenated graphene.

  5. Angularly resolved X-ray photoelectron spectroscopy investigation of PTFE after prolonged space exposure

    NASA Technical Reports Server (NTRS)

    Dalins, I.; Karimi, M.

    1992-01-01

    Monochromatized angularly resolved X-ray photoelectron spectroscopy (ARXPS) was used to study PTFE (Teflon) that had been exposed to an earth orbital environment for approximately six years. The primary interest of the research is on a very reactive component of this environment (atomic oxygen) which, because of the typical orbital velocities of a spacecraft, impinge on exposed surfaces with 5 eV energy. This presentation deals with the method of analysis, the findings as they pertain to a rather complex carbon, oxygen, and fluorine XPS peak analysis, and the character of the valence bands. An improved bias referencing method, based on ARXPS, is also demonstrated for evaluating specimen charging effects. It was found that the polymer molecule tends to resist the atomic oxygen attack by reorienting itself, so that the most electronegative CF3 groups are facing the incoming hyperthermal oxygen atoms. The implications of these findings to ground-based laboratory studies are discussed.

  6. X-ray photoelectron and mass spectroscopic study of electron irradiation and thermal stability of polytetrafluoroethylene

    NASA Technical Reports Server (NTRS)

    Wheeler, Donald R.; Pepper, Stephen V.

    1990-01-01

    Polytetrafluoroethylene (PTFE) was subjected to 3 keV electron bombardment and then heated in vacuum to 300 C. The behavior of the material as a function of radiation dose and temperature was studied by X-ray photoelectron spectroscopy (XPS) of the surface and mass spectroscopy of the species evolved. A quantitative comparison of the radiation dose rate with that in other reported studies showed that, for a given total dose, the damage observed by XPS is greater for higher dose rates. Lightly damaged material heated to 300 C evolved saturated fluorocarbon species, whereas unsaturated fluorocarbon species evolved from heavily damaged material. After heating the heavily damaged material, those features in the XPS that were associated with damage diminished, giving the appearance that the radiation damage annealed. The apparent annealing of the radiation damage was found to be due to the covering of the network by saturated fragments that easily diffused through the decomposed material to the surface region upon heating.

  7. Determination of InN/Diamond Heterojunction Band Offset by X-ray Photoelectron Spectroscopy

    PubMed Central

    2011-01-01

    Diamond is not only a free standing highly transparent window but also a promising carrier confinement layer for InN based devices, yet little is known of the band offsets in InN/diamond system. X-ray photoelectron spectroscopy was used to measure the energy discontinuity in the valence band offset (VBO) of InN/diamond heterostructure. The value of VBO was determined to be 0.39 ± 0.08 eV and a type-I heterojunction with a conduction band offset (CBO) of 4.42 ± 0.08 eV was obtained. The accurate determination of VBO and CBO is important for the application of III-N alloys based electronic devices.

  8. X-Ray Photoelectron Spectroscopy (XPS) of Bacteriorhodopsin Analogues Synthesized from Fluorophenyl Retinals

    NASA Astrophysics Data System (ADS)

    Takahashi, Masae; Takahashi, Takashi; Tokunaga, Fumio; Murano, Kentaro; Tsujimoto, Kazuo; Sagawa, Takasi

    1984-04-01

    The two external point-charge (TEPC) model for bacteriorhodopsin (bR) has been examined by X-ray photoelectron spectroscopy (XPS) and CNDO/S molecular orbital calculations. A main concern was given to a point charge near the β-ionone ring. XPS measurements were carried out on fluorophenyl retinal (F-ret) and their derivatives (Schiff base, protonated Schiff base and bacteriorhodopsin analogues (F-bR)), paying close attention to the chemical shift of the F 1s core level. No meaningful differences were observed among these species although numerical calculations on an assumption of the TEPC model have predicted the chemical shift of about 3 eV between F-ret and F-bR. This fact has arisen a serious question to the validity of the TEPC model. The same conclusion has been reached by the present study of absorption maxima of F-ret and their derivatives.

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

    NASA Astrophysics Data System (ADS)

    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 HfO2 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 × 10-6 for 445 nm illumination.

  10. X-ray laser-induced time-of-flight photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Nelson, Art J.; Dunn, James; van Buuren, Tony W.; Hunter, Jim; Smith, Ray F.; Hemmers, Oliver; Lindle, Dennis W.

    2003-12-01

    X-ray laser induced time-of-flight photoelectron spectroscopy has been used to probe the core-level and valence band electronic structure of room-temperature bulk materials with picosecond time resolution. The LLNL COMET compact tabletop x-ray laser source provides the necessary high photon flux, high energy, monochromaticity, picosecond pulse duration, and coherence for probing ultrafast changes in the chemical and electronic structure of these materials. Valence band and core-level spectra were recorded for transition metal surfaces. In situ sputter etching with Ar ions at 30° incidence will be implemented to improve the surface purity and consequently increase core-level and valence-band photoemission intensity. This work demonstrates a powerful new technique for probing reaction dynamics and for probing changes of local order on surfaces on their fundamental timescales. Future work will include the study of fundamental phenomena such as non-thermal melting, chemical bond formation, intermediate reaction steps, and the existence of transient reaction products.

  11. In situ high-resolution X-ray photoelectron spectroscopy - Fundamental insights in surface reactions

    NASA Astrophysics Data System (ADS)

    Papp, Christian; Steinrück, Hans-Peter

    2013-11-01

    Since the advent of third generation synchrotron light sources optimized for providing soft X-rays up to 2 keV, X-ray photoelectron spectroscopy (XPS) has been developed to be an outstanding tool to study surface properties and surface reactions at an unprecedented level. The high resolution allows identifying various surface species, and for small molecules even the vibrational fine structure can be resolved in the XP spectra. The high photon flux reduces the required measuring time per spectrum to the domain of a few seconds or even less, which enables to follow surface processes in situ. Moreover, it also provides access to very small coverages down to below 0.1% of a monolayer, enabling the investigation of minority species or processes at defect sites. The photon energy can be adjusted according to the requirement of a particular experiment, i.e., to maximize or minimize the surface sensitivity or the photoionization cross-section of the substrate or the adsorbate. For a few instruments worldwide, a next step forward was taken by combining in situ high-resolution spectrometers with supersonic molecular beams. These beams allow to control and vary the kinetic and internal energies of the incident molecules and provide a local pressure of up to ~10-5 mbar, which can be switched on and off in a controllable way, thus offering a well-defined time structure to study adsorption or reaction processes.

  12. X-ray photoelectron spectroscopy and luminescent properties of Y2O3:Bi3+ phosphor

    NASA Astrophysics Data System (ADS)

    Jafer, R. M.; Coetsee, E.; Yousif, A.; Kroon, R. E.; Ntwaeaborwa, O. M.; Swart, H. C.

    2015-03-01

    X-ray photoelectron spectroscopy (XPS) results provided proof for the blue and green emission of Bi3+ in the Y2O3:Bi3+ phosphor. The Y2O3:Bi3+ phosphor was successfully prepared by the combustion process during the investigation of down-conversion materials for Si solar cell application. The X-ray diffraction (XRD) patterns indicated that a single-phase cubic crystal structure with the Ia3 space group was formed. X-ray photoelectron spectroscopy (XPS) showed that the Bi3+ ion replaces the Y3+ ion in two different coordination sites in the Y2O3 crystal structure. The O 1s peak shows five peaks, two which correlate with the O2- ion in Y2O3 in the two different sites, two which correlate with O2- in Bi2O3 in the two different sites and the remaining peak relates to hydroxide. The Y 3d spectrum shows two peaks for the Y3+ ion in the Y2O3 structure in two different sites and the Bi 4f spectrum shows the Bi3+ ion in the two different sites in Bi2O3. The photoluminescence (PL) results showed three broad emission bands in the blue and green regions under ultraviolet excitation, which were also present for panchromatic cathodoluminescence (CL) results. These three peaks have maxima at ∼3.4, 3.0 and 2.5 eV. The PL emission ∼3.0 eV (blue emission) showed two excitation bands centered at ∼3.7 and 3.4 eV while the PL emission at ∼2.5 eV (green emission) showed a broad excitation band from ∼4 to 3.4 eV. The panchromatic CL images were obtained for selected wavelengths at (2.99 ± 0.08) eV (for blue emission) and (2.34 ± 0.06) eV (for green emission). These luminescence results correlate with the XPS results that show that there are two different Bi3+ sites in the host lattice.

  13. Effect of iron oxide reductive dissolution on the transformation and immobilization of arsenic in soils: New insights from X-ray photoelectron and X-ray absorption spectroscopy.

    PubMed

    Fan, Jian-Xin; Wang, Yu-Jun; Liu, Cun; Wang, Li-Hua; Yang, Ke; Zhou, Dong-Mei; Li, Wei; Sparks, Donald L

    2014-08-30

    The geochemical behavior and speciation of arsenic (As) in paddy soils is strongly controlled by soil redox conditions and the sequestration by soil iron oxyhydroxides. Hence, the effects of iron oxide reductive dissolution on the adsorption, transformation and precipitation of As(III) and As(V) in soils were investigated using batch experiments and synchrotron based techniques to gain a deeper understanding at both macroscopic and microscopic scales. The results of batch sorption experiments revealed that the sorption capacity of As(V) on anoxic soil was much higher than that on control soil. Synchrotron based X-ray fluorescence (μ-XRF) mapping studies indicated that As was heterogeneously distributed and was mainly associated with iron in the soil. X-ray absorption near edge structure (XANES), micro-X-ray absorption near edge structure (μ-XANES) and X-ray photoelectron spectroscopy (XPS) analyses revealed that the primary speciation of As in the soil is As(V). These results further suggested that, when As(V) was introduced into the anoxic soil, the rapid coprecipitation of As(V) with ferric/ferrous ion prevented its reduction to As(III), and was the main mechanism controlling the immobilization of As. This research could improve the current understanding of soil As chemistry in paddy and wetland soils. PMID:25064258

  14. Reactive ZnO/Ti/ZnO interfaces studied by hard x-ray photoelectron spectroscopy

    SciTech Connect

    Knut, Ronny Lindblad, Rebecka; Rensmo, Håkan; Karis, Olof; Grachev, Sergey; Faou, Jean-Yvon; Søndergård, Elin

    2014-01-28

    The chemistry and intermixing at buried interfaces in sputter deposited ZnO/Ti/ZnO thin layers were studied by hard x-ray photoelectron spectroscopy. The long mean free path of the photoelectrons allowed for detailed studies of the oxidation state, band bending effects, and intrinsic doping of the buried interfaces. Oxidation of the Ti layer was observed when ZnO was deposited on top. When Ti is deposited onto ZnO, Zn Auger peaks acquire a metallic character indicating a strong reduction of ZnO at the interface. Annealing of the stack at 200 °C results in further reduction of ZnO and oxidation of Ti. Above 300 °C, oxygen transport from the bulk of the ZnO layer takes place, leading to re-oxidation of ZnO at the interface and further oxidation of Ti layer. Heating above 500 °C leads to an intermixing of the layers and the formation of a Zn{sub x}TiO{sub y} compound.

  15. Investigation of Ohmic mechanism for chlorine-treated p-type GaN using x-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Chen, Po-Sung; Lee, Ching-Ting

    2006-08-01

    To investigate the function and mechanism of oxidation, the surface of the chlorine-treated p-type GaN semiconductor was analyzed using x-ray photoelectron spectroscopy. The chlorinated surface treatment was performed by electrolyzing HCl chemical solution to generate HClO, which in turn could be used to oxidize the p-type GaN. The chlorinated surface treatment enhances the formation of GaOx on the GaN surface and removing GaOx layer from the surface thereafter leads to the creation of additional Ga vacancies. Consequently, more holes are generated as a result of the generated Ga vacancies. Therefore, a relatively higher Ohmic performance with a specific contact resistance of 6.1×10-6Ωcm2 can be obtained for Ni /Au metal contact subsequently patterned on the chlorine-treated p-type GaN via the enhanced formation of GaOx.

  16. Light-induced changes in an alkali metal atomic vapor cell coating studied by X-ray photoelectron spectroscopy

    SciTech Connect

    Hibberd, A. M.; Bernasek, S. L.; Seltzer, S. J.; Balabas, M. V.; Morse, M.; Budker, D.

    2013-09-07

    The light-induced desorption of Rb atoms from a paraffin coating is studied with depth-profiling X-ray photoelectron spectroscopy (XPS) using tunable synchrotron radiation. Following Rb exposure, shifts of the C1s signal to higher binding energies, as well as the appearance of lower binding energy components in the O1s region, were observed. These effects were diminished after irradiation with desorbing light. Additionally, following desorbing-light irradiation, changes in the depth-dependent concentration of carbon were observed. These observations offer an insight into the microscopic changes that occur during light-induced atomic desorption and demonstrate the utility of XPS in understanding atom-coating interactions.

  17. Probing buried organic-organic and metal-organic heterointerfaces by hard x-ray photoelectron spectroscopy

    SciTech Connect

    Shibuta, Masahiro; Eguchi, Toyoaki; Watanabe, Yoshio; Nakajima, Atsushi; Son, Jin-Young; Oji, Hiroshi

    2012-11-26

    We present a nondestructive characterization method for buried hetero-interfaces for organic/organic and metal/organic systems using hard x-ray photoelectron spectroscopy (HAXPES) which can probe electronic states at depths deeper than {approx}10 nm. A significant interface-derived signal showing a strong chemical interaction is observed for Au deposited onto a C{sub 60} film, while there is no such additional feature for copper phthalocyanine deposited onto a C{sub 60} film reflecting the weak interaction between the molecules in the latter case. A depth analysis with HAXPES reveals that a Au-C{sub 60} intermixed layer with a thickness of 5.1 nm is formed at the interface.

  18. X-ray photoelectron spectroscopy studies of plasma-modified PET surface and alumina/PET interface

    NASA Astrophysics Data System (ADS)

    Cueff, R.; Baud, G.; Benmalek, M.; Besse, J. P.; Butruille, J. R.; Jacquet, M.

    1997-07-01

    X-ray photoelectron spectroscopy was used to study the chemical effects of a reactive plasma treatment on the PET surface and to investigate the chemical interactions involved at the alumina/PET interface. The treatment of the PET by a carbon dooxide plasma introduces new oxygen reactive species on the polymer surface. Evidence of this chemical modification is given by the appearance of additional carbonyl bonds. The interfacial study reveals a reaction of alumina with the oxygen atoms of the carbonyl bonds of PET (plasma-induced carbonyl bonds and carbonyl bonds of the ester groups). This chemical interaction results in the formation of AlOC interfacial bonds in the early stages of deposition.

  19. N-derived signals in the x-ray photoelectron spectra of N-doped anatase TiO2

    NASA Astrophysics Data System (ADS)

    Yu, Y. P.; Xing, X. J.; Xu, L. M.; Wu, S. X.; Li, S. W.

    2009-06-01

    The plasma-assisted molecular beam epitaxial anatase TiO2-xNx (x <0.3) films were chosen to investigate the N-derived variation in the x-ray photoelectron spectroscopy (XPS). With increasing nitrogen concentration, the small chemical shift and the shoulder of the main peak emerge in the N 1s, O 1s, or Ti 2p3/2 core level spectra. In combination with the experimental results obtained from x-ray diffraction and atomic force microscopy, the variations in the spectra could be ascribed to the microstructural distortion. This distortion, induced by the N3- substitution for lattice O2-, could slightly decrease the average ionicity of the Ti-O (or N) bonds. In addition, the other N 1s features (at 399.8 and 401.8 eV) and the oxygen vacancy are also discussed. For the N-doped TiO2, this work introduces a correlation between the microstructural properties and the XPS signals.

  20. X-ray photoelectron spectroscopy analysis of aluminum and copper cleaning procedures for the Advanced Photon Source

    SciTech Connect

    Rosenberg, R.A.; McDowell, M.W.; Noonan, J.R. )

    1994-07-01

    The Advanced Photon Source (APS), presently under construction, will produce x rays of unprecedented brightness. The storage ring where the x rays will be produced will be constructed from an extruded 6063 aluminum alloy, while transition pieces (flanges, etc.) will be made from a 2219 aluminum alloy. In addition, cooled photon absorbers will be placed in strategic locations throughout the ring to intercept the majority of the unused high power-density radiation. These will be made of either CDA-101 (OFHC) copper or glidcop (a dispersion strengthened copper alloy). Before any of these components can be assembled they must be cleaned to remove surface contaminants so that the ultrahigh vacuum ([lt]0.1 nTorr) necessary for successful operation can be achieved. Many recipes for cleaning aluminum and copper exist; however, most of them involve the use of chemicals that present safety and/or environmental concerns. We have undertaken an x-ray photoelectron spectroscopy study of the effects of a variety of commercially available cleaners on the surface cleanliness of aluminum and copper. Several important results have been identified in this study. A simple alkaline detergent in an ultrasonic bath cleans aluminum alloys as effectively as the more aggressive cleaning solutions. The detergent can be used at 65 [degree]C to clean the 6063 alloy and at 50 [degree]C to clean the 2219 alloy. A citric acid based cleaner was found to be effective at cleaning copper, although the surface oxidizes rapidly. To date, we have been unable to find a universal cleaning procedure, i.e., one that is optimal for cleaning both Al and Cu.

  1. X-ray photoelectron spectra structure and chemical bond nature in NpO2

    NASA Astrophysics Data System (ADS)

    Teterin, Yu. A.; Teterin, A. Yu.; Ivanov, K. E.; Ryzhkov, M. V.; Maslakov, K. I.; Kalmykov, St. N.; Petrov, V. G.; Enina, D. A.

    2014-01-01

    Quantitative analysis was done of the x-ray photoelectron spectra structure in the binding energy (BE) range of 0 to ˜35 eV for neptunium dioxide (NpO2) valence electrons. The BEs and structure of the core electronic shells (˜35-1250 eV) as well as the relativistic discrete variation calculation results for the finite fragment of the NpO2 lattice and the data of other authors were taken into account. The experimental data show that the many-body effects and the multiplet splitting contribute to the spectral structure much less than the effects of formation of the outer (0-˜15 eV) and the inner (˜15-˜35 eV) valence molecular orbitals (OVMO and IVMO, respectively). The filled Np 5f electronic states were shown to form in the NpO2 valence band. The Np 6p electrons participate in formation of both the IVMO and the OVMO (bands). The filled Np 6p3/2 and the O 2s electronic shells were found to take the maximum part in the IVMO formation. The MO composition and the sequence order in the BE range 0-˜35 eV in NpO2 were established. The experimental and theoretical data allowed a quantitative MO scheme for NpO2, which is fundamental for both understanding the chemical bond nature in neptunium dioxide and the interpretation of other x-ray spectra of NpO2.

  2. X-ray Photoelectron Spectroscopy Study of Argon-Plasma-Treated Fluoropolymers

    NASA Technical Reports Server (NTRS)

    Golub, Morton A.; Lopata, Eugene S.; Finney, Lorie S.

    1994-01-01

    Films of poly(tetrafluoroethylene) (PTFE) and of a tetrafluoroethylene-perfluoroalkyl vinyl ether (approximately 49:1) copolymer (PFA) were exposed to a radio-frequency argon plasma and then examined by X-ray photoelectron spectroscopy (XPS). The use of fluoropolymer films nearly free of surface hydrocarbon contamination as well as the use of a monochromatized X-ray source for XPS removed two factors contributing to conflicting reports on the effect of exposure time on the fluorine-to-carbon (F/C) and oxygen-to-carbon (O/C) ratios for several Ar-plasma-treated fluoropolymers. Contrary to literature indications, a common pattern was found for PTFE and PFA: a moderate decrease in F/C ratio (from 1.99 to 1.40, and from 1.97 to 1.57, respectively), together with a moderate increase in O/C ratio (from negligible to about 0.10, and from 0.012 to about O.10, respectively) at very short exposures, after which the F/C ratios remained essentially constant on prolonged exposures, while the O/C ratios for PTFE and PFA leveled off at 0.11 and 0.15, respectively. The XPS C(sub 1s), spectra for these polymers exposed to the Ar plasma for 20 min were similar and presented, besides a prominent peak at 292.0 eV (CF2,) and a minor peak at 294.0 or 294.1 eV (CF3), a composite band of four curve-resolved peaks (approximately 285-290 eV) representing various CH, CC, CO, CN, and CF functionalities.

  3. First-principles core-level X-ray photoelectron spectroscopy calculation on arsenic defects in silicon crystal

    SciTech Connect

    Kishi, Hiroki; Miyazawa, Miki; Matsushima, Naoki; Yamauchi, Jun

    2014-02-21

    We investigate the X-ray photoelectron spectroscopy (XPS) binding energies of As 3d in Si for various defects in neutral and charged states by first-principles calculation. It is found that the complexes of a substitutional As and a vacancy in charged and neutral states explain the experimentally observed unknown peak very well.

  4. X-ray photoelectron spectroscopic evidence for bacteria-enhanced dissolution of hornblende

    NASA Astrophysics Data System (ADS)

    Kalinowski, B. E.; Liermann, L. J.; Brantley, S. L.; Barnes, A.; Pantano, C. G.

    2000-04-01

    An Arthrobacter species capable of extracting Fe from hornblende was isolated from a soil from the Adirondacks, NY (USA). This bacteria isolate, used in batch experiments with hornblende, accelerated the release of Fe from hornblende without measurably affecting Al release. The isolate produces both low molecular weight organic acids (LMWOA) and a catecholate siderophore. Polished hornblende (glass and crystal) discs were analyzed with X-ray photoelectron spectroscopy (XPS) before and after incubation with growing Arthrobacter sp. to investigate whether the bacteria caused a distinguishable chemical signature on the upper 100 Å of mineral surface. After removal of the arthrobacter grown on hornblende crystal or glass substrates using lysozyme, XPS revealed surface depletion of Fe for samples grown for several days in buffered (crystal) and unbuffered (crystal and glass) media. Fe/Si ratios of hornblende surfaces dissolved under biotic conditions are significantly lower than Fe/Si ratios on surfaces dissolved under abiotic conditions for similar amounts of time. Enhanced Fe release and the formation of Fe-depleted surfaces is inferred to be caused by catechol complexation at the mineral surface. Because natural siderophore was not isolated in sufficient quantities to run bacteria-free leaching experiments, parallel investigations were run with a commercially available siderophore (desferrioxamine B). Desferrioxamine B was observed to enhance release of Fe, Si, and Al from hornblende both with and without added bacteria. Formation of desferrioxamine-Fe surface complexes were probed by studying the multiple splitting and shift in intensities of the N 1s line analyzed by XPS on siderophore ± Fe on gold surfaces and siderophore + hornblende crystal surfaces. Based upon the observed formation of an hydroxamate (desferrioxamine) surface complex on hornblende, we infer that catecholate siderophores, such as those produced by the arthrobacter, also complex on the

  5. An in situ x-ray photoelectron spectroscopy study of the initial stages of rf magnetron sputter deposition of indium tin oxide on p-type Si substrate

    SciTech Connect

    Rein, M. H.; Holt, A. O.; Hohmann, M. V.; Klein, A.; Thogersen, A.; Mayandi, J.; Monakhov, E. V.

    2013-01-14

    The interface between indium tin oxide and p-type silicon is studied by in situ X-ray photoelectron spectroscopy (XPS). This is done by performing XPS without breaking vacuum after deposition of ultrathin layers in sequences. Elemental tin and indium are shown to be present at the interface, both after 2 and 10 s of deposition. In addition, the silicon oxide layer at the interface is shown to be composed of mainly silicon suboxides rather than silicon dioxide.

  6. Photoelectron fluxes observed by FAST compared with model predictions incorporating SNOE observations of the solar soft X-ray irradiance

    NASA Astrophysics Data System (ADS)

    Bailey, S. M.; Peterson, W. K.; Solomon, S. C.; Carlson, C. W.; McFadden, J. P.

    2001-12-01

    Photoelectrons are those electrons produced when atoms or molecules in the upper atmosphere are photoionized. These electrons carry the excess energy of the photon remaining from the ionization and can have energies up to and greater than 1 keV. Photoelectrons are important in that they play a significant role in the energetics of the upper atmosphere, resulting in ionization, dissociation, and excitation of atoms and molecules. There have been long standing issues with regard to understanding the magnitude of the terrestrial photoelectron flux as models have not been able to reproduce the observations without scaling the solar soft X-ray irradiance by factors of two to four. The Fast Auroral Snapshot (FAST) spacecraft was launched in August of 1996. While its primary goals focus on the study of auroral energetic particles, in January of 1999 it began making low-latitude observations. From measurements by the FAST energetic electron sensor, upward flowing photoelectron fluxes in the energy range of 50 eV to 1 keV have been obtained. These measurements are in agreement with earlier measurements of the terrestrial photoelectron flux. The Student Nitric Oxide Explorer (SNOE) spacecraft was launched in February of 1998. Since then it has been making daily observations of the solar soft X-ray irradiance in bandpasses of 2 - 7, 6 - 19, and 17 - 20 nm. SNOE observes larger values of the solar soft X-ray irradiance than reported by earlier observations or predicted by empirical models; however, the SNOE observations are in agreement with many suggestions of the solar soft X-ray irradiance obtained from geophysical observations such as airglow and electron densities. These irradiance measurements are used in a photoelectron model that includes transport. Observations of photoelectron fluxes for the first solar rotation of 1999 are modeled. The model photoelectron spectra are in good agreement with the observed photoelectron spectra over most of the 50 eV to 1 keV energy

  7. X-ray computed tomography for additive manufacturing: a review

    NASA Astrophysics Data System (ADS)

    Thompson, A.; Maskery, I.; Leach, R. K.

    2016-07-01

    In this review, the use of x-ray computed tomography (XCT) is examined, identifying the requirement for volumetric dimensional measurements in industrial verification of additively manufactured (AM) parts. The XCT technology and AM processes are summarised, and their historical use is documented. The use of XCT and AM as tools for medical reverse engineering is discussed, and the transition of XCT from a tool used solely for imaging to a vital metrological instrument is documented. The current states of the combined technologies are then examined in detail, separated into porosity measurements and general dimensional measurements. In the conclusions of this review, the limitation of resolution on improvement of porosity measurements and the lack of research regarding the measurement of surface texture are identified as the primary barriers to ongoing adoption of XCT in AM. The limitations of both AM and XCT regarding slow speeds and high costs, when compared to other manufacturing and measurement techniques, are also noted as general barriers to continued adoption of XCT and AM.

  8. Surface composition analysis of HF vapour cleaned silicon by X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Ermolieff, A.; Martin, F.; Amouroux, A.; Marthon, S.; Westendorp, J. F. M.

    1991-06-01

    X-ray photoelectron spectroscopy (XPS) measurements on silicon surfaces treated by HF gaseous cleaning are described. Various cleaning recipes, which essentially differ by the amount of water present during the reaction were studied; the composition of the silicon surface was measured in terms of monolayer coverage of oxygen, fluorine and carbon. These gaseous cleaned surfaces are compared with those of commonly deglazed silicon samples by using an aqueous HF bath. The F(1s), O(1s), Si(2p), C(1s) photoelectron lines were monitored, and concentrations determined as usual by integration of the lines after removal of the non-linear backgroune. The F(1s), C(1s) and Si(2p) lines were decomposed into several components corresponding to different chemical bonds. The results show that the amount of fluorine is directly correlated with the amount of oxygen: the higher the oxygen level on the sample, the more important is the fluorine content till 0.7 ML, essentially in a O sbnd Si sbnd F bonding state. For more aggresive etching leaving less than one monolayer of oxygen, the Si sbnd F bond becomes predominant. The ratio of the SiF to OSiF concentrations is a significant signature of the deoxidation state of the surface. Hydrophobicity of the water appears in the range of 25% Si sbnd F bonds. With very aggresive etching processes, 67% Si sbnd F bonds and 33% O sbnd Si sbnd F bonds are reached and the total amount of fluoride drops below 0.3 ML. For comparison, only Si sbnd F bonds are observed after a wet etching in a dilute HF bath without a rinse with a much lower fluorine concentration. The balance between Si sbnd F and O sbnd Si sbnd F remains stable and seems to be representative of the surface states provided by the etching process.

  9. Effect of Space Radiation Processing on Lunar Soil Surface Chemistry: X-Ray Photoelectron Spectroscopy Studies

    NASA Technical Reports Server (NTRS)

    Dukes, C.; Loeffler, M.J.; Baragiola, R.; Christoffersen, R.; Keller, J.

    2009-01-01

    Current understanding of the chemistry and microstructure of the surfaces of lunar soil grains is dominated by a reference frame derived mainly from electron microscopy observations [e.g. 1,2]. These studies have shown that the outermost 10-100 nm of grain surfaces in mature lunar soil finest fractions have been modified by the combined effects of solar wind exposure, surface deposition of vapors and accretion of impact melt products [1,2]. These processes produce surface-correlated nanophase Feo, host grain amorphization, formation of surface patinas and other complex changes [1,2]. What is less well understood is how these changes are reflected directly at the surface, defined as the outermost 1-5 atomic monolayers, a region not easily chemically characterized by TEM. We are currently employing X-ray Photoelectron Spectroscopy (XPS) to study the surface chemistry of lunar soil samples that have been previously studied by TEM. This work includes modification of the grain surfaces by in situ irradiation with ions at solar wind energies to better understand how irradiated surfaces in lunar grains change their chemistry once exposed to ambient conditions on earth.

  10. In Situ Ambient Pressure X-ray Photoelectron Spectroscopy Studies of Lithium-Oxygen Redox Reactions

    NASA Astrophysics Data System (ADS)

    Lu, Yi-Chun; Crumlin, Ethan J.; Veith, Gabriel M.; Harding, Jonathon R.; Mutoro, Eva; Baggetto, Loïc; Dudney, Nancy J.; Liu, Zhi; Shao-Horn, Yang

    2012-10-01

    The lack of fundamental understanding of the oxygen reduction and oxygen evolution in nonaqueous electrolytes significantly hinders the development of rechargeable lithium-air batteries. Here we employ a solid-state Li4+xTi5O12/LiPON/LixV2O5 cell and examine in situ the chemistry of Li-O2 reaction products on LixV2O5 as a function of applied voltage under ultra high vacuum (UHV) and at 500 mtorr of oxygen pressure using ambient pressure X-ray photoelectron spectroscopy (APXPS). Under UHV, lithium intercalated into LixV2O5 while molecular oxygen was reduced to form lithium peroxide on LixV2O5 in the presence of oxygen upon discharge. Interestingly, the oxidation of Li2O2 began at much lower overpotentials (~240 mV) than the charge overpotentials of conventional Li-O2 cells with aprotic electrolytes (~1000 mV). Our study provides the first evidence of reversible lithium peroxide formation and decomposition in situ on an oxide surface using a solid-state cell, and new insights into the reaction mechanism of Li-O2 chemistry.

  11. Light-induced atom desorption from glass surfaces characterized by X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Kumagai, Ryo; Hatakeyama, Atsushi

    2016-07-01

    We analyzed the surfaces of vitreous silica (quartz) and borosilicate glass (Pyrex) substrates exposed to rubidium (Rb) vapor by X-ray photoelectron spectroscopy (XPS) to understand the surface conditions of alkali metal vapor cells. XPS spectra indicated that Rb atoms adopted different bonding states in quartz and Pyrex. Furthermore, Rb atoms in quartz remained in the near-surface region, while they diffused into the bulk in Pyrex. For these characterized surfaces, we measured light-induced atom desorption (LIAD) of Rb atoms. Clear differences in time evolution, photon energy dependence, and substrate temperature dependence were found; the decay of LIAD by continuous ultraviolet irradiation for quartz was faster than that for Pyrex, a monotonic increase in LIAD with increasing photon energy from 1.8 to 4.3 eV was more prominent for quartz, and LIAD from quartz was more efficient at higher temperatures in the range from 300 to 580 K, while that from Pyrex was almost independent of temperature.

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

    SciTech Connect

    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.

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

    DOE PAGESBeta

    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

  14. Ultrafast x-ray photoelectron spectroscopy in the microsecond time domain

    SciTech Connect

    Höfert, O.; Gleichweit, C.; Steinrück, H.-P.; Papp, C.

    2013-09-15

    We introduce a new approach for ultrafast in situ high-resolution X-ray photoelectron spectroscopy (XPS) to study surface processes and reaction kinetics on the microsecond timescale. The main idea is to follow the intensity at a fixed binding energy using a commercial 7 channeltron electron analyzer with a modified signal processing setup. This concept allows for flexible switching between measuring conventional XP spectra and ultrafast XPS. The experimental modifications are described in detail. As an example, we present measurements for the adsorption and desorption of CO on Pt(111), performed at the synchrotron radiation facility BESSY II, with a time resolution of 500 μs. Due to the ultrafast measurements, we are able to follow adsorption and desorption in situ at pressures of 2 × 10{sup −6} mbar and temperatures up to 500 K. The data are consistently analyzed using a simple model in line with data obtained with conventional fast XPS at temperatures below 460 K. Technically, our new approach allows measurement on even shorter timescales, down to 20 μs.

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

    SciTech Connect

    Delmelle, Renaud; Borgschulte, Andreas; Probst, Benjamin; Alberto, Roger; Züttel, 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.

  16. Hydrazine reduction of transition metal oxides - In situ characterization using X-ray photoelectron spectroscopy

    NASA Technical Reports Server (NTRS)

    Littrell, D. M.; Tatarchuk, B. J.

    1986-01-01

    The transition metal oxides (TMOs) V2O5, FeO3, Co3O4, NiO, CuO, and ZnO were exposed to hydrazine at various pressures. The metallic surfaces were surveyed by in situ X-ray photoelectron spectroscopy to determine the irrelative rate of reduction by hydrazine. The most easily reducible oxide, CuO, could be reduced to the metallic state at room temperature and 10 to the -6th torr. The reaction is first order with respect to CuO, with an activation energy of about 35 kJ/mol. Two types of adsorption were seen to occur at 295 K: (1) a reversible component in which the measured N:Cu ratio increased to 0.60 at hydrazine pressures up to 0.5 torr, and (2) an irreversible component, with a N:Cu ratio of 0.28, which could not be removed by extended vacuum pumping. The results of this study are useful for the identification of TMO's that can be used as solid neatallizers of hydrazine spills, and for the preparation of metal surfaces for electroplating and evaporative thin-film coating.

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

    NASA Astrophysics Data System (ADS)

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

    2015-05-01

    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 H2 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 CO2 hydrogenation and the hydrogenation of a water reduction catalyst for photocatalytic H2 production, but it opens the possibility of the new in situ characterisation of energy materials and catalysts.

  18. Compositional aspects of iron Fischer-Tropsch catalysts: an x-ray photoelectron

    SciTech Connect

    Kuivila, C.S.

    1987-01-01

    Iron catalysts employed in the Fischer-Tropsch synthesis consist of metallic, carbide, and oxide phases. The catalytic and compositional behavior of prereduced and unreduced iron catalysts were investigated in this study. Catalytic behavior was evaluated by measuring the rates of hydrocarbon formation in a 3:1 H/sub 2//CO mixture at one atmosphere and 250/sup 0/C. Iron phases which evolved near the catalyst surfaces were characterized by x-ray photoelectron spectroscopy, and bulk phases present following the synthesis reactions were determined by Mossbauer spectroscopy. At low conversion levels, prereduced iron catalysts were gradually converted to iron carbide. At total CO conversion levels in the range of 30 to 40%, prereduced catalysts were converted primarily to iron carbide, although some surface oxide phases also formed. Unreduced Fe/sub 2/O/sub 3/ exhibited no initial synthesis activity, but underwent gradual activation and eventually became more active than the prereduced catalysts. The various phases of the iron catalysts were related to varying olefin production rates.

  19. X-Ray Photoelectron Spectroscopic Study of Oxidation of InP

    NASA Astrophysics Data System (ADS)

    Shibata, Noboru; Ikoma, Hideaki

    1992-12-01

    InP was oxidized chemically (in boiling deionized water), thermally (dry oxygen, 260°C, 30 min) and chemically under light illumination from a xenon arc lamp. The chemical compositions and their depth distributions from the surface of these oxides as well as the InP native oxide (naturally grown) were studied by angle-resolved X-ray photoelectron spectroscopy (XPS) and XPS combined with in situ Ar+ ion etching. In any oxide, indium is first oxidized to form In2O3 perhaps due to depletion of phosphorus from the InP surface induced by contact annealing, etc. InPO3 and/or InPO4 are then successively grown on an In2O3 or In2O3 rich layer. In and P atoms diffuse through the already grown In2O3 layer and react with oxidant at the surface to form InPO3 and/or InPO4. Light illumination was found to strongly enhance oxidation of InP, and substantially increase InPO3 and InPO4.

  20. Characterization of acidity in ZSM-5 zeolites: An x-ray photoelectron and IR spectroscopy study

    SciTech Connect

    Borade, R.; Sayari, A.; Adnot, A.; Kaliaguine, S. )

    1990-07-26

    An x-ray photoelectron spectroscopic (XPS) method is proposed for the identification and quantitation of Broensted and Lewis acid sites in ZSM-5 zeolites. The method consists of deconvoluting the N{sub 1s}XPS level of chemisorbed pyridine and measuring the relative intensities of the peak components. It was found that pyridine is chemisorbed in three different states on ZSM-5 zeolites corresponding to N{sub 1s} binding energy of 398.7, 400.0, and 401.8 eV, respectively. The first peak at 398.7 eV was assigned to N{sub 1s} level of pyridine adsorbed on Lewis sites, while the second and third were assigned to N{sub 1s} levels of pyridine adsorbed on relatively weak and strong Broensted acid sites, respectively. Comparison of the concentrations of the various acid sites as determined from the relative intensities of the N{sub 1s} components with IR spectroscopic data showed that XPS has potential applications in the identification and the quantitative determination of Broensted and Lewis acid sites in zeolites.

  1. X-ray photoelectron spectroscopy study of thin TiO2 films cosputtered with Al

    NASA Astrophysics Data System (ADS)

    Hsu, Jin-Cherng; Wang, Paul W.; Lee, Cheng-Chung

    2006-06-01

    In this study, titanium dioxide (TiO2) films were fabricated by cosputtering of a titanium (Ti) target and an aluminum (Al) slice in a smaller area by an ion-beam sputtering deposition method. The sputtered films were postannealed at 450 °C. The x-ray photoelectron spectroscopy spectra were categorized by their oxygen bonding variations, which include high-binding-energy oxygen, (HBO), bridging oxygen, low-binding-energy oxygen, and shifts of the binding energies (BEs) of oxygen (O) and Ti signals. The enhancement of HBO and higher BE shifts of the O 1s spectra as a function of cosputtered Al in the film imply the formation of an Al—O—Ti linkage. Corresponding changes in the Ti 2p spectra further confirm the modification of properties of the cosputtered film that results from the variation of the chemical bonding environment. An observed correlation between the chemical structure and optical absorption of the Al cosputtered films can be used to modify the optical properties of the film.

  2. X-ray photoelectron spectroscopy surface analysis of aluminum ion stress in barley roots. [Hordeum vulgare

    SciTech Connect

    Millard, M.M.; Foy, C.D.; Coradetti, C.A.; Reinsel, M.D. )

    1990-06-01

    X-ray photoelectron spectroscopy (XPS) has been used to analyze root surface changes when Dayton barley (Hordeum vulgare) (Al tolerant) and Kearney barley (Al sensitive) seedlings were grown in nutrient solution in the presence and absence of 37.0 micromolar Al. The electron spectra from root surfaces contained strong lines in order of decreasing intensity from organic forms of carbon, oxygen, and nitrogen and weak lines due to inorganic elements in the form of anions and cations on the surface. The surface composition of root tips from Kearney was C, 65.6%; 0, 26.8%; N, 4.4% and tips from Dayton was C, 72.7%; O, 23.6%; N, 1.9%, grown in the absence of aluminum. Electron lines characteristic of nitrate, potassium, chloride, phosphate were also present in the spectra from those roots. Dayton roots grown in the presence of 37.0 micromolar aluminum contained 2.1% aluminum while Kearney contained 1.3% aluminum. The ratio of aluminum to phosphate was close to 1.0. Dayton roots usually contained twice as much aluminum phosphate in the surface region as Kearney. Dayton may be less susceptible to Al toxic effects by accumulation of aluminum phosphate on the root surface which then acts as a barrier to the transport of aluminum into the interior of the roots.

  3. Internal Photoemission and X-Ray Photoelectron Spectroscopic Studies of Sulfur-Passivated GaAs

    NASA Astrophysics Data System (ADS)

    Sato, Kenji; Ikoma, Hideaki

    1993-02-01

    Internal photoemission and X-ray photoelectron spectroscopic (XPS) measurements were performed to investigate the effect of sulfur passivation on the GaAs surface and the degradation of the GaAs surface exposed to air ambient after the passivation. The reverse bias dependence of the Schottky barrier height was very small in the as-sulfur-treated sample and was mainly explained by the image force lowering effect. However, it increased as this sample was exposed to air, indicating an increase in the interface state density. The XPS studies showed that both the Ga and As oxides were hardly observed in the sulfur-passivated samples. This indicates that sulfur passivation strongly suppresses oxidation of GaAs. However, a small amount of elemental arsenic was observed with a trace of the As suboxides (such as AsO) after exposure to air and it increased as the exposure time was increased. These results were probably correlated with the increase in the bias dependence of the Schottky barrier height in samples exposed to air after the passivation. Thermal oxidation of GaAs was found to be retarded by sulfur passivation until oxidation time was about 10 min at 300°C. A possible model of suppression of oxidation by sulfur passivation was also discussed.

  4. A versatile instrument for ambient pressure x-ray photoelectron spectroscopy: The Lund cell approach

    NASA Astrophysics Data System (ADS)

    Knudsen, Jan; Andersen, Jesper N.; Schnadt, Joachim

    2016-04-01

    During the past one and a half decades ambient pressure x-ray photoelectron spectroscopy (APXPS) has grown to become a mature technique for the real-time investigation of both solid and liquid surfaces in the presence of a gas or vapour phase. APXPS has been or is being implemented at most major synchrotron radiation facilities and in quite a large number of home laboratories. While most APXPS instruments operate using a standard vacuum chamber as the sample environment, more recently new instruments have been developed which focus on the possibility of custom-designed sample environments with exchangeable ambient pressure cells (AP cells). A particular kind of AP cell solution has been driven by the development of the APXPS instrument for the SPECIES beamline of the MAX IV Laboratory: the solution makes use of a moveable AP cell which for APXPS measurements is docked to the electron energy analyser inside the ultrahigh vacuum instrument. Only the inner volume of the AP cell is filled with gas, while the surrounding vacuum chamber remains under vacuum conditions. The design enables the direct connection of UHV experiments to APXPS experiments, and the swift exchange of AP cells allows different custom-designed sample environments. Moreover, the AP cell design allows the gas-filled inner volume to remain small, which is highly beneficial for experiments in which fast gas exchange is required. Here we report on the design of several AP cells and use a number of cases to exemplify the utility of our approach.

  5. Surface structure determination of Pd on W(100) using X-ray photoelectron diffraction

    NASA Astrophysics Data System (ADS)

    Lussani, F. C.; de Siervo, A.; de Figueiredo, J. J. S.; Pancotti, A.; Landers, R.

    2011-11-01

    Ferromagnetic ordering in non-ferromagnetic transition metals induced by structural effects such as lattice expansion and stacking faults have been predicted by several theoretical studies. Different surfaces such as Nb(100), W(100) and C(0001) have been suggested as potential templates which could drive a Pd ultrathin film to a stable ferromagnetic state, depending on growth packing, film thickness and lateral lattice parameter. In this work we present an X-ray photoelectron diffraction (XPD) study of sub-monolayer to a few layers of Pd grown on W(100) and its surface structure determination. XPD patterns of Pd 3d and W 4f peaks were measured using synchrotron radiation with photon energy of 1810 eV provided by the SXS beamline at the Brazilian Synchrotron Light Laboratory. Our results indicate that the first few monolayers of Pd grow on W(100) with bcc packing and lateral lattice parameter dramatically changed in comparison with the Pd(fcc) bulk values. Based on these results we also present a discussion on the magnetic properties of this system derived from spin-polarized DFT calculation.

  6. Ultrafast x-ray photoelectron spectroscopy in the microsecond time domain

    NASA Astrophysics Data System (ADS)

    Höfert, O.; Gleichweit, C.; Steinrück, H.-P.; Papp, C.

    2013-09-01

    We introduce a new approach for ultrafast in situ high-resolution X-ray photoelectron spectroscopy (XPS) to study surface processes and reaction kinetics on the microsecond timescale. The main idea is to follow the intensity at a fixed binding energy using a commercial 7 channeltron electron analyzer with a modified signal processing setup. This concept allows for flexible switching between measuring conventional XP spectra and ultrafast XPS. The experimental modifications are described in detail. As an example, we present measurements for the adsorption and desorption of CO on Pt(111), performed at the synchrotron radiation facility BESSY II, with a time resolution of 500 μs. Due to the ultrafast measurements, we are able to follow adsorption and desorption in situ at pressures of 2 × 10-6 mbar and temperatures up to 500 K. The data are consistently analyzed using a simple model in line with data obtained with conventional fast XPS at temperatures below 460 K. Technically, our new approach allows measurement on even shorter timescales, down to 20 μs.

  7. Investigation of the surface composition of electrodeposited black chromium by X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Survilienė, S.; Češūnienė, A.; Jasulaitienė, V.; Jurevičiūtė, I.

    2015-01-01

    The paper reviews black chromium electrodeposited from a trivalent chromium bath containing ZnO as a second main component. The chemical compositions of the top layers of the black chromium coatings were studied by the X-ray photoelectron spectroscopy method. The surface of black chromium was found to be almost entirely covered with organic substances. To gain information on the state of each element in the deposit bulk, the layer-by-layer etching of the black chromium surface with argon gas was used. Analysis of XPS spectra has shown that the top layers of black chromium without zinc are composed of various Cr(III) components, organic substances and metallic Cr, whereas metallic Cr is almost absent in black chromium containing some amount of Zn(II) compounds. The ratios of metal/oxide phases were found to be 10/27 and 2/28 for black chromium without and with zinc, respectively. It has been determined that owing to the presence of ZnO in the Cr(III) bath, the percentage of metallic chromium is substantially reduced in black chromium which is quite important for good solar selective characteristics of the coating. The results confirm some of earlier observations and provide new information on the composition of the near-surface layers.

  8. In Situ Ambient Pressure X-ray Photoelectron Spectroscopy Studies of Lithium-Oxygen Redox Reactions

    PubMed Central

    Lu, Yi-Chun; Crumlin, Ethan J.; Veith, Gabriel M.; Harding, Jonathon R.; Mutoro, Eva; Baggetto, Loïc; Dudney, Nancy J.; Liu, Zhi; Shao-Horn, Yang

    2012-01-01

    The lack of fundamental understanding of the oxygen reduction and oxygen evolution in nonaqueous electrolytes significantly hinders the development of rechargeable lithium-air batteries. Here we employ a solid-state Li4+xTi5O12/LiPON/LixV2O5 cell and examine in situ the chemistry of Li-O2 reaction products on LixV2O5 as a function of applied voltage under ultra high vacuum (UHV) and at 500 mtorr of oxygen pressure using ambient pressure X-ray photoelectron spectroscopy (APXPS). Under UHV, lithium intercalated into LixV2O5 while molecular oxygen was reduced to form lithium peroxide on LixV2O5 in the presence of oxygen upon discharge. Interestingly, the oxidation of Li2O2 began at much lower overpotentials (~240 mV) than the charge overpotentials of conventional Li-O2 cells with aprotic electrolytes (~1000 mV). Our study provides the first evidence of reversible lithium peroxide formation and decomposition in situ on an oxide surface using a solid-state cell, and new insights into the reaction mechanism of Li-O2 chemistry. PMID:23056907

  9. X-ray photoelectron spectroscopy studies of MgB 2 for valence state of Mg

    NASA Astrophysics Data System (ADS)

    A. Talapatra; Bandyopadhyay, S. K.; Sen, Pintu; Barat, P.; Mukherjee, S.; Mukherjee, M.

    2005-03-01

    Core level X-ray photoelectron spectroscopy (XPS) studies have been carried out on polycrystalline MgB 2 pellets over the whole binding energy range with a view to having an idea of the charge state of magnesium (Mg). We observe three distinct peaks in Mg 2p spectra at 49.3 eV (trace), 51.3 eV (major) and 54.0 eV (trace), corresponding to metallic Mg, MgB 2 and MgCO 3 or, divalent Mg species, respectively. Similar trend has been noticed in Mg 2s spectra. The binding energy of Mg in MgB 2 is lower than that corresponding to Mg(2+), indicative of the fact that the charge state of Mg in MgB 2 is less than (2+). Lowering of the formal charge of Mg promotes the σ → π electron transfer in boron (B) giving rise to holes on the top of the σ-band which are involved in coupling with B E 2g phonons for superconductivity. Through this charge transfer, Mg plays a positive role in hole superconductivity. B 1s spectra consist of three peaks corresponding to MgB 2, boron and B 2O 3. There is also evidence of MgO due to surface oxidation as seen from O 1s spectra.

  10. Thickness determination of molecularly thin lubricant films by angle-dependent X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Pang, Chongjun; Bai, Mingwu

    2007-03-01

    An angle-dependent X-ray photoelectron spectroscopy (XPS) method used to measure the thickness of molecularly thin lubricants was developed. The method was built based on an island model of patched overlayer on a flat substrate by using the photoemission signal solely from the lubricant film. Typical molecularly thin Zdol films on the CHx overcoat of unused commercial magnetic disks were measured to verify the metrology. The lubricant thickness determined by the metrology was equal to the recent result by thermostatic high vacuum atomic force microscopy. The measured deduction in the thickness of the molecularly thin lubricant films, successively irradiated by the monochromatic source operated at 14 kV/250 W, was as low as 1 Ǻ during the first irradiation hour. XPS spectra showed that no hydrocarbons, water or oxygen were adsorbed over the Zdol outer surfaces in the tested XPS conditions. The inelastic mean free path (IMFP) of C 1s in Zdol or in CHx was found to be independent of take off angle (TOA) when TOA < 40°. The IMFP of C 1s in Zdol was ˜63.5 Ǻ and the lubricant island thickness was ˜35 Ǻ.

  11. CHARACTERIZING SURFACE LAYERS IN NITINOL USING X-RAY PHOTOELECTRON SPECTROSCOPY

    SciTech Connect

    Christopfel, R.; Mehta, A.

    2008-01-01

    Nitinol is a shape memory alloy whose properties allow for large reversible deformations and a return to its original geometry. This nickel-titanium (NiTi) alloy has become a material used widely in the biomedical fi eld as a stent to open up collapsed arteries. Both ambient and biological conditions cause surface oxidation in these devices which in turn change its biocompatibility. The thickness of oxidized layers can cause fractures in the material if too large and can allow for penetration if too thin. Depending on the type and abundance of the chemical species on or near the surface, highly toxic metal ions can leak into the body causing cell damage or even cell death. Thus, biocompatibility of such devices is crucial. By using highly surface sensitive x-ray photoelectron spectroscopy to probe the surface of these structures, it is possible to decipher both layer composition and layer thickness. Two samples, both of which were mechanically polished, were investigated. Of the two samples, one was then exposed to a phosphate buffered saline (PBS) solution to mimic the chemical properties of blood, while the other remained unexposed. Although both samples were found to have oxide layers of appropriate thickness (on the order of a few nm), it was found that the sample exposed to the saline solution had a slightly thicker oxide layer and more signifi cantly, a phosphate layer very near the surface suggesting toxic metal components are well contained within the sample. These are considerable indications of a biocompatible device.

  12. In situ ambient pressure X-ray photoelectron spectroscopy studies of lithium-oxygen redox reactions.

    PubMed

    Lu, Yi-Chun; Crumlin, Ethan J; Veith, Gabriel M; Harding, Jonathon R; Mutoro, Eva; Baggetto, Loïc; Dudney, Nancy J; Liu, Zhi; Shao-Horn, Yang

    2012-01-01

    The lack of fundamental understanding of the oxygen reduction and oxygen evolution in nonaqueous electrolytes significantly hinders the development of rechargeable lithium-air batteries. Here we employ a solid-state Li(4+x)Ti(5)O(12)/LiPON/Li(x)V(2)O(5) cell and examine in situ the chemistry of Li-O(2) reaction products on Li(x)V(2)O(5) as a function of applied voltage under ultra high vacuum (UHV) and at 500 mtorr of oxygen pressure using ambient pressure X-ray photoelectron spectroscopy (APXPS). Under UHV, lithium intercalated into Li(x)V(2)O(5) while molecular oxygen was reduced to form lithium peroxide on Li(x)V(2)O(5) in the presence of oxygen upon discharge. Interestingly, the oxidation of Li(2)O(2) began at much lower overpotentials (~240 mV) than the charge overpotentials of conventional Li-O(2) cells with aprotic electrolytes (~1000 mV). Our study provides the first evidence of reversible lithium peroxide formation and decomposition in situ on an oxide surface using a solid-state cell, and new insights into the reaction mechanism of Li-O(2) chemistry. PMID:23056907

  13. Challenges for lithium species identification in complementary Auger and X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Hoffmann, M.; Zier, M.; Oswald, S.; Eckert, J.

    2015-08-01

    The combination of high spatial resolution and near-surface chemical information makes Auger electron spectroscopy (AES) a powerful tool for comprehensive surface analysis. The recent interest in lithium metal as an active material in lithium sulphur or lithium air batteries increases the demand for a thorough knowledge of the reactions happening at the electrode interface. Applying AES to the complex surfaces of batteries, however, requires a detailed understanding of the interactions occurring with the highly reactive materials during investigation, especially when using metallic lithium with its passivation layers formed even under glove box atmosphere. The article is focused on the influence of electron beam damage and residual gas under ultra-high vacuum conditions on the observations made. Immediate irradiation effects are shown to highly depend on electron dose leading to misinterpretation the surface composition and a non-sufficient stability of the sample. The results are further supported by coupled X-ray photoelectron spectroscopy (XPS) measurements that help to understand the beam induced phenomena. An improved output of the spectroscopic measurement could be achieved employing AES mappings. This allows an improved insight into the local distribution of different lithium compounds in the material surface and can also be applied to other battery active materials.

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

    SciTech Connect

    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.

  15. Self-detection of x-ray Fresnel transmissivity using photoelectron-induced gas ionization

    NASA Astrophysics Data System (ADS)

    Stoupin, Stanislav

    2016-01-01

    Electric response of an x-ray mirror enclosed in a gas flow ionization chamber was studied under the conditions of total external reflection for hard x-rays. It is shown that the electric response of the system as a function of the incidence angle is defined by x-ray Fresnel transmissivity and photon-electron attenuation properties of the mirror material. A simple interpretation of quantum yield of the system is presented. The approach could serve as a basis for non-invasive in situ diagnostics of hard x-ray optics, easy access to complementary x-ray transmissivity data in x-ray reflectivity experiments, and might also pave the way to advanced schemes for angle and energy resolving x-ray detectors.

  16. An X-ray photoelectron spectroscopy study of the thermal nitridation of SiO2/Si

    NASA Technical Reports Server (NTRS)

    Vasquez, R. P.; Madhukar, A.; Grunthaner, F. J.; Naiman, M. L.

    1986-01-01

    The dependence of the nitrogen distribution in thermally nitrided SiO2 films on the nitridation time and temperature has been studied by means of X-ray photoelectron spectroscopy (XPS). The photoelectron peak intensities were measured by fitting Voigt profiles to the XPS spectra and were used to calculate the film composition as a function of film depth, applying an analytical method described in detail. The times of appearance of the maxima in interfacial nitrogen concentration are shown for 800, 1000, and 1150 C, and the data are related to a kinetic model of Vasquez and Madhukar (1985), which considers the effect of interfacial strain on the nitridation kinetics. In addition, the intensity of a fluorine marker (from the HF used in the etching step) was found to correlate with the nitrogen concentration. It is postulated that the F bonds preferentially to defects. This hypothesis and the measured F intensities are consistent with the proposed strain-dependent energy of defect formation.

  17. ASCITOVG - FORTRAN PROGRAM FOR X-RAY PHOTOELECTRON SPECTROSCOPY DATA REFORMATTING

    NASA Technical Reports Server (NTRS)

    Able, P. B.

    1994-01-01

    It is often desirable to use a central, more powerful computer to analyze data captured on a local machine. ASCITOVG is a program for use on an IBM PC series computer which creates binary format files from columns of ASCII-format numbers. The resultant files are suitable for interactive analysis on a DEC PDP-11/73 under the Micro-RSX operating system running the VGS-5000 Enhanced Data Processing (EDP) software package. EDP performs data analysis interactively with a color graphics display, speeding up the analysis considerably when compared with batch job processing. Its interactive analysis capabilities also allow the researcher to watch for spurious data that might go undetected when some form of automatic spectrum processing is used. The incompatibility in floating-point number representations of an IBM PC and a DEC computer were resolved by a FORTRAN subroutine that correctly converts single-precision, floating-point numbers on the PC so that they can be directly read by DEC computers, such as a VAX. The subroutine also can convert binary DEC files (single-precision, floating-point numbers) to IBM PC format. This may prove a more efficient method of moving data from, for instance, a VAX-cluster down to a local IBM PC for further examination, manipulation, or display. The input data file used by ASCITOVG is simply a text file in the form of a column of ASCII numbers, with each value followed by a carriage return. These can be the output of a data collection routine or can even be keyed in through the use of a program editor. The data file header required by the EDP programs for an x-ray photoelectron spectrum is also written to the file. The spectrum parameters, entered by the user when the program is run, are coded into the header format used internally by all of the VGS-5000 series EDP packages. Any file transfer protocol having provision for binary data can be used to transmit the resulting file from the PC to the DEC machine. Each EDP data file has at least

  18. [Characterization of biochar by X-ray photoelectron spectroscopy and 13C nuclear magnetic resonance].

    PubMed

    Xu, Dong-yu; Jin, Jie; Yan, Yu; Han, Lan-fang; Kang, Ming-jie; Wang, Zi-ying; Zhao, Ye; Sun, Ke

    2014-12-01

    The wood (willow branch) and grass (rice straw) materials were pyrolyzed at different temperatures (300, 450 and 600 °C) to obtain the biochars used in the present study. The biochars were characterized using elementary analysis, X-ray photoelectron spectroscopy (XPS) and solid state 13C cross-polarization and magic angle spinning nuclear magnetic resonance spectroscopy (13C NMR) to illuminate the structure and composition of the biochars which were derived from the different thermal temperatures and biomass. The results showed that the H/C, O/C and (O+N)/C ratios of the biochars decreased with the increase in the pyrolysis temperatures. The surface polarity and ash content of the grass-derived biochars were higher than those of the wood-derived biochars. The minerals of the wood-derived biochars were mainly covered by the organic matter; in contrast, parts of the mineral surfaces of the grass-derived biochars were not covered by organic matter? The 13C NMR of the low temperature-derived biochars revealed a large contribution of aromatic carbon, aliphatic carbon, carboxyl and carbonyl carbon, while the high temperature-derived biochars contained a large amount of aromatic carbon. Moreover, the wood-derived biochars produced at low heat treatment temperatures contained more lignin residues than grass-derived ones, probably due to the existence of high lignin content in the feedstock soures of wood-derived biochars. The results of the study would be useful for environmental application of biochars. PMID:25881450

  19. Surface structure of human mucin using X-ray photoelectron spectroscopy.

    PubMed

    Russell, B G; Moddeman, W E; Birkbeck, J C; Wright, S E; Millington, D S; Stevens, R D; Dombrowski, K E

    1998-01-01

    X-ray photoelectron spectroscopy (XPS) is a surface sensitive analytical technique that measures the binding energy of electrons in atoms and molecules on the surface of a material. XPS was used to determine the distribution of the oligosaccharide side chains in the glycoprotein, MUC1 mucin. Low-resolution XPS spectra provided elemental composition of MUC1 mucin (fully glycosylated), mucin polypeptide (nonglycosylated), and carbohydrates found in mucin. The nitrogen content of MUC1 mucin was determined to be intermediate between the mucin polypeptide and the carbohydrates. Assuming a uniform distribution of carbohydrate on MUC1 mucin, the average thickness of the carbohydrate layer was calculated to be 4.9 nm using the low-resolution N 1s signals. High-resolution XPS spectra give detailed information about the chemical bonding of the surface molecules. Calculations based on the high-resolution O 1s spectra showed a carbohydrate thickness of 6.6 nm. These experimentally determined values agree reasonably well with an estimated 5 nm of carbohydrate thickness from a simple model which assume that the core protein is a rodlike molecule approximately 5 nm in diameter. Although the carbohydrate coating on the MUC1 mucin appears to be thick enough to cover the core protein entirely, fully glycosylated breast milk MUC1 mucin is susceptible to proteolytic digestion without removal of any oligosaccharide side chain, suggesting areas of exposed core protein. A possible explanation is that the oligosaccharide side chains may form patches of carbohydrate along the core protein with regions of exposed core protein. PMID:9706384

  20. X-ray photoelectron spectroscopy (XPS) investigation of the surface film on magnesium powders.

    PubMed

    Burke, Paul J; Bayindir, Zeynel; Kipouros, Georges J

    2012-05-01

    Magnesium (Mg) and its alloys are attractive for use in automotive and aerospace applications because of their low density and good mechanical properties. However, difficulty in forming magnesium and the limited number of available commercial alloys limit their use. Powder metallurgy may be a suitable solution for forming near-net-shape parts. However, sintering pure magnesium presents difficulties due to surface film that forms on the magnesium powder particles. The present work investigates the composition of the surface film that forms on the surface of pure magnesium powders exposed to atmospheric conditions and on pure magnesium powders after compaction under uniaxial pressing at a pressure of 500 MPa and sintering under argon at 600 °C for 40 minutes. Initially, focused ion beam microscopy was utilized to determine the thickness of the surface layer of the magnesium powder and found it to be ~10 nm. The X-ray photoelectron analysis of the green magnesium sample prior to sintering confirmed the presence of MgO, MgCO(3)·3H(2)O, and Mg(OH)(2) in the surface layer of the powder with a core of pure magnesium. The outer portion of the surface layer was found to contain MgCO(3)·3H(2)O and Mg(OH)(2), while the inner portion of the layer is primarily MgO. After sintering, the MgCO(3)·3H(2)O was found to be almost completely absent, and the amount of Mg(OH)(2) was also decreased significantly. This is postulated to occur by decomposition of the compounds to MgO and gases during the high temperature of sintering. An increase in the MgO content after sintering supports this theory. PMID:22524956

  1. Summary: Update to ASTM guide E 1523 to charge control and charge referencing techniques in x-ray photoelectron spectroscopy

    SciTech Connect

    Baer, D.R.

    2005-05-01

    An updated version of the American Society for Testing and Materials (ASTM) guide E 1523 to the methods to charge control and charge referencing techniques in x-ray photoelectron spectroscopy has been released by ASTM [Annual Book of ASTM Standards Surface Analysis (American Society for Testing and Materials, West Conshohocken, PA, 2004), Vol. 03.06]. The guide is meant to acquaint x-ray photoelectron spectroscopy (XPS) users with the various charge control and charge referencing techniques that are and have been used in the acquisition and interpretation of XPS data from surfaces of insulating specimens. The current guide has been expanded to include new references as well as recommendations for reporting information on charge control and charge referencing. The previous version of the document had been published in 1997 [D. R. Baer and K. D. Bomben, J. Vac. Sci. Technol. A 16, 754 (1998)].

  2. Numerical modeling of radiation physics in kinetic plasmas [IV] - Isochoric heating by intense X-ray laser-produced photoelectrons

    NASA Astrophysics Data System (ADS)

    Royle, Ryan; Sentoku, Yasuhiko

    2014-10-01

    An intense, hard X-ray laser such as an XFEL is an attractive light source since it can directly heat solid matter isochorically to a temperature of millions of degrees on a time scale of a few tens of femtoseconds, which is much shorter than the plasma expansion time scale. The X-ray laser interaction with carbon, aluminum, silicon, and copper is studied with a particle-in-cell code that solves the photoionization and X-ray transport self-consistently. Photoionization is the dominant absorption mechanism and non-thermal photoelectrons are produced with energy near the X-ray photon energy. The photoelectrons' stopping range is a few microns and they are quickly thermalized in tens of femtoseconds. As a result, a hot plasma column is formed behind the laser pulse with a temperature of more than 100,000 kelvin (>10 eV) and energy density greater than 1011 J/m3. The heating depth and temperature depend on the material and are also controllable by changing the photon energy of the incident laser light.

  3. X-ray photoelectron spectroscopic studies of graphitic materials and interfacial interactions in carbon-fiber-reinforced polymer composites

    NASA Astrophysics Data System (ADS)

    Viswanathan, Hema L.

    This dissertation involves the X-ray photoelectron spectroscopic (XPS) study of the chemistry associated with carbon fiber-reinforced composites fabricated using PAN-based carbon fibers and a thermoplastic polyimide resin. The mechanical properties of the ultimate composite are significantly affected by the nature of the fiber/matrix interface. Interfacial interaction can be promoted by the electrochemical modification of the fiber surface. The determination of carbon fiber microstructure was conducted through angle-resolved valence band photoemission studies of highly ordered graphite. The change in orientation of the basal planes and reactive edge sites with take-off angle provided a method for the determination of surface microstructure. The electronic structure of solid-state graphite was described using a band structure model and the results obtained were compared with the multiple scattered wave X a calculations. PAN-based fibers were electrochemically oxidized and studied using monochromatic X-radiation. The extremely narrow natural linewidth of the monochromatized Al K a radiation allowed previously unresolved features to be seen. In addition, sample decomposition due to radiative heat from the X-ray source is eliminated. Fibers that were pretreated by the manufacturer were subjected to further electrochemical oxidation. The fibers behaved in an erratic and non-reproducible manner. The surface treatment was removed by heating the fibers in vacuum, followed by XPS analysis and electrochemical oxidation. The fiber/matrix interface was simulated by coating a very thin layer of the polyimide resin on the surface of the fiber followed by XPS analysis. The validity of a proposed structure for the resin was confirmed by comparison with ab initio calculations conducted on the resin repeat unit. A high level of fiber/matrix interaction was observed for electrochemically oxidized fibers. The possibility of solvent interaction with the fiber surface was eliminated by

  4. Coordination defects in bismuth-modified arsenic selenide glasses: High-resolution x-ray photoelectron spectroscopy measurements

    SciTech Connect

    Golovchak, Roman; Shpotyuk, Oleh

    2008-05-01

    The possibility of coordination defects formation in Bi-modified chalcogenide glasses is examined by high-resolution x-ray photoelectron spectroscopy. The results provide evidence for the formation of positively charged fourfold coordinated defects on As and Bi sites in glasses with low Bi concentration. At high Bi concentration, mixed As{sub 2}Se{sub 3}-Bi{sub 2}Se{sub 3} nanocrystallites are formed in the investigated Se-rich As-Se glasses.

  5. In Situ Ambient Pressure X-ray Photoelectron Spectroscopy Studies of Lithium-Oxygen Redox Reactions

    SciTech Connect

    Lu, Yi-Chun; Crumlin, Ethan J.; Veith, Gabriel M.; Harding, Jonathon R.; Mutoro, Eva; Baggetto, Loïc; Dudney, Nancy J.; Liu, Zhi; Shao-Horn, Yang

    2012-10-08

    The lack of fundamental understanding of the oxygen reduction and oxygen evolution in nonaqueous electrolytes significantly hinders the development of rechargeable lithium-air batteries. Here we employ a solid-state Li4+xTi5O12/LiPON/LixV2O5 cell and examine in situ the chemistry of Li-O2 reaction products on LixV2O5 as a function of applied voltage under ultra high vacuum (UHV) and near ambient-pressure of oxygen using X-ray photoelectron spectroscopy (APXPS). Oxygen reduction and evolution reactions take place on the surface of the mixed electronic and Li+ ionic conductor, LixV2O5, which eliminate parasitic reactions between oxygen reduction/evolution reaction intermediates and aprotic electrolytes used in Li-O2 batteries reported to date. Under UHV, reversible lithium intercalation and de-intercalation from LixV2O5 was noted, where the changes in the vanadium valence state revealed from XPS in this study were comparable to that reported previously from Li/LixV2O5 thin film batteries. In presence of oxygen near ambient pressure, the LixV2O5 surface was covered gradually by the reaction product of oxygen reduction, namely lithium peroxide (Li2O2) (approximately 1-2 unit cells) upon discharge. Interestingly, the LixV2O5 surface became re-exposed upon charging, and the oxidation of Li2O2 began at much lower overpotentials (~240 mV) than the charge overpotentials of Li-O2 cells (~1000 mV) with aprotic electrolytes, which can be attributed to subnanometer-thick Li2O2 with surfaces free of contaminants such as carbonate species. Our study provides first evidence of reversible lithium peroxide formation and decomposition in situ on an oxide surface using a solid-state cell, and new insights into the reaction mechanism of Li-O2 chemistry.

  6. X-Ray Photoelectron Spectroscopy and the Role of Relaxation Energy in Understanding Chemical Shifts

    ERIC Educational Resources Information Center

    Ellison, Frank O.; White, Michael G.

    1976-01-01

    Discusses the measurement of electrons ejected from a system which is being irradiated with X-rays or ultraviolet photons, and a theoretical model for calculating core-electron ionization energies. (MLH)

  7. X-ray photoelectron spectroscopy study of the passive films formed on thermally sprayed and wrought Inconel 625

    NASA Astrophysics Data System (ADS)

    Bakare, M. S.; Voisey, K. T.; Roe, M. J.; McCartney, D. G.

    2010-11-01

    There is a well known performance gap in corrosion resistance between thermally sprayed corrosion resistant coatings and the equivalent bulk materials. Interconnected porosity has an important and well known effect, however there are additional relevant microstructural effects. Previous work has shown that a compositional difference exists between the regions of resolidified and non-melted material that exist in the as-sprayed coatings. The resolidified regions are depleted in oxide forming elements due to formation of oxides during coating deposition. Formation of galvanic cells between these different regions is believed to decrease the corrosion resistance of the coating. In order to increase understanding of the details of this effect, this work uses X-ray photoelectron spectroscopy (XPS) to study the passive films formed on thermally sprayed coatings (HVOF) and bulk Inconel 625, a commercially available corrosion resistant Ni-Cr-Mo-Nb alloy. Passive films produced by potentiodynamic scanning to 400 mV in 0.5 M sulphuric acid were compared with air-formed films. The poorer corrosion performance of the thermally sprayed coatings was attributed to Ni(OH) 2, which forms a loose, non-adherent and therefore non-protective film. The good corrosion resistance of wrought Inconel 625 is due to formation of Cr, Mo and Nb oxides.

  8. X-ray photoelectron spectroscopy of CdSe nanocrystals with applications to studies of the nanocrystal surface

    SciTech Connect

    Katari, J.E.B. ); Colvin, V.L.; Alivisatos, A.P. Univ. of California, Berkeley CA )

    1994-04-14

    We report the use of X-ray photoelectron spectroscopy (XPS) to determine the surface composition of semiconductor nanocrystals. Crystalline, nearly monodisperse CdSe nanocrystals ranging in radius from 9 to 30 A were chemically synthesized and covalently bound to Au and Si surfaces for study. XPS core level peak positions for Cd and Se were in agreement with those of bulk CdSe. We have determined that the majority of Se atoms on the surface are unbonded as prepared and that Cd atoms are bonded to the surface ligand, tri-n-octylphosphine oxide, to the extent that such bonding is sterically allowed. We have determined that the total ligand saturation of the nanocrystal surface varies from 60% in the smaller nanocrystals to 30% in the larger nanocrystals. In addition, we have determined that upon exposure of the nanocrystals to air Se surface sites are oxidized, forming a SeO[sub 2] surface film which causes the nanocrystals to degrade over time. The nanocrystal surface can be modified by dispersing the crystals in pyridine. Nearly all of the P ligands are removed in this case, leaving behind primarily unsaturated Cd and Se surface atoms. In this case, both Cd and Se oxidize upon exposure to air. 35 refs., 17 figs., 1 tab.

  9. Oxidation of UO 2 fuel pellets in air at 503 and 543 K studied using X-ray photoelectron spectroscopy and X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Tempest, P. A.; Tucker, P. M.; Tyler, J. W.

    1988-02-01

    An understanding of the low temperature oxidation behaviour of UO 2 pellets in air is important in the unlikely event of gas ingress to a fuel can during handling or storage. The main parameter of concern is the production time of U 3O 8 particulate as a function of temperature. Factors which affect the UO2 → U3O8 transformation have been investigated by sequentially oxidising UO 2 fuel pellets in air at 503 and 543 K and monitoring the growth of U 3O and U 3O 7 using X-ray photoelectron spectroscopy, X-ray diffraction and scanning electron microscopy. Initially oxidation proceeded at a linear rate by the inward diffusion of oxygen to form a complete layer of substoichiometric U 3O 7. This phase was tetragonal with a {c}/{a} ratio of 1.015, significantly less than the value of 1.03 measured on UO 2 powder when oxidised under identical conditions. This difference and the preferred orientation exhibited by surface grains were caused by growth stresses induced in the pellet surface. Both intergranular and transgranular cracking occurred and became nucleation sites for the growth of U 3O 8. The linear oxidation period associated with U 3O 7 growth was much shorter at 543 than at 503 K and U 3O 8 nucleated earlier. Spallation and the production of particulate were only observed during the formation of U 3O 8 when a 30% increase in volume arose from the U3O7 → U3O8 phase change.

  10. High-resolution soft X-ray beamline ADRESS at the Swiss Light Source for resonant inelastic X-ray scattering and angle-resolved photoelectron spectroscopies

    PubMed Central

    Strocov, V. N.; Schmitt, T.; Flechsig, U.; Schmidt, T.; Imhof, A.; Chen, Q.; Raabe, J.; Betemps, R.; Zimoch, D.; Krempasky, J.; Wang, X.; Grioni, M.; Piazzalunga, A.; Patthey, L.

    2010-01-01

    The concepts and technical realisation of the high-resolution soft X-ray beamline ADRESS operating in the energy range from 300 to 1600 eV and intended for resonant inelastic X-ray scattering (RIXS) and angle-resolved photoelectron spectroscopy (ARPES) are described. The photon source is an undulator of novel fixed-gap design where longitudinal movement of permanent magnetic arrays controls not only the light polarization (including circular and 0–180° rotatable linear polarizations) but also the energy without changing the gap. The beamline optics is based on the well established scheme of plane-grating monochromator operating in collimated light. The ultimate resolving power E/ΔE is above 33000 at 1 keV photon energy. The choice of blazed versus lamellar gratings and optimization of their profile parameters is described. Owing to glancing angles on the mirrors as well as optimized groove densities and profiles of the gratings, the beamline is capable of delivering high photon flux up to 1 × 1013 photons s−1 (0.01% BW)−1 at 1 keV. Ellipsoidal refocusing optics used for the RIXS endstation demagnifies the vertical spot size down to 4 µm, which allows slitless operation and thus maximal transmission of the high-resolution RIXS spectrometer delivering E/ΔE > 11000 at 1 keV photon energy. Apart from the beamline optics, an overview of the control system is given, the diagnostics and software tools are described, and strategies used for the optical alignment are discussed. An introduction to the concepts and instrumental realisation of the ARPES and RIXS endstations is given. PMID:20724785

  11. High-resolution soft X-ray beamline ADRESS at the Swiss Light Source for resonant inelastic X-ray scattering and angle-resolved photoelectron spectroscopies.

    PubMed

    Strocov, V N; Schmitt, T; Flechsig, U; Schmidt, T; Imhof, A; Chen, Q; Raabe, J; Betemps, R; Zimoch, D; Krempasky, J; Wang, X; Grioni, M; Piazzalunga, A; Patthey, L

    2010-09-01

    The concepts and technical realisation of the high-resolution soft X-ray beamline ADRESS operating in the energy range from 300 to 1600 eV and intended for resonant inelastic X-ray scattering (RIXS) and angle-resolved photoelectron spectroscopy (ARPES) are described. The photon source is an undulator of novel fixed-gap design where longitudinal movement of permanent magnetic arrays controls not only the light polarization (including circular and 0-180 degrees rotatable linear polarizations) but also the energy without changing the gap. The beamline optics is based on the well established scheme of plane-grating monochromator operating in collimated light. The ultimate resolving power E/DeltaE is above 33000 at 1 keV photon energy. The choice of blazed versus lamellar gratings and optimization of their profile parameters is described. Owing to glancing angles on the mirrors as well as optimized groove densities and profiles of the gratings, the beamline is capable of delivering high photon flux up to 1 x 10(13) photons s(-1) (0.01% BW)(-1) at 1 keV. Ellipsoidal refocusing optics used for the RIXS endstation demagnifies the vertical spot size down to 4 microm, which allows slitless operation and thus maximal transmission of the high-resolution RIXS spectrometer delivering E/DeltaE > 11000 at 1 keV photon energy. Apart from the beamline optics, an overview of the control system is given, the diagnostics and software tools are described, and strategies used for the optical alignment are discussed. An introduction to the concepts and instrumental realisation of the ARPES and RIXS endstations is given. PMID:20724785

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

    SciTech Connect

    Rheinheimer, Vanessa; Casanova, Ignasi

    2014-06-01

    Electron-beam evaporation was used to produce thin films of β-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.

  13. Time-resolved x-ray photoelectron spectroscopy techniques for real-time studies of interfacial charge transfer dynamics

    SciTech Connect

    Shavorskiy, Andrey; Hertlein, Marcus; Guo Jinghua; Tyliszczak, Tolek; Cordones, Amy; Vura-Weis, Josh; Siefermann, Katrin; Slaughter, Daniel; Sturm, Felix; Weise, Fabian; Khurmi, Champak; Belkacem, Ali; Weber, Thorsten; Gessner, Oliver; Bluhm, Hendrik; Strader, Matthew; Cho, Hana; Coslovich, Giacomo; Kaindl, Robert A.; Lin, Ming-Fu; and others

    2013-04-19

    X-ray based spectroscopy techniques are particularly well suited to gain access to local oxidation states and electronic dynamics in complex systems with atomic pinpoint accuracy. Traditionally, these techniques are applied in a quasi-static fashion that usually highlights the steady-state properties of a system rather than the fast dynamics that often define the system function on a molecular level. Novel x-ray spectroscopy techniques enabled by free electron lasers (FELs) and synchrotron based pump-probe schemes provide the opportunity to monitor intramolecular and interfacial charge transfer processes in real-time and with element and chemical specificity. Two complementary time-domain xray photoelectron spectroscopy techniques are presented that are applied at the Linac Coherent Light Source (LCLS) and the Advanced Light Source (ALS) to study charge transfer processes in N3 dye-sensitized ZnO semiconductor nanocrystals, which are at the heart of emerging light-harvesting technologies.

  14. Study of Charge Trap Sites in SiN Films by Hard X-ray Photoelectron Spectroscopy

    NASA Astrophysics Data System (ADS)

    Kosemura, Daisuke; Takei, Munehisa; Nagata, Kohki; Akamatsu, Hiroaki; Hattori, Maki; Katayama, Daisuke; Nishita, Tatsuo; Hirota, Yoshihiro; Machida, Masatake; Son, Jin-Young; Koganezawa, Tomoyuki; Hirosawa, Ichiro; Ogura, Atsushi

    2010-04-01

    Hard X-ray photoelectron spectroscopy (HAX-PES) was performed at SPring-8, and has enabled us to study the bulk properties of SiN films deposited by microwave plasma-enhanced chemical vapor deposition and deeply buried SiN/SiO2 interfaces, owing to the large inelastic mean free path of a photoelectron with a high kinetic energy. The defect states in the SiN films were examined by HAX-PES in order to verify the charge-trapping mechanism in a silicon-oxide-nitride-oxide-silicon flash memory device. X-ray reflectometry (XRR) was also performed at SPring-8. There is a complementary relationship between photoelectron spectroscopy and XRR. This methodology is proposed in this paper as a powerful tool for examining material properties. The detailed depth profile analysis of the chemical states in the SiN films obtained by angle-resolved HAX-PES also helped us to examine the charge-trapping mechanism.

  15. Sub-nanosecond time-resolved ambient-pressure X-ray photoelectron spectroscopy setup for pulsed and constant wave X-ray light sources

    SciTech Connect

    Shavorskiy, Andrey; Slaughter, Daniel S.; Zegkinoglou, Ioannis; Rude, Bruce S.; Bluhm, Hendrik; Neppl, Stefan; Cryan, James P.; Siefermann, Katrin R.; Weise, Fabian; Lin, Ming-Fu; Bacellar, Camila; Ziemkiewicz, Michael P.; Fraund, Matthew W.; Khurmi, Champak; Wright, Travis W.; Schoenlein, Robert W.; Gessner, Oliver; Hertlein, Marcus P.; Tyliszczak, Tolek; Huse, Nils; and others

    2014-09-15

    An apparatus for sub-nanosecond time-resolved ambient-pressure X-ray photoelectron spectroscopy studies with pulsed and constant wave X-ray light sources is presented. A differentially pumped hemispherical electron analyzer is equipped with a delay-line detector that simultaneously records the position and arrival time of every single electron at the exit aperture of the hemisphere with ∼0.1 mm spatial resolution and ∼150 ps temporal accuracy. The kinetic energies of the photoelectrons are encoded in the hit positions along the dispersive axis of the two-dimensional detector. Pump-probe time-delays are provided by the electron arrival times relative to the pump pulse timing. An average time-resolution of (780 ± 20) ps (FWHM) is demonstrated for a hemisphere pass energy E{sub p} = 150 eV and an electron kinetic energy range KE = 503–508 eV. The time-resolution of the setup is limited by the electron time-of-flight (TOF) spread related to the electron trajectory distribution within the analyzer hemisphere and within the electrostatic lens system that images the interaction volume onto the hemisphere entrance slit. The TOF spread for electrons with KE = 430 eV varies between ∼9 ns at a pass energy of 50 eV and ∼1 ns at pass energies between 200 eV and 400 eV. The correlation between the retarding ratio and the TOF spread is evaluated by means of both analytical descriptions of the electron trajectories within the analyzer hemisphere and computer simulations of the entire trajectories including the electrostatic lens system. In agreement with previous studies, we find that the by far dominant contribution to the TOF spread is acquired within the hemisphere. However, both experiment and computer simulations show that the lens system indirectly affects the time resolution of the setup to a significant extent by inducing a strong dependence of the angular spread of electron trajectories entering the hemisphere on the retarding ratio. The scaling of the angular

  16. Applications of X-Ray Photoelectron Spectroscopy. Part I. High T(c) Superconductors. Part II. Polymer Degradation.

    NASA Astrophysics Data System (ADS)

    Allan, Kristi Ann

    1990-08-01

    X-ray Photoelectron Spectroscopy (XPS) was applied to two different areas of research: (1) high T _{rm c} cuprate superconductors, (2) X-ray induced polymer degradation. The metallic perovskite LaCuO_3 was synthesized using a high oxygen pressure synthesis. In the XPS spectra of this compound the Cu (2p_ {3/2}) peak exhibited a shift to higher binding energy and the L_3VV Auger kinetic energy is lower than that of CuO. These shifts are representative of Cu(III) in an octahedral site linked to neighboring Cu(III) via a single 180^ circ Cu-O-Cu bridge in a metallic phase similar to copper found in the CuO_2 sheets of the cuprate superconductors. This spectrum is therefore a useful standard for comparison with the XPS spectra of new high T_{rm c} cuprate superconductors. XPS measurements of Tl_{rm 2 - y}Ba_2CuO _{rm 6 - x} as a function of oxygen content to determine the oxidation/reduction mechanism of the CuO_2 sheet. Oxidation/reduction of the CuO_2 sheets beyond or below the formal valence of Cu^{2+} is one of the necessary conditions to induce superconductivity. By employing two new chemical analyses and XPS we determined that the oxidation/reduction mechanism of the CuO _2 sheets is achieved internally by the overlap of the Tl:6s band with the CuO_2 conduction band. Changes in the oxygen content resulted in (1) changes in the phase as evidenced by the appearance or lack of T_{rm c}, (2) changes in the crystal symmetry, and (3) changes in the c axis lattice parameter obtained from X-ray diffraction measurements. Thallium is extruded during the annealing process and this was verified by both the X-ray diffraction and the XPS measurements. Recently, in a study of the anchoring of organometallic compounds on polyvinyl alcohol (PVA, -(CH_2 -HCOH)_{rm n} -), we observed X-ray exposure-dependent changes in the polymer composition. This motivated the detailed study of the X-ray induced compositional modifications of a solvent cast polyvinyl alcohol (PVA) polymer films

  17. X-ray photoelectron spectroscopic study of surface chemistry of dibenzyl disulfide on steel under mild and severe wear conditions

    NASA Technical Reports Server (NTRS)

    Wheeler, D. R.

    1978-01-01

    X-ray photoelectron spectroscopy was used to characterize the chemical composition of 304 stainless steel surfaces run in oil containing dibenzyl disulfide under both mild and severe wear conditions. In severe wear a sulfide was formed at the expense of the normal oxide. This was due to either chemical attack on the oxide or reaction with clean metal exposed by the wear process. In the mild wear scars there was no evidence of either sulfide or mercaptide. The oxide, however, was approximately twice as thick as the normal oxide on an unworn surface. The change in surface chemistry was primarily a function of wear rate rather than load.

  18. Application of maximum-entropy spectral estimation to deconvolution of XPS data. [X-ray Photoelectron Spectroscopy

    NASA Technical Reports Server (NTRS)

    Vasquez, R. P.; Klein, J. D.; Barton, J. J.; Grunthaner, F. J.

    1981-01-01

    A comparison is made between maximum-entropy spectral estimation and traditional methods of deconvolution used in electron spectroscopy. The maximum-entropy method is found to have higher resolution-enhancement capabilities and, if the broadening function is known, can be used with no adjustable parameters with a high degree of reliability. The method and its use in practice are briefly described, and a criterion is given for choosing the optimal order for the prediction filter based on the prediction-error power sequence. The method is demonstrated on a test case and applied to X-ray photoelectron spectra.

  19. Origin of resistivity change in NiO thin films studied by hard x-ray photoelectron spectroscopy

    SciTech Connect

    Calka, P.; Martinez, E.; Lafond, D.; Minoret, S.; Guedj, C.; Tirano, S.; Detlefs, B.; Roy, J.; Zegenhagen, J.

    2011-06-15

    We investigated origins of the resistivity change during the forming of NiO based resistive random access memories in a nondestructive way using hard x-ray photoelectron spectroscopy. Energy shifts and bandgap states observed after switching suggest that oxygen vacancies are created in the low resistive state. As a result conduction may occur via defects such as electrons traps and metallic nickel impurities. Migration of oxygen atoms seems to be the driving mechanism. This provides concrete evidence of the major role played by oxygen defects in decreasing resistivity. This is a key point since oxygen vacancies are particularly unstable and thus difficult to identify by physico-chemical analyses.

  20. Interaction of nitric oxide with Pt(1 0 0). A fast X-ray photoelectron spectroscopy study

    NASA Astrophysics Data System (ADS)

    Rienks, E. D. L.; Bakker, J. W.; Baraldi, A.; Carabineiro, S. A. C.; Lizzit, S.; Weststrate, C. J.; Nieuwenhuys, B. E.

    2002-09-01

    The interaction of nitric oxide (NO) with the clean, reconstructed (1 0 0) surface of platinum is studied using synchrotron X-ray photoelectron spectroscopy. It is found that molecular adsorption at 200 K yields two different molecular NO species. Above 250 K, NO is found to adsorb both dissociatively and molecularly, giving rise to an oxygen/NO coadsorption structure with a molecular coverage that is half of that at 200 K. At 375 K, adsorption is found to be exclusively dissociative. Furthermore, it is found that NO dissociation yields two different atomic oxygen species. No significant coverage of atomic nitrogen is observed indicating fast combination of nitrogen atoms upon NO dissociation.

  1. Effects of applying bias voltage on metal-coated pentacene films on SiO2 studied by hard X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Hirosawa, Ichiro; Watanabe, Takeshi; Oji, Hiroshi; Yasuno, Satoshi; Koganezawa, Tomoyuki; Tada, Keisuke; Yoshimoto, Noriyuki

    2016-03-01

    The effects of bias voltage application on C 1s photoelectron kinetic energies in Au- and Ag-coated pentacene films on SiO2 were studied by hard X-ray photoelectron spectroscopy. It was observed that the kinetic energies of C 1s were smaller in shallow regions in contact with metals than in mid regions of the pentacene films. The differences in C 1s kinetic energy between the shallow and mid regions of the Ag-coated pentacene films were slightly larger than those of the Au-coated films. The differences in the kinetic energies were decreased by applying negative voltages. The larger effect of voltage application was observed in the Ag-coated film than in the Au-coated film. In addition, partially reduced Si atoms in SiO2 were found at the interface to the pentacene film.

  2. Nanocrystalline tin oxide: Possible origin of its weak ferromagnetism deduced from nuclear magnetic resonance and X-ray photoelectron spectroscopies

    NASA Astrophysics Data System (ADS)

    Zhang, Feng; Lian, Yadong; Gu, Min; Yu, Ji; Tang, Tong B.; Sun, Jian; Zhang, Weiyi

    2016-09-01

    Nanocrystalline tin oxide was fabricated, with molar ratio O/Sn determined as 1.40, 1.55, 1.79, 1.92 and 1.96 from X-ray photoelectron spectroscopy. They displayed weak ferromagnetism, the sample with O/Sn = 1.55 showing the maximum saturation magnetization reaching almost 8 ×10-3 emu /g at room temperature. 119Sn nuclear magnetic resonance allowed the deduction, based on four resolved resonance peaks, that their Sn ions had four possible coordination numbers, namely 3, 4, 5 and 6. The relative fraction of 4-coordinated cations was the one found to bear positive linear correlation with saturation magnetization of the sample. It is surmised that magnetism in tin oxide results mainly from 4-coordination Sn ions, of valance about +3, as estimated from the binding energies of their 3d photoelectron emission levels.

  3. Forward scattering in hard X-ray photoelectron spectroscopy: Structural investigation of buried Mn–Ga films

    SciTech Connect

    ViolBarbosa, Carlos E. Ouardi, Siham; Fecher, Gerhard H. Felser, Claudia; Kubota, Takahide; Mizukami, Shigemi; Miyazaki, Terunobu; Ikenaga, Eiji

    2015-02-02

    X-ray photoelectron diffraction (XPD) in combination with hard X-ray photoelectron spectroscopy (HAXPES) has been used to study the structure of buried layers in thin multilayer films. A detailed layer-by-layer investigation was performed using the element-specific, local-probe character of XPD. In the present work, angular-resolved HAXPES at a photon energy of 7.94 keV photon energy was used to investigate a Cr/Mn{sub 62}Ga{sub 38}/Mg/MgO multilayer system. Differences in the angular distributions of electrons emitted from Mn and Ga atoms revealed that the structure of Mn{sub 62}Ga{sub 38} changes from L1{sub 0} towards D0{sub 22} for increasing annealing temperatures. A c/a ratio of 1.81 ± 0.06 was determined for the buried Mn{sub 62}Ga{sub 38} layer in a D0{sub 22} structure from the XPD experiment. The improvement of the structural order of the Mn{sub 62}Ga{sub 38} layer is accompanied by an improvement of the structure of the overlying MgO layer.

  4. A novel X-ray photoelectron spectroscopy study of the Al/SiO2 interface

    NASA Technical Reports Server (NTRS)

    Hecht, M. H.; Vasquez, R. P.; Grunthaner, F. J.; Zamani, N.; Maserjian, J.

    1985-01-01

    The nondestructive measurement of the chemical and physical characteristics of the interface between bulk SiO2 and thick aluminum films is reported. Both X-ray phototelectron spectroscopy (XPS) and electrical measurements of unannealed, resistively evaporated Al films on thermal SiO2 indicate an atomically abrupt interface. Post metallization annealing at 450 C induces reduction of the SiO2 by the aluminum, at a rate consistent with the bulk reaction rate. The XPS measurement is performed from the SiO2 side after the removal of the Si substrate with XeF2 gas and thinning of the SiO2 layer with HF:ETOH. This represents a powerful new approach to the study of metal-insulator and related interfaces.

  5. XPS studies of structure-induced radiation effects at the Si/SiO2 interface. [X ray Photoelectron Spectroscopy

    NASA Technical Reports Server (NTRS)

    Grunthaner, F. J.; Lewis, B. F.; Zamini, N.; Maserjian, J.; Madhukar, A.

    1980-01-01

    The interfacial structures of radiation hard and soft oxides grown by dry and wet processes on silicon substrates have been examined by high-resolution X-ray photoelectron spectroscopy. It is found that the primary difference in the local atomic structure at the Si/SiO2 interface is the significantly higher concentration of strained 120 deg SiO2 bonds and SiO interfacial species in soft samples. Results of in situ radiation damage experiments using low energy electrons (0-20 eV) are reported which correlate with the presence of a strained layer of SiO2 (20 A) at the interface. The results are interpreted in terms of a structural model for hole and electron trap generation by ionizing radiation.

  6. Photoelectron Experiments and Studies of X-Ray Absorption Near Edge Structure in Alkaline-Earth and Rare - Fluorides.

    NASA Astrophysics Data System (ADS)

    Gao, Yuan

    Alkaline-earth fluorides and rare-earth trifluorides possess technological importance for applications in multi -layer electronic device structures and opto-electronic devices. Interfaces between thin films of YbF _3 and Si(111) substrates were studied by photoelectron spectroscopy and x-ray absorption spectroscopy using synchrotron radiation. Results of YbF_3 /Si(111) were compared with those of TmF _3/Si(111). While electrons in the Si valence band are prevented from occupying the empty 4f levels in TmF_3 at the interface by the on -site Coulomb repulsion energy, the charge transfer from Si to YbF_3 is possible because the totally filled 4f states in Yb still lie below the Si valence band maximum. The theory of x-ray absorption near edge structure (XANES) is incomplete except for a few particularly simple special cases. A Bragg reflection model was developed to qualitatively explain the oscillations in XANES, in terms of the scattering of the photoelectron wave between families of lattice planes as set out by the Bragg condition for backscattering. The model was found to represent the data for systems with nearly free electron like conduction bands reasonably well. High resolution CaF_2 fluorine K edge XANES was used as a prototype to understand XANES in more depth on systems with strong core hole effects. Unlike previous work which involved multiple scattering cluster calculations that include only short range order effects, both the long range order and the symmetry breaking core holes are included in a new bandstructure approach in which the core hole is treated with a supercell technique. A first principles calculation with the use of pseudopotentials successfully reproduced all the main features of the first 15 eV of the fluorine K edge in CaF_2 which had not been explained with the cluster calculations. A comparison of the theoretical and experimental fluorine K edges in CaF_2 and BaF _2 was used to identify the structure related features. The possibility

  7. X-ray photoelectron spectroscopy analysis of cleaning procedures for synchrotron radiation beamline materials at the Advanced Photon Source

    SciTech Connect

    Li, Y.; Ryding, D.; Liu, C.; Kuzay, T.M.; McDowell, M.W.; Rosenberg, R.A.

    1995-05-01

    TZM (a high-temperature molybdenum alloy), machinable tungsten, and 304 stainless steel were cleaned using environmentally safe, commercially available cleaning detergents. The surface cleanliness was evaluated by x-ray photoelectron spectroscopy. It was found that a simple alkaline detergent is very effective at removal of organic and inorganic surface contaminants or foreign particle residue from machining processes. The detergent can be used with ultrasonic agitation at 140 {degree}F to clean the TZM molybdenum, machinable tungsten, and 304 stainless steel. A citric-acid-based detergent was also found to be effective at cleaning metal oxides, such as iron oxide, molybdenum oxide, as well as tungsten oxides, at mild temperatures with ultrasonic agitation, and it can be used to replace strong inorganic acids to improve cleaning safety and minimize waste disposal and other environmental problems. The efficiency of removing the metal oxides depends on both cleaning temperature and time. {copyright} {ital 1995} {ital American} {ital Vacuum} {ital Society}

  8. X-ray photoelectron spectroscopy studies of bond structure between polyvinyl alcohol and a titanate cross-coupling agent

    SciTech Connect

    Guelguen, M.A.; Popoola, O.O.; Kriven, W.M.

    1995-06-01

    Chemical interactions between polyvinyl alcohol (PVA) and triethanol amine titanate chelate were studied using x-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). The titanate chelate cross coupled the PVA solution and produced a viscous gel. The gel had a three- dimensional network structure containing --C{sub PVA}--O--Ti--O--C{sub PVA}--organic complexes. A new C(1{ital s}) signature at 285.7 eV and an O(1{ital s}) signature at 531.25 eV were associated with the formation of these complexes. The water of the PVA solution was physically retained in the gelled structure and was readily available for chemical reactions. The removal of this entrapped water was irreversible and lead to a collapsed film of Ti-cross-linked PVA.

  9. Assessment of the Quality of Newly Formed Bone around Titanium Alloy Implants by Using X-Ray Photoelectron Spectroscopy.

    PubMed

    Nakada, Hiroshi; Sakae, Toshiro; Tanimoto, Yasuhiro; Teranishi, Mari; Kato, Takao; Watanabe, Takehiro; Saeki, Hiroyuki; Kawai, Yasuhiko; Legeros, Racquel Z

    2012-01-01

    The aim of this study was to evaluate differences in bones quality between newly formed bone and cortical bone formed around titanium alloy implants by using X-ray photoelectron spectroscopy. As a result of narrow scan measurement at 4 weeks, the newly formed bone of C1s, P2p, O1s, and Ca2p were observed at a different peak range and strength compared with a cortical bone. At 8 weeks, the peak range and strength of newly formed bone were similar to those of cortical bone at C1s, P2p, and Ca2p, but not O1s. The results from this analysis indicate that the peaks and quantities of each element of newly formed bone were similar to those of cortical bone at 8 weeks, suggestive of a strong physicochemical resemblance. PMID:22778740

  10. X-ray photoelectron spectroscopy study of para-substituted benzoic acids chemisorbed to aluminum oxide thin films

    SciTech Connect

    Kreil, Justin; Ellingsworth, Edward; Szulczewski, Greg

    2013-11-15

    A series of para-substituted, halogenated (F, Cl, Br, and I) benzoic acid monolayers were prepared on the native oxide of aluminum surfaces by solution self-assembly and spin-coating techniques. The monolayers were characterized by x-ray photoelectron spectroscopy (XPS) and water contact angles. Several general trends are apparent. First, the polarity of the solvent is critical to monolayer formation. Protic polar solvents produced low coverage monolayers; in contrast, nonpolar solvents produced higher coverage monolayers. Second, solution deposition yields a higher surface coverage than spin coating. Third, the thickness of the monolayers determined from XPS suggests the plane of the aromatic ring is perpendicular to the surface with the carboxylate functional group most likely binding in a bidentate chelating geometry. Fourth, the saturation coverage (∼2.7 × 10{sup 14} molecules cm{sup −2}) is independent of the para-substituent.

  11. Band alignment at a MgO/GaSb heterointerface using x-ray photoelectron spectroscopy measurements

    NASA Astrophysics Data System (ADS)

    Li, Ruxue; Wei, Zhipeng; Liu, Xue; Li, Yongfeng; Fang, Xuan; Tang, Jilong; Fang, Dan; Gao, Xian; Wang, Dengkui; Hao, Yongqin; Yao, Bin; Ma, Xiaohui; Wang, Xiaohua

    2016-07-01

    The valence band offset (ΔE V) of a MgO/GaSb heterostructure was determined using x-ray photoelectron spectroscopy measurements. A ΔE V value of 2.84 ± 0.10 eV was calculated by using Ga 3d3/2 and Mg 2p1/2 binding energies as references. Taking the empirical band gaps of 7.83 eV and 0.73 eV for MgO and GaSb thin films into consideration, respectively, we obtained the type-I band alignment of a MgO/GaSb heterostructure with a conduction band offset (ΔE c) of 4.26 ± 0.10 eV, suggesting a nested interface band alignment.

  12. Calculation of X-ray photoelectron spectra with the use of the normalized elimination of the small component method

    NASA Astrophysics Data System (ADS)

    Klooster, Rob; Broer, Ria; Filatov, Michael

    2012-02-01

    A method for the calculation of X-ray photoelectron spectra (XPS) based on the use of the normalized elimination of the small component (NESC) formalism combined with the restricted active space state interaction (RASSI) approach with atomic mean field integrals (AMFI) is developed. Benchmark calculations carried out for the 4f XPS of U5+show that the NESC/RASSI/AMFI method is capable of reproducing the results of the full 4-component relativistic calculations with excellent accuracy. The NESC/RASSI/AMFI method is applied to study the 4p and 5p XPS of ytterbium phosphide YbP. The results of the calculations suggest an alternative interpretation of the satellite peaks in the 4p XPS of YbP.

  13. Employing X-ray Photoelectron Spectroscopy for Determining Layer Homogeneity in Mixed Polar Self-Assembled Monolayers.

    PubMed

    Hehn, Iris; Schuster, Swen; Wächter, Tobias; Abu-Husein, Tarek; Terfort, Andreas; Zharnikov, Michael; Zojer, Egbert

    2016-08-01

    Self-assembled monolayers (SAMs) containing embedded dipolar groups offer the particular advantage of changing the electronic properties of a surface without affecting the SAM-ambient interface. Here we show that such systems can also be used for continuously tuning metal work functions by growing mixed monolayers consisting of molecules with different orientations of the embedded dipolar groups. To avoid injection hot-spots when using the SAM-modified electrodes in devices, a homogeneous mixing of the two components is crucial. We show that a combination of high-resolution X-ray photoelectron spectroscopy with state-of-the-art simulations is an ideal tool for probing the electrostatic homogeneity of the layers and thus for determining phase separation processes in polar adsorbate assemblies down to inhomogeneities at the molecular level. PMID:27429041

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

    SciTech Connect

    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.

  15. Characterization of SiC fibers by soft x-ray photoelectron and photoabsorption spectroscopies and scanning Auger microscopy

    SciTech Connect

    Ma, Qing; McDowell, M.W.; Rosenberg, R.A.

    1996-08-01

    Synchrotron radiation soft x-ray photoelectron and photoabsorption spectroscopy was used to characterize commercially obtained SiC fibers produced by CVD on a W core and followed by a C passivating layer. Depth profiling of the fiber through the C/SiC interface was done by making Si 2p and C 1s core level PES and PAS, as well as scanning Auger microscopy, measurements following Ar{sup +} sputtering. No significant changes in either photoemission or absorption or Auger line shapes were observed versus depth, indicating no significant interfacial reaction. The line shapes of the carbonaceous coatings are predominantely graphite-like and those of the CVD SiC coatings are microcrystalline, with disorder present to some extent in both cases.

  16. Austenitic and duplex stainless steels in simulated physiological solution characterized by electrochemical and X-ray photoelectron spectroscopy studies.

    PubMed

    Kocijan, Aleksandra; Conradi, Marjetka; Schön, Peter M

    2012-04-01

    A study of oxide layers grown on 2205 duplex stainless steel (DSS) and AISI 316L austenitic stainless steel in simulated physiological solution is presented here in order to establish the possibility of replacement of AISI 316 L with 2205 DSS in biomedical applications. The results of the potentiodynamic measurements show that the extent of the passive range significantly increased for DSS 2205 compared to AISI 316L stainless steel. Cyclic voltammetry was used to investigate electrochemical processes taking place on the steel surfaces. Oxide layers formed by electrochemical oxidation at different oxidation potentials were studied by X-ray photoelectron spectroscopy, and their compositions were analyzed as a function of depth. The main constituents on both the investigated materials were Cr- and Fe-oxides. Atomic force microscopy topography studies revealed the higher corrosion resistance of the DSS 2205 compared to the AISI 316L under the chosen experimental conditions. PMID:22331841

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

    SciTech Connect

    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.

  18. X-ray photoelectron spectroscopy study of the chemical structure of thermally nitrided SiO2

    NASA Technical Reports Server (NTRS)

    Vasquez, R. P.; Hecht, M. H.; Grunthaner, F. J.; Naiman, M. L.

    1984-01-01

    X-ray photoelectron spectroscopy has been used to study the composition of 100-A thermally grown SiO2 films that have been thermally nitrided in ammonia. The SiO(x)N(y)/Si interface was studied both by chemical depth profiling of the oxynitride and by removal of the Si substrate with XeF2. It is found that N is distributed throughout the film, but with the concentration higher at the surface and in a region centered 25 A from the film/substrate interface. The interface region itself is found to be oxygen-rich relative to the rest of the film. Possible models which can explain these results are discussed.

  19. Understanding Chemical versus Electrostatic Shifts in X-ray Photoelectron Spectra of Organic Self-Assembled Monolayers

    PubMed Central

    2016-01-01

    The focus of the present article is on understanding the insight that X-ray photoelectron spectroscopy (XPS) measurements can provide when studying self-assembled monolayers. Comparing density functional theory calculations to experimental data on deliberately chosen model systems, we show that both the chemical environment and electrostatic effects arising from a superposition of molecular dipoles influence the measured core-level binding energies to a significant degree. The crucial role of the often overlooked electrostatic effects in polar self-assembled monolayers (SAMs) is unambiguously demonstrated by changing the dipole density through varying the SAM coverage. As a consequence of this effect, care has to be taken when extracting chemical information from the XP spectra of ordered organic adsorbate layers. Our results, furthermore, imply that XPS is a powerful tool for probing local variations in the electrostatic energy in nanoscopic systems, especially in SAMs. PMID:26937264

  20. X-ray photoelectron spectroscopic study of Ge2Sb2Te5 etched by fluorocarbon inductively coupled plasmas

    NASA Astrophysics Data System (ADS)

    Kang, S.-K.; Oh, J. S.; Park, B. J.; Kim, S. W.; Lim, J. T.; Yeom, G. Y.; Kang, C. J.; Min, G. J.

    2008-07-01

    X-ray photoelectron spectroscopy was used to determine the level of surface fluorination damage of Ge2Sb2Te5 (GST) etched by fluorocarbon gases at different F/C ratios. When blank GST was etched, the gas with a higher F/C ratio produced a thinner C-F polymer on the etched surface but fluorinated Ge, Sb, and Te compounds were observed in the remaining GST. When the sidewall of the etched GST features was investigated, a thicker fluorinated layer was observed on the GST sidewall etched by the higher F/C ratio gas, indicating more fluorination due to the difficulty in preventing F diffusion into the GST through the thinner C-F layer.

  1. Band alignment of HfO2/AlN heterojunction investigated by X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Ye, Gang; Wang, Hong; Ji, Rong

    2016-04-01

    The band alignment between AlN and Atomic-Layer-Deposited (ALD) HfO2 was determined by X-ray photoelectron spectroscopy (XPS). The shift of Al 2p core-levels to lower binding energies with the decrease of take-off angles θ indicated upward band bending occurred at the AlN surface. Based on the angle-resolved XPS measurements combined with numerical calculations, valence band discontinuity ΔEV of 0.4 ± 0.2 eV at HfO2/AlN interface was determined by taking AlN surface band bending into account. By taking the band gap of HfO2 and AlN as 5.8 eV and 6.2 eV, respectively, a type-II band line-up was found between HfO2 and AlN.

  2. Surface Evaluation by X-Ray Photoelectron Spectroscopy of High Performance Polyimide Foams After Exposure to Oxygen Plasma

    NASA Technical Reports Server (NTRS)

    Melendez, Orlando; Hampton, Michael D.; Williams, Martha K.; Brown, Sylvia F.; Nelson, Gordon L.; Weiser, Erik S.

    2002-01-01

    Aromatic polyimides have been attractive in the aerospace and electronics industries for applications such as cryogenic insulation, flame retardant panels and structural subcomponents. Newer to the arena of polyimides is the synthesis of polyimide foams and their applications. In the present work, three different, closely related, polyimide foams developed by NASA Langley Research Center (LaRC) are studied by X-ray Photoelectron Spectroscopy (XPS) after exposure to radio frequency generated Oxygen Plasma. Although polyimide films exposure to atomic oxygen and plasma have been studied previously and reported, the data relate to films and not foams. Foams have much more surface area and thus present new information to be explored. Understanding degradation mechanisms and properties versus structure, foam versus solid is of interest and fundamental to the application and protection of foams exposed to atomic oxygen in Low Earth Orbit (LEO).

  3. Study of high-temperature oxidation of ultrathin fe films on Pt(100) by using X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Nahm, T.-U.

    2016-05-01

    High-temperature oxidation of iron thin films deposited on Pt(100) surfaces was studied by using X-ray photoelectron spectroscopy (XPS). Upon an oxygen exposure of 300 Langmuir onto a 7.5- monolayer (ML) Fe film at 830 K, about 2 monolayers of the Fe film were oxidized as Fe3O4 while the remaining Fe atoms diffused into the substrate. For 1.25-, 2.5-, and 3.75-monolayer Fe films, only about a monolayer of the Fe film was oxidized as FeO, regardless of the number of Fe atoms. The oxide layers on the 7.5-monolayer Fe film were observed to be stable upon post-annealing at 1030 K.

  4. X-ray photoelectron spectroscopy analysis of cleaning procedures for synchrotron radiation beamline materials at the Advanced Photon Source

    SciTech Connect

    Li, Y.; Ryding, D.; Liu, C.; Kuzay, T.M.; McDowell, M.W.; Rosenberg, R.A.

    1994-12-31

    TZM (a high temperature molybdenum alloy), machinable tungsten, and 304 stainless steel were cleaned using environmentally safe, commercially available cleaning detergents. The surface cleanliness was evaluated by x-ray photoelectron spectroscopy (XPS). It was found that a simple alkaline detergent is very effective at removal of organic and inorganic surface contaminants or foreign particle residue from machining processes. The detergent can be used with ultrasonic agitation at 140 F to clean the TZM molybdenum, machinable tungsten, and 304 stainless steel. A citric-acid-based detergent was also found to be effective at cleaning metal oxides, such as iron oxide, molybdenum oxide, as well as tungsten oxides at mild temperatures with ultrasonic agitation, and it can be used to replace strong inorganic acids to improve cleaning safety and minimize waste disposal and other environmental problems. The efficiency of removing the metal oxides depends on both cleaning temperature and time.

  5. Origins of sp(3)C peaks in C1s X-ray Photoelectron Spectra of Carbon Materials.

    PubMed

    Fujimoto, Ayaka; Yamada, Yasuhiro; Koinuma, Michio; Sato, Satoshi

    2016-06-21

    X-ray photoelectron spectroscopy (XPS) is among the most powerful techniques to analyze defective structures of carbon materials such as graphene and activated carbon. However, reported assignments of defects, especially sp(3)C and sp(2)C, are questionable. Most reports assign sp(3)C peaks to be higher than sp(2)C peaks, whereas a few reports assign sp(3)C peaks to be lower than sp(2)C peaks. Our group previously reported that calculated binding energies of sp(3)C were basically lower than those of sp(2)C. This work clarified that one of the reasons for the prevailing ambiguous assignments of sp(3)C peaks is charging effects of diamond. PMID:27264720

  6. Surface chemical composition of human maxillary first premolar as assessed by X-ray photoelectron spectroscopy (XPS)

    NASA Astrophysics Data System (ADS)

    Lou, Leo; Nelson, Alan E.; Heo, Giseon; Major, Paul W.

    2008-08-01

    The surface chemical composition of dental enamel has been postulated as a contributing factor in the variation of bond strength of brackets bonded to teeth, and hence, the probability of bracket failure during orthodontic treatment. This study systematically investigated the chemical composition of 98 bonding surfaces of human maxillary premolars using X-ray photoelectron spectroscopy (XPS) to ascertain compositional differences between right and left first premolars. The major elements detected in all samples were calcium, phosphorus, oxygen, nitrogen and carbon. Surface compositions were highly variable between samples and several elements were found to be highly correlated. No statistical significant difference in the chemical composition of the maxillary right and left first premolars was found ( p > 0.05). Knowledge of the chemical composition of enamel surfaces will facilitate future studies that relate this information to the variations in dental enamel bond strength.

  7. Thermal stability of electron-irradiated poly(tetrafluoroethylene) - X-ray photoelectron and mass spectroscopic study

    NASA Technical Reports Server (NTRS)

    Wheeler, Donald R.; Pepper, Stephen V.

    1990-01-01

    Polytetrafluoroethylene (PTFE) was subjected to 3 keV electron bombardment and then heated in vacuum to 300 C. The behavior of the material as a function of radiation dose and temperature was studied by X-ray photoelectron spectroscopy (XPS) of the surface and mass spectroscopy of the species evolved. Lightly damaged material heated to 300 C evolved saturated fluorocarbon species, whereas unsaturated fluorocarbon species were evolved from heavily damaged material. After heating the heavily damaged material, those features in the XPS spectrum that were associated with damage diminished, giving the appearance that the radiation damage had annealed. The observations were interpreted by incorporating mass transport of severed chain fragments and thermal decomposition of severely damaged material into the branched and cross-linked network model of irradiated PTFE. The apparent annealing of the radiation damage was due to covering of the network by saturated fragments that easily diffused through the decomposed material to the surface region upon heating.

  8. Energy band alignment of InGaZnO{sub 4}/Si heterojunction determined by x-ray photoelectron spectroscopy

    SciTech Connect

    Xie Zhangyi; Lu Hongliang; Xu Saisheng; Geng Yang; Sun Qingqing; Ding Shijin; Zhang, David Wei

    2012-12-17

    X-ray photoelectron spectroscopy was utilized to determine the valence band offset ({Delta}E{sub V}) of the InGaZnO{sub 4} (IGZO)/Si heterojunction. The IGZO films were grown on Si (100) using radio frequency magnetron sputtering. A value of {Delta}E{sub V} = 2.53 eV was obtained by using In 3d{sub 5/2}, Ga 2p{sub 3/2} core energy levels as references. Taking into consideration the experimental band gap of 3.20 eV of the IGZO, this would result in a conduction band offset {Delta}E{sub C} = 0.45 eV in this heterostructure.

  9. Application of ESCA to the determination of stoichiometry in sputtered coatings and interface regions. [X-ray photoelectron spectroscopy

    NASA Technical Reports Server (NTRS)

    Wheeler, D. R.

    1978-01-01

    X-ray Photoelectron Spectroscopy (XPS) was used to characterize radiofrequency sputter deposited films of several refractory compounds. Both the bulk film properties such as purity and stoichiometry and the character of the interfacial region between the film and substrate were examined. The materials were CrB2, MoS2, Mo2C, and Mo2B5 deposited on 440C steel. It was found that oxygen from the sputtering target was the primary impurity in all cases. Biasing improves the film purity. The effect of biasing on film stoichiometry is different for each compound. Comparison of the interfacial composition with friction data suggests that adhesion of these films is improved if a region of mixed film and iron oxides can be formed.

  10. X-ray photoelectron spectroscopy study on the chemistry involved in tin oxide film growth during chemical vapor deposition processes

    SciTech Connect

    Mannie, Gilbere J. A.; Gerritsen, Gijsbert; Abbenhuis, Hendrikus C. L.; Deelen, Joop van; Niemantsverdriet, J. W.; Thuene, Peter C.

    2013-01-15

    The chemistry of atmospheric pressure chemical vapor deposition (APCVD) processes is believed to be complex, and detailed reports on reaction mechanisms are scarce. Here, the authors investigated the reaction mechanism of monobutyl tinchloride (MBTC) and water during SnO{sub 2} thin film growth using x-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). XPS results indicate an acid-base hydrolysis reaction mechanism, which is tested with multilayer experiments, demonstrating self-terminating growth. In-house developed TEM wafers are used to visualize nucleation during these multilayer experiments, and results are compared with TEM results of APCVD samples. Results show almost identical nucleation behavior implying that their growth mechanism is identical. Our experiments suggest that in APCVD, when using MBTC and water, SnO{sub 2} film growth occurs via a heterolytic bond splitting of the Sn-Cl bonds without the need to invoke gas-phase radical or coordination chemistry of the MBTC precursor.

  11. Employing X-ray Photoelectron Spectroscopy for Determining Layer Homogeneity in Mixed Polar Self-Assembled Monolayers

    PubMed Central

    2016-01-01

    Self-assembled monolayers (SAMs) containing embedded dipolar groups offer the particular advantage of changing the electronic properties of a surface without affecting the SAM–ambient interface. Here we show that such systems can also be used for continuously tuning metal work functions by growing mixed monolayers consisting of molecules with different orientations of the embedded dipolar groups. To avoid injection hot-spots when using the SAM-modified electrodes in devices, a homogeneous mixing of the two components is crucial. We show that a combination of high-resolution X-ray photoelectron spectroscopy with state-of-the-art simulations is an ideal tool for probing the electrostatic homogeneity of the layers and thus for determining phase separation processes in polar adsorbate assemblies down to inhomogeneities at the molecular level. PMID:27429041

  12. Electronic structure of the carbon nanotube tips studied by x-ray-absorption spectroscopy and scanning photoelectron microscopy

    NASA Astrophysics Data System (ADS)

    Chiou, J. W.; Yueh, C. L.; Jan, J. C.; Tsai, H. M.; Pong, W. F.; Hong, I.-H.; Klauser, R.; Tsai, M.-H.; Chang, Y. K.; Chen, Y. Y.; Wu, C. T.; Chen, K. H.; Wei, S. L.; Wen, C. Y.; Chen, L. C.; Chuang, T. J.

    2002-11-01

    Angle-dependent x-ray absorption near edge structure (XANES) and scanning photoelectron microscopy (SPEM) measurements have been performed to differentiate local electronic structures of the tips and sidewalls of highly aligned carbon nanotubes. The intensities of both π*- and σ*-band C K-edge XANES features are found to be significantly enhanced at the tip. SPEM results also show that the tips have a larger density of states and a higher C 1s binding energy than those of sidewalls. The increase of the tip XANES and SPEM intensities are quite uniform over an energy range wider than 10 eV in contrast to earlier finding that the enhancement is only near the Fermi level.

  13. X-ray photoelectron spectroscopy and micro-Raman analysis of conductive RuO2 thin films

    NASA Astrophysics Data System (ADS)

    Bhaskar, S.; Dobal, P. S.; Majumder, S. B.; Katiyar, R. S.

    2001-03-01

    Ruthenium oxide (RuO2) was synthesized in thin film and powder forms using the solution chemistry technique. The oxide electrodes on Si substrates were characterized in terms of their structure, composition, stoichiometry, and conductivity. X-ray lattice parameter calculations and micro-Raman analysis revealed the rutile structure in the material. Both films and powders exhibited an unassigned Raman band at about 477 cm-1 in their Raman spectra. Performing peak frequency calculations for B2g and A1g modes of RuO2 using the rigid-ion model, which ruled out the possibility that this band originated from disorder induced symmetry, allowed silent mode. Based on the x-ray photoelectron spectroscopy (XPS) and temperature dependent Raman studies, this band was assigned to hydrated RuO2. XPS characterizations of our samples revealed minute surface contamination of oxygen and chlorine, probably due to the film preparation and high temperature deposition processes. Films with uniform microstructure, low surface roughness, and good electrical properties meet the requirements for serving as the bottom electrode for the ferroelectric capacitor.

  14. Reduction of Vanadium Oxide (VOx) under High Vacuum Conditions as Investigated by X-Ray Photoelectron Spectroscopy

    NASA Astrophysics Data System (ADS)

    Chourasia, A.

    2015-03-01

    Vanadium oxide thin films were formed by depositing thin films of vanadium on quartz substrates and oxidizing them in an atmosphere of oxygen. The deposition was done by the e-beam technique. The oxide films were annealed at different temperatures for different times under high vacuum conditions. The technique of x-ray photoelectron spectroscopy has been employed to study the changes in the oxidation states of vanadium and oxygen in such films. The spectral features in the vanadium 2p, oxygen 1s, and the x-ray excited Auger regions were investigated. The Auger parameter has been utilized to study the changes. The complete oxidation of elemental vanadium to V2O5 was observed to occur at 700°C. At any other temperature, a mixture of oxides consisting of V2O5 and VO2 was observed in the films. Annealing of the films resulted in the gradual loss of oxygen followed by reduction in the oxidation state from +5 to 0. The reduction was observed to depend upon the annealing temperature and the annealing time. Organized Research, TAMU-Commerce.

  15. X-ray photoelectron spectroscopic and morphologic studies of Ru nanoparticles deposited onto highly oriented pyrolytic graphite

    NASA Astrophysics Data System (ADS)

    Bavand, R.; Yelon, A.; Sacher, E.

    2015-11-01

    Ruthenium nanoparticles (Ru NPs) function as effective catalysts in specific reactions, such as methanation and Fischer-Tropsch syntheses. It is our purpose to physicochemically characterize their surfaces, at which catalysis occurs, by surface-sensitive X-ray photoelectron spectroscopy (XPS), using the symmetric peak component anaylsis technique developed in our laboratory to reveal previously hidden components. Ru NPs were deposited by evaporation (0.25-1.5 nm nominal deposition range) onto highly oriented pyrolytic graphite (HOPG). In addition to their surfaces being characterized by XPS, an indication of morphology was obtained from transmission electron microscopy (TEM). Our use of symmetric peak component XPS analysis has revealed detailed information on a previously unidentified surface oxide initially formed, as well as on the valence electronic structure and its variation with NP size, information that is of potential importance in the use of these NPs in catalysis. Each of the several Ru core XPS spectra characterized (3d, 3p and 3s) was found to be composed of three symmetric components. Together with two metal oxide O1s components, these give evidence of a rather complex, previously unidentified oxide that is initially formed. The Ru valence band (4d and 5s) spectra clearly demonstrate a loss of metallicity, a simultaneous increase of the Kubo gap, and an abrupt transfer in valence electron density from the 4d to the 5s orbitals (known as electron spill-over), as the NP size decreases below 0.5 nm. TEM photomicrographs, as a function of deposition rate, show that, at a rate that gives insufficient time for the NP condensation energy to dissipate, the initially well-separated NPs are capable of diffusing laterally and aggregating. This indicates weak NP bonding to the HOPG substrate. Carbide is formed, at both high and low deposition rates, at Ru deposition thicknesses greater than 0.25 nm, its formation explained by Ru NPs reacting with residual

  16. Evaluation of band offset at amorphous-Si/BaSi2 interfaces by hard x-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Takabe, Ryota; Takeuchi, Hiroki; Du, Weijie; Ito, Keita; Toko, Kaoru; Ueda, Shigenori; Kimura, Akio; Suemasu, Takashi

    2016-04-01

    The 730 nm-thick undoped BaSi2 films capped with 5 nm-thick amorphous Si (a-Si) intended for solar cell applications were grown on Si(111) by molecular beam epitaxy. The valence band (VB) offset at the interface between the BaSi2 and the a-Si was measured by hard x-ray photoelectron spectroscopy to understand the carrier transport properties by the determination of the band offset at this heterointerface. We performed the depth-analysis by varying the take-off angle of photoelectrons as 15°, 30°, and 90° with respect to the sample surface to obtain the VB spectra of the BaSi2 and the a-Si separately. It was found that the barrier height of the a-Si for holes in the BaSi2 is approximately -0.2 eV, whereas the barrier height for electrons is approximately 0.6 eV. This result means that the holes generated in the BaSi2 layer under solar radiation could be selectively extracted through the a-Si/BaSi2 interface, promoting the carrier separation in the BaSi2 layer. We therefore conclude that the a-Si/BaSi2 interface is beneficial for BaSi2 solar cells.

  17. First stages of surface steel nitriding: X-ray photoelectron spectroscopy and electrical measurements

    NASA Astrophysics Data System (ADS)

    Flori, M.; Gruzza, B.; Bideux, L.; Monier, G.; Robert-Goumet, C.; Benamara, Z.

    2009-08-01

    Quantitative and qualitative analysis techniques were employed to study the first stages of ultra-high vacuum plasma nitriding of the 42CrMo4 steel. At constant treatment temperature, maintained for all samples at about 360 °C, we have established the influence of treatment time on the chemical composition, thickness and electrical properties of the nitrided layer. In this purpose it was used a stacking atomic layer model describing the sample surface, which takes into account the attenuation depth of photoelectrons by the atomic monolayers. So, we have found that after 2 h of nitriding in laboratory conditions, 70% of the nitrided layer was composed of iron oxide. Also, I- V measurements indicate an influence of the nitride overlayer with increasing treatment time.

  18. Auger electron nanoscale mapping and x-ray photoelectron spectroscopy combined with gas cluster ion beam sputtering to study an organic bulk heterojunction

    SciTech Connect

    Heon Kim, Seong; Heo, Sung; Ihn, Soo-Ghang; Yun, Sungyoung; Hwan Park, Jong; Chung, Yeonji; Lee, Eunha; Park, Gyeongsu; Yun, Dong-Jin

    2014-06-16

    The lateral and vertical distributions of organic p/n bulk heterojunctions for an organic solar cell device are, respectively, investigated using nanometer-scale Auger electron mapping and using X-ray photoelectron spectroscopy (XPS) with Ar gas cluster ion beam (GCIB) sputtering. The concentration of sulfur, present only in the p-type material, is traced to verify the distribution of p-type (donor) and n-type (acceptor) materials in the blended structure. In the vertical direction, a considerable change in atomic sulfur concentration is observed using XPS depth profiling with Ar GCIB sputtering. In addition, Auger electron mapping of sulfur reveals the lateral 2-dimensional distribution of p- and n-type materials. The combination of Auger electron mapping with Ar GCIB sputtering should thereby allow the construction of 3-dimensional distributions of p- and n-type materials in organic photovoltaic cells.

  19. X-Ray photoelectron spectroscopy study of radiofrequency-sputtered titanium, carbide, molybdenum carbide, and titanium boride coatings and their friction properties

    NASA Technical Reports Server (NTRS)

    Brainard, W. A.; Wheeler, D. R.

    1977-01-01

    Radiofrequency sputtered coatings of titanium carbide, molybdenum carbide and titanium boride were tested as wear resistant coatings on stainless steel in a pin on disk apparatus. X-ray photoelectron spectroscopy (XPS) was used to analyze the sputtered films with regard to both bulk and interface composition in order to obtain maximum film performance. Significant improvements in friction behavior were obtained when properly biased films were deposited on deliberately preoxidized substrates. XPS depth profile data showed thick graded interfaces for bias deposited films even when adherence was poor. The addition of 10 percent hydrogen to the sputtering gas produced coatings with thin poorly adherent interfaces. Results suggest that some of the common practices in the field of sputtering may be detrimental to achieving maximum adherence and optimum composition for these refractory compounds.

  20. Investigation of the near-surface structures of polar InN films by chemical-state-discriminated hard X-ray photoelectron diffraction

    SciTech Connect

    Yang, A. L.; Yamashita, Y.; Kobata, M.; Yoshikawa, H.; Sakata, O.; Kobayashi, K.; Matsushita, T.; Pis, I.; Imura, M.; Yamaguchi, T.; Nanishi, Y.

    2013-01-21

    Near-surface structures of polar InN films were investigated by laboratory-based hard X-ray photoelectron diffraction (HXPD) with chemical-state-discrimination. HXPD patterns from In 3d{sub 5/2} and N 1s core levels of the In-polar and N-polar InN films were different from each other and compared with the simulation results using a multiple-scattering cluster model. It was found that the near-surface structure of the In-polar InN film was close to the ideal wurtzite structure. On the other hand, on the N-polar InN film, defects-rich surface was formed. In addition, the existence of the In-polar domains was observed in the HXPD patterns.

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

    SciTech Connect

    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.

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

    NASA Astrophysics Data System (ADS)

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

    2015-04-01

    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 Si2+ and Al2+ cation mobility under the influence of voltage potential between the cathode and anode will be discussed in detail.

  3. Negatively charged subnanometer-sized silicon clusters and their reversible migration into AFI zeolite pores studied with X-ray photoelectron spectroscopy and ultraviolet photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Choo, Cheow-keong; Sakamoto, Takashi; Tanaka, Katsumi; Nakata, Ryouhei; Asakawa, Tetsuo

    1999-02-01

    Subnanometer sized silicon clusters were deposited on AFI zeolite (AlPO 4-5: one-dimensional channel diameter <0.73 nm) by pulsed laser ablation of silicon wafer. Their electronic structures were elucidated in situ by X-ray photoelectron spectroscopy (XPS) and ultraviolet photoelectron spectroscopy (UPS). Core level Si 2p spectra were analyzed into five components, Si(I) to Si(V). Si(I) and Si(II) species selectively increased with a constant ratio during pulsed laser silicon ablation. Their binding energies (BEs) were below 99.5 eV implying negatively charged states. Charge transfer occurred between silicon clusters and framework oxygen and phosphor ions. It was interpreted that the stability of negative charge is due to large electron affinity of silicon clusters. The intensity of XPS signals decreased as a function of time and at the same time the channels were blocked. These results were interpreted due to migration of silicon clusters into zeolite pores. The estimated activation energy (57 kJ/mol) suggests that rate-determining step of the migration is reflected by a weak adsorbed state of silicon clusters similar to physisorbed state. The silicon clusters were partially oxidized at 573 K, which was interpreted as a driving force of backward migration from zeolite pores to the external surface. The composition of silicon cluster was discussed based on homogeneous dispersion of single species.

  4. On background subtraction for quantitative analysis of X-ray photoelectron spectra of rare earth fluorides

    NASA Astrophysics Data System (ADS)

    Schnellbügel, A.; Anton, R.

    2001-10-01

    The applicability of Tougaard's method of a "universal" form of background correction in photoelectron spectra was investigated for thin films of the wide gap insulators YbF x, DyF x, SmF x, and YF x. These films were produced by ion assisted deposition with varying fluorine content x⩽3, caused by preferential sputtering. For YbF x, in particular, acceptable accuracy was obtained for x⩾2.4 by shifting the universal background function by the band gap energy, while for x<2.4, no reasonable fit of the experimental background could be obtained. More realistic profiles of the inelastic scattering background were calculated on the basis of published fast-electron energy-loss data of DyF 3, which yielded highly accurate quantification of spectra of YbF x in the whole range of x between 2 and 3. This was confirmed by measurements of the intensity ratios of the 4f peaks of Yb 2+ and Yb 3+, representing valence states 2 and 3, respectively, which are directly correlated with the fluorine content. Stoichiometry values from XPS data were compared with Rutherford backscattering analysis and yielded good agreement.

  5. Atmospheric pressure X-ray photoelectron spectroscopy apparatus: Bridging the pressure gap.

    PubMed

    Velasco-Vélez, J J; Pfeifer, V; Hävecker, M; Wang, R; Centeno, A; Zurutuza, A; Algara-Siller, G; Stotz, E; Skorupska, K; Teschner, D; Kube, P; Braeuninger-Weimer, P; Hofmann, S; Schlögl, R; Knop-Gericke, A

    2016-05-01

    One of the main goals in catalysis is the characterization of solid/gas interfaces in a reaction environment. The electronic structure and chemical composition of surfaces become heavily influenced by the surrounding environment. However, the lack of surface sensitive techniques that are able to monitor these modifications under high pressure conditions hinders the understanding of such processes. This limitation is known throughout the community as the "pressure gap." We have developed a novel experimental setup that provides chemical information on a molecular level under atmospheric pressure and in presence of reactive gases and at elevated temperatures. This approach is based on separating the vacuum environment from the high-pressure environment by a silicon nitride grid-that contains an array of micrometer-sized holes-coated with a bilayer of graphene. Using this configuration, we have investigated the local electronic structure of catalysts by means of photoelectron spectroscopy and in presence of gases at 1 atm. The reaction products were monitored online by mass spectrometry and gas chromatography. The successful operation of this setup was demonstrated with three different examples: the oxidation/reduction reaction of iridium (noble metal) and copper (transition metal) nanoparticles and with the hydrogenation of propyne on Pd black catalyst (powder). PMID:27250406

  6. On PbTiO{sub 3}-(111)-Pt interfacial layers and their x-ray photoelectron spectroscopy signature

    SciTech Connect

    Habouti, S.; Solterbeck, C-H.; Es-Souni, M.; Zaporojtchenko, V.

    2008-11-15

    In this work emphasis is placed on the investigation of interfacial layers between sol-gel processed PbTiO{sub 3} (PTO) thin films and (111)Pt terminated silicon substrates. The methods used are x-ray diffraction, x-ray photoelectron spectroscopy (XPS) combined with depth profiling, and atomic force microscopy (AFM). In order to avoid artifacts related to ion bombardment, e.g., reduction of Pb ions and preferential sputtering, gentle argon ion bombardment conditions were first derived. AFM investigations of native and ion bombarded films at different stages of depth profiling show that the films are homogenously sputtered, whereby the film roughness remains practically unchanged in the course of sputtering. An annealing treatment at 550 deg. C under reducing atmosphere was used to provoke the formation of an interfacial intermetallic (111)Pt{sub x}Pb phase, which is shown to coexist with an amorphous oxide film. This could allow us to establish the XPS signature of the intermetallic phase. A negative shift of the Pt (4f) binding energy and a large full width at half maximum of the Pb (4f) peak are the attributes of this signature. PTO-film annealing in air at temperatures between 350 and 600 deg. C leads to the formation of the perovskite phase, starting at 500 deg. C, directly from the amorphous phase. Based on its derived XPS signature it is shown that the intermetallic phase still exists at the interface with variable thickness depending on the annealing temperature. The pronounced (111) texture of the PTO-crystallized films is thought to be the direct consequence of this intermetallic template layer. It is also shown that the outermost surface of the PTO film is enriched with PbO as a result of segregation phenomena.

  7. Scanning electron and atomic force microscopy, and raman and x-ray photoelectron spectroscopy characterization of near-isogenic soft and hard wheat kernels and corresponding flours

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Atomic force microscopy (AFM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS) are used to investigate vitreous (hard) and non-vitreous (soft) wheat kernels and their corresponding wheat flours. AFM data reveal two different microstructures. The vitreous kernel reveals a granular text...

  8. X-Ray Photoelectron Spectroscopy Study of the Effect of Hydrocarbon Contamination on Poly(Tetrafluoroethylene) Exposed to a Nitrogen Plasma

    NASA Technical Reports Server (NTRS)

    Golub, Morton A.; Lopata, Eugene S.; Finney, Lorie S.

    1993-01-01

    In this note, we show that X-ray photoelectron Spectroscopy (XPS) data and the changes in surface properties attending exposure of poly(tetrafluoroethylene) (PTFE) films to a nitrogen plasma can likewise be misinterpreted when the interfering role of minor surface hydrocarbon contamination is not taken into account.

  9. X-Ray Photoelectron Spectroscopy Study of the Effect of Hydrocarbon Contamination on Poly(Tetrafluoroethylene) Exposed to a Nitrogen Plasma

    NASA Technical Reports Server (NTRS)

    Golub, Morton A.; Lopata, Eugene S.; Finney, Lorie S.

    1993-01-01

    It has been shown that unless the surface of poly(tetrafluoroethylene)(PTFE) is free of hydrocarbon contamination, anomalous changes in the oxygen and fluorine contents, as measured by X-ray photoelectron spectroscopy (XPS), and hence also the surface properties, may be improperly ascribed to a PTFE film exposed to a oxygen plasma.

  10. Catalyst Chemical State during CO Oxidation Reaction on Cu(111) Studied with Ambient-Pressure X-ray Photoelectron Spectroscopy and Near Edge X-ray Adsorption Fine Structure Spectroscopy.

    PubMed

    Eren, Baran; Heine, Christian; Bluhm, Hendrik; Somorjai, Gabor A; Salmeron, Miquel

    2015-09-01

    The chemical structure of a Cu(111) model catalyst during the CO oxidation reaction in the CO+O2 pressure range of 10-300 mTorr at 298-413 K was studied in situ using surface sensitive X-ray photoelectron and adsorption spectroscopy techniques [X-ray photoelectron spectroscopy (XPS) and near edge X-ray adsorption fine structure spectroscopy (NEXAFS)]. For O2:CO partial pressure ratios below 1:3, the surface is covered by chemisorbed O and by a thin (∼1 nm) Cu2O layer, which covers completely the surface for ratios above 1:3 between 333 and 413 K. The Cu2O film increases in thickness and exceeds the escape depth (∼3-4 nm) of the XPS and NEXAFS photoelectrons used for analysis at 413 K. No CuO formation was detected under the reaction conditions used in this work. The main reaction intermediate was found to be CO2(δ-), with a coverage that correlates with the amount of Cu2O, suggesting that this phase is the most active for CO oxidation. PMID:26275662

  11. X-Ray Dichroism in Photoelectron Spectroscopy for Direct Element Specific Surface Magnetometry of Nanomagnetic Structures

    NASA Astrophysics Data System (ADS)

    Tobin, James G.

    1997-03-01

    Element specific surface magnetometry remains a central goal of synchrotron radiation based studies of nanomagnetic structures. One appealing possibility is the combination of xray absorption dichroism measurements and the theoretical framework provided by the "sum rules."[1] Unfortunately, sum rule analyses are hampered by several limitations [2], including delocalization of the final state, multi-electronic phenomena and the presence of surface dipoles. An alternative experiment, Magnetic Xray Dichroism in Photoelectron Spectroscopy, holds out promise based upon its elemental specificity, surface sensitivity and high resolution. Computational simulations by Tamura et al [3] demonstrated the relationship between exchange and spin orbit splittings and experimental data of linear and circular dichroisms. Now we [4] have developed an analytical framework which allows for the direct extraction of core level exchange splittings from circular and linear dichroic photoemission data. By extending a model initially proposed by Venus [5], it is possible to show a linear relation between normalized dichroism peaks in the experimental data and the underlying exchange splitting. Since it is reasonable to expect that exchange splittings and magnetic moments track together [6], this measurement thus becomes a powerful new tool for direct surface magnetometry, without recourse to time consuming and difficult spectral simulations. The theoretical derivation will be supported by high resolution linear and circular dichroism data collected at the Spectromicroscopy Facility of the Advanced Light Source. [7,8] This work was performed under the auspices of the U.S. Department of Energy by LLNL under contract No. W-7405-ENG-48. 1. B.T. Thole et al, Phys. Rev. Lett. 68,1943 (1992); P. Carra et al. Phys. Rev. Lett. 70, 694 (1993). 2. J.G. Tobin et al Phys. Rev. B 52, 6530 (1995). 3. E. Tamura et al, Phys. Rev. Lett 73, 1533 (1994) 4. J.G. Tobin, K.W. Goodman, F.O. Schumann, R.F. Willis, J

  12. Dynamic secondary ion mass spectrometry and X-ray photoelectron spectroscopy on artistic bronze and copper artificial patinas

    NASA Astrophysics Data System (ADS)

    Balta, I. Z.; Pederzoli, S.; Iacob, E.; Bersani, M.

    2009-04-01

    To prevent the natural processes of decay and to develop and improve the treatments of conservation and restoration of artistic bronzes meaning statues and sculptures, it is important understanding the patination processes and the knowledge of artificially corroded surfaces. Chemical and physical characterization of artificial patinas obtained on artistic bronzes and coppers by using the 19th century Western traditional patination techniques and recipes by means of SEM-EDS, light microscopy and ATR/FT-IR has been done in previous studies [I.Z. Balta, L. Robbiola, Characterization of artificial black patinas on artistic cast bronze and pure copper by using SEM-EDS and light microscopy, in: Proceedings of the 13th European Microscopy Congress, 22-27 August 2004, Antwerp, Belgium, EMC 2004 CD-Rom Conference Preprints; I.Z. Balta, L. Robbiola, Traditional artificial artistic bronze and copper patinas—an investigation by SEM-EDS and ATR/FT-IR, in: Proceedings of the 8th International Conference on Non Destructive Investigations and Microanalysis for the Diagnostics and Conservation of the Cultural and Environmental Heritage, 15-19 May 2005, Lecce, Italy, ART'05 CD-Rom Conference Preprints]. Differences in morphology (structure, thickness, porosity, adherence, compactity, uniformity, homogeneity) and also in composition, on both artistic cast bronze and pure copper patinas, were clearly evidenced. Further in-depth investigation is required to be carried out in order to better understand the patinas mechanisms of formation and the layers kinetics of growth. The elemental and chemical analysis, either on a surface monolayer or in a depth profile, by using the Secondary Ion Mass Spectrometry (SIMS) and X-ray Photoelectron Spectroscopy (XPS) techniques, can provide this kind of information, unique at trace-level sensitivity. SIMS has proved to be a suitable analytical technique for analyzing small amounts of material with high atomic sensitivity (ppm or even ppb) and high

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

    SciTech Connect

    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.

  14. Quantitative determination of the oxidation state of iron in biotite using x-ray photoelectron spectroscopy: I. Calibration

    SciTech Connect

    Raeburn, S.P.; Ilton, E.S.; Veblen, D.R.

    1997-11-01

    X-ray photoelectron spectroscopy (XPS) analyses of Fe(III)/{Sigma}Fe were calibrated with nine single crystals of biotite of known Fe(III)/{Sigma}Fe content. Peak shape parameters for the component Fe{sup 2+} and Fe{sup 3+} Fe 3p peaks were obtained by a constrained lease squares fitting method that minimized the difference between Fe(III)/{Sigma}Fe determined by XPS and wet chemistry/electron microprobe (WCEM) analyses. Fe{sup 2+} and Fe{sup 3+} peak separation was estimated from the separation of minima in the second derivative of Fe 3p spectra. The single set of derived peak parameters yielded a good linear correlation (r = 0.87) between XPS and WCEM values over the sample displaying progressive oxidation during XPS analysis resulted in Fe{sup 2} and Fe{sup 3+} component peak shapes largely consistent with the constrained least squares fitting methods. Beam damage, which appeared to be restricted to three single crystals with low {Sigma}Fe, low Fe/Mg, and high Fe(II)/{Sigma}Fe, caused increases in Fe(III)/{Sigma}Fe that were proportional to the duration of sample exposure. 60 refs., 6 figs., 7 tabs.

  15. Chemical composition of the SiO2/InSb interface as determined by X-ray photoelectron spectroscopy

    NASA Technical Reports Server (NTRS)

    Vasquez, R. P.; Grunthaner, F. J.

    1981-01-01

    In connection with the relatively poor insulating characteristics of the native oxides of most III-V compound semiconductors, there has been interest in the development of deposited dielectric layers for surface passivation and MOS device fabrication on III-V compound semiconductor substrates. The chemical system of SiO2 deposited on single-crystal InSb substrates has been proposed for the fabrication of IR CCD. The considered investigation is concerned with a detailed examination of the chemical nature of the interactions between deposited and native oxides using X-ray photoelectron spectroscopy (XPS) in conjunction with a chemical-etching technique for depth profiling. The compositional structure of the interfaces obtained in the SiO2/native oxide/InSb system is derived on the basis of an intensity analysis of XPS spectra. Thermal oxidation of the InSb substrate is found to result in an In-rich native oxide and excess elemental Sb at the native oxide/substrate interface.

  16. Quantitative determination of the oxidation state of iron in biotite using x-ray photoelectron spectroscopy: II. In situ analyses

    SciTech Connect

    Raeburn, S.P. |; Ilton, E.S.; Veblen, D.R.

    1997-11-01

    X-ray photoelectron spectroscopy (XPS) was used to determine Fe(III)/{Sigma}Fe in individual biotite crystals in thin sections of ten metapelites and one syenite. The in situ XPS analyses of Fe(III)/{Sigma}Fe in biotite crystals in the metapelites were compared with published Fe(III)/{Sigma}Fe values determined by Moessbauer spectroscopy (MS) for mineral separates from the same hand samples. The difference between Fe(III)/{Sigma}Fe by the two techniques was greatest for samples with the lowest Fe(III)/{Sigma}Fe (by MS). For eight metamorphic biotites with Fe(III)/{Sigma}Fe = 9-27% comparison of the two techniques yielded a linear correlation of r = 0.94 and a statistically acceptable fit of [Fe(III)/{Sigma}Fe]{sub xps} = [Fe(III)/{Sigma}Fe]{sub ms}. The difference between Fe(III)/{Sigma}Fe by the two techniques was greater for two samples with Fe(III)/{Sigma}Fe {le} 6% (by MS). For biotite in the syenite sample, Fe(III)/{Sigma}Fe determined by both in situ XPS and bulk wet chemistry/electron probe microanalysis were similar. This contribution demonstrates that XPS can be used to analyze bulk Fe(III)/{Sigma}Fe in minerals in thin sections when appropriate precautions taken to avoid oxidation of the near-surface during preparation of samples. 25 refs., 3 figs., 4 tabs.

  17. Study of the interface Si-nc/SiO 2 by infrared spectroscopic ellipsometry and X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Stenger, I.; Gallas, B.; Siozade, L.; Fisson, S.; Vuye, G.; Chenot, S.; Rivory, J.

    2007-04-01

    SiO x films (1< x<2), 0.5 μm thick, have been elaborated by electron-gun evaporation. A thermal annealing of these films induced a phase separation leading to the formation of Si nanocrystals embedded in a SiO 2 matrix. These films have been studied by infrared spectroscopic ellipsometry and by X-ray photoelectron spectroscopy (XPS). The effective dielectric function of the thin films has been extracted in the 600-5000 cm -1 range which allowed us to deduce the dielectric function of the matrix surrounding the Si-nc. A study of the Transverse Optical (TO) vibration mode has revealed the presence of SiO x into the matrix. Before XPS measurements, the films have been etched in fluorhydric acid to remove the superficial SiO 2 layer formed during air exposure. The Si 2p core-level emission has been recorded. The decomposition of the Si 2p peak into contributions of the usual five tetrahedrons Si-(Si 4-nO n) ( n=0-4) has also revealed the presence of a SiO x phase. Consistency between infra-red and XPS results is discussed.

  18. Surface Termination Conversion during SrTiO3 Thin Film Growth Revealed by X-ray Photoelectron Spectroscopy.

    PubMed

    Baeumer, Christoph; Xu, Chencheng; Gunkel, Felix; Raab, Nicolas; Heinen, Ronja Anika; Koehl, Annemarie; Dittmann, Regina

    2015-01-01

    Emerging electrical and magnetic properties of oxide interfaces are often dominated by the termination and stoichiometry of substrates and thin films, which depend critically on the growth conditions. Currently, these quantities have to be measured separately with different sophisticated techniques. This report will demonstrate that the analysis of angle dependent X-ray photoelectron intensity ratios provides a unique tool to determine both termination and stoichiometry simultaneously in a straightforward experiment. Fitting the experimental angle dependence with a simple analytical model directly yields both values. The model is calibrated through the determination of the termination of SrTiO3 single crystals after systematic pulsed laser deposition of sub-monolayer thin films of SrO. We then use the model to demonstrate that during homoepitaxial SrTiO3 growth, excess Sr cations are consumed in a self-organized surface termination conversion before cation defects are incorporated into the film. We show that this termination conversion results in insulating properties of interfaces between polar perovskites and SrTiO3 thin films. These insights about oxide thin film growth can be utilized for interface engineering of oxide heterostructures. In particular, they suggest a recipe for obtaining two-dimensional electron gases at thin film interfaces: SrTiO3 should be deposited slightly Ti-rich to conserve the TiO2-termination. PMID:26189436

  19. Surface Termination Conversion during SrTiO3 Thin Film Growth Revealed by X-ray Photoelectron Spectroscopy

    NASA Astrophysics Data System (ADS)

    Baeumer, Christoph; Xu, Chencheng; Gunkel, Felix; Raab, Nicolas; Heinen, Ronja Anika; Koehl, Annemarie; Dittmann, Regina

    2015-07-01

    Emerging electrical and magnetic properties of oxide interfaces are often dominated by the termination and stoichiometry of substrates and thin films, which depend critically on the growth conditions. Currently, these quantities have to be measured separately with different sophisticated techniques. This report will demonstrate that the analysis of angle dependent X-ray photoelectron intensity ratios provides a unique tool to determine both termination and stoichiometry simultaneously in a straightforward experiment. Fitting the experimental angle dependence with a simple analytical model directly yields both values. The model is calibrated through the determination of the termination of SrTiO3 single crystals after systematic pulsed laser deposition of sub-monolayer thin films of SrO. We then use the model to demonstrate that during homoepitaxial SrTiO3 growth, excess Sr cations are consumed in a self-organized surface termination conversion before cation defects are incorporated into the film. We show that this termination conversion results in insulating properties of interfaces between polar perovskites and SrTiO3 thin films. These insights about oxide thin film growth can be utilized for interface engineering of oxide heterostructures. In particular, they suggest a recipe for obtaining two-dimensional electron gases at thin film interfaces: SrTiO3 should be deposited slightly Ti-rich to conserve the TiO2-termination.

  20. Photoelectric characteristics of silicon P—N junction with nanopillar texture: Analysis of X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Liu, Jing; Wang, Jia-Ou; Yi, Fu-Ting; Wu, Rui; Zhang, Nian; Ibrahim, Kurash

    2014-09-01

    Silicon nanopillars are fabricated by inductively coupled plasma (ICP) dry etching with the cesium chloride (CsCl) islands as masks originally from self-assembly. Wafers with nanopillar texture or planar surface are subjected to phosphorus (P) diffusion by liquid dopant source (POCl3) at 870 °C to form P—N junctions with a depth of 300 nm. The X-ray photoelectron spectroscopy (XPS) is used to measure the Si 2p core levels of P—N junction wafer with nanopillar texture and planar surface. With a visible light excitation, the P—N junction produces a new electric potential for photoelectric characteristic, which causes the Si 2p core level to have a energy shift compared with the spectrum without the visible light. The energy shift of the Si 2p core level is -0.27 eV for the planar P—N junction and -0.18 eV for the nanopillar one. The difference in Si 2p energy shift is due to more space lattice defects and chemical bond breaks for nanopillar compared with the planar one.

  1. UV-Raman spectroscopy, X-ray photoelectron spectroscopy, and temperature programmed desorption studies of model and bulk heterogeneous catalysts

    SciTech Connect

    Tewell, Craig R.

    2002-08-19

    X-ray photoelectron spectroscopy (XPS) and Temperature Programmed Desorption (TPD) have been used to investigate the surface structure of model heterogeneous catalysts in ultra-high vacuum (UHV). UV-Raman spectroscopy has been used to probe the structure of bulk model catalysts in ambient and reaction conditions. The structural information obtained through UV-Raman spectroscopy has been correlated with both the UHV surface analysis and reaction results. The present day propylene and ethylene polymerization catalysts (Ziegler-Natta catalysts) are prepared by deposition of TiCl{sub 4} and a Al(Et){sub 3} co-catalyst on a microporous Mg-ethoxide support that is prepared from MgCl{sub 2} and ethanol. A model thin film catalyst is prepared by depositing metallic Mg on a Au foil in a UHV chamber in a background of TiCl{sub 4} in the gas phase. XPS results indicate that the Mg is completely oxidized to MgCl{sub 2} by TiCl{sub 4} resulting in a thin film of MgCl{sub 2}/TiCl{sub x}, where x = 2, 3, and 4. To prepare an active catalyst, the thin film of MgCl{sub 2}/TiCl{sub x} on Au foil is enclosed in a high pressure cell contained within the UHV chamber and exposed to {approx}1 Torr of Al(Et){sub 3}.

  2. Compositional depth profile of a native oxide LPCVD MNOS structure using X-ray photoelectron spectroscopy and chemical etching

    NASA Technical Reports Server (NTRS)

    Wurzbach, J. A.; Grunthaner, F. J.

    1983-01-01

    It is pointed out that there is no report of an unambiguous analysis of the composition and interfacial structure of MNOS (metal-nitride oxide semiconductor) systems, despite the technological importance of these systems. The present investigation is concerned with a study of an MNOS structure on the basis of a technique involving the use of X-ray photoelectron spectroscopy (XPS) with a controlled stopped-flow chemical-etching procedure. XPS is sensitive to the structure of surface layers, while stopped-flow etching permits the controlled removal of overlying material on a scale of atomic layers, to expose new surface layers as a function of thickness. Therefore, with careful analysis of observed intensities at measured depths, this combination of techniques provides depth resolution between 5 and 10 A. According to the obtained data there is intact SiO2 at the substrate interface. There appears to be a thin layer containing excess bonds to silicon on top of the SiO2.

  3. In-situ X-ray photoelectron spectroscopy studies of water on metals and oxides at ambient conditions

    SciTech Connect

    Salmeron, Miquel; Yamamoto, S.; Bluhm, H.; Andersson, K.; Ketteler, G.; Ogasawara, H.; Salmeron, M.; Nilsson, A.

    2007-10-29

    X-ray photoelectron spectroscopy (XPS) is a powerful tool for surface and interface analysis, providing the elemental composition of surfaces and the local chemical environment of adsorbed species. Conventional XPS experiments have been limited to ultrahigh vacuum (UHV) conditions due to a short mean free path of electrons in a gas phase. The recent advances in instrumentation coupled with third-generation synchrotron radiation sources enables in-situ XPS measurements at pressures above 5 Torr. In this review, we describe the basic design of the ambient pressure XPS setup that combines differential pumping with an electrostatic focusing. We present examples of the application of in-situ XPS to studies of water adsorption on the surface of metals and oxides including Cu(110), Cu(111), TiO2(110) under environmental conditions of water vapor pressure. On all these surfaces we observe a general trend where hydroxyl groups form first, followed by molecular water adsorption. The importance of surface OH groups and their hydrogen bonding to water molecules in water adsorption on surfaces is discussed in detail.

  4. X-ray photoelectron spectroscopy analysis of boron defects in silicon crystal: A first-principles study

    NASA Astrophysics Data System (ADS)

    Yamauchi, Jun; Yoshimoto, Yoshihide; Suwa, Yuji

    2016-05-01

    We carried out a comprehensive study on the B 1s core-level X-ray photoelectron spectroscopy (XPS) binding energies and formation energies for boron defects in crystalline silicon by first-principles calculation with careful evaluation of the local potential boundary condition for the model system using the supercell corresponding to 1000 Si atoms. It is reconfirmed that the cubo-octahedral B12 cluster in silicon crystal is unstable and exists at the saddle point decaying to the icosahedral and S4 B12 clusters. The electrically active clusters without any postannealing of ion-implanted Si are identified as icosahedral B12 clusters. The experimentally proposed threefold coordinated B is also identified as a ⟨ 001 ⟩ B - Si defect. For an as-doped sample prepared by plasma doping, the calculated XPS spectra for complexes consisting of vacancies and substitutional B atoms are consistent with the experimental spectra. It is proposed that, assuming that the XPS peak at 187.1 eV is due to substitutional B (Bs), the experimental XPS peaks at 187.9 and 186.7 eV correspond to interstitial B at the H-site and ⟨ 001 ⟩ B - Si defects, respectively. In the annealed samples, the complex of Bs and interstitial Si near the T-site is proposed as a candidate for the experimental XPS peak at 188.3 eV.

  5. X-ray Photoelectron Spectroscopy of Pyridinium-Based Ionic Liquids: Comparison to Imidazolium- and Pyrrolidinium-Based Analogues.

    PubMed

    Men, Shuang; Mitchell, Daniel S; Lovelock, Kevin R J; Licence, Peter

    2015-07-20

    We investigate eight 1-alkylpyridinium-based ionic liquids of the form [Cn Py][A] by using X-ray photoelectron spectroscopy (XPS). The electronic environment of each element of the ionic liquids is analyzed. In particular, a reliable fitting model is developed for the C 1s region that applies to each of the ionic liquids. This model allows the accurate charge correction of binding energies and the determination of reliable and reproducible binding energies for each ionic liquid. Shake-up/off phenomena are determinedfor both C 1s and N 1s spectra. The electronic interaction between cations and anions is investigated for both simple ionic liquids and an example of an ionic-liquid mixture; the effect of the anion on the electronic environment of the cation is also explored. Throughout the study, a detailed comparison is made between [C8 Py][A] and analogues including 1-octyl-1-methylpyrrolidinium- ([C8 C1 Pyrr][A]), and 1-octyl-3-methylimidazolium- ([C8 C1 Im][A]) based samples, where X is common to all ionic liquids. PMID:25952131

  6. X-ray photoelectron spectroscopy and secondary electron yield analysis of Al and Cu samples exposed to an accelerator environment.

    SciTech Connect

    Rosenberg, R. A.; McDowell, M. W.; Ma, Q.; Harkay, K. C.; XFD; APS-USR; ASD

    2003-09-01

    It is well known that exposure to an accelerator environment can cause ''conditioning'' of the vacuum chamber surfaces. In order to understand the manner in which the surface structure might influence the production of gases and electrons in the accelerator, such surfaces should be studied both before and after exposure to accelerator conditions. Numerous studies have been performed on representative materials prior to being inserted into an accelerator, but very little has been done on materials that have ''lived'' in the accelerator for extended periods. In the present work, we mounted Al and Cu coupons at different positions in a section of the Advanced Photon Source storage ring and removed them following exposures ranging from 6 to 18 months. X-ray photoelectron spectroscopy (XPS) of the surface was performed before and after exposure. Changes were observed that depended on the location and whether the coupon was facing the chamber interior or chamber wall. These results will be presented and compared to XPS and secondary electron yield data obtained from laboratory measurements meant to simulate the accelerator conditions.

  7. Structure of Se-rich As-Se glasses by high-resolution x-ray photoelectron spectroscopy

    SciTech Connect

    Golovchak, R.; Kovalskiy, A.; Miller, A. C.; Jain, H.; Shpotyuk, O.

    2007-09-15

    To establish the validity of various proposed structural models, we have investigated the structure of the binary As{sub x}Se{sub 100-x} chalcogenide glass family (x{<=}40) by high-resolution x-ray photoelectron spectroscopy. From the composition dependence of the valence band, the contributions to the density of states from the 4p lone pair electrons of Se and the 4p bonding states and 4s electrons of Se and As are identified in the top part of the band. The analysis of Se 3d and As 3d core-level spectra supports the so-called chain crossing model for the atomic structure of Se-rich As{sub x}Se{sub 100-x} bulk glasses. The results also indicate small deviations ({approx}3-8%) from this model, especially for glass compositions with short Se chains (25

  8. X-Ray Photoelectron Spectroscopy Study of the Heating Effects on Pd/6H-SiC Schottky Structure

    NASA Technical Reports Server (NTRS)

    Chen, Liang-Yu; Hunter, Gary W.; Neudeck, Philip G.; Knight, Dak

    1998-01-01

    X-ray photoelectron spectroscopy is used to study the effects of heat treatment on the Pd/6H-SiC Schottky diode structure. After heating the structure at 425 C for 140 h, a very thin surface layer of PdO mixed with SiO(x) formed on the palladium surface of the Schottky structure. Heat treatment promoted interfacial diffusion and reaction which significantly broadened the interfacial region. In the interfacial region, the palladium concentration decreases with depth, and the interfacial products are Pd(x)Si (x = 1,2,3,4). In the high Pd concentration regions, Pd4Si is the major silicide component while gr and Pd2Si are major components in the low Pd concentration region. At the center of the interface, where the total palladium concentration equals that of silicon, the concentrations of palladium associated with various palladium silicides (Pd(x)Si, x= 1,2,3,4) are approximately equal. The surface passivation layer composed of PdO and SiO, may significantly affect the electronic and catalytic properties of the surface of the Schottky diode which plays a major role in gas detection. The electronic properties of the Schottky structure may be dominated by a (Pd+Pd(x)Si)/SiC interface. In order to stabilize the properties of the Schottky structure the surface and interface diffusion and reactions must be controlled.

  9. An XPS study of the stability of Fomblin Z25 on the native oxide of aluminum. [x ray photoelectron spectroscopy

    NASA Technical Reports Server (NTRS)

    Herrera-Fierro, Pilar; Pepper, Stephen V.; Jones, William R.

    1991-01-01

    Thin films of Fomblin Z25, a perfluoropolyalkylether lubricant, were vapor deposited onto clean, oxidized aluminum and sapphire surfaces, and their behavior at different temperatures was studied using x ray photoelectron spectroscopy (XPS) and thermal desorption spectroscopy (TDS). It was found that the interfacial fluid molecules decompose on the native oxide at room temperature, and continue to decompose at elevated temperatures, as previous studies had shown to occur on clean metal. TDS indicated that different degradation mechanisms were operative for clean and oxidized aluminum. On sapphire substrates, no reaction was observed at room temperature. Our conclusion is that the native oxide of aluminum is neither passive nor protective towards Fomblin Z25. At high temperatures (150 C) degradation of the polymer on sapphire produced a debris layer at the interface with a chemical composition similar to the one formed on aluminum oxide. Rubbing a Fomblin film on a single crystal sapphire also induced the decomposition of the lubricant in contact with the interface and the formulation of a debris layer.

  10. X-ray photoelectron spectroscopy study of the stability of Fomblin Z25 on the native oxide of aluminum

    NASA Technical Reports Server (NTRS)

    Herrera-Fierro, Pilar; Pepper, Stephen V.; Jones, William R.

    1992-01-01

    Thin films of Fomblin Z25, a perfluoropolyalkylether lubricant, were vapor deposited onto clean, oxidized aluminum, and onto sapphire surfaces, and their behavior at different temperatures was studied using X-ray photoelectron spectroscopy and temperature desorption spectroscopy (TDS). The interfacial fluid molecules decompose on the native oxide at room temperature, and continue to decompose at elevated temperatures, as previous studies had shown to occur on the clean metal. TDS indicated that different degradation mechanisms were operative for clean and oxidized aluminum. On sapphire substrates, no reaction was observed at room temperature. The native oxide of aluminum is neither passive nor protective towards Fomblin Z25. At higher temperatures (150 C), degradation of the polymer on sapphire produced a debris layer at the interface with a chemical composition similar to the one formed on aluminum oxide. Rubbing a Fomblin film on a single crystal sapphire also induced the decomposition of the lubricant in contact with the interface and the formation of a debris layer.

  11. In situ x-ray photoelectron spectroscopy studies of gas/solidinterfaces at near-ambient conditions

    SciTech Connect

    Bluhm, Hendrik; Havecker, Michael; Knop-Gericke, Axel; Kiskinova,Maya; Schlogl, Robert; Salmeron, Miquel

    2007-12-03

    X-ray photoelectron spectroscopy (XPS) is a quantitative, chemically specific technique with a probing depth of a few angstroms to a few nanometers. It is therefore ideally suited to investigate the chemical nature of the surfaces of catalysts. Because of the scattering of electrons by gas molecules, XPS is generally performed under vacuum conditions. However, for thermodynamic and/or kinetic reasons, the catalyst's chemical state observed under vacuum reaction conditions is not necessarily the same as that of a catalyst under realistic operating pressures. Therefore, investigations of catalysts should ideally be performed under reaction conditions, i.e., in the presence of a gas or gas mixtures. Using differentially pumped chambers separated by small apertures, XPS can operate at pressures of up to 1 Torr, and with a recently developed differentially pumped lens system, the pressure limit has been raised to about 10 Torr. Here, we describe the technical aspects of high-pressure XPS and discuss recent applications of this technique to oxidation and heterogeneous catalytic reactions on metal surfaces.

  12. Investigation of composition and chemical state of elements in iron boride by the method of X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Alyoshin, V. G.; Kharlamov, A. I.; Prokopenko, V. M.

    1981-06-01

    The composition and chemical state of iron and boron in the surface layer of iron boride under different kinds of pretreatment of samples have been investigated by the method of X-ray photo-electron spectroscopy. It has been found that in the initial sample there is oxygen chemically combined with iron and boron atoms. Upon heating (450°C) in hydrogen, in argon, and in vacuo there occurs removal of oxygen only from iron atoms (no pure iron was found to be formed). Boron oxidizes and there probably appears a new surface combination of boron with oxygen in which the bonding energy of 1 s electrons is higher than that in B 2O 3. Treatment of the iron boride surface with argon ions and with protons ensures uniform removal of oxygen from iron and boron atoms. It has been found that thermal treatment of iron boride leads to depletion of iron atoms from the sample surface layer, and pickling with argon ions and with protons leads to strong enrichment. Iron boride samples subjected to Ar + and H + bombardment tend to undergo significant oxidation when subsequently exposed to air at room temperature.

  13. Valence band offset of β-Ga2O3/wurtzite GaN heterostructure measured by X-ray photoelectron spectroscopy

    PubMed Central

    2012-01-01

    A sample of the β-Ga2O3/wurtzite GaN heterostructure has been grown by dry thermal oxidation of GaN on a sapphire substrate. X-ray diffraction measurements show that the β-Ga2O3 layer was formed epitaxially on GaN. The valence band offset of the β-Ga2O3/wurtzite GaN heterostructure is measured by X-ray photoelectron spectroscopy. It is demonstrated that the valence band of the β-Ga2O3/GaN structure is 1.40 ± 0.08 eV. PMID:23046910

  14. Interface electronic properties of co-evaporated MAPbI3 on ZnO(0001): In situ X-ray photoelectron spectroscopy and ultraviolet photoelectron spectroscopy study

    NASA Astrophysics Data System (ADS)

    Zhou, Xianzhong; Li, Xiaoli; Liu, Yuan; Huang, Feng; Zhong, Dingyong

    2016-03-01

    In this work, the interface electronic properties of ZnO(0001)/CH3NH3PbI3 were investigated by both X-ray and ultraviolet photoelectron spectroscopy. The CH3NH3PbI3 thin films were grown on single crystalline ZnO(0001) substrate in situ by co-evaporation of PbI2 and CH3NH3I at room temperature with various thickness from 1.5 nm to 190 nm. It was found that the conduction band minimum of ZnO lies 0.3 eV below that of CH3NH3PbI3, while the valence band maximum of ZnO lies 2.1 eV below that of CH3NH3PbI3, implying that the electrons can be effectively transported from CH3NH3PbI3 to ZnO, and the holes can be blocked in the same time. A PbI2 rich layer was initially formed at the interface of ZnO(0001)/CH3NH3PbI3 during the growth. As a consequence, an interface barrier was built up which may prevent the electron transport at the interface.

  15. Aluminum position in Rb-feldspar as determined by X-ray photoelectron spectroscopy.

    PubMed

    Kyono, Atsushi; Kimata, Mitsuyoshi; Hatta, Tamao

    2003-09-01

    Al/Si configurations in some natural and synthetic Rb-feldspars have been examined carefully by EMPA and XPS analyses. Our results indicate that a small amount of H2O and excess Si and Al are incorporated in hydrothermally synthesized Rb-feldspar. The quantities of excess Al are 0.056 atoms per formula unit and are negatively correlated with those of the Rb, suggesting the presence of excess Al occupying non-tetrahedral sites in feldspar structures. This leads to incorporation of Al(Al3Si)O8 endmember into Rb-feldspars, estimated as one appropriate endmember indication for unusual chemistry of feldspars. In addition, Si2p, Al2p and O1s XPS signals of Rb-feldspars shift drastically toward the higher energy side than those of any natural feldspars. These provide conclusive evidence not only for existence of perceptible excess Si and Al, but also for Al at both extra-framework and tetrahedral sites in feldspar structures. PMID:14504785

  16. X-ray radiation-induced addition of oxygen atoms to protein residues.

    PubMed

    Wang, Jimin

    2016-08-01

    The additions of oxygen and peroxide to residues that result when proteins are exposed to the free radicals produced using the Fenton reaction or X-rays have been studied for over a century. Nevertheless little is known about the impact these modifications have on protein crystal structures. Here evidence is presented that both kinds of modifications occur in protein crystals on a significant scale during the collection of X-ray diffraction data. For example, at least 538 of the 5,351 residues of protein molecules in the crystal used to obtain the structure for photosystem II described by the PDB accession number 3ARC became oxygenated during data collection. PMID:27074249

  17. Study of Surface Cleaning Methods and Pyrolysis Temperature on Nano-Structured Carbon Films using X-ray Photoelectron Spectroscopy

    SciTech Connect

    Kerber, Pranita B.; Porter, Lisa M.; McCullough, L. A.; Kowalewski, Tomasz; Engelhard, Mark H.; Baer, Donald R.

    2012-10-12

    Nanostructured carbon (ns-C) films fabricated by stabilization and pyrolysis of di-block copolymers are of interest for a variety of electrical/electronic applications due to their chemical inertness, high-temperature insensitivity, very high surface area, and tunable electrical resistivity over a wide range [Kulkarni et al., Synth. Met. 159, (2009) 177]. Because of their high porosity and associated high specific surface area, controlled surface cleaning studies are important for fabricating electronic devices from these films. In this study, quantification of surface composition and surface cleaning studies on ns-C films synthesized by carbonization of di-block copolymers of polyacrylonitrile-b-poly(n-butyl acrylate) (PAN-b-PBA) at two different temperatures were carried out. X-ray photoelectron spectroscopy was used for elemental analysis and to determine the efficacy of various surface cleaning methods for ns-C films and to examine the polymer residues in the films. The in-situ surface cleaning methods included: HF vapor treatment, vacuum annealing, and exposure to UV-ozone. Quantitative analysis of high-resolution XPS scans showed 11 at. % of nitrogen present in the films pyrolyzed at 600 °C, suggesting incomplete denitrogenation of the copolymer films. The nitrogen atomic concentration reduced significantly for films pyrolyzed at 900 °C confirming extensive denitrogenation at that temperature. Furthermore, quantitative analysis of nitrogen sub-peaks indicated higher loss of nitrogen atoms residing at the edge of graphitic clusters relative to that of nitrogen atoms within the graphitic cluster, suggesting higher graphitization with increasing pyrolysis temperature. Of the surface cleaning methods investigated, in-situ annealing of the films at 300 °C for 40 min was found to be the most efficacious in removing adventitious carbon and oxygen impurities from the surface.

  18. Study of surface cleaning methods and pyrolysis temperatures on nanostructured carbon films using x-ray photoelectron spectroscopy

    SciTech Connect

    Kerber, Pranita; Porter, Lisa M.; McCullough, Lynne A.; Kowalewski, Tomasz; Engelhard, Mark; Baer, Donald

    2012-11-15

    Nanostructured carbon (ns-C) films fabricated by stabilization and pyrolysis of diblock copolymers are of interest for a variety of electrical/electronic applications due to their chemical inertness, high-temperature insensitivity, very high surface area, and tunable electrical resistivity over a wide range [Kulkarni et al., Synth. Met. 159, 177 (2009)]. Because of their high porosity and associated high specific surface area, controlled surface cleaning studies are important for fabricating electronic devices from these films. In this study, quantification of surface composition and surface cleaning studies on ns-C films synthesized by carbonization of diblock copolymers of polyacrylonitrile-b-poly(n-butyl acrylate) at two different temperatures were carried out. X-ray photoelectron spectroscopy was used for elemental analysis and to determine the efficacy of various surface cleaning methods for ns-C films and to examine the polymer residues in the films. The in-situ surface cleaning methods included HF vapor treatment, vacuum annealing, and exposure to UV-ozone. Quantitative analysis of high-resolution XPS scans showed 11 at. % nitrogen was present in the films pyrolyzed at 600 Degree-Sign C, suggesting incomplete denitrogenation of the copolymer films. The nitrogen atomic concentration decreased significantly for films pyrolyzed at 900 Degree-Sign C confirming extensive denitrogenation at that temperature. Furthermore, quantitative analysis of nitrogen subpeaks indicated higher loss of nitrogen atoms residing at the edge of graphitic clusters relative to that of nitrogen atoms within the graphitic clusters, suggesting higher graphitization with increasing pyrolysis temperature. Of the surface cleaning methods investigated, in-situ annealing of the films at 300 Degree-Sign C for 40 min was found to be the most efficacious in removing adventitious carbon and oxygen impurities from the surface.

  19. X-ray photoelectron spectroscopy study of the growth kinetics of biomimetically grown hydroxyapatite thin-film coatings

    NASA Astrophysics Data System (ADS)

    McLeod, K.; Kumar, S.; Dutta, N. K.; Smart, R. St. C.; Voelcker, N. H.; Anderson, G. I.

    2010-09-01

    Hydroxyapatite (HA) thin-film coatings grown biomimetically using simulated body fluid (SBF) are desirable for a range of applications such as improved fixation of fine- and complex-shaped orthopedic and dental implants, tissue engineering scaffolds and localized and sustained drug delivery. There is a dearth of knowledge on two key aspects of SBF-grown HA coatings: (i) the growth kinetics over short deposition periods, hours rather than weeks; and (ii) possible difference between the coatings deposited with and without periodic SBF replenishment. A study centred on these aspects is reported. X-ray photoelectron spectroscopy (XPS) has been used to study the growth kinetics of SBF-grown HA coatings for deposition periods ranging from 0.5 h to 21 days. The coatings were deposited with and without periodic replenishment of SBF. The XPS studies revealed that: (i) a continuous, stable HA coating fully covered the titanium substrate after a growth period of 13 h without SBF replenishment; (ii) thicker HA coatings about 1 μm in thickness resulted after a growth period of 21 days, both with and without SBF replenishment; and (iii) the Ca/P ratio at the surface of the HA coating was significantly lower than that in its bulk. No significant difference between HA grown with and without periodic replenishment of SBF was found. The coatings were determined to be carbonated, a characteristic desirable for improved implant fixation. The atomic force and scanning electron microscopies results suggested that heterogeneous nucleation and growth are the primary deposition mode for these coatings. Primary osteoblast cell studies demonstrated the biocompatibility of these coatings, i.e., osteoblast colony coverage of approximately 80%, similar to the control substrate (tissue culture polystyrene).

  20. Angle resolved x-ray photoelectron spectroscopy (ARXPS) analysis of lanthanum oxide for micro-flexography printing

    NASA Astrophysics Data System (ADS)

    Hassan, S.; Yusof, M. S.; Embong, Z.; Maksud, M. I.

    2016-01-01

    Micro-flexography printing was developed in patterning technique from micron to nano scale range to be used for graphic, electronic and bio-medical device on variable substrates. In this work, lanthanum oxide (La2O3) has been used as a rare earth metal candidate as depositing agent. This metal deposit was embedded on Carbon (C) and Silica (Si) wafer substrate using Magnetron Sputtering technique. The choose of Lanthanum as a target is due to its wide application in producing electronic devices such as thin film battery and printed circuit board. The La2O3 deposited on the surface of Si wafer substrate was then analyzed using Angle Resolve X-Ray Photoelectron Spectroscopy (ARXPS). The position for each synthetic component in the narrow scan of Lanthanum (La) 3d and O 1s are referred to the electron binding energy (eV). The La 3d narrow scan revealed that the oxide species of this particular metal is mainly contributed by La2O3 and La(OH)3. The information of oxygen species, O2- component from O 1s narrow scan indicated that there are four types of species which are contributed from the bulk (O2-), two chemisorb component (La2O3) and La(OH)3 and physisorp component (OH). Here, it is proposed that from the adhesive and surface chemical properties of La, it is suitable as an alternative medium for micro-flexography printing technique in printing multiple fine solid lines at nano scale. Hence, this paper will describe the capability of this particular metal as rare earth metal for use in of micro-flexography printing practice. The review of other parameters contributing to print fine lines will also be described later.

  1. Quantitative X-ray photoelectron spectroscopy-based depth profiling of bioleached arsenopyrite surface by Acidithiobacillus ferrooxidans

    NASA Astrophysics Data System (ADS)

    Zhu, Tingting; Lu, Xiancai; Liu, Huan; Li, Juan; Zhu, Xiangyu; Lu, Jianjun; Wang, Rucheng

    2014-02-01

    In supergene environments, microbial activities significantly enhance sulfide oxidation and result in the release of heavy metals, causing serious contamination of soils and waters. As the most commonly encountered arsenic mineral in nature, arsenopyrite (FeAsS) accounts for arsenic contaminants in various environments. In order to investigate the geochemical behavior of arsenic during microbial oxidation of arsenopyrite, (2 3 0) surfaces of arsenopyrite slices were characterized after acidic (pH 2.00) and oxidative decomposition with or without an acidophilic microorganism Acidithiobacillus ferrooxidans. The morphology as well as chemical and elemental depth profiles of the oxidized arsenopyrite surface were investigated by scanning electron microscopy and X-ray photoelectron spectroscopy. With the mediation of bacteria, cell-shaped and acicular pits were observed on the reacted arsenopyrite surface, and the concentration of released arsenic species in solution was 50 times as high as that of the abiotic reaction after 10 days reaction. Fine-scale XPS depth profiles of the reacted arsenopyrite surfaces after both microbial and abiotic oxidation provided insights into the changes in chemical states of the elements in arsenopyrite surface layers. Within the 450 nm surface layer of abiotically oxidized arsenopyrite, Fe(III)-oxides appeared and gradually increased towards the surface, and detectable sulfite and monovalent arsenic appeared above 50 nm. In comparison, higher contents of ferric sulfate, sulfite, and arsenite were found in the surface layer of approximately 3 μm of the microbially oxidized arsenopyrite. Intermediates, such as Fe(III)-AsS and S0, were detectable in the presence of bacteria. Changes of oxidative species derived from XPS depth profiles show the oxidation sequence is Fe > As = S in abiotic oxidation, and Fe > S > As in microbial oxidation. Based on these results, a possible reaction path of microbial oxidation was proposed in a concept model.

  2. Probing ultrathin film continuity and interface abruptness with x-ray photoelectron spectroscopy and low-energy ion scattering

    SciTech Connect

    Zhang, Wenyu; Nahm, Rambert K.; Engstrom, James R.; Ma, Paul F.

    2013-11-15

    The authors have examined ultrathin (≤10 Å) tantalum nitride (TaN{sub x}) thin films deposited by atomic layer deposition (ALD) on three surfaces relevant to interconnect layers in microelectronic devices: thermally grown SiO{sub 2}; a Cu thin film grown by physical vapor deposition, and a carbon-doped SiO{sub 2} porous low-κ thin film. The authors have employed ex situ angle-resolved x-ray photoelectron spectroscopy (ARXPS), low-energy ion scattering spectroscopy (LEISS), and atomic force microscopy (AFM) to determine the continuity of these thin films, and by implication, the abruptness of the thin film/substrate interface. On SiO{sub 2} and low-κ, the authors find similar results: both ARXPS and AFM indicate that smooth, uniform thin films are deposited, consistent with nearly layer-by-layer growth of TaN{sub x} on these surfaces. Examination of these films using LEISS reveals that while the 10 Å TaN{sub x} thin films are continuous, the 5 Å TaN{sub x} thin films are not continuous and may possess on the order of ∼10% exposed substrate in the form of small subnanometer inclusions. On Cu, the situation is quite different. The TaN{sub x} thin films on these surfaces are not continuous, and our results point to a mixed layer of TaN{sub x} and Cu forming during ALD. In all cases, if one were to rely solely on results from ARXPS, the picture would be incomplete as the results from LEISS are ultimately decisive concerning thin film continuity.

  3. X-ray photoelectron spectroscopy/Ar sup + ion profile study of thin oxide layers on InP

    SciTech Connect

    Thurgate, S.M.; Erickson, N.E. )

    1990-09-01

    The effect of incremental ion bombardment on the surface layers of an aqua regia etched InP sample was studied by monitoring the components of the In 3{ital d}{sub 5/2} and O 1{ital s} x-ray photoelectron spectroscopy (XPS) lines as the sample was bombarded with low energy (1 keV) Ar{sup +} ions. The changes in the stoichiometry of the surface produced large shifts in the position of the In 3{ital d} and O 1{ital s} lines that were not paralleled by shifts in the P 2{ital p} line. Analysis of these shifts indicated that the surface was covered with a mixture of indium hydroxide and indium phosphate, with the phosphate closer to the InP substrate. It is proposed that this layer structure is due to differences in the dissolution rates of the oxidation products in the acid etch and the effect of the distilled water rinse. It may be possible to alter the composition of such oxides by carefully tailoring the etch conditions to optimize the kinetics for the particular oxide phase required. The analysis of the XPS lines also showed that the InP substrate was damaged at very low ion doses, and finally decomposed by the ion beam. When the ion cleaned'' sample was exposed to oxygen, a different oxide system was produced which consisted largely of In{sub 2}O{sub 3} and InPO{sub 4} (or In(PO{sub 3} ){sub {ital x}}). This model of the oxidized surface of InP is consistent with other measurements and we conclude that ion milling together with XPS and careful curve fitting can be used to find the nature of the thin oxides on InP.

  4. Chemical bonding and electronic structures of microcline, orthoclase and the plagioclase series by X-ray photoelectron spectroscopy.

    PubMed

    Kloprogge, J Theo; Wood, Barry J

    2015-02-25

    A detailed analysis was undertaken of the X-ray photoelectron spectra obtained from microcline, orthoclase and several samples of plagioclase with varying Na/Ca ratio. Comparison of the spectra was made based on the chemical bonding and structural differences in the Al- and Si-coordination within each specimen. The spectra for Si 2p and Al 2p vary with the change in symmetry between microcline and orthoclase, while in plagioclase an increase in Al-O-Si linkages results in a small but observable decrease in binding energy. The overall shapes of the O 1s peaks observed in all spectra are similar and show shifts similar to those observed for Si 2p and Al 2p. The lower-VB spectra for microcline and orthoclase are similar intermediate between α-SiO2 and α-Al2O3 in terms of binding energies. In the plagioclase series increasing coupled substitution of Na and Si for Ca and Al results in a change of the overall shape of the spectra, showing a distinct broadening associated with the presence of two separate but overlapping bands similar to the 21 eV band observed for quartz and the 23 eV band observed for corundum. The bonding character for microcline and orthoclase is more covalent than that of α-Al2O3, but less than that of α-SiO2. In contrast, the plagioclase samples show two distinct bonding characters that are comparable with those of α-SiO2 and α-Al2O3. PMID:25261735

  5. Following the molecular motion of near-resonant excited CO on Pt(111): A simulated x-ray photoelectron diffraction study based on molecular dynamics calculations

    PubMed Central

    Greif, Michael; Nagy, Tibor; Soloviov, Maksym; Castiglioni, Luca; Hengsberger, Matthias; Meuwly, Markus; Osterwalder, Jürg

    2015-01-01

    A THz-pump and x-ray-probe experiment is simulated where x-ray photoelectron diffraction (XPD) patterns record the coherent vibrational motion of carbon monoxide molecules adsorbed on a Pt(111) surface. Using molecular dynamics simulations, the excitation of frustrated wagging-type motion of the CO molecules by a few-cycle pulse of 2 THz radiation is calculated. From the atomic coordinates, the time-resolved XPD patterns of the C 1s core level photoelectrons are generated. Due to the direct structural information in these data provided by the forward scattering maximum along the carbon-oxygen direction, the sequence of these patterns represents the equivalent of a molecular movie. PMID:26798798

  6. X-ray photoelectron and optical absorption spectroscopic studies on the dye chlorodiane blue, used as a carrier generation molecule in organic photoconductors

    SciTech Connect

    Pacansky, J.; Waltman, R.J.

    1992-07-01

    The dye chlorodiane blue, used as a carrier generation molecule in organic photoconductors, is characterized via optical absorption and X-ray photoelectron spectroscopy, and the results are interpreted on the basis of ab initio quantum mechanical molecular models. These data indicate that chlorodiane blue exists as azo-enol and hydrazone-quinone chemical structures and it is the hydrazone-quinone form that provides the higher xerographic gain in electrophotographic applications. Optimized geometries, atomic charges, and molecular orbital plots and energies are reported for both the azo-enol and hydrazone-quinone forms of chlorodiane blue. The two structural forms of the dye are experimentally distinguishable via both optical absorption and X-ray photoelectron spectroscopy, and the wavelength and chemical shifts, respectively, are interpreted via the theoretical results. 29 refs., 9 figs., 4 tabs.

  7. The evolution of Ga and As core levels in the formation of Fe/GaAs (001): A high resolution soft x-ray photoelectron spectroscopic study

    SciTech Connect

    Thompson, Jamie D. W.; Neal, James R.; Shen, Tiehan H.; Morton, Simon A.; Tobin, James G.; Dan Waddill, G.; Matthew, Jim A. D.; Greig, Denis; Hopkinson, Mark

    2008-07-15

    A high resolution soft x-ray photoelectron spectroscopic study of Ga and As 3d core levels has been conducted for Fe/GaAs (001) as a function of Fe thickness. This work has provided unambiguous evidence of substrate disrupting chemical reactions induced by the Fe overlayer--a quantitative analysis of the acquired spectra indicates significantly differing behavior of Ga and As during Fe growth, and our observations have been compared with existing theoretical models. Our results demonstrate that the outdiffusing Ga and As remain largely confined to the interface region, forming a thin intermixed layer. Whereas at low coverages Fe has little influence on the underlying GaAs substrate, the onset of substrate disruption when the Fe thickness reaches 3.5 A results in major changes in the energy distribution curves (EDCs) of both As and Ga 3d cores. Our quantitative analysis suggests the presence of two additional As environments of metallic character: one bound to the interfacial region and another which, as confirmed by in situ oxidation experiments, surface segregates and persists over a wide range of overlayer thickness. Analysis of the corresponding Ga 3d EDCs found not two, but three additional environments--also metallic in nature. Two of the three are interface resident whereas the third undergoes outdiffusion at low Fe coverages. Based on the variations of the integrated intensities of each component, we present a schematic of the proposed chemical makeup of the Fe/GaAs (001) system.

  8. The evolution of Ga and As core levels in the formation of Fe/GaAs (001):A high resolution soft x-ray photoelectron spectroscopic study

    SciTech Connect

    Thompson, Jamie; Neal, James; Shen, Tiehan; Morton, Simon; Tobin, James; Waddill, George Dan; Matthew, Jim; Greig, Denis; Hopkinson, Mark

    2008-07-14

    A high resolution soft x-ray photoelectron spectroscopic study of Ga and As 3d core levels has been conducted for Fe/GaAs (001) as a function of Fe thickness. This work has provided unambiguous evidence of substrate disrupting chemical reactions induced by the Fe overlayer--a quantitative analysis of the acquired spectra indicates significantly differing behavior of Ga and As during Fe growth, and our observations have been compared with existing theoretical models. Our results demonstrate that the outdiffusing Ga and As remain largely confined to the interface region, forming a thin intermixed layer. Whereas at low coverages Fe has little influence on the underlying GaAs substrate, the onset of substrate disruption when the Fe thickness reaches 3.5 Angstrom results in major changes in the energy distribution curves (EDCs) of both As and Ga 3d cores. Our quantitative analysis suggests the presence of two additional As environments of metallic character: one bound to the interfacial region and another which, as confirmed by in situ oxidation experiments, surface segregates and persists over a wide range of overlayer thickness. Analysis of the corresponding Ga 3d EDCs found not two, but three additional environments--also metallic in nature. Two of the three are interface resident whereas the third undergoes outdiffusion at low Fe coverages. Based on the variations of the integrated intensities of each component, we present a schematic of the proposed chemical makeup of the Fe/GaAs (001) system.

  9. Synchrotron X-ray CT characterization of titanium parts fabricated by additive manufacturing. Part I. Morphology.

    PubMed

    Scarlett, Nicola Vivienne Yorke; Tyson, Peter; Fraser, Darren; Mayo, Sheridan; Maksimenko, Anton

    2016-07-01

    Synchrotron X-ray tomography has been applied to the study of titanium parts fabricated by additive manufacturing (AM). The AM method employed here was the Arcam EBM(®) (electron beam melting) process which uses powdered titanium alloy, Ti64 (Ti alloy with approximately 6%Al and 4%V), as the feed and an electron beam for the sintering/welding. The experiment was conducted on the Imaging and Medical Beamline of the Australian Synchrotron. Samples were chosen to examine the effect of build direction and complexity of design on the surface morphology and final dimensions of the piece. PMID:27359150

  10. Al capping layers for nondestructive x-ray photoelectron spectroscopy analyses of transition-metal nitride thin films

    SciTech Connect

    Greczynski, Grzegorz Hultman, Lars; Petrov, Ivan; Greene, J. E.

    2015-09-15

    X-ray photoelectron spectroscopy (XPS) compositional analyses of materials that have been air exposed typically require ion etching in order to remove contaminated surface layers. However, the etching step can lead to changes in sample surface and near-surface compositions due to preferential elemental sputter ejection and forward recoil implantation; this is a particular problem for metal/gas compounds and alloys such as nitrides and oxides. Here, the authors use TiN as a model system and compare XPS analysis results from three sets of polycrystalline TiN/Si(001) films deposited by reactive magnetron sputtering in a separate vacuum chamber. The films are either (1) air-exposed for ≤10 min prior to insertion into the ultrahigh-vacuum (UHV) XPS system; (2) air-exposed and subject to ion etching, using different ion energies and beam incidence angles, in the XPS chamber prior to analysis; or (3) Al-capped in-situ in the deposition system prior to air-exposure and loading into the XPS instrument. The authors show that thin, 1.5–6.0 nm, Al capping layers provide effective barriers to oxidation and contamination of TiN surfaces, thus allowing nondestructive acquisition of high-resolution core-level spectra representative of clean samples, and, hence, correct bonding assignments. The Ti 2p and N 1s satellite features, which are sensitive to ion bombardment, exhibit high intensities comparable to those obtained from single-crystal TiN/MgO(001) films grown and analyzed in-situ in a UHV XPS system and there is no indication of Al/TiN interfacial reactions. XPS-determined N/Ti concentrations acquired from Al/TiN samples agree very well with Rutherford backscattering and elastic recoil analysis results while ion-etched air-exposed samples exhibit strong N loss due to preferential resputtering. The intensities and shapes of the Ti 2p and N 1s core level signals from Al/TiN/Si(001) samples do not change following long-term (up to 70 days) exposure to ambient conditions

  11. X-ray photoelectron spectroscopy and structural analysis of amorphous SiOxNy films deposited at low temperatures

    NASA Astrophysics Data System (ADS)

    Cova, P.; Poulin, S.; Masut, R. A.

    2005-11-01

    We establish, using a tetrahedral model, the bonding properties of amorphous silicon oxynitride (a-SiOxNy) films deposited at low temperatures (LTs) by electron-cyclotron resonance chemical-vapor deposition (ECRCVD) on several substrates and under various conditions of gas flows and total gas pressure in a dilute mixture of SiH4+N2 in Ar. The atomic percentage of each tetrahedral unit incorporated in the film network is calculated from the deconvolution of the high-resolution x-ray photoelectron spectroscopy (XPS) spectra in the Si 2p3/2 region and corroborated by the results obtained from both survey scans and the high-resolution XPS spectra in the N 1s region. The Si3N4 phase is the most important one and the only bonding unit which is incorporated in all our LT ECRCVD SiOxNy films. The incorporation of all the other component tetrahedrons depends strongly on growth conditions. The threshold values of the N/Si atomic ratio for which intrinsic defects, such as Si-Si bonds, are not incorporated in the network depend on the O/Si ratio incorporated in the films, mainly due to the competition between oxygen and nitrogen atoms in their reaction with silicon dangling bonds. The effect of the total gas pressure on the atomic percentages of the oxidation states present in the LT ECRCVD SiOxNy films is qualitatively similar to the effect of the ion bombarding energy or the plasma density. O-N bonds are present only in samples having high amount of oxygen and nitrogen in their networks. For these films, our results show unambiguously the presence of the N-Si2O tetrahedron and suggest that N-Si3-νOν tetrahedrons with ν>=2 are not incorporated in their networks. A correlation is observed between the N-Si2O and the Si-O3(ON) tetrahedrons whose component peak is localized at (104.0+/-0.2) eV in the Si 2p3/2 region of the XPS data, which suggests that both bonding units coexist in these films as some sort of complex bonding configuration.

  12. CO(2)-selective methanol steam reforming on In-doped Pd studied by in situ X-ray photoelectron spectroscopy.

    PubMed

    Rameshan, Christoph; Lorenz, Harald; Mayr, Lukas; Penner, Simon; Zemlyanov, Dmitry; Arrigo, Rosa; Haevecker, Michael; Blume, Raoul; Knop-Gericke, Axel; Schlögl, Robert; Klötzer, Bernhard

    2012-11-01

    In situ X-ray photoelectron spectroscopy (in situ XPS) was used to study the structural and catalytic properties of Pd-In near-surface intermetallic phases in correlation with previously studied PdZn and PdGa.Room temperature deposition of ∼4 monolayer equivalents (MLEs) of In metal on Pd foil and subsequent annealing to 453 K in vacuum yields a ∼1:1 Pd/In near-surface multilayer intermetallic phase. This Pd(1)In(1) phase exhibits a similar "Cu-like" electronic structure and indium depth distribution as its methanol steam reforming (MSR)-selective multilayer Pd(1)Zn(1) counterpart.Catalytic characterization of the multilayer Pd(1)In(1) phase in MSR yielded a CO(2)-selectivity of almost 100% between 493 and 550 K. In contrast to previously studied In(2)O(3)-supported PdIn nanoparticles and pure In(2)O(3), intermediate formaldehyde is only partially converted to CO(2) using this Pd(1)In(1) phase. Strongly correlated with PdZn, on an In-diluted PdIn intermetallic phase with "Pd-like" electronic structure, prepared by thermal annealing at 623 K, methanol steam reforming is suppressed and enhanced CO formation via full methanol dehydrogenation is observed.To achieve CO(2)-TOF values on the isolated Pd(1)In(1) intermetallic phase as high as on supported PdIn/In(2)O(3), at least 593 K reaction temperature is required. A bimetal-oxide synergism, with both bimetallic and oxide synergistically contributing to the observed catalytic activity and selectivity, manifests itself by accelerated formaldehyde-to-CO(2) conversion at markedly lowered temperatures as compared to separate oxide and bimetal. Combination of suppression of full methanol dehydrogenation to CO on Pd(1)In(1) inhibited inverse water-gas-shift reaction on In(2)O(3) and fast water activation/conversion of formaldehyde is the key to the low-temperature activity and high CO(2)-selectivity of the supported catalyst. PMID:23226689

  13. CO2-selective methanol steam reforming on In-doped Pd studied by in situ X-ray photoelectron spectroscopy

    PubMed Central

    Rameshan, Christoph; Lorenz, Harald; Mayr, Lukas; Penner, Simon; Zemlyanov, Dmitry; Arrigo, Rosa; Haevecker, Michael; Blume, Raoul; Knop-Gericke, Axel; Schlögl, Robert; Klötzer, Bernhard

    2012-01-01

    In situ X-ray photoelectron spectroscopy (in situ XPS) was used to study the structural and catalytic properties of Pd–In near-surface intermetallic phases in correlation with previously studied PdZn and PdGa. Room temperature deposition of ∼4 monolayer equivalents (MLEs) of In metal on Pd foil and subsequent annealing to 453 K in vacuum yields a ∼1:1 Pd/In near-surface multilayer intermetallic phase. This Pd1In1 phase exhibits a similar “Cu-like” electronic structure and indium depth distribution as its methanol steam reforming (MSR)-selective multilayer Pd1Zn1 counterpart. Catalytic characterization of the multilayer Pd1In1 phase in MSR yielded a CO2-selectivity of almost 100% between 493 and 550 K. In contrast to previously studied In2O3-supported PdIn nanoparticles and pure In2O3, intermediate formaldehyde is only partially converted to CO2 using this Pd1In1 phase. Strongly correlated with PdZn, on an In-diluted PdIn intermetallic phase with “Pd-like” electronic structure, prepared by thermal annealing at 623 K, methanol steam reforming is suppressed and enhanced CO formation via full methanol dehydrogenation is observed. To achieve CO2-TOF values on the isolated Pd1In1 intermetallic phase as high as on supported PdIn/In2O3, at least 593 K reaction temperature is required. A bimetal-oxide synergism, with both bimetallic and oxide synergistically contributing to the observed catalytic activity and selectivity, manifests itself by accelerated formaldehyde-to-CO2 conversion at markedly lowered temperatures as compared to separate oxide and bimetal. Combination of suppression of full methanol dehydrogenation to CO on Pd1In1 inhibited inverse water–gas-shift reaction on In2O3 and fast water activation/conversion of formaldehyde is the key to the low-temperature activity and high CO2-selectivity of the supported catalyst. PMID:23226689

  14. Electron transfer reactions on Cs/MoS2(0002) with chlorine, oxygen, and water: High resolution x-ray photoelectron spectroscopy and theoretical study

    NASA Astrophysics Data System (ADS)

    Park, Ken T.; Hess, James S.; Klier, Kamil

    1999-07-01

    Supra-valence electron transfer from surface Cs-doped MoS2(0002) to electron acceptor adsorbates was investigated by high resolution x-ray photoelectron spectroscopy (HRXPS) in the valence band region and above the valence band maximum (VBM). Deposition of a sub-monolayer amount of Cs onto the basal plane of MoS2 introduced a new electron density of states at ca. 1.25 eV above VBM. Angle-resolved HRXPS and theoretical analysis located this electron density in the MoS2 layer. Upon the reaction with Cl2, this Cs-induced photoelectron almost completely disappeared and the Cs 3d and Cl 2p core levels indicated the formation of a surface Cs-chloride species. The Cs-covered MoS2(0002) surface also reacted with O2 to form surface peroxides and superoxides, as evidenced by two distinct binding energies of the O 1s core level peaks. However, the reaction with water proved to be more difficult: Exposure of the Cs-covered MoS2(0002) surface to H2O at 10-5 Torr did not result in electron transfer reaction, but the Cs/MoS2(0002) surface exposed to H2O at 1 Torr showed a substantial decrease in the density of states above VBM as well as formation of a surface-hydroxide, indicated by the O 1s core level position. Theoretical calculations using a full-potential linearized augmented plane wave density functional theory (FLAPW-DFT) confirm the conclusion based on experimental intensity anisotropy of the new peak: the Cs 6s electron transfers into the MoS2 substrate, forming the Cs/MoS2 electron donor-acceptor complex with Csδ+. In addition, all phenomena observed during the adsorption of electron donor-acceptor molecules are quantitatively accounted by the theory.

  15. Toward new techniques to measure heterogeneous oxidation of aerosol: Electrodynamic Balance-Mass Spectrometry (EDB-MS) and Aerosol X-ray Photoelectron Spectroscopy

    NASA Astrophysics Data System (ADS)

    Jacobs, M. I.; Heine, N.; Xu, B.; Davies, J. F.; Kirk, B. B.; Kostko, O.; Alayoglu, S.; Wilson, K. R.; Ahmed, M.

    2015-12-01

    The chemical composition and physical properties of aerosol can be changed via heterogeneous oxidation with the OH radical. However, the physical state of the aerosol influences the kinetics of this reaction; liquid particles with a high diffusion coefficient are expected to be well mixed and homogenously oxidized, while oxidation of solid, diffusion-limited aerosol is expected to occur primarily on the surface, creating steep chemical gradients within the particle. We are working to develop several new techniques to study the heterogeneous oxidation of different types of aerosol. We are developing a "modular" electrodynamic balance (EDB) that will enable us to study heterogeneous oxidation at aqueous interfaces using a mass-spectrometer (and potentially other detection techniques). Using a direct analysis in real time (DART) interface, preliminary droplet train measurements have demonstrated single-droplet mass spectrometry to be possible. With long reaction times in our EDB, we will be able to study heterogeneous oxidation of a wide variety of organic species in aqueous droplets. Additionally, we are working to use aerosol photoemission and velocity map imaging (VMI) to study the surface of aerosol particles as they undergo heterogeneous oxidation. With VMI, we're able to collect electrons with a 4π collection efficiency over conventional electron energy analyzers. Preliminary results looking at the ozonolysis of squalene using ultraviolet photoelectron spectroscopy (UPS) show that heterogeneous oxidation kinetic data can be extracted from photoelectron spectra. By moving to X-ray photoemission spectroscopy (XPS), we will determine elemental and chemical composition of the aerosol surface. Thus, aerosol XPS will provide information on the steep chemical gradients that form as diffusion-limited aerosol undergo heterogeneous oxidation.

  16. Beam Damage of Poly(Vinyl Chloride) [PVC] Film as Observed by X-ray Photoelectron Spectroscopy

    SciTech Connect

    Engelhard, Mark H.; Krishna, Abhilash; Kulkarni, Pranita B.; Lee, Chi-Ying M.; Baer, Donald R.

    2003-03-08

    XPS spectra of a spin-coated film poly(vinyl chloride) (PVC) were collected over a period of 243 minutes at 303 K to determine specimen damage during long exposures to monochromatic Al Ka x-rays. For this PVC film we measured the loss of chlorine as a function of time by rastering a focused 104.6 w 100 um diameter x-ray beam over a 1.4 mm x 0.2 mm area on the sample.

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

    SciTech Connect

    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.

  18. Impact of water vapour and carbon dioxide on surface composition of C{sub 3}A polymorphs studied by X-ray photoelectron spectroscopy

    SciTech Connect

    Dubina, E.; Plank, J.; Black, L.

    2015-07-15

    The surface specific analytical method, X-ray photoelectron spectroscopy (XPS), has been used to study the effects of water vapour and CO{sub 2} on the cubic and orthorhombic polymorphs of C{sub 3}A. Significant differences between the two polymorphs were observed in the XPS spectra. Upon exposure to water vapour, both polymorphs produced C{sub 4}AH{sub 13} on their surfaces. Additionally, the sodium-doped o-C{sub 3}A developed NaOH and traces of C{sub 3}AH{sub 6} on its surface. Subsequent carbonation yielded mono carboaluminate on both polymorphs. Large amounts of Na{sub 2}CO{sub 3} also formed on the surface of o-C{sub 3}A as a result of carbonation of NaOH. Furthermore, the extent of carbonation was much more pronounced for o-C{sub 3}A{sub o} than for c-C{sub 3}A.

  19. X-ray Photoelectron Spectroscopy ofGaP_{1-x}N_x Photocorroded as a Result of Hydrogen Productionthrough Water Electrolysis

    SciTech Connect

    Mayer, Marie A.; /Illinois U., Urbana /SLAC

    2006-09-27

    Photoelectrochemical (PEC) cells produce hydrogen gas through the sunlight driven electrolysis of water. By extracting hydrogen and oxygen from water and storing solar energy in the H-H bond, they offer a promising renewable energy technology. Addition of dilute amounts of nitrogen to III-V semiconductors has been shown to dramatically increase the stability of these materials for hydrogen production. In an effort to learn more about the origin of semiconductor photocorrosion in PEC cells, three samples of p-type GaP with varying levels of nitrogen content (0%, 0.2%, 2%) were photocorroded and examined by X-ray Photoelectron Spectroscopy (XPS). GaPN samples were observed to be more efficient during the hydrogen production process than the pure GaP samples. Sample surfaces contained gallium oxides in the form of Ga{sub 2}O{sub 3} and Ga(OH){sub 3} and phosphorus oxide (P{sub 2}O{sub 5}), as well as surface oxides from exposure to air. A significant shift in intensity from bulk to surface peaks dramatic nitrogen segregation to the surface during photoelectrochemical hydrogen production. Further investigations, including using a scanning electron microscope to investigate sample topography and inductively coupled plasma mass spectroscopy (ICP-MS) analysis for solution analyses, are under way to determine the mechanism for these changes.

  20. Micro-x-ray fluorescence, micro-x-ray absorption spectroscopy, and micro-x-ray diffraction investigation of lead speciation after the addition of different phosphorus amendments to a smelter-contaminated soil.

    PubMed

    Baker, Lucas R; Pierzynski, Gary M; Hettiarachchi, Ganga M; Scheckel, Kirk G; Newville, Matthew

    2014-03-01

    The stabilization of Pb on additions of P to contaminated soils and mine spoil materials has been well documented. It is clear from the literature that different P sources result in different efficacies of Pb stabilization in the same contaminated material. We hypothesized that the differences in the efficacy of Pb stabilization in contaminated soils on fluid or granular P amendment addition is due to different P reaction processes in and around fertilizer granules and fluid droplets. We used a combination of several synchrotron-based techniques (i.e., spatially resolved micro-X-ray fluorescence, micro-X-ray absorption near-edge structure spectroscopy, and micro-X-ray diffraction) to speciate Pb at two incubation times in a smelter-contaminated soil on addition of several fluid and granular P amendments. The results indicated that the Pb phosphate mineral plumbogummite was an intermediate phase of pyromorphite formation. Additionally, all fluid and granular P sources were able to induce Pb phosphate formation, but fluid phosphoric acid (PA) was the most effective with time and distance from the treatment. Granular phosphate rock and triple super phosphate (TSP) amendments reacted to generate Pb phosphate minerals, with TSP being more effective at greater distances from the point of application. As a result, PA and TSP were the most effective P amendments at inducing Pb phosphate formation, but caution needs to be exercised when adding large amounts of soluble P to the environment. PMID:25602650

  1. Kaolinite flocculation induced by smectite addition - a transmission X-ray microscopic study.

    PubMed

    Zbik, Marek S; Song, Yen-Fang; Frost, Ray L

    2010-09-01

    The influence of smectite addition on kaolinite suspensions in water was investigated by transmission X-ray microscopy (TXM) and Scanning Electron Microscopy (SEM). Sedimentation test screening was also conducted. Micrographs were processed by the STatistic IMage Analysing (STIMAN) program and structural parameters were calculated. From the results of the sedimentation tests important influences of small smectite additions to about 3wt.% on kaolinite suspension flocculation has been found. In order to determine the reason for this smectite impact on kaolinite suspension, macroscopic behaviour micro-structural examination using Transmission X-ray Microscope (TXM) and SEM has been undertaken. TXM & SEM micrographs of freeze-dried kaolinite-smectite suspensions with up to 20% smectite showed a high degree of orientation of the fabric made of highly oriented particles and greatest density when 3wt.% of smectite was added to the 10wt.% dense kaolinite suspension. In contrast, suspensions containing pure kaolinite do not show such platelet mutual orientation but homogenous network of randomly oriented kaolinite platelets. This suggests that in kaolinite-smectite suspensions, smectite forms highly oriented basic framework into which kaolinite platelets may bond in face to face preferential contacts strengthening structure and allowing them to show plastic behaviour which is cause of platelets orientation. PMID:20621806

  2. X-ray photoelectron spectroscopy and diffraction investigation of a metal-oxide-semiconductor heterostructure: Pt/Gd2O3/Si(111)

    NASA Astrophysics Data System (ADS)

    Ferrah, D.; El Kazzi, M.; Niu, G.; Botella, C.; Penuelas, J.; Robach, Y.; Louahadj, L.; Bachelet, R.; Largeau, L.; Saint-Girons, G.; Liu, Q.; Vilquin, B.; Grenet, G.

    2015-04-01

    Platinum thin films deposited by physical vapor deposition (PVD) on Gd2O3/Si(111) templates are investigated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and X-ray photoelectron diffraction (XPD). Both XRD and XPD give clear evidence that Gd2O3 grows (111)-oriented and single-domain on Si(111) with mirror epitaxial relationship viz., [1bar10] Gd2O3(111)//[11bar0] Si(111). On Gd2O3/Si(111), Pt is partially crystallized with (111) orientation. There are two epitaxial domains and a slightly visible (111) fiber texture. The in-plane relationships of these Pt(111) domains with Gd2O3(111) are a direct one: [11bar0] Pt(111)//[11bar0] Gd2O3(111) and a mirror one: [1bar10] Pt(111)//[11bar0] Gd2O3(111). XPS reveals that Pt4f exhibits a metallic behavior even for small amounts of Pt but very small chemical shifts suggest that Pt environment is different at the interface with Gd2O3. These XPS chemical shifts have been correlated with features in XPD azimuth curves, which could be related with the existence of hexagonal α-PtO2(0001)layer.

  3. Line shapes and satellites in high-resolution x-ray photoelectron spectra of large pi-conjugated organic molecules.

    PubMed

    Schöll, A; Zou, Y; Jung, M; Schmidt, Th; Fink, R; Umbach, E

    2004-11-22

    We present a high-resolution C1s and O1 s x-ray photoemission (XPS) study for condensed films of pi-conjugated organic molecules, namely, of the anhydrides 3,4,9,10-perylene-tetracarboxylic acid dianhydride, 1,4,5,8-naphthalene-tetracarboxylic acid dianhydride, 1,8-naphthalene dicarboxylic acid anhydride, and benzoperylene-(1,8)-dicarboxylic acid anhydride as well as the quinoic acenaphthenequinone. Although the functional groups are identical for the anhydrides, the molecules show very different photoemission fine structure thus providing a detailed fingerprint. A simultaneous peak fit analysis of the XPS spectra of all molecules allows to consistently determine the ionization potentials of all chemically different carbon and oxygen atoms. Additional structures in the C1s and O1s spectra are interpreted as shakeup satellites and assigned with the help of singles and doubles configuration interaction calculations. These satellites provide further information on multielectron excitations and must be taken into account for quantitative investigations. PMID:15549902

  4. Beam damage of poly(vinyl chloride) [PVC] as observed by x-ray photoelectron spectroscopy at 143 K, 303 K and 373 K.

    SciTech Connect

    Engelhard, Mark H.; Baer, Donald R.; Lea, Alan S.

    2003-03-08

    X-ray beam damage is often observed during surface analysis of beam sensitive materials as indicated in the introduction to this issue and in a wide variety of references. While damage occurs in a wide range of materials, those that are most susceptible to damage are materials that contain low energy covalent bonds such as polymers or other organic materials. Even amongst the relatively easily damaged polymers, there is a wide range of damage rates. The data reported in this submission was collected in the interest of comparing the rates of damage produced by x-ray and electron irradiation of different materials. The focus of this submission is x-ray damage of bulk poly(vinyl chloride) PVC since it is a readily available material. The temperature of the sample holder was controlled during irradiation of the PVC in order to determine the extent to which localized sample heating affects the rate of damage. PVC degrades by photoionization, resulting in the production of HCl through H and Cl bond cleavage. Bulk PVC has previously been the focus of an x-ray damage study involving many laboratories throughout the world. For comparison to the bulk PVC data, damage rates for thin films of poly(2-chloroethyl methacrylate) (PCEMA) are also reported for the same three temperatures. Measurements of several relatively common materials on one instrument can provide a data base that allows damage rates on one instrument to be linked or compared to other damage data in the literature. In addition to the PCEMA films and bulk PVC, other data collected at the same x-ray parameters include thin films of PVC (for which damage rates are essentially identical to the bulk material) and of poly(acrylonitrile) PAN which is more stable that either PCEMA or PVC. An additional set of PVC data for a different instrument is also included in the volume. X-ray beams used for XPS produce less damage in materials than electrons used for AES analysis. This is due to both th e weaker interaction

  5. Analysis of electronic structure of amorphous InGaZnO/SiO{sub 2} interface by angle-resolved X-ray photoelectron spectroscopy

    SciTech Connect

    Ueoka, Y.; Ishikawa, Y.; Maejima, N.; Matsui, F.; Matsui, H.; Yamazaki, H.; Urakawa, S.; Horita, M.; Daimon, H.; Uraoka, Y.

    2013-10-28

    The electronic structures of amorphous indium gallium zinc oxide (a-IGZO) on a SiO{sub 2} layers before and after annealing were observed by constant final state X-ray photoelectron spectroscopy (CFS-XPS) and X-ray adsorption near-edge structure spectroscopy (XANES). From the results of angle-resolved CFS-XPS, the change in the electronic state was clearly observed in the a-IGZO bulk rather than in the a-IGZO/SiO{sub 2} interface. This suggests that the electronic structures of the a-IGZO bulk strongly affected the thin-film transistor characteristics. The results of XANES indicated an increase in the number of tail states upon atmospheric annealing (AT). We consider that the increase in the number of tail states decreased the channel mobility of AT samples.

  6. Study of band offsets at the Cu2SnS3/In2O3: Sn interface using x-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Dias, Sandra; Krupanidhi, S. B.

    2015-06-01

    Cu2SnS3 thins films were deposited onto In2O3: Sn coated soda lime glass substrates by spin coating technique. The films have been structurally characterized using x-ray Diffraction (XRD) and Atomic Force Microscopy (AFM). The morphology of the films was studied using Field Emission Scanning Electron Microscopy (FESEM). The optical properties of the films were determined using UV-vis-NIR spectrophotometer. The electrical properties were measured using Hall effect measurements. The energy band offsets at the Cu2SnS3/In2O3: Sn interface were calculated using x-ray photoelectron spectroscopy (XPS). The valence band offset was found to be -3.4 ± 0.24 eV. From the valence band offset value, the conduction band offset is calculated to be -1.95 ± 0.34 eV. The energy band alignment indicates a type-II misaligned heterostructure formation.

  7. Development of a single-shot CCD-based data acquisition system for time-resolved X-ray photoelectron spectroscopy at an X-ray free-electron laser facility.

    PubMed

    Oura, Masaki; Wagai, Tatsuya; Chainani, Ashish; Miyawaki, Jun; Sato, Hiromi; Matsunami, Masaharu; Eguchi, Ritsuko; Kiss, Takayuki; Yamaguchi, Takashi; Nakatani, Yasuhiro; Togashi, Tadashi; Katayama, Tetsuo; Ogawa, Kanade; Yabashi, Makina; Tanaka, Yoshihito; Kohmura, Yoshiki; Tamasaku, Kenji; Shin, Shik; Ishikawa, Tetsuya

    2014-01-01

    In order to utilize high-brilliance photon sources, such as X-ray free-electron lasers (XFELs), for advanced time-resolved photoelectron spectroscopy (TR-PES), a single-shot CCD-based data acquisition system combined with a high-resolution hemispherical electron energy analyzer has been developed. The system's design enables it to be controlled by an external trigger signal for single-shot pump-probe-type TR-PES. The basic performance of the system is demonstrated with an offline test, followed by online core-level photoelectron and Auger electron spectroscopy in 'single-shot image', 'shot-to-shot image (image-to-image storage or block storage)' and `shot-to-shot sweep' modes at soft X-ray undulator beamline BL17SU of SPring-8. In the offline test the typical repetition rate for image-to-image storage mode has been confirmed to be about 15 Hz using a conventional pulse-generator. The function for correcting the shot-to-shot intensity fluctuations of the exciting photon beam, an important requirement for the TR-PES experiments at FEL sources, has been successfully tested at BL17SU by measuring Au 4f photoelectrons with intentionally controlled photon flux. The system has also been applied to hard X-ray PES (HAXPES) in `ordinary sweep' mode as well as shot-to-shot image mode at the 27 m-long undulator beamline BL19LXU of SPring-8 and also at the SACLA XFEL facility. The XFEL-induced Ti 1s core-level spectrum of La-doped SrTiO3 is reported as a function of incident power density. The Ti 1s core-level spectrum obtained at low power density is consistent with the spectrum obtained using the synchrotron source. At high power densities the Ti 1s core-level spectra show space-charge effects which are analysed using a known mean-field model for ultrafast electron packet propagation. The results successfully confirm the capability of the present data acquisition system for carrying out the core-level HAXPES studies of condensed matter induced by the XFEL. PMID:24365935

  8. Assigning Oxidation States to Organic Compounds via Predictions from X-ray Photoelectron Spectroscopy: A Discussion of Approaches and Recommended Improvements

    SciTech Connect

    Gupta, Vipul; Ganegoda, Hasitha; Engelhard, Mark H.; Terry, Jeff H.; Linford, Matthew R.

    2014-02-11

    The traditional assignment of oxidation numbers to organic molecules is problematic. Accordingly, in 1999, Calzaferri proposed a simple and elegant solution that is based on the similar electronegativities of carbon and hydrogen: hydrogen would be assigned an oxidation number of zero when bonded to carbon. Here we show that X-ray photoelectron spectroscopy (XPS), a core electron spectroscopy that is sensitive to oxidation states of elements, confirms his suggestion. In particular, in this work we: (i) list the typical rules for assigning oxidation numbers, (ii) discuss the traditional assignment of oxidation numbers to organic molecules, (iii) review Calzaferri’s solution, (iv) introduce X-ray photoelectron spectroscopy (XPS), (v) show the consistency of Calzaferri’s suggestion with XPS results, (vi) provide supporting examples from the literature, (vii) provide examples from our own research, and (viii) further confirm the Calzaferri suggestion/photoelectron spectroscopy results by discussing two organic well-known reactions. We end by reechoing Calzaferri’s suggestion that the traditional rules for assigning oxidation numbers to organic molecules be modified.

  9. A high pressure x-ray photoelectron spectroscopy experimental method for characterization of solid-liquid interfaces demonstrated with a Li-ion battery system

    NASA Astrophysics Data System (ADS)

    Maibach, Julia; Xu, Chao; Eriksson, Susanna K.; Åhlund, John; Gustafsson, Torbjörn; Siegbahn, Hans; Rensmo, Hâkan; Edström, Kristina; Hahlin, Maria

    2015-04-01

    We report a methodology for a direct investigation of the solid/liquid interface using high pressure x-ray photoelectron spectroscopy (HPXPS). The technique was demonstrated with an electrochemical system represented by a Li-ion battery using a silicon electrode and a liquid electrolyte of LiClO4 in propylene carbonate (PC) cycled versus metallic lithium. For the first time the presence of a liquid electrolyte was realized using a transfer procedure where the sample was introduced into a 2 mbar N2 environment in the analysis chamber without an intermediate ultrahigh vacuum (UHV) step in the load lock. The procedure was characterized in detail concerning lateral drop gradients as well as stability of measurement conditions over time. The X-ray photoelectron spectroscopy (XPS) measurements demonstrate that the solid substrate and the liquid electrolyte can be observed simultaneously. The results show that the solid electrolyte interphase (SEI) composition for the wet electrode is stable within the probing time and generally agrees well with traditional UHV studies. Since the methodology can easily be adjusted to various high pressure photoelectron spectroscopy systems, extending the approach towards operando solid/liquid interface studies using liquid electrolytes seems now feasible.

  10. A high pressure x-ray photoelectron spectroscopy experimental method for characterization of solid-liquid interfaces demonstrated with a Li-ion battery system

    SciTech Connect

    Maibach, Julia; Xu, Chao; Gustafsson, Torbjörn; Edström, Kristina; Eriksson, Susanna K.; Åhlund, John; Siegbahn, Hans; Rensmo, Håkan; Hahlin, Maria

    2015-04-15

    We report a methodology for a direct investigation of the solid/liquid interface using high pressure x-ray photoelectron spectroscopy (HPXPS). The technique was demonstrated with an electrochemical system represented by a Li-ion battery using a silicon electrode and a liquid electrolyte of LiClO{sub 4} in propylene carbonate (PC) cycled versus metallic lithium. For the first time the presence of a liquid electrolyte was realized using a transfer procedure where the sample was introduced into a 2 mbar N{sub 2} environment in the analysis chamber without an intermediate ultrahigh vacuum (UHV) step in the load lock. The procedure was characterized in detail concerning lateral drop gradients as well as stability of measurement conditions over time. The X-ray photoelectron spectroscopy (XPS) measurements demonstrate that the solid substrate and the liquid electrolyte can be observed simultaneously. The results show that the solid electrolyte interphase (SEI) composition for the wet electrode is stable within the probing time and generally agrees well with traditional UHV studies. Since the methodology can easily be adjusted to various high pressure photoelectron spectroscopy systems, extending the approach towards operando solid/liquid interface studies using liquid electrolytes seems now feasible.

  11. X-ray photoelectron spectroscopic study of the oxide film on an aluminum-tin alloy in 3.5% sodium chloride solution

    SciTech Connect

    Venugopal, A.; Selvam, P.; Raja, V.S.; Veluchamy, P.; Minoura, H.

    1997-10-01

    Oxide films on Al and an Al-Sn alloy were analyzed by x-ray photoelectron spectroscopy (XPS) after immersion in 3.5% sodium chloride (NaCl) solution. Results showed Sn exhibited both Sn{sup 2+} and Sn{sup 4+} oxidation stats in the oxide film. It was proposed that incorporation of these cations in the film would result in generation of more anionic and cationic vacancies in aluminum oxide (Al{sub 2}O{sub 3}), leading to active dissolution of Al.

  12. X-ray photoelectron spectroscopic analysis of oxidized Fe-16Cr-16Ni-2Mn-1Mo-2Si austenitic stainless steel

    SciTech Connect

    Poston, J.A., Jr.; Siriwardane, R.V.; Dunning, J.S.; Alman, D.E.; Rawers, J.C.

    2007-03-30

    Depth profile analysis (argon ion etching/X-ray photoelectron spectroscopy) was conducted on a series of Fe–16Cr–16Ni–2Mn–1Mo–2Si austenitic stainless steel samples oxidized at 973 and 1073 K with exposure times of 25, 100, 193, 436 and 700 h. Surface and near surface rearrangement following oxidation resulted in a region of high Cr concentration on all oxidized samples. Temperature and time dependence to O2 penetration depth was observed. In general, O2 penetration depth was found to increase with increasing exposure up to 436 h. No increase in depth was observed between 436 and 700 h exposure time.

  13. Electron-hole recombination on ZnO(0001) single-crystal surface studied by time-resolved soft X-ray photoelectron spectroscopy

    SciTech Connect

    Yukawa, R.; Yamamoto, S.; Ogawa, M.; Yamamoto, Sh.; Fujikawa, K.; Hobara, R.; Matsuda, I.; Ozawa, K.; Emori, M.; Sakama, H.; Kitagawa, S.; Daimon, H.

    2014-10-13

    Time-resolved soft X-ray photoelectron spectroscopy (PES) experiments were performed with time scales from picoseconds to nanoseconds to trace relaxation of surface photovoltage on the ZnO(0001) single crystal surface in real time. The band diagram of the surface has been obtained numerically using PES data, showing a depletion layer which extends to 1 μm. Temporal evolution of the photovoltage effect is well explained by a recombination process of a thermionic model, giving the photoexcited carrier lifetime of about 1 ps at the surface under the flat band condition. This lifetime agrees with a temporal range reported by the previous time-resolved optical experiments.

  14. X-ray photoelectron spectroscopic study of surface chemistry of dibenzyl-disulfide on steel under mild and severe wear conditions

    NASA Technical Reports Server (NTRS)

    Wheeler, D. R.

    1977-01-01

    Wear tests were performed on 304 stainless steel lubricated with pure mineral oil with and without dibenzyl-disulfide. Both mild and severe wear were observed. The type of wear was distinguished by a marked change in wear rate, friction coefficient, and wear scar appearance. The chemical composition of the wear scar surface was examined with X-ray photoelectron spectroscopy in conjunction with argon ion sputter etching. In severe wear scars, a sulfide was formed at the expense of the normal oxide layer. In mild wear scars, there were only superficial sulfur compounds, but there was a substantial increase in the oxide thickness.

  15. X-ray photoelectron spectroscopy study of radiofrequency sputtered chromium bromide, molybdenum disilicide, and molybdenum disulfide coatings and their friction properties

    NASA Technical Reports Server (NTRS)

    Wheeler, D. R.; Brainard, W. A.

    1977-01-01

    Radiofrequency sputtered coatings of CRB2, MOSI2, and MOS2 were examined by X-ray photoelectron spectroscopy. The effects of sputtering target history, deposition time, RF power level, and substrate bias on film composition were studied. Friction tests were run on RF sputtered surfaces of 440-C steel to correlate XPS data with lubricating properties. Significant deviations from stoichiometry and high oxide levels for all three compounds were related to target outgassing. The effect of biasing on these two factors depended on the compound. Improved stoichiometry correlated well with good friction and wear properties.

  16. Understanding the electronic structure of IrO2 using hard-X-ray photoelectron spectroscopy and density-functional theory.

    PubMed

    Kahk, J M; Poll, C G; Oropeza, F E; Ablett, J M; Céolin, D; Rueff, J-P; Agrestini, S; Utsumi, Y; Tsuei, K D; Liao, Y F; Borgatti, F; Panaccione, G; Regoutz, A; Egdell, R G; Morgan, B J; Scanlon, D O; Payne, D J

    2014-03-21

    The electronic structure of IrO2 has been investigated using hard x-ray photoelectron spectroscopy and density-functional theory. Excellent agreement is observed between theory and experiment. We show that the electronic structure of IrO2 involves crystal field splitting of the iridium 5d orbitals in a distorted octahedral field. The behavior of IrO2 closely follows the theoretical predictions of Goodenough for conductive rutile-structured oxides [J. B. Goodenough, J. Solid State Chem. 3, 490 (1971). PMID:24702416

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

    SciTech Connect

    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}.

  18. X-Ray Photoelectron Spectroscopy and Scanning Electrochemical Microscopy Studies of Branched Multiwalled Carbon Nanotube Paper Modified by Electrochemical Grafting and Click Chemistry

    NASA Astrophysics Data System (ADS)

    Coates, Megan; Nyokong, Tebello

    2013-06-01

    Modification of nanomaterials through electrochemical grafting is a useful approach to introduce linking groups on to the surface of these structures. This work shows the possibility of applying electrochemical grafting to branched multiwalled carbon nanotube paper with an electrical resistance of 0.1 ohm-cm, and subsequent reaction of the grafted 4-azidobenzenediazonium with ethynylferrocene through the Sharpless click chemistry reaction. A comparison is made between this paper electrode and adsorbed single-walled carbon nanotubes on a glassy carbon electrode, with electrochemistry, X-ray photoelectron spectroscopy and scanning electrochemical microscopy used for characterization.

  19. X-ray photoelectron spectroscopy investigation of the Schottky barrier at low-k a-SiO(C):H/Cu interfaces

    SciTech Connect

    King, S. W.; French, M.; Jaehnig, M.; Kuhn, M.; French, B.

    2011-11-14

    In order to understand the fundamental mechanisms involved in electrical leakage in low-k/Cu interconnects, we have utilized x-ray photoelectron spectroscopy to determine the Schottky barrier present at interfaces formed by plasma enhanced chemical vapor deposition of low-k a-SiO{sub x}C{sub y}:H thin films on polished Cu substrates. We find the Schottky Barrier at this interface to range widely from 1 to >4 eV and to be dependent on the amount of network carbon incorporated into the a-SiOC:H thin films.

  20. Structure analyses using X-ray photoelectron spectroscopy and X-ray absorption near edge structure for amorphous MS3 (M: Ti, Mo) electrodes in all-solid-state lithium batteries

    NASA Astrophysics Data System (ADS)

    Matsuyama, Takuya; Deguchi, Minako; Mitsuhara, Kei; Ohta, Toshiaki; Mori, Takuya; Orikasa, Yuki; Uchimoto, Yoshiharu; Kowada, Yoshiyuki; Hayashi, Akitoshi; Tatsumisago, Masahiro

    2016-05-01

    Electronic structure changes of sulfurs in amorphous TiS3 and MoS3 for positive electrodes of all-solid-state lithium batteries are examined by X-ray photoelectron spectroscopy (XPS) and the X-ray absorption near edge structure (XANES). The all-solid-state cell with amorphous TiS3 electrode shows the reversible capacity of about 510 mAh g-1 for 10 cycles with sulfur-redox in amorphous TiS3 during charge-discharge process. On the other hand, the cell with amorphous MoS3 shows the 1st reversible capacity of about 720 mAh g-1. The obtained capacity is based on the redox of both sulfur and molybdenum in amorphous MoS3. The irreversible capacity of about 50 mAh g-1 is observed at the 1st cycle, which is attributed to the irreversible electronic structure change of sulfur during the 1st cycle. The electronic structure of sulfur in amorphous MoS3 after the 10th charge is similar to that after the 1st charge. Therefore, the all-solid-state cell with amorphous MoS3 electrode shows relatively good cyclability after the 1st cycle.

  1. X-ray Photoelectron Spectroscopy Study of Al- and N- Co-Doped p-Type ZnO Thin Films

    SciTech Connect

    Yuan, G. D.; Ye, Z. Z.; Huang, J. Y.; Zhu, L. P.; Perkins, C. L.; Zhang, S. B.

    2009-01-01

    The chemical state of nitrogen, aluminum, oxygen and zinc in Al-N co-doped p-type ZnO thin films was investigated by X-ray photoelectron spectroscopy (XPS). N{sub 1s} peak were detected in both the two p-type ZnO thin films, showing two components. The higher binding energy peak may be due to the Al-No-H species, and the lower one perhaps derive from the (NH{sub 2}){sup -} cluster for the ammonia introduction. These two peaks both contribute to the p-type behavior in the ZnO films. A symmetry 74.4 eV binding energy in Al{sub 2p3/2} photoelectron peaks revealed an Al-N bonding state, a key factor to the co-doping method.

  2. Polarity of semipolar wurtzite crystals: X-ray photoelectron diffraction from GaN(101⁻1) and GaN(202⁻1) surfaces

    SciTech Connect

    Romanyuk, O. Jiříček, P.; Bartoš, I.; Paskova, T.

    2014-09-14

    Polarity of semipolar GaN(101⁻1) (101⁻1⁻) and GaN(202⁻1) (202⁻1⁻) surfaces was determined with X-ray photoelectron diffraction (XPD) using a standard MgKα source. The photoelectron emission from N 1s core level measured in the a-plane of the crystals shows significant differences for the two crystal orientations within the polar angle range of 80–100° from the (0001) normal. It was demonstrated that XPD polar plots recorded in the a-plane are similar for each polarity of the GaN(101⁻1) and GaN(202⁻1) crystals if referred to (0001) crystal axes. For polarity determinations of all important GaN(h0h⁻l) semipolar surfaces, the above given polar angle range is suitable.

  3. Weathering properties of treated southern yellow pine wood examined by X-ray photoelectron spectroscopy, scanning electron microscopy and physical characterization

    NASA Astrophysics Data System (ADS)

    Salaita, Ghaleb N.; Ma, Frank M. S.; Parker, Trudy C.; Hoflund, Gar B.

    2008-04-01

    In this study the weathering behavior of southern yellow pine (SYP) wood samples pretreated in different solutions has been examined using X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and various types of physical characterization regarding material loss and discoloration. The treatment solutions include water as a control, a commercially available water repellent (WR) wood treating additive and polyethylene glycol (PEG) products including PEG PLUS™, PEG 8000 solutions and Compound 20M in varying concentrations. All contained the wood preservative chromated copper arsenate (CCA). One sample was treated with a CCA solution only. The treatments were carried out at 20 °C and 150 psig for 1/2 h after exposure to vacuum (28 mmHg) for 15 min. Simulated weathering was achieved in an Atlas 65-W Weather-Ometer for 2000 h with both light and dark periods and rain. The temperature ranged from 23 °C during the dark cycle to 35 °C during the light cycle. With weathering the XPS O/C ratios increase due to oxidation of the surface. Exposure to UV light results in bond breakage and reaction with oxygen in the presence of air to form organic functional groups such as ?, ?, C dbnd O and/or O-C-O. These oxidized products can protect the underlying wood from deterioration if they are insoluble in water and remain on the surface as a protective coating. If soluble, rain washes the compounds away and assists in the degradation. Correlated changes are observed in the XPS O/C ratios, the high-resolution XPS C 1s spectra, the SEM micrographs and physical measurements including thickness alteration, weight loss, and discoloration by yellowing or whitening of the weathered wood. The PEG treatments are effective in protecting wood with the 2% PEG PLUS treatment providing the best weathering behavior similar to that of the CCA treatment. The WR and water treatments yield the poorest weathering properties.

  4. Near-Ambient-Pressure X-ray Photoelectron Spectroscopy Study of Methane-Induced Carbon Deposition on Clean and Copper-Modified Polycrystalline Nickel Materials

    PubMed Central

    2015-01-01

    In order to simulate solid-oxide fuel cell (SOFC)-related coking mechanisms of Ni, methane-induced surface carbide and carbon growth was studied under close-to-real conditions by synchrotron-based near-ambient-pressure (NAP) X-ray photoelectron spectroscopy (XPS) in the temperature region between 250 and 600 °C. Two complementary polycrystalline Ni samples were used, namely, Ni foam—serving as a model structure for bulk Ni in cermet materials such as Ni/YSZ—and Ni foil. The growth mechanism of graphene/graphite species was found to be closely related to that previously described for ethylene-induced graphene growth on Ni(111). After a sufficiently long “incubation” period of the Ni foam in methane at 0.2 mbar and temperatures around 400 °C, cooling down to ∼250 °C, and keeping the sample at this temperature for 50–60 min, initial formation of a near-surface carbide phase was observed, which exhibited the same spectroscopic fingerprint as the C2H4 induced Ni2C phase on Ni(111). Only in the presence of this carbidic species, subsequent graphene/graphite nucleation and growth was observed. Vice versa, the absence of this species excluded further graphene/graphite formation. At temperatures above 400 °C, decomposition/bulk dissolution of the graphene/graphite phase was observed on the rather “open” surface of the Ni foam. In contrast, Ni foil showed—under otherwise identical conditions—predominant formation of unreactive amorphous carbon, which can only be removed at ≥500 °C by oxidative clean-off. Moreover, the complete suppression of carbide and subsequent graphene/graphite formation by Cu-alloying of the Ni foam and by addition of water to the methane atmosphere was verified. PMID:26692914

  5. Influence of electron irradiation and heating on secondary electron yields from non-evaporable getter films observed with in situ x-ray photoelectron spectroscopy

    SciTech Connect

    Nishiwaki, Michiru; Kato, Shigeki

    2007-07-15

    Nonevaporable getter (NEG) film has been used for the beam ducts of particle accelerators as a pump having a large area. NEG film has been considered to have a low outgas rate induced by energetic particle irradiation and a low secondary electron yield (SEY). In this article, we focused on SEY measurements and in situ surface characterization of four NEG film samples using x-ray photoelectron spectroscopy (XPS). The NEG samples were TiZrV thin films deposited by magnetron sputtering at 100 or 300 deg. C on stainless steel. In addition, NEG samples saturated by CO gas exposure were prepared. SEY and XPS measurements of the surfaces of NEG samples were carried out under the conditions of as received, after electron beam irradiation, and after heating at 200 deg. C for 24 h. The maximum SEY values of the primary electron energy dependence, {delta}{sub max}, of all NEG samples decreased to around 1 by electron beam irradiation owing to a change in the carbon impurities, such as carbon oxide, carbon hydroxide, and hydrocarbon, to graphite state (graphitization) during the irradiation. After heating, {delta}{sub max} values of the NEG samples without CO gas exposure were also around 1 owing to the carbonization of Ti, Zr, and V. The {delta}{sub max}{approx_equal}1 was remarkably lower than that of copper baked under the same conditions. However, in saturated NEG samples, metal carbides were not produced to a significant extent by heating, and the {delta}{sub max} values did not decrease, showing values of 1.5-1.7.

  6. X-ray photoelectron spectroscopy study of high-k CeO{sub 2}/La{sub 2}O{sub 3} stacked dielectrics

    SciTech Connect

    Zhang, Jieqiong; Wong, Hei; Yu, Danqun; Kakushima, Kuniyuki; Iwai, Hiroshi

    2014-11-15

    This work presents a detailed study on the chemical composition and bond structures of CeO{sub 2}/La{sub 2}O{sub 3} stacked gate dielectrics based on x-ray photoelectron spectroscopy (XPS) measurements at different depths. The chemical bonding structures in the interfacial layers were revealed by Gaussian decompositions of Ce 3d, La 3d, Si 2s, and O 1s photoemission spectra at different depths. We found that La atoms can diffuse into the CeO{sub 2} layer and a cerium-lanthanum complex oxide was formed in between the CeO{sub 2} and La{sub 2}O{sub 3} films. Ce{sup 3+} and Ce{sup 4+} states always coexist in the as-deposited CeO{sub 2} film. Quantitative analyses were also conducted. The amount of CeO{sub 2} phase decreases by about 8% as approaching the CeO{sub 2}/La{sub 2}O{sub 3} interface. In addition, as compared with the single layer La{sub 2}O{sub 3} sample, the CeO{sub 2}/La{sub 2}O{sub 3} stack exhibits a larger extent of silicon oxidation at the La{sub 2}O{sub 3}/Si interface. For the CeO{sub 2}/La{sub 2}O{sub 3} gate stack, the out-diffused lanthanum atoms can promote the reduction of CeO{sub 2} which produce more atomic oxygen. This result confirms the significant improvement of electrical properties of CeO{sub 2}/La{sub 2}O{sub 3} gated devices as the excess oxygen would help to reduce the oxygen vacancies in the film and would suppress the formation of interfacial La-silicide also.

  7. Evaluation of valence band top and electron affinity of SiO2 and Si-based semiconductors using X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Fujimura, Nobuyuki; Ohta, Akio; Makihara, Katsunori; Miyazaki, Seiichi

    2016-08-01

    An evaluation method for the energy level of the valence band (VB) top from the vacuum level (VL) for metals, dielectrics, and semiconductors from the results of X-ray photoelectron spectroscopy (XPS) is presented for the accurate determination of the energy band diagram for materials of interest. In this method, the VB top can be determined by the energy difference between the onset of VB signals and the cut-off energy for secondary photoelectrons by considering the X-ray excitation energy (hν). The energy level of the VB top for three kinds of Si-based materials (H-terminated Si, wet-cleaned 4H-SiC, and thermally grown SiO2) has been investigated by XPS under monochromatized Al Kα radiation (hν = 1486.6 eV). We have also demonstrated the determination of the electron affinity for the samples by this measurement technique in combination with the measured and reported energy bandgaps (E g).

  8. Angle-resolved X-ray photoelectron spectroscopy study of poly(vinylidene fluoride)/poly(N-dodecylacrylamide) Langmuir-Blodgett nanofilms

    NASA Astrophysics Data System (ADS)

    Zhu, Huie; Gao, Yu; Yamamoto, Shunsuke; Miyashita, Tokuji; Mitsuishi, Masaya

    2016-03-01

    Our earlier research prepared ferroelectric poly(vinylidene fluoride) (PVDF) homopolymer monolayers at the air-water interface using amphiphilic poly(N-dodecylacrylamide) (pDDA) nanosheets with Langmuir-Blodgett (LB) technique. However, the miscibility of solvent for PVDF with the water sub-phase in the Langmuir trough makes the film composition unclear in spite of the feeding ratio of \\text{PVDF}:\\text{pDDA} (50:1). In this study, angle-resolved X-ray photoelectron spectroscopy (AR-XPS) was used to investigate the surface chemical composition and the depth profile of the PVDF/pDDA LB nanofilms. The X-ray photoelectron spectroscopy (XPS) spectra confirmed by the detection of fluorine atoms that PVDF molecules were deposited successfully onto the substrate. The constant chemical composition with increasing takeoff angle from 15 to 75° reflects a well-regular layer structure of the PVDF LB nanofilm. The mixing ratio of \\text{PVDF}:\\text{pDDA} is 33:1, which contributes 89.8 wt % PVDF and 10.2 wt % in the PVDF/pDDA LB nanofilms.

  9. Study of energy band discontinuity in NiZnO/ZnO heterostructure using X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Dewan, Sheetal; Tomar, Monika; Goyal, Anshu; Kapoor, A. K.; Tandon, R. P.; Gupta, Vinay

    2016-05-01

    A heterostructure based on ZnO and Ni doped ZnO (NiZnO) thin films has been prepared on c-plane sapphire substrate by pulsed laser deposition technique. X-ray photo electron spectroscopy has been utilized to study the energy band discontinuities, i.e., valence band offset ( Δ E v ) and conduction band offset ( Δ E c ) at the interface of NiZnO and ZnO thin films. A type-II band alignment is identified at the interface of prepared heterostructure from the computed data, which is attractive for the realization of efficient optoelectronic devices.

  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

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

    SciTech Connect

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

    SciTech Connect

    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.

  13. Real-time observation of the dry oxidation of the Si (100) surface with ambient pressure x-ray photoelectron spectroscopy

    SciTech Connect

    Enta, Y.; Mun, B.S.; Rossi, M.; Ross Jr, P.N.; Hussain, Zahid; Fadley, C.S.; Lee, K.-S.; Kim, S.-K.

    2007-09-20

    We have applied ambient-pressure x-ray photoelectron spectroscopy with Si 2p chemical shifts to study the real-time dry oxidation of Si(100), using pressures in the range of 0.01-1 Torr and temperatures of 300-530 oC, and examining the oxide thickness range from 0 to ~;;25 Angstrom. The oxidation rate is initially very high (with rates of up to ~;;225 Angstrom/h) and then, after a certain initial thickness of the oxide in the range of 6-22 Angstrom is formed, decreases to a slow state (with rates of ~;;1.5-4.0 Angstrom/h). Neither the rapid nor the slow regime is explained by the standard Deal-Grove model for Si oxidation.

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

    SciTech Connect

    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.

  15. 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

    Imam, H.; Ahmed, Doaa; Eldakrouri, Ashraf

    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.

  16. Performance of a size-selected nanocluster deposition facility and in situ characterization of grown films by x-ray photoelectron spectroscopy

    SciTech Connect

    Mondal, Shyamal; Bhattacharyya, S. R.

    2014-06-15

    We report here on a newly installed gas aggregation type nanocluster deposition unit based on magnetron sputtering ion source with mass selection of the clusters by quadrupole mass filter. The system is ultra high vacuum compatible and is equipped with an in situ X-ray Photoelectron Spectroscopy facility, giving compositional information of the films formed by nanoclusters deposition on a substrate. Detailed descriptions and working of the components of the system are presented. For the characterization of the nanocluster source and associated mass filter for size selected clusters, the dependence of output performance as a function of aggregation length, sputter gas flow and magnetron power of the cluster source have been studied. Copper nanoclusters deposited on Silicon (100) surface and on transmission electron microscope grids are, respectively, studied with scanning electron microscopy and transmission electron microscopy for the morphology.

  17. X-ray photoelectron spectroscopy and friction studies of nickel-zinc and manganese-zinc ferrites in contact with metals

    NASA Technical Reports Server (NTRS)

    Miyoshi, K.; Buckley, D. H.

    1983-01-01

    X-ray photoelectron spectroscopy analysis and sliding friction experiments were conducted with hot-pressed, polycrystalline Ni-Zn and Mn-Zn ferrites in sliding contact with various transition metals at room temperature in a vacuum of 30 nPa. The results indicate that the coefficients of friction for Ni-Zn and Mn-Zn ferrites in contact with metals are related to the relative chemical activity in these metals: the more active the metal, the higher is the coefficient of friction. The coefficients of friction for the ferrites correlate with the free energy of formation of the lowest metal oxide. The interfacial bond can be regarded as a chemical bond between the metal atoms and the oxygen anions in the ferrite surfaces. The adsorption of oxygen on clean metal and ferrite surfaces increases the coefficients of friction for the Ni-Zn and Mn-Zn ferrite-metal interfaces.

  18. Electronic structure of ultrathin Fe films on TiO[sub 2](110) studied with soft-x-ray photoelectron spectroscopy and resonant photoemission

    SciTech Connect

    Diebold, U. Department of Physics, Tulane University, New Orleans, Louisiana 70118-5698 ); Tao, H. ); Shinn, N.D. ); Madey, T.E. )

    1994-11-15

    We report on soft-x-ray photoelectron spectroscopy (SXPS) of a TiO[sub 2](110) surface during deposition of Fe in the monolayer regime. At low fractional monolayer coverages, the adsorbed Fe atoms are oxidized and Ti cations at the interface become reduced due to Fe adsorption. SXPS from shallow core levels and valence bands show that Fe starts to exhibit metallic character at a coverage of approximately 0.7 equivalent monolayers. Two well separated defect states appear in the band gap of TiO[sub 2] at iron coverages well below one monolayer. We use resonant photoemission to obtain information on the partial density of states, and we assign these defect states as being Fe-derived and Ti-derived states, located at the Fe and Ti sites, respectively. We suggest that a position change of oxygen is involved in the bonding of Fe on the TiO[sub 2](110) surface.

  19. Initial stages of ITO/Si interface formation: In situ x-ray photoelectron spectroscopy measurements upon magnetron sputtering and atomistic modelling using density functional theory

    SciTech Connect

    Løvvik, O. M.; Diplas, S.; Ulyashin, A.; Romanyuk, A.

    2014-02-28

    Initial stages of indium tin oxide (ITO) growth on a polished Si substrate upon magnetron sputtering were studied experimentally using in-situ x-ray photoelectron spectroscopy measurements. The presence of pure indium and tin, as well as Si bonded to oxygen at the ITO/Si interface were observed. The experimental observations were compared with several atomistic models of ITO/Si interfaces. A periodic model of the ITO/Si interface was constructed, giving detailed information about the local environment at the interface. Molecular dynamics based on density functional theory was performed, showing how metal-oxygen bonds are broken on behalf of silicon-oxygen bonds. These theoretical results support and provide an explanation for the present as well as previous ex-situ and in-situ experimental observations pointing to the creation of metallic In and Sn along with the growth of SiO{sub x} at the ITO/Si interface.

  20. Hard x-ray photoelectron spectroscopy study on band alignment at poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate)/ZnO interface

    NASA Astrophysics Data System (ADS)

    Nagata, T.; Oh, S.; Yamashita, Y.; Yoshikawa, H.; Hayakawa, R.; Kobayashi, K.; Chikyow, T.; Wakayama, Y.

    2012-10-01

    We used hard x-ray photoelectron spectroscopy to investigate the interfacial electronic states of a poly(styrenesulfonate) doped poly(3,4-ethylenedioxythiophene) (PEDOT:PSS) contact on a ZnO single crystal. An understanding of the interfacial band structure is useful for putting the organic contact to practical use. We observed upward band bending of the ZnO layer a few nanometers from the interface. The detected ZnO bulk region exhibited a flat band structure, meaning that the PEDOT:PSS does not greatly deplete the ZnO layer. The band bending caused the charge injection barrier formation with the result that the contact exhibited the Schottky property.

  1. The nature of the water nucleation sites on TiO2(110) surfacesrelvealed by ambient pressure x-ray photoelectron spectroscopy

    SciTech Connect

    Ketteler, Guido; Yamamoto, Susumu; Bluhm, Hendrik; Andersson,Klas; Starr, David E.; Ogletree, D. Frank; Ogasawara, Hirohito; Nilsson,Anders; Salmeron, Miquel

    2007-05-01

    X-ray photoelectron spectroscopy at ambient conditions of pressure (up to 1.5 Torr) and temperature (265K

  2. Synthesis, conductivity, and X-ray photoelectron spectrum of Bi 2Sr 2CuO 7+X. A new ternary bismuth-oxide system exhibiting metallic conductivity

    NASA Astrophysics Data System (ADS)

    Porter, Leigh Christopher; Appelman, Evan; Beno, Mark A.; Cariss, Carolyn S.; Carlson, K. Douglas; Cohen, Harry; Geiser, Urs; Thorn, R. J.; Williams, Jack M.

    1988-06-01

    The preparation and some of the properties relating to the superconductive state of the newly discovered ternary bismuth oxide, Bi 2Sr 2Cu 2O 7+x, are described. Conductivity behavior ranging from semiconductive to metallic is observed when four-probe AC resistivity measurements are carried out on pressed pellet specimens that have been annealed under different conditions. From a determination of the total oxygen present by an iodometric titration, it was found that metallic conductivity was associated with a higher oxygen content. An X-ray photoelectron experiment was carried out in order to determine whether bismuth or copper was present as the mixed-valent species. The XPS spectrum of the Bi 4 f orbital electrons in the oxide was nearly identical to that observed in Bi 2O 3, with no evidence of any Bi 5+.

  3. Synthesis conductivity, and x ray photoelectron spectrum of Bi2Sr2Cu(sub 7+x). A new ternary bismuth-oxide system exhibiting metallic conductivity

    NASA Astrophysics Data System (ADS)

    Porter, Leigh Christopher; Appleman, Evan; Beno, Mark A.; Cariss, Carolyn S.; Carlson, K. Douglas; Cohen, Harry; Geiser, Urs; Thorn, R. J.; Williams, John M.

    The preparation and some of the properties relating to the superconductive state of the newly discovered ternary bismuth oxides, Bi2Sr2Cu2O(7+x), are described. Conductivity behavior ranging from semiconductive to metallic is observed when four-probe ac resistivity measurements are carried out on pressed pellet specimens that have been annealed under different conditions. From a determination of the total oxygen present by an iodometric titration, it was found that metallic conductivity was associated with a higher oxygen content. An x ray photoelectron experiment was carried out in order to determine whether bismuth or copper was present as the mixed valent species. The XPS spectrum of the Bi 4f orbital electrons in the oxides was nearly identical to that observed in Bi2O3, with no evidence of any Bi5(+).

  4. Band alignment study of lattice-matched In{sub 0.49}Ga{sub 0.51}P and Ge using x-ray photoelectron spectroscopy

    SciTech Connect

    Owen, Man Hon Samuel E-mail: yeo@ieee.org; Zhou, Qian; Gong, Xiao; Yeo, Yee-Chia E-mail: yeo@ieee.org; Zhang, Zheng; Pan, Ji Sheng; Loke, Wan Khai; Wicaksono, Satrio; Yoon, Soon Fatt; Tok, Eng Soon

    2014-09-08

    Lattice-matched In{sub 0.49}Ga{sub 0.51}P was grown on a p-type Ge(100) substrate with a 10° off-cut towards the (111) by low temperature molecular beam epitaxy, and the band-alignment of In{sub 0.49}Ga{sub 0.51}P on Ge substrate was obtained by high resolution x-ray photoelectron spectroscopy. The valence band offset for the InGaP/Ge(100) interface was found to be 0.64 ± 0.12 eV, with a corresponding conduction band offset of 0.60 ± 0.12 eV. The InGaP/Ge interface is found to be of the type I band alignment.

  5. X-ray photoelectron spectroscopic studies of carbon fiber surfaces. 22. Comparison between surface treatment of untreated and previously surface-treated fibers

    SciTech Connect

    Wang, Y.Q.; Viswanathan, H.; Audi, A.A.; Sherwood, P.M.A.

    2000-04-01

    IM7 PAN-based carbon fibers, with a proprietary surface treatment applied by the manufacturer, were analyzed by X-ray photoelectron spectroscopy (XPS). The surface treatment applied by the manufacturer was removed by heating in a vacuum. The fibers detreated in this manner were then subjected to electrochemical treatment. The electrochemical behavior of the as-received fibers and detreated fibers were measured and analyzed. When the same electrochemical treatment was applied to the as-received fibers with their commercial surface treatment intact, a different surface chemistry was observed for the detreated fibers. This study shows that the surface chemistry of treated fibers depends closely on the initial surface chemistry of the fibers and its detreatment. This work shows the importance of using untreated or detreated fibers as precursors for applying reproducible surface treatment so that one can understand and control the surface chemistry of fibers and their interfacial interaction in composites.

  6. Probing the Reversible Changes in Electronic Structure Induced by Liquid Electrolyte Gating in WO3 Thin Films by Hard X-ray Photoelectron Spectroscopy

    NASA Astrophysics Data System (ADS)

    Karel, Julie; Viol Barbosa, Carlos; Altendorf, Simone; Kiss, Janos; Utsumi, Yuki; Samant, Mahesh; Tjeng, Liu Hao; Felser, Claudia; Parkin, Stuart

    2015-03-01

    Tungsten trioxide (WO3) is a d0 transition metal oxide that has attracted broad interest from both application and fundamental materials physics standpoints. It has been studied for use in photoelectrochemical hydrogen generation, smart windows, gas sensors and has been shown to exhibit high temperature surface superconductivity when doped with K or Cs. Many of these studies necessitate modifications in the carrier concentration and in particular oxygen deficiencies. In this work, we utilize liquid electrolyte gating to create oxygen vacancies in WO3 thin films, a process we will show is reversible. The modifications in the electronic structure (core levels and valance band) resulting from the gating are probed by hard X-ray photoelectron spectroscopy. Electrolyte gating leads to a significant population of W 5d states in the conduction band and an enormous change in the W 4f core levels. Ab initio density functional theory is used to help describe the origin of these modifications in the electronic structure.

  7. X-ray photoelectron spectroscopy study of energy-band alignments of ZnO on buffer layer Lu2O3

    NASA Astrophysics Data System (ADS)

    Chen, Shanshan; Pan, Xinhua; Xu, Chenxiao; Huang, Jingyun; Ye, Zhizhen

    2016-02-01

    Lu2O3 was used as the buffer layer of the epitaxy of ZnO film on Si substrate by plasma-assisted molecular beam epitaxy. X-ray photoelectron spectroscopy was used to determine the band alignment at ZnO/Lu2O3 interface. The conduction band offset (CBO) and valence band offset (VBO) of the ZnO/Lu2O3 heterojunction are calculated to be 1.77 eV and 0.66 eV, respectively, with a type-I band alignment. And the ratio of CBO and VBO (ΔEc / ΔEv) is estimated to be about 2.68. The large ΔEv and ΔEc reveal that Lu2O3 is an ideal barrier layer in Si-based ZnO optoelectronic devices.

  8. Non-destructive assessment of the polarity of GaN nanowire ensembles using low-energy electron diffraction and x-ray photoelectron diffraction

    SciTech Connect

    Romanyuk, O. Jiříček, P.; Bartoš, I.; Fernández-Garrido, S.; Geelhaar, L.; Brandt, O.; Paskova, T.

    2015-01-12

    We investigate GaN nanowire ensembles spontaneously formed in plasma-assisted molecular beam epitaxy by non-destructive low-energy electron diffraction (LEED) and x-ray photoelectron diffraction (XPD). We show that GaN nanowire ensembles prepared on AlN-buffered 6H-SiC(0001{sup ¯}) substrates with well-defined N polarity exhibit similar LEED intensity-voltage curves and angular distribution of photo-emitted electrons as N-polar free-standing GaN layers. Therefore, as in the case of GaN layers, LEED and XPD are found to be suitable techniques to assess the polarity of GaN nanowire ensembles on a macroscopic scale. The analysis of GaN nanowire ensembles prepared on bare Si(111) allows us to conclude that, on this non-polar substrate, the majority of nanowires is also N-polar.

  9. Investigation of chemical distribution in the oxide bulk layer in Ti/HfO{sub 2}/Pt memory devices using x-ray photoelectron spectroscopy

    SciTech Connect

    Jiang, Ran; Du, Xianghao; Han, Zuyin; Sun, Weideng

    2015-04-27

    Resistive switching (RS) of Ti/HfO{sub 2}/Pt memory devices was studied using X-ray photoelectron spectroscopy. Hf{sup 4+} monotonously decreases with depth increasing towards to HfO{sub 2}/Pt interface in low resistance state, while a fluctuation distribution of Hf{sup 4+} is shown in high resistance state (HRS) and in the pristine Ti/HfO{sub 2}/Pt devices (without any SET or RESET process). It is explained by the existence of locally accumulated oxygen vacancies (clusters) in the oxide bulk layer in HRS and pristine states. A dynamic model of RS processes was proposed that the oxygen vacancy clusters dominantly determines the resistivity by the connecting/rupture between the neighbor cluster sites in the bulk.

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

    NASA Astrophysics Data System (ADS)

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

    2015-08-01

    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.

  11. Auger electron spectroscopy and x-ray photoelectron spectroscopy of the biocorrosion of copper by Gum Arabic, BCS and Pseudomonas atlantica exopolymer

    SciTech Connect

    Jolley, J.G.; Geesey, G.G.; Hankins, M.R.; Wright, R.B.; Wichlacz, P.L.

    1987-01-01

    Thin films (3.4 nm) of copper on germanium substrates were exposed to 10% Gum Arabic aqueous solution, 1% BCS (aqueous and simulated sea water solutions) and 0.5% Pseudomonas atlantica exopolymer (aqueous and simulated sea water solutions). Pre- and post-exposure characterization were done by Auger electron spectroscopy and x-ray photoelectron spectroscopy. Ancillary graphite furnace atomic absorption spectroscopy was used to monitor the removal process of the copper thin film from the germanium substrate. Results indicate that the copper was oxidized by the Gum Arabic and BCS, and some was removed from the Cu/Ge interface by all three polymers and incorporated into the polymer matrix. Thus biocorrosion of copper was exhibited by the Gum Arabic, BCS and Pseudomonas atlantica exopolymer. 14 refs., 4 figs., 3 tabs.

  12. X-Ray Photoelectron Spectroscopy Study of GaAs (001) and InP (001) Cleaning Procedures Prior to Molecular Beam Epitaxy

    NASA Astrophysics Data System (ADS)

    Contour, J. P.; Massies, J.; Saletes, A.

    1985-07-01

    The effect of chemical etching by H2S04/H202/H20 (5/1/1) mixtures and of mechanopolishing by bromine-methanol diluted solution on GaAs (001) and InP (001) substrates for molecular beam epitaxy (MBE) has been studied using X-ray photoelectron spectroscopy (XPS). The final rinse in running deionized water does not produce any passivating oxide layer on the substrate surface. Oxidation observed on GaAs and InP after these cleaning procedures occurs during substrate handling in air. The H2S04/H202/H20 mixture produces arsenic rich surface layers having an atomic ratio As/Ga of 1.15, whereas the bromine-methanol mechanopolishing leads to an arsenic or phosphorus depleted surface with atomic ratios As/Ga=0.7 and P/In=0.65.

  13. X-ray photoelectron spectroscopy studies of initial growth mechanism of CdTe layers grown on (100)GaAs by organometallic vapor phase epitaxy

    NASA Astrophysics Data System (ADS)

    Sone, Syuji; Ekawa, Mitsuru; Yasuda, Kazuhito; Sugiura, Yoshiyuki; Saji, Manabu; Tanaka, Akikazu

    1990-02-01

    Variations of the GaAs surface conditions and the adsorption of the precursor elements of Cd and Te on the (100)GaAs substrate were studied by x-ray photoelectron spectroscopy at the initial stage of CdTe growth by organometallic vapor phase epitaxy. The stoichiometry of GaAs substrates was found to recover by annealing in the H2 environment (500 °C, 5 min), while the surface was initially in an As-rich condition after etching with H2SO4:H2O2:H2O (5:1:1). The preferential adsorption of Te on the GaAs surface was also observed. <100> oriented growth was obtained routinely when the GaAs surface was fully stabilized with Te after the H2 anneal under the above conditions. <111> oriented growth resulted when dimethylcadmium was first introduced after the anneal.

  14. Oxides on GaAs and InAs surfaces: An x-ray-photoelectron-spectroscopy study of reference compounds and thin oxide layers

    NASA Astrophysics Data System (ADS)

    Hollinger, G.; Skheyta-Kabbani, R.; Gendry, M.

    1994-04-01

    The chemical composition of thin native oxide layers grown on GaAs and InAs by ultraviolet (UV)/ozone and thermal oxidation is investigated using x-ray-photoelectron spectroscopy. Core-level binding energies, core-level intensities, and valence-band spectra are compared with data for bulk crystalline binary or ternary As, In, and Ga oxides. The chemical compositions, which vary strongly from GaAs to InAs and from thermal to UV oxidation, appear to be controlled by both thermodynamic and kinetic factors. Only for GaAs thermal oxidation are the products predicted at thermodynamic equilibrium obtained. In all cases the native oxides can be described as single phase nonstoichiometric compounds and not as a macroscopic mixture of stoichiometric binary oxides.

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

    SciTech Connect

    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.

  16. The role of cesium suboxides in low-work-function surface layers studied by X-ray photoelectron spectroscopy - Ag-O-Cs

    NASA Technical Reports Server (NTRS)

    Yang, S.-J.; Bates, C. W., Jr.

    1980-01-01

    The oxidation of cesium on silver substrates has been studied using photoyield measurements and X-ray photoelectron spectroscopy. The occurrence of two O1s peaks in the core-level spectrum at 527.5 and 531.5-eV binding energy for cesium and oxygen exposures giving the optimum photoyield proves that two oxides of cesium exist in high-photoyield surfaces, and not Cs2O alone as previously thought. From the shape and position of the cesium peaks and the Auger parameter, the assignment of the O1s peaks at 527.5- and 531.5-eV binding energies to oxygen in Cs2O and Cs11O3, respectively, can be made. Hence the total cesium-oxygen layer is a mixed phase consisting of Cs2O + Cs11O3, approximately 20-40 A thick.

  17. The effect of Sr and Bi on the Si(100) surface oxidation - Auger electron spectroscopy, low energy electron diffraction, and X-ray photoelectron spectroscopy study

    NASA Technical Reports Server (NTRS)

    Fan, W. C.; Mesarwi, A.; Ignatiev, A.

    1990-01-01

    The effect of Sr and Bi on the oxidation of the Si(100) surface has been studied by Auger electron spectroscopy, low electron diffraction, and X-ray photoelectron spectroscopy. A dramatic enhancement, by a factor of 10, of the Si oxidation has been observed for Si(100) with a Sr overlayer. The SR-enhanced Si oxidation has been studied as a function of O2 exposure and Sr coverage. In contrast to the oxidation promotion of Sr on Si, it has been also observed that a Bi overlayer on Si(100) reduced Si oxidation significantly. Sr adsorption on the Si(100) with a Bi overlayer enhances Si oxidation only at Sr coverage of greater than 0.3 ML.

  18. Structure, Mobility, and Composition of Transition Metal Catalyst Surfaces. High-Pressure Scanning Tunneling Microscopy and Ambient-Pressure X-ray Photoelectron Spectroscopy Studies

    SciTech Connect

    Zhu, Zhongwei

    2013-12-06

    Surface structure, mobility, and composition of transition metal catalysts were studied by high-pressure scanning tunneling microscopy (HP-STM) and ambient-pressure X-ray photoelectron spectroscopy (AP-XPS) at high gas pressures. HP-STM makes it possible to determine the atomic or molecular rearrangement at catalyst surfaces, particularly at the low-coordinated active surface sites. AP-XPS monitors changes in elemental composition and chemical states of catalysts in response to variations in gas environments. Stepped Pt and Cu single crystals, the hexagonally reconstructed Pt(100) single crystal, and Pt-based bimetallic nanoparticles with controlled size, shape and composition, were employed as the model catalysts for experiments in this thesis.

  19. Elucidating the electronic structure of supported gold nanoparticles and its relevance to catalysis by means of hard X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Reinecke, Benjamin N.; Kuhl, Kendra P.; Ogasawara, Hirohito; Li, Lin; Voss, Johannes; Abild-Pedersen, Frank; Nilsson, Anders; Jaramillo, Thomas F.

    2016-08-01

    We report on the electronic structure of Au (gold) nanoparticles supported onto TiO2 with a goal of elucidating the most important effects that contribute to their high catalytic activity. We synthesize and characterize with high resolution transmission electron microscopy (HRTEM) 3.4, 5.3, and 9.5 nm diameter TiO2-supported Au nanoparticles with nearly spherical shape and measure their valence band using Au 5d subshell sensitive hard X-ray photoelectron spectroscopy (HAXPES) conducted at Spring-8. Based on density functional theory (DFT) calculations of various Au surface structures, we interpret the observed changes in the Au 5d valence band structure as a function of size in terms of an increasing percentage of Au atoms at corners/edges for decreasing particle size. This work elucidates how Au coordination number impacts the electronic structure of Au nanoparticles, ultimately giving rise to their well-known catalytic activity.

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

    NASA Astrophysics Data System (ADS)

    Imam, H.; Ahmed, Doaa; Eldakrouri, Ashraf

    2013-06-01

    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.

  1. X-ray photoelectron spectroscopy characterization of a nonsuperconducting Y-Ba-Cu-O superconductor-normal-metal-superconductor barrier material

    NASA Technical Reports Server (NTRS)

    Vasquez, R. P.; Hunt, B. D.; Foote, M. C.; Bajuk, L. J.

    1992-01-01

    A film of a novel nonsuperconducting Y-Ba-Cu-O (YBCO) barrier material was grown using conditions similar to those reported by Agostinelli et al. (1991) for forming a cubic semiconducting (c-YBCO) phase, and the material was characterized using X-ray photoelectron spectroscopy (XPS). A comparison of the XPS spectra of this material to those obtained from the orthorhombic and tetragonal phases of YBCO (o-YBCO and t-YBCO, respectively) showed that the barrier material had spectral characteristics different from those of o-YBCO and t-YBCO, particularly in the O 1s region. Features associated with the Cu-O chain and surface-reconstructed Cu-O planes were absent, consistent with expectations for the simple perovskite crystal structure of c-YBCO proposed by Agostinelli et al.

  2. Ammonia plasma treated polyethylene films for adsorption or covalent immobilization of trypsin: quantitative correlation between X-ray photoelectron spectroscopy data and enzyme activity.

    PubMed

    Ghasemi, Mahsa; Minier, Michel J G; Tatoulian, Michaël; Chehimi, Mohamed M; Arefi-Khonsari, Farzaneh

    2011-09-01

    The ammonia plasma process was used for generating reactive groups, particularly primary amine functions on the surface of polyethylene (PE) films, to immobilize the enzyme trypsin. The attachment of the enzyme was achieved by directly applying an aqueous solution of trypsin to the plasma-activated surface or by using glutaraldehyde as a chemical linker. In both cases, the utilization of sodium cyanoborohydride efficiently stabilized the immobilization. The surfaces were analyzed by X-ray photoelectron spectroscopy (XPS) and enzymatic activity measurements. Active trypsin was successfully immobilized on the surface with a mean activity of 0.09 ± 0.02 U/cm(2). The study of the stability of the immobilized enzyme during repetitive assays showed that some activity could be maintained during several months. An original quantitative correlation between the immobilized enzyme activity and the XPS signal intensity of the S 2p electrons present in the sulfur-containing amino acid residues was evidenced. PMID:21770448

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

    SciTech Connect

    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.

  4. Electronic structure of ZnO nanorods studied by angle-dependent x-ray absorption spectroscopy and scanning photoelectron microscopy

    NASA Astrophysics Data System (ADS)

    Chiou, J. W.; Jan, J. C.; Tsai, H. M.; Bao, C. W.; Pong, W. F.; Tsai, M.-H.; Hong, I.-H.; Klauser, R.; Lee, J. F.; Wu, J. J.; Liu, S. C.

    2004-05-01

    Angle-dependent x-ray absorption near-edge structure (XANES) and scanning photoelectron microscopy measurements were performed to differentiate local electronic structures at the tips and sidewalls of highly aligned ZnO nanorods. The overall intensity of the O K-edge XANES spectra is greatly enhanced for small photon incident angles. In contrast, the overall intensity of the Zn K-edge XANES is much less sensitive to the photon incident angle. Both valence-band photoemission and O K-edge XANES spectra show substantial enhancement of O 2p derived states near the valence band maximum and conduction band minimum, respectively. The spatially resolved Zn 3d core level spectra from tip and sidewall regions show the lack of chemical shift. All the results consistently suggest that the tip surfaces of the highly aligned ZnO nanorods are terminated by O ions and the nanorods are oriented in the [0001¯] direction.

  5. Kinetic study of GeO disproportionation into a GeO{sub 2}/Ge system using x-ray photoelectron spectroscopy

    SciTech Connect

    Wang Shengkai; Liu Honggang; Toriumi, Akira

    2012-08-06

    GeO disproportionation into GeO{sub 2} and Ge is studied through x-ray photoelectron spectroscopy. Direct evidence for the reaction 2GeO {yields} GeO{sub 2} + Ge after annealing in ultra-high vacuum is presented. Activation energy for GeO disproportionation is found to be about 0.7 {+-} 0.2 eV through kinetic and thermodynamic calculations. A kinetic model of GeO disproportionation is established by considering oxygen transfer in the GeO network. The relationship between GeO disproportionation and GeO desorption induced by GeO{sub 2}/Ge interfacial reaction is discussed, and the apparent contradiction between GeO desorption via interfacial redox reaction and GeO disproportionation into Ge and GeO{sub 2} is explained by considering the oxygen vacancy.

  6. Investigations on surface chemical analysis using X-ray photoelectron spectroscopy and optical properties of Dy3+-doped LiNa3P2O7 phosphor

    NASA Astrophysics Data System (ADS)

    Munirathnam, K.; Dillip, G. R.; Chaurasia, Shivanand; Joo, S. W.; Deva Prasad Raju, B.; John Sushma, N.

    2016-08-01

    Near white-light emitting LiNa3P2O7:Dy3+ phosphors were prepared by a conventional solid-state reaction method. The orthorhombic crystal structure of the phosphors was confirmed using X-ray diffraction (XRD), and the valence states of the surface elements were determined from the binding energies of Li 1s, O 1s, Na 1s, P 2p, and Dy 3d by X-ray photoelectron spectroscopy (XPS). Attenuated total reflectance (ATR) - Fourier transform infrared (FT-IR) spectroscopy was employed to identify the pyrophosphate groups in the phosphors. Diffuse reflectance spectra (DRS) show the absorption bands of the Dy3+ ions in the host material. Intense blue (481 nm) and yellow (575 nm) emissions were obtained at an excitation wavelength of 351 nm and are attributed to the 4F9/2 → 6H15/2 and 4F9/2 → 6H13/2 transitions of Dy3+ ions, respectively. The combination of these two intense bands generates light emission in the near-white region of the chromaticity diagram.

  7. Analysis of bi-layer oxide on austenitic stainless steel, 316L, exposed to Lead-Bismuth Eutectic (LBE) by X-ray Photoelectron Spectroscopy (XPS)

    NASA Astrophysics Data System (ADS)

    Koury, D.; Johnson, A. L.; Ho, T.; Farley, J. W.

    2013-09-01

    Corrosion of the austenitic stainless steel alloy 316L by Lead-Bismuth Eutectic (LBE) was studied using X-ray Photoelectron Spectroscopy (XPS) with Sputter-Depth Profiling (SDP), and compared to data taken by Scanning Electron Microscopy (SEM) and Energy Dispersive X-rays (EDXs). Exposed and unexposed samples were compared. Annealed 316L samples, exposed to LBE for durations of 1000, 2000 and 3000 h, developed bi-layer oxides up to 30 μm thick. Analysis of the charge-states of the 2p3/2 peaks of iron, chromium, and nickel in the oxide layers reveal an inner layer consisting of iron and chromium oxides (likely spinel-structured) and an outer layer consisting of iron oxides (Fe3O4). Cold-rolled 316L samples, exposed for the same durations, form a chromium-rich, thin (⩽1 μm) oxide with some oxidized iron in the outermost ˜200 nm of the oxide layer. This is the first experiment to investigate what components of the 316L are oxidized by LBE exposure. It is shown here that nickel is metallic in the inner layer.

  8. X-ray photoelectron spectroscopy analysis of TlInGaAsN semiconductor system and their annealing-induced structural changes

    SciTech Connect

    Kim, Kang Min; Kim, Woo-Byoung; Krishnamurthy, Daivasigamani; Ishimaru, Manabu; Kobayashi, Hikaru; Hasegawa, Shigehiko; Asahi, Hajime

    2010-12-15

    TlInGaAsN thin films grown by gas-source molecular-beam epitaxy were investigated by x-ray photoelectron spectroscopy (XPS) to analyze the Tl incorporation and to study the annealing-induced transformation of the atomic configurations. XPS analysis revealed that the Tl composition in the grown TlInGaAsN is around 1.5% and that the dominant atomic configuration of the TlInGaAsN changes from the In-As and Ga-N bonds to the In-N and Ga-As bonds by 700 deg. C rapid thermal annealing. High-resolution x-ray diffraction and reciprocal space mapping measurements showed that no significant out-diffusion of the elements occurs in the TlInGaAsN/TlGaAsN quantum wells (QWs) even after the same annealing. It is concluded that the blueshift in the photoluminescence peak for the TlInGaAsN/TlGaAsN QWs after annealing is attributed to the transformation of the atomic configuration in TlInGaAsN.

  9. Energy-Dispersive X-Ray Fluorescence Spectrometry: A Long Overdue Addition to the Chemistry Curriculum

    ERIC Educational Resources Information Center

    Palmer, Peter T.

    2011-01-01

    Portable Energy-Dispersive X-Ray Fluorescence (XRF) analyzers have undergone significant improvements over the past decade. Salient advantages of XRF for elemental analysis include minimal sample preparation, multielement analysis capabilities, detection limits in the low parts per million (ppm) range, and analysis times on the order of 1 min.…

  10. Interaction of bovine serum albumin and lysozyme with stainless steel studied by time-of-flight secondary ion mass spectrometry and X-ray photoelectron spectroscopy.

    PubMed

    Hedberg, Yolanda S; Killian, Manuela S; Blomberg, Eva; Virtanen, Sannakaisa; Schmuki, Patrik; Odnevall Wallinder, Inger

    2012-11-27

    An in-depth mechanistic understanding of the interaction between stainless steel surfaces and proteins is essential from a corrosion and protein-induced metal release perspective when stainless steel is used in surgical implants and in food applications. The interaction between lysozyme (LSZ) from chicken egg white and bovine serum albumin (BSA) and AISI 316L stainless steel surfaces was studied ex situ by means of X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS) after different adsorption time periods (0.5, 24, and 168 h). The effect of XPS measurements, storage (aging), sodium dodecyl sulfate (SDS), and elevated temperature (up to 200 °C) on the protein layers, as well as changes in surface oxide composition, were investigated. Both BSA and LSZ adsorption induced an enrichment of chromium in the oxide layer. BSA induced significant changes to the entire oxide, while LSZ only induced a depletion of iron at the utmost layer. SDS was not able to remove preadsorbed proteins completely, despite its high concentration and relatively long treatment time (up to 36.5 h), but induced partial denaturation of the protein coatings. High-temperature treatment (200 °C) and XPS exposure (X-ray irradiation and/or photoelectron emission) induced significant denaturation of both proteins. The heating treatment up to 200 °C removed some proteins, far from all. Amino acid fragment intensities determined from ToF-SIMS are discussed in terms of significant differences with adsorption time, between the proteins, and between freshly adsorbed and aged samples. Stainless steel-protein interactions were shown to be strong and protein-dependent. The findings assist in the understanding of previous studies of metal release and surface changes upon exposure to similar protein solutions. PMID:23116183

  11. Correlations Between Variations in Solar EUV and Soft X-Ray Irradiance and Photoelectron Energy Spectra Observed on Mars and Earth

    NASA Technical Reports Server (NTRS)

    Peterson, W. K.; Brain, D. A.; Mitchell, D. L.; Bailey, S. M.; Chamberlin, P. C.

    2013-01-01

    Solar extreme ultraviolet (EUV; 10-120 nm) and soft X-ray (XUV; 0-10 nm) radiation are major heat sources for the Mars thermosphere as well as the primary source of ionization that creates the ionosphere. In investigations of Mars thermospheric chemistry and dynamics, solar irradiance models are used to account for variations in this radiation. Because of limited proxies, irradiance models do a poor job of tracking the significant variations in irradiance intensity in the EUV and XUV ranges over solar rotation time scales when the Mars-Sun-Earth angle is large. Recent results from Earth observations show that variations in photoelectron energy spectra are useful monitors of EUV and XUV irradiance variability. Here we investigate photoelectron energy spectra observed by the Mars Global Surveyor (MGS) Electron Reflectometer (ER) and the FAST satellite during the interval in 2005 when Earth, Mars, and the Sun were aligned. The Earth photoelectron data in selected bands correlate well with calculations based on 1 nm resolution observations above 27 nm supplemented by broadband observations and a solar model in the 0-27 nm range. At Mars, we find that instrumental and orbital limitations to the identifications of photoelectron energy spectra in MGS/ER data preclude their use as a monitor of solar EUV and XUV variability. However, observations with higher temporal and energy resolution obtained at lower altitudes on Mars might allow the separation of the solar wind and ionospheric components of electron energy spectra so that they could be used as reliable monitors of variations in solar EUV and XUV irradiance than the time shifted, Earth-based, F(10.7) index currently used.

  12. Correlations between variations in solar EUV and soft X-ray irradiance and photoelectron energy spectra observed on Mars and Earth

    NASA Astrophysics Data System (ADS)

    Peterson, W. K.; Brain, D. A.; Mitchell, D. L.; Bailey, S. M.; Chamberlin, P. C.

    2013-11-01

    extreme ultraviolet (EUV; 10-120 nm) and soft X-ray (XUV; 0-10 nm) radiation are major heat sources for the Mars thermosphere as well as the primary source of ionization that creates the ionosphere. In investigations of Mars thermospheric chemistry and dynamics, solar irradiance models are used to account for variations in this radiation. Because of limited proxies, irradiance models do a poor job of tracking the significant variations in irradiance intensity in the EUV and XUV ranges over solar rotation time scales when the Mars-Sun-Earth angle is large. Recent results from Earth observations show that variations in photoelectron energy spectra are useful monitors of EUV and XUV irradiance variability. Here we investigate photoelectron energy spectra observed by the Mars Global Surveyor (MGS) Electron Reflectometer (ER) and the FAST satellite during the interval in 2005 when Earth, Mars, and the Sun were aligned. The Earth photoelectron data in selected bands correlate well with calculations based on 1 nm resolution observations above 27 nm supplemented by broadband observations and a solar model in the 0-27 nm range. At Mars, we find that instrumental and orbital limitations to the identifications of photoelectron energy spectra in MGS/ER data preclude their use as a monitor of solar EUV and XUV variability. However, observations with higher temporal and energy resolution obtained at lower altitudes on Mars might allow the separation of the solar wind and ionospheric components of electron energy spectra so that they could be used as reliable monitors of variations in solar EUV and XUV irradiance than the time shifted, Earth-based, F10.7 index currently used.

  13. X-Ray Photoelectron and Anger Electron Spectroscopic Studies of Chemical Shifts in Amorphous Ge-Se System

    NASA Astrophysics Data System (ADS)

    Ueno, Tokihiro

    1983-09-01

    The chemical shifts of the Ge 3d, 3p3/2,1/2 and Se 3d, 3p3/2,1/2 photoelectron lines were measured for the amorphous Ge-Se system and those of the Ge photoelectron lines are corrected for Auger parameter shifts. According to the valence shell potential model, the ratio of the chemical shift in the amorphous Ge-Se system to that in stoichiometric GeSe2 can be approximated by the ratio of the Ge-Se bond number in the Ge-Se system to that in GeSe2. The chemical shift ratios evaluated from the experimental results reveal bond structures at non-stoichiometric compositions. In the excess-Ge range, GeSe is composed of atomic clusters of three-fold co-ordinated Ge and Se atoms, and Ge2Se3 contains atomic clusters of Se3Ge-GeSe3 units. In the excess-Se range, GeSe3 includes GeSe4 tetrahedral units, and Se-Se chains and/or Se8 rings.

  14. Direct observation of bias-dependence potential distribution in metal/HfO{sub 2} gate stack structures by hard x-ray photoelectron spectroscopy under device operation

    SciTech Connect

    Yamashita, Y.; Yoshikawa, H.; Kobayashi, K.; Chikyo, T.

    2014-01-28

    Although gate stack structures with high-k materials have been extensively investigated, there are some issues to be solved for the formation of high quality gate stack structures. In the present study, we employed hard x-ray photoelectron spectroscopy in operating devices. This method allows us to investigate bias dependent electronic states, while keeping device structures intact. Using this method, we have investigated electronic states and potential distribution in gate metal/HfO{sub 2} gate stack structures under device operation. Analysis of the core levels shifts as a function of the bias voltage indicated that a potential drop occurred at the Pt/HfO{sub 2} interface for a Pt/HfO{sub 2} gate structure, while a potential gradient was not observed at the Ru/HfO{sub 2} interface for a Ru/HfO{sub 2} gate structure. Angle resolved photoelectron spectroscopy revealed that a thicker SiO{sub 2} layer was formed at the Pt/HfO{sub 2} interface, indicating that the origin of potential drop at Pt/HfO{sub 2} interface is formation of the thick SiO{sub 2} layer at the interface. The formation of the thick SiO{sub 2} layer at the metal/high-k interface might concern the Fermi level pinning, which is observed in metal/high-k gate stack structures.

  15. Operando x-ray photoelectron emission microscopy for studying forward and reverse biased silicon p-n junctions.

    PubMed

    Barrett, N; Gottlob, D M; Mathieu, C; Lubin, C; Passicousset, J; Renault, O; Martinez, E

    2016-05-01

    Significant progress in the understanding of surfaces and interfaces of materials for new technologies requires operando studies, i.e., measurement of chemical, electronic, and magnetic properties under external stimulus (such as mechanical strain, optical illumination, or electric fields) applied in situ in order to approach real operating conditions. Electron microscopy attracts much interest, thanks to its ability to determine semiconductor doping at various scales in devices. Spectroscopic photoelectron emission microscopy (PEEM) is particularly powerful since it combines high spatial and energy resolution, allowing a comprehensive analysis of local work function, chemistry, and electronic structure using secondary, core level, and valence band electrons, respectively. Here we present the first operando spectroscopic PEEM study of a planar Si p-n junction under forward and reverse bias. The method can be used to characterize a vast range of materials at near device scales such as resistive oxides, conducting bridge memories and domain wall arrays in ferroelectrics photovoltaic devices. PMID:27250431

  16. Operando x-ray photoelectron emission microscopy for studying forward and reverse biased silicon p-n junctions

    NASA Astrophysics Data System (ADS)

    Barrett, N.; Gottlob, D. M.; Mathieu, C.; Lubin, C.; Passicousset, J.; Renault, O.; Martinez, E.

    2016-05-01

    Significant progress in the understanding of surfaces and interfaces of materials for new technologies requires operando studies, i.e., measurement of chemical, electronic, and magnetic properties under external stimulus (such as mechanical strain, optical illumination, or electric fields) applied in situ in order to approach real operating conditions. Electron microscopy attracts much interest, thanks to its ability to determine semiconductor doping at various scales in devices. Spectroscopic photoelectron emission microscopy (PEEM) is particularly powerful since it combines high spatial and energy resolution, allowing a comprehensive analysis of local work function, chemistry, and electronic structure using secondary, core level, and valence band electrons, respectively. Here we present the first operando spectroscopic PEEM study of a planar Si p-n junction under forward and reverse bias. The method can be used to characterize a vast range of materials at near device scales such as resistive oxides, conducting bridge memories and domain wall arrays in ferroelectrics photovoltaic devices.

  17. Hard X-ray Standing-Wave Photoelectron Spectroscopy Study of Cobalt-Iron-Boron/Magnesium Oxide Magnetic Tunnel Junction Multilayers

    NASA Astrophysics Data System (ADS)

    Greer, Albert Anthony

    As one key aspect of the area of spin-based electronics or spintronics, the magnetic tunnel junction (MTJ) holds special promise for magnetic memory, and possibly also logic devices. In an MTJ, two ferromagnetic layers are separated by a very thin nonmagnetic insulating layer and the key effect is based on the spin-dependent tunneling of electrons through the insulating layer and is called tunnel magnetoresistance (TMR). Resistance is lower when the two ferromagnetic layers are oriented parallel to one another, and higher when they are anti-parallel. Recent work reveals that MTJs with a Ta/CoFeB/MgO/CoFeB/Ta structure show three optimal characteristics: 1) high thermal stability on the nanoscale, 2) a high TMR ratio, and 3) low switching current for current-induced switching of magnetization across the interface. Studies suggest that B diffusion from the initially amorphous CoFeB layer into the MgO causes CoFeB crystallization such that TMR-increasing perpendicular anisotropy (PMA) arises at the MgO/CoFeB interface. Furthermore, the TMR ratio is likewise regulated by B diffusion into the Ta layer. Scientists are currently exploring the structure/properties relationships of these buried interfaces in magnetic nanostructures. One effective method for probing the composition, structure, and properties of buried layers is the newly-developed technique of standing-wave, hard x-ray photoelectron spectroscopy or SW-HAXPES. In this method, a standing wave is generated by Bragg reflection from a synthetic multilayer mirror upon which the sample is deposited. This standing wave can be scanned vertically through the sample by varying the incidence angle around the Bragg angle, giving a rocking curve (RC) scan. Using SW-HAXPES, we studied the B distribution in a Ta/Co0.2Fe0.6B0.2/MgO sample. We obtained hard x-ray standing-wave data, as well as conventional variable takeoff angle XPS (angle-resolved XPS or ARXPS) data at SPring-8 in Japan, as well as complimentary soft x-ray

  18. A study of reversible gamma-induced structural transformations in vitreous Ge23.5Sb11.8S64.7 by high-resolution X-ray photoelectron spectroscopy.

    PubMed

    Kovalskiy, Andriy; Jain, Himanshu; Miller, Alfred C; Golovchak, Roman Ya; Shpotyuk, Oleh I

    2006-11-16

    The structural origin of reversible gamma-induced effects in vitreous Ge(23.5)Sb(11.8)S(64.7) has been investigated by high-resolution X-ray photoelectron spectroscopy (XPS). The changes in valence band spectrum from gamma-irradiation suggest a decrease of sulfur lone pair electron concentration accompanied by changes in bonding states of S and Ge. The appearance of additional doublets in the core-level XPS spectra of Ge, Sb, and S atoms for gamma-irradiated sample is described by the formation of over- and under-coordinated charged defect pairs (Ge(3)(-)-S(3)(+)) as a result of radiation treatment. The results verify the switching of Ge-S covalent bonds into S-S bonds as the main microstructural mechanism for gamma-induced optical effects in this glass. PMID:17092046

  19. Cation distribution in co-doped ZnAl2O4 nanoparticles studied by X-ray photoelectron spectroscopy and 27Al solid-state NMR spectroscopy.

    PubMed

    Duan, Xiulan; Yuan, Duorong; Yu, Fapeng

    2011-06-20

    Co(x)Zn(1-x)Al(2)O(4) (x = 0.01-0.6) nanoparticles were synthesized by the citrate sol-gel method and were characterized by X-ray powder diffraction and transmission electron microscopy to identify the crystalline phase and determine the particle size. X-ray photoelectron spectroscopy and (27)Al solid-state NMR spectroscopy were used to study the distribution of the cations in the tetrahedral and octahedral sites in Co(x)Zn(1-x)Al(2)O(4) nanoparticles as a function of particle size and composition. The results show that all of the as-synthesized samples exhibit spinel-type single phase; the crystallite size of the samples is about 20-50 nm and increases with increasing annealing temperature and decreases with Co-enrichment. Zn(2+) ions are located in large proportions in the tetrahedral sites and in small proportions in the octahedral sites in Co(x)Zn(1-x)Al(2)O(4) nanoparticles. The fraction of octahedral Zn(2+) increases with increasing Co concentration and decreases with increasing particle size. Besides the tetrahedral and octahedral coordinations, the presence of the second octahedrally coordinated Al(3+) ions is observed in the nanoparticles. The change of the inversion parameter (2 times the fraction of Al(3+) ions in tetrahedral sites) with Co concentration and particle size is consistent with that of the Zn fraction in octahedral sites. Analysis of the absorption properties indicates that Co(2+) ions are located in the tetrahedral sites as well as in the octahedral sites in the nanoparticles. The inversion degree of Co(2+) decreases with increasing particle size. PMID:21612229

  20. Band alignment of atomic layer deposited MgO/Zn0.8Al0.2O heterointerface determined by charge corrected X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Yan, Baojun; Liu, Shulin; Yang, Yuzhen; Heng, Yuekun

    2016-05-01

    Pure magnesium (MgO) and zinc oxide doped with aluminum oxide (Zn0.8Al0.2O) were prepared via atomic layer deposition. We have studied the structure and band gap of bulk Zn0.8Al0.2O material by X-ray diffractometer (XRD) and Tauc method, and the band offsets and alignment of atomic layer deposited MgO/Zn0.8Al0.2O heterointerface were investigated systematically using X-ray photoelectron spectroscopy (XPS) in this study. Different methodologies, such as neutralizing electron gun, the use of C 1s peak recalibration and zero charging method, were applied to recover the actual position of the core levels in insulator materials which were easily influenced by differential charging phenomena. Schematic band alignment diagram, valence band offset (ΔEV) and conduction band offset (ΔEC) for the interface of the MgO/Zn0.8Al0.2O heterostructure have been constructed. An accurate value of ΔEV = 0.72 ± 0.11 eV was obtained from various combinations of core levels of heterojunction with varied MgO thickness. Given the experimental band gaps of 7.83 eV for MgO and 5.29 eV for Zn0.8Al0.2O, a type-II heterojunction with a ΔEC of 3.26 ± 0.11 eV was found. Band offsets and alignment studies of these heterojunctions are important for gaining deep consideration to the design of various optoelectronic devices based on such heterointerface.

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

    SciTech Connect

    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

  2. Addition of missing loops and domains to protein models by x-ray solution scattering.

    PubMed Central

    Petoukhov, Maxim V; Eady, Nigel A J; Brown, Katherine A; Svergun, Dmitri I

    2002-01-01

    Inherent flexibility and conformational heterogeneity in proteins can often result in the absence of loops and even entire domains in structures determined by x-ray crystallographic or NMR methods. X-ray solution scattering offers the possibility of obtaining complementary information regarding the structures of these disordered protein regions. Methods are presented for adding missing loops or domains by fixing a known structure and building the unknown regions to fit the experimental scattering data obtained from the entire particle. Simulated annealing was used to minimize a scoring function containing the discrepancy between the experimental and calculated patterns and the relevant penalty terms. In low-resolution models where interface location between known and unknown parts is not available, a gas of dummy residues represents the missing domain. In high-resolution models where the interface is known, loops or domains are represented as interconnected chains (or ensembles of residues with spring forces between the C(alpha) atoms), attached to known position(s) in the available structure. Native-like folds of missing fragments can be obtained by imposing residue-specific constraints. After validation in simulated examples, the methods have been applied to add missing loops or domains to several proteins where partial structures were available. PMID:12496082

  3. X-ray photoelectron diffraction study of thin Cu films grown on clean Ru(0001) and O-precovered Ru(0001)

    NASA Astrophysics Data System (ADS)

    Ruebush, S. D.; Couch, R. E.; Thevuthasan, S.; Fadley, C. S.

    1999-02-01

    We have studied the epitaxial growth modes and near-surface interlayer relaxation of thin Cu films on Ru(0001) using X-ray photoelectron diffraction (XPD), measuring experimental Cu 2p 3/2 ( Ekin=556 eV) and Ru 3d ( Ekin=1206 eV) intensities over one-third of the nearly full 2 π solid angle above the surface for Cu coverages from submonolayer up to 40 monolayers. Reference Cu 2p 3/2 data for a clean Cu(111) surface have also been obtained from Naumović et al. and in our laboratory. These data have been compared to single scattering cluster (SSC) and more accurate multiple scattering cluster (MSC) calculations via a sum of five R-factors to derive precise structural information. MSC calculations are found to give a more accurate description for layers of ≥4 ML thickness, and comparisons of experiment and theory are also improved by allowing more accurately for the effective degree of angular averaging involved. Calculations for thicker layers are also found to converge by ˜5 ML. Our analysis indicates that the first Cu layer grows pseudomorphically on Ru(0001), in agreement with prior studies. An R-factor analysis comparing MSC and SSC calculations to experimental results further indicates that the Cu-Ru interlayer spacing at 1 monolayer (ML) is about 2.15 Å, in excellent agreement with prior low-energy ion scattering (LEIS) and low-energy electron diffraction (LEED) experimental studies, as well as with prior linearized augmented plane-wave (LAPW) calculations. At higher coverages, comparison of our data to SSC and MSC calculations for various atomic clusters indicates that the short-range structure is fcc Cu(111)-like, but with significant interlayer contraction which persists up to ≥5 ML coverage. Prior STM work by Behm et al. has shown a series of misfit dislocation structures in the top layer of the Cu film at higher coverages from 2 to 4 ML. Our data indicate that these misfit dislocation structures thread to the Cu/Ru interface rather than occurring

  4. Measurement of valence-band offset at native oxide/BaSi2 interfaces by hard x-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Takabe, Ryota; Du, Weijie; Ito, Keita; Takeuchi, Hiroki; Toko, Kaoru; Ueda, Shigenori; Kimura, Akio; Suemasu, Takashi

    2016-01-01

    Undoped n-type BaSi2 films were grown on Si(111) by molecular beam epitaxy, and the valence band (VB) offset at the interface between the BaSi2 and its native oxide was measured by hard x-ray photoelectron spectroscopy (HAXPES) at room temperature. HAXPES enabled us to investigate the electronic states of the buried BaSi2 layer non-destructively thanks to its large analysis depth. We performed the depth-analysis by varying the take-off angle (TOA) of photoelectrons as 15°, 30°, and 90° with respect to the sample surface and succeeded to obtain the VB spectra of the BaSi2 and the native oxide separately. The VB maximum was located at -1.0 eV from the Fermi energy for the BaSi2 and -4.9 eV for the native oxide. We found that the band bending did not occur near the native oxide/BaSi2 interface. This result was clarified by the fact that the core-level emission peaks did not shift regardless of TOA (i.e., analysis depth). Thus, the barrier height of the native oxide for the minority-carriers in the undoped n-BaSi2 (holes) was determined to be 3.9 eV. No band bending in the BaSi2 close to the interface also suggests that the large minority-carrier lifetime in undoped n-BaSi2 films capped with native oxide is attributed not to the band bending in the BaSi2, which pushes away photogenerated minority carriers from the defective surface region, but to the decrease of defective states by the native oxide.

  5. Synchrotron X-ray CT characterization of titanium parts fabricated by additive manufacturing. Part II. Defects.

    PubMed

    Scarlett, Nicola Vivienne Yorke; Tyson, Peter; Fraser, Darren; Mayo, Sheridan; Maksimenko, Anton

    2016-07-01

    Synchrotron X-ray tomography (SXRT) has been applied to the study of defects within three-dimensional printed titanium parts. These parts were made using the Arcam EBM(®) (electron beam melting) process which uses powdered titanium alloy, Ti64 (Ti alloy with approximately 6%Al and 4%V) as the feed and an electron beam for the sintering/welding. The experiment was conducted on the Imaging and Medical Beamline of the Australian Synchrotron. The samples represent a selection of complex shapes with a variety of internal morphologies. Inspection via SXRT has revealed a number of defects which may not otherwise have been seen. The location and nature of such defects combined with detailed knowledge of the process conditions can contribute to understanding the interplay between design and manufacturing strategy. This fundamental understanding may subsequently be incorporated into process modelling, prediction of properties and the development of robust methodologies for the production of defect-free parts. PMID:27359151

  6. Atomic scale structure of the 5-fold surface of an AlPdMn quasicrystal: A quantitative X-Ray photoelectron diffraction analysis

    SciTech Connect

    Zheng, Jin-Cheng; Huan, C.H.A.; Wee, A.T.S.; Van Hove, M.A.; Fadley, C.S.; Shi, F.J.; Rotenberg, E.; Barman, S.R.; Paggel, J.J.; Horn, K.; Ebert, Ph.; Urban, K.

    2004-02-11

    The atomic scale structure of the 5-fold symmetric surface of an AlPdMn quasicrystal is investigated quantitatively by comparing x-ray photoelectron diffraction (XPD) simulations to experiment. The observed 5-fold symmetry of the diffraction patterns indicates that the surface is quasicrystalline with no hint of a reconstruction from the bulk structure. In analyzing the experimental data, many possible bulk terminations have been tested. Those few that fit best to the data have in common that they contain an Al-rich surface layer followed by a dense mixed Al/Pd/Mn layer. These best terminations, while not identical to each other, are suggested to form terraces coexisting on a real surface. Structural relaxations of the quasicrystal surface are also analyzed: mixing several best-fit terminations gives average best-fit interlayer spacing changes of Dd12 = -0.057 Angstrom, Dd24 = +0.159 Angstrom. These results are in good agreement with a prior structure determination by LEED on a sample that was prepared in a different manner.

  7. A promising concept for using near-surface measuring angles in angle-resolved x-ray photoelectron spectroscopy considering elastic scattering effects

    SciTech Connect

    Oswald, S.; Oswald, F.

    2011-02-01

    The increasing number of applications of very thin films requires both reliable thin-layer and interface characterization. A powerful method for characterization in the nanometer thickness range is the angle-resolved x-ray photoelectron spectroscopy (ARXPS). This is a nondestructive depth-profiling method, which can provide elemental content as well as chemical information. Two of the drawbacks of ARXPS are, that it requires dedicated mathematical modeling and that, at least up until now, its use has been restricted away from near-surface angles. In this paper we present a method for the mathematical description of a few, hitherto unaccounted, measurement effects in order to improve the simulations of ARXPS data for complex surface structures. As an immediate application, we propose a simple algorithm to consider the effects of elastic scattering in the standard ARXPS data interpretation, which in principle would allow the use of the whole angular range for the analysis; thus leading to a significant increase in the usable information content from the measurements. The potential of this approach is demonstrated with model calculations for a few thin film examples.

  8. A study of the O/Ag(111) system with scanning tunneling microscopy and x-ray photoelectron spectroscopy at ambient pressures

    NASA Astrophysics Data System (ADS)

    Heine, Christian; Eren, Baran; Lechner, Barbara A. J.; Salmeron, Miquel

    2016-10-01

    The interaction of O2 with the Ag(111) surface was studied with scanning tunneling microscopy (STM) in the pressure range from 10- 9 Torr to 1 atm at room temperature and with X-ray photoelectron spectroscopy (XPS) up to 0.3 Torr O2 in the temperature range from RT to 413 K. STM images show that the Ag(111) surface topography is little affected in regions with large flat terraces, except for the appearance of mobile features due to oxygen atoms at pressures above 0.01 Torr. In regions where the step density is high, the surface became rough under 0.01 Torr of O2, due to the local oxidation of Ag. Various chemical states of oxygen due to chemisorbed, oxide and subsurface species were identified by XPS as a function of pressure and temperature. The findings from the STM images and XPS measurements indicate that formation of an oxide phase, the thermodynamically stable form at room temperature under ambient O2 pressure, is kinetically hindered in the flat terrace areas but proceeds readily in regions with high-step density.

  9. Distinct and dramatic water dissociation on GaP(111) tracked by near-ambient pressure X-ray photoelectron spectroscopy.

    PubMed

    Zhang, Xueqiang; Ptasinska, Sylwia

    2015-02-01

    Water adsorption and dissociation on a GaP(111) crystal surface are investigated using near-ambient pressure X-ray photoelectron spectroscopy (NAP XPS) in a wide range of pressures (∼10(-10)-5 mbar) and temperatures (∼300-773 K). Dynamic changes in chemical evolution at the H2O/GaP(111) interface are reflected in Ga 2p3/2, O 1s, and P 2p spectra. In the pressure-dependent study performed at room temperature, an enhancement of surface Ga hydroxylation and oxidation with an increase in H2O pressure is observed. In the temperature-dependent study performed at elevated pressures, two distinct regions can be defined in which drastic changes occur in the surface chemistry. Below 673 K, the surface Ga hydroxylation and oxidation progress continuously. However, above 673 K, a large-scale conversion of surface O-Ga-OH species into non-stoichiometric Ga hydroxide along with oxidation of surface P atoms occurs through an intermediate state. The NAP XPS technique enabled us to experimentally track the chemistry at the H2O/GaP interface under near-realistic conditions, thereby providing evidence to compare with recent theoretical efforts to improve the understanding of water-splitting mechanisms and photo-corrosion on semiconductor surfaces. PMID:25559043

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

    PubMed

    Fears, T M; Doucet, M; Browning, J F; Baldwin, J K S; Winiarz, J G; Kaiser, H; Taub, H; Sacci, R L; Veith, G M

    2016-05-18

    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 × 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 were 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 suggests 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, which is required to remove the electrolyte residue prior to ex situ analysis, demonstrating the necessity of performing SEI characterization in situ. PMID:27149427

  11. An XPS study of the adherence of refractory carbide, silicide, and boride RF-sputtered wear-resistant coatings. [X-ray Photoelectron Spectroscopy of steel surfaces

    NASA Technical Reports Server (NTRS)

    Brainard, W. A.; Wheeler, D. R.

    1978-01-01

    Radio frequency sputtering was used to deposit refractory carbide, silicide, and boride coatings on 440-C steel substrates. Both sputter etched and pre-oxidized substrates were used and the films were deposited with and without a substrate bias. The composition of the coatings was determined as a function of depth by X-ray photoelectron spectroscopy combined with argon ion etching. Friction and wear tests were conducted to evaluate coating adherence. In the interfacial region there was evidence that bias may produce a graded interface for some compounds. Biasing, while generally improving bulk film stoichiometry, can adversely affect adherence by removing interfacial oxide layers. Oxides of all film constituents except carbon and iron were present in all cases but the iron oxide coverage was only complete on the preoxidized substrates. The film and iron oxides were mixed in the MoSi2 and Mo2C films but layered in the Mo2B5 films. In the case of mixed oxides, preoxidation enhanced film adherence. In the layered case it did not.

  12. Chemistry of L-proline on Pd(1 1 1): Temperature-programmed desorption and X-ray photoelectron spectroscopic study

    NASA Astrophysics Data System (ADS)

    Gao, Feng; Wang, Yilin; Burkholder, Luke; Tysoe, W. T.

    2007-09-01

    The surface chemistry of proline is explored on Pd(1 1 1) using a combination of temperature-programmed desorption (TPD) and X-ray photoelectron spectroscopy. Proline adsorbs on Pd(1 1 1) at temperatures of 250 K and below into second and subsequent layers prior to the saturation of the first layer, where approximately 70% of the adsorbed proline is present in its zwitterionic form. Molecular proline desorbs between ˜315 K and ˜333 K depending on coverage. When adsorbed at ˜300 K, only the first monolayer is formed, and the proline is present as zwitterions, oriented such that all of the carbons are detected equally by XPS. Proline decomposes by scission of the C-COO bond, where the carboxylate moiety desorbs as carbon monoxide and carbon dioxide, while the nitrogen-containing moiety desorbs as to HCN, and evolves pyrrole at ˜390 K, pyrrolidine at ˜410 K, and final species that desorbs at ˜450 K that cannot be unequivocally assigned but may be 2-butenenitrile (CH 3-CH dbnd CH-CN), 3-butenenitrile (CH 2dbnd CH-CH 2-CN), 2-methyl-2-propenenitrile (CH 2dbnd C(CH 3)-CN) or cyclopropanecarbonitrile.

  13. 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

    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.

  14. Voltage contrast X-ray photoelectron spectroscopy reveals graphene-substrate interaction in graphene devices fabricated on the C- and Si- faces of SiC

    SciTech Connect

    Aydogan, Pinar; Suzer, Sefik; Arslan, Engin; Cakmakyapan, Semih; Ozbay, Ekmel; Strupinski, Wlodek

    2015-09-21

    We report on an X-ray photoelectron spectroscopy (XPS) study of two graphene based devices that were analyzed by imposing a significant current under +3 V bias. The devices were fabricated as graphene layers(s) on hexagonal SiC substrates, either on the C- or Si-terminated faces. Position dependent potential distributions (IR-drop), as measured by variations in the binding energy of a C1s peak are observed to be sporadic for the C-face graphene sample, but very smooth for the Si-face one, although the latter is less conductive. We attribute these sporadic variations in the C-face device to the incomplete electrical decoupling between the graphene layer(s) with the underlying buffer and/or substrate layers. Variations in the Si2p and O1s peaks of the underlayer(s) shed further light into the electrical interaction between graphene and other layers. Since the potential variations are amplified only under applied bias (voltage-contrast), our methodology gives unique, chemically specific electrical information that is difficult to obtain by other techniques.

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

    DOE PAGESBeta

    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

  16. Structural investigation on Ge{sub x}Sb{sub 10}Se{sub 90−x} glasses using x-ray photoelectron spectra

    SciTech Connect

    Wei, Wen-Hou; Xiang, Shen; Xu, Si-Wei; Wang, Rong-Ping; Fang, Liang

    2014-05-14

    The structure of Ge{sub x}Sb{sub 10}Se{sub 90−x} glasses (x = 7.5, 10, 15, 20, 25, 27.5, 30, and 32.5 at. %) has been investigated by x-ray photoelectron spectroscopy (XPS). Different structural units have been extracted and characterized by decomposing XPS core level spectra, the evolution of the relative concentration of each structural unit indicates that, the relative contributions of Se-trimers and Se-Se-Ge(Sb) structure decrease with increasing Ge content until they become zero at chemically stoichiometric glasses of Ge{sub 25}Sb{sub 10}Se{sub 65}, and then the homopolar bonds like Ge-Ge and Sb-Sb begin to appear in the spectra. Increase of homopolar bonds will extend band-tails into the gap and narrow the optical band gap. Thus, the glass with a stoichiometric composition generally has fewer defective bonds and larger optical bandgap.

  17. Manganese nanoclusters and MnSi{sub {approx}1.7} nanowires formed on Si(110): A comparative x-ray photoelectron spectroscopy study

    SciTech Connect

    Zou Zhiqiang; Shi Gaoming; Liu Xiaoyong; Sun Limin

    2013-01-14

    The growth of Mn on a Si(110) surface at room temperature (RT) and 550 Degree-Sign C has been investigated by scanning tunneling spectroscopy (STM) and X-ray photoelectron spectroscopy (XPS). STM observation shows that the growth at 550 Degree-Sign C results in the formation of nanowires (NWs), while that at RT produces only nanoclusters. The Mn 2p XPS spectra unambiguously reveal that the NWs are composed of MnSi{sub {approx}1.7} and the nanoclusters are composed of Mn. Curve-fitting analysis of the spectra shows that 64.9% of the NWs were oxidized due to atmospheric exposure during sample transfer, while the Mn nanoclusters were completely oxidized under the same conditions. This fact indicates that the MnSi{sub {approx}1.7} NWs have better oxidation resistance than the Mn clusters, which can be attributed to the protection effect of the SiO{sub 2} layer formed on the NWs and the smaller surface to volume ratio of the NWs comparing with the clusters. The binding energy of Mn 2p for the NWs exhibits a negative shift of {approx}0.5 eV with respect to the Mn metallic state, which is similar to the silicide state of earlier transition metals Ti and Cr, but different from that of later transition metals Fe and Ni. This negative shift can be attributed to the contribution of Madelung potential.

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

    SciTech Connect

    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.

  19. Integrated X-ray photoelectron spectroscopy and DFT characterization of benzene adsorption on Pt(111), Pt(355) and Pt(322) surfaces.

    PubMed

    Zhang, Renqin; Hensley, Alyssa J; McEwen, Jean-Sabin; Wickert, Sandra; Darlatt, Erik; Fischer, Kristina; Schöppke, Matthias; Denecke, Reinhard; Streber, Regine; Lorenz, Michael; Papp, Christian; Steinrück, Hans-Peter

    2013-12-21

    We systematically investigate the adsorption of benzene on Pt(111), Pt(355) and Pt(322) surfaces by high-resolution X-ray photoelectron spectroscopy (XPS) and first-principle calculations based on density functional theory (DFT), including van der Waals corrections. By comparing the adsorption energies at 1/9, 1/16 and 1/25 ML on Pt(111), we find significant lateral interactions exist between the benzene molecules at 1/9 ML. The adsorption behavior on Pt(355) and Pt(322) is very different. While on Pt(355) a step species is clearly identified in the C 1s spectra at low coverages followed by occupation of a terrace species at high coverages, no evidence for a step species is found on Pt(322). These different adsorption sites are confirmed by extensive DFT calculations, where the most favorable adsorption configurations on Pt(355) and Pt(322) are also found to vary: a highly distorted across the step molecule is found on Pt(355) while a less distorted configuration adjacent to the step molecule is deduced for Pt(322). The theoretically proposed C 1s core level binding energy shifts between these most favorable configurations and the terrace species are found to correlate well with experiment: for Pt(355), two adsorbate states are found, separated by ~0.4 eV in XPS and 0.3 eV in the calculations, in contrast to only one state on Pt(322). PMID:24189500

  20. Structural origin of Si-2p core-level shifts from Si(100)-c[4x2] surface: A spectral x-ray photoelectron diffraction study

    SciTech Connect

    Chen, X.; Tonner, B.P.; Denlinger, J.

    1997-04-01

    The authors have performed angle-resolved x-ray photoelectron diffraction (XPD) from a Si(100)-c(4x2) surface to study the structural origin of Si-2p core-level shifts. In the experiment, the highly resolved surface Si-2p core-level spectra were measured as a fine grid of hemisphere and photon energies, using the SpectroMicroscopy Facility {open_quotes}ultraESCA{close_quotes} instrument. By carefully decomposing the spectra into several surface peaks, the authors are able to obtain surface-atom resolved XPD patterns. Using a multiple scattering analysis, they derived a detailed atomic model for the Si(100)-c(4x2) surface. In this model, the asymmetric dimers were found tilted by 11.5 plus/minus 2.0 degrees with bond length of 2.32 plus/minus 0.05{angstrom}. By matching model XPD patterns to experiment, the authors can identify which atoms in the reconstructed surface are responsible for specific photoemission lines in the 2p spectrum.

  1. Electronic and geometric properties of Au nanoparticles on Highly Ordered Pyrolytic Graphite (HOPG) studied using X-ray Photoelectron Spectroscopy (XPS) and Scanning Tunneling Microscopy (STM).

    PubMed

    Lopez-Salido, Ignacio; Lim, Dong Chan; Dietsche, Rainer; Bertram, Nils; Kim, Young Dok

    2006-01-26

    Au nanoparticles grown on mildly sputtered Highly Ordered Pyrolytic Graphite (HOPG) surfaces were studied using Scanning Tunneling Microscopy (STM) and X-ray Photoelectron Spectroscopy (XPS). The results were compared with those of Ag nanoparticles on the same substrate. By varying the defect densities of HOPG and the Au coverages, one can create Au nanoparticles in various sizes. At high Au coverages, the structures of the Au films significantly deviate from the ideal truncated octahedral form: the existence of many steps between different Au atomic layers can be observed, most likely due to a high activation barrier of the diffusion of Au atoms across the step edges. This implies that the particle growth at room temperature is strongly limited by kinetic factors. Hexagonal shapes of Au structures could be identified, indicating preferential growth of Au nanostructures along the (111) direction normal to the surface. In the case of Au, XPS studies reveal a weaker core level shift with decreasing particle size compared to the 3d level in similarly sized Ag particles. Also taking into account the Auger analysis of the Ag particles, the core level shifts of the metal nanoparticles on HOPG can be understood in terms of the metal/substrate charge transfer. Ag is (partially) positively charged, whereas Au negatively charged on HOPG. It is demonstrated that XPS can be a useful tool to study metal-support interactions, which plays an important role for heterogeneous catalysis, for example. PMID:16471654

  2. Surface properties of Streptococcus salivarius HB and nonfibrillar mutants: measurement of zeta potential and elemental composition with X-ray photoelectron spectroscopy.

    PubMed Central

    van der Mei, H C; Léonard, A J; Weerkamp, A H; Rouxhet, P G; Busscher, H J

    1988-01-01

    To characterize the functional cell surface, the zeta potentials and elemental surface composition of Streptococcus salivarius HB and a range of mutants with known molecular surface structures were determined. Zeta potentials of fully hydrated cells were measured as a function of pH in dilute potassium phosphate solutions, yielding isoelectric points of the strains. Elemental composition (O, C, N, and P) of the outer 2 to 5 nm of the freeze-dried cell surfaces were measured by X-ray photoelectron spectroscopy. An increasing loss of proteinaceous fibrillar surface antigens of the mutants was found to be accompanied by a progressive decrease in the N/C ratio from 0.104 in the parent strain HB to 0.053 in mutant HBC12. Simultaneously, the value of the isoelectric point shifted from 3.0 to 1.3. In a previous study (A.H. Weerkamp, H.C. van der Mei, and J. W. Slot, Infect. Immun. 55:438-455, 1987) on the cell surfaces of the same strains, it was shown that removal of fibrils led to increased exposure of (lipo)teichoic acid at the surface, which explains the low isoelectric point caused by the low pKa of the phosphate groups. PMID:3372474

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

    SciTech Connect

    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. X-ray photoelectron spectroscopy study on Fe and Co catalysts during the first stages of ethanol chemical vapor deposition for single-walled carbon nanotube growth

    SciTech Connect

    Oida, Satoshi; McFeely, Fenton R.; Bol, Ageeth A.

    2011-03-15

    Optimized chemical vapor deposition processes for single-walled carbon nanotube (SWCNT) can lead to the growth of dense, vertically aligned, mm-long forests of SWCNTs. Precise control of the growth process is however still difficult, mainly because of poor understanding of the interplay between catalyst, substrate and reaction gas. In this paper we use x-ray photoelectron spectroscopy (XPS) to study the interplay between Fe or Co catalysts, SiO{sub 2} and Al{sub 2}O{sub 3} substrates and ethanol during the first stages of SWCNT forest growth. With XPS we observe that ethanol oxidizes Fe catalysts at carbon nanotube (CNT) growth temperatures, which leads to reduced carbon nanotube growth. Ethanol needs to be decomposed by a hot filament or other technique to create a reducing atmosphere and reactive carbon species in order to grow vertically aligned single-walled carbon nanotubes from Fe catalysts. Furthermore, we show that Al{sub 2}O{sub 3}, unlike SiO{sub 2}, plays an active role in CNT growth using ethanol CVD. From our study we conclude that metallic Fe on Al{sub 2}O{sub 3} is the most optimal catalyst/substrate combination for high-yield SWCNT forest growth, using hot filament CVD with ethanol as the carbon containing gas.

  5. New insight brought by density functional theory on the chemical state of alaninol on Cu(100): Energetics and interpretation of x-ray photoelectron spectroscopy data

    NASA Astrophysics Data System (ADS)

    Irrera, S.; Costa, D.

    2008-03-01

    In recent years, an increasing interest has been focused on the adsorption of molecules on surfaces due to the importance of technologies based on the interaction of organic systems with metals and oxides for biosensors, catalysis, and molecularly imprinted polymer technology. A particularly attractive area is the study of chiral surfaces, as these can act as heterogeneous catalysts and sensors in the stereochemical industrial processes. This work reports on an ab initio simulation of chemisorption of the D-alaninol on Cu (100). This system has been investigated systematically by using the Vienna ab initio simulation Package (VASP) which performs density functional theory (DFT) calculations in periodic boundary conditions. Molecular dynamics at 300K is performed to explore all the possible geometries, finally, optimized at 0K to obtain the adsorption modes. C 1s, O 1s, and N 1s, core level shift (CLS) calculations of those adsorption modes have been evaluated and compared with x-ray photoelectron spectroscopy experimental data. Energetic and CLS indicate that both chemical functions, the NH2 and the dehydrogenated hydroxyl, are involved in the bonding to the surface at low coverage. Atomic hydrogen coadsorbs in a fourfold hollow site. An atomistic thermodynamics approach suggests that at room temperature under UHV conditions, coadsorbed hydrogen has recombined as H2 and desorbed from the surface.

  6. Characterization of carbon surface chemistry by combined temperature programmed desorption with in situ X-ray photoelectron spectrometry and temperature programmed desorption with mass spectrometry analysis.

    PubMed

    Brender, Patrice; Gadiou, Roger; Rietsch, Jean-Christophe; Fioux, Philippe; Dentzer, Joseph; Ponche, Arnaud; Vix-Guterl, Cathie

    2012-03-01

    The analysis of the surface chemistry of carbon materials is of prime importance in numerous applications, but it is still a challenge to identify and quantify the surface functional groups which are present on a given carbon. Temperature programmed desorption with mass spectrometry analysis (TPD-MS) and X-ray photoelectron spectroscopy with an in situ heating device (TPD-XPS) were combined in order to improve the characterization of carbon surface chemistry. TPD-MS analysis allowed the quantitative analysis of the released gases as a function of temperature, while the use of a TPD device inside the XPS setup enabled the determination of the functional groups that remain on the surface at the same temperatures. TPD-MS results were then used to add constraints on the deconvolution of the O1s envelope of the XPS spectra. Furthermore, a better knowledge of the evolution of oxygen functional groups with temperature during a thermal treatment could be obtained. Hence, we show here that the combination of these two methods allows to increase the reliability of the analysis of the surface chemistry of carbon materials. PMID:22242697

  7. In situ SERS and X-ray photoelectron spectroscopy studies on the pH-dependant adsorption of anthraquinone-2-carboxylic acid on silver electrode

    NASA Astrophysics Data System (ADS)

    Li, Dan; Jia, Shaojie; Fodjo, Essy Kouadio; Xu, Hu; Wang, Yuhong; Deng, Wei

    2016-03-01

    In this study, in situ surface-enhanced Raman scattering (SERS) spectroelectrochemistry and angle-resolved X-ray photoelectron spectroscopy (AR-XPS) are used to investigate the redox reaction and adsorption behavior of anthraquinone-2-carboxylic acid (AQ-2-COOH) on an Ag electrode at different pH values. The obtained results indicate that AQ-2-COOH is adsorbed tilted on the Ag electrode through O-atom of ring carbonyl in a potential range from -0.3 to -0.5 V vs. SCE, but the orientation turns to more tilted orientation with both O-atom of the ring carbonyl and carboxylate group in positive potential region for pH 6.0 and 7.4. However, at pH 10.0, the orientation adopts tilted conformation constantly on the Ag electrode with both O-atom of the anthraquinone ring and carboxylate group in the potential range from -0.3 to -0.5 V vs. SCE or at positive potentials. Moreover, the adsorption behavior of AQ-2-COOH has been further confirmed by AR-XPS on the Ag surface. Proposed reasons for the observed changes in orientation are presented.

  8. Hard X-ray photoelectron spectroscopy of LixNi1-xO epitaxial thin films with a high lithium content

    NASA Astrophysics Data System (ADS)

    Kumara, L. S. R.; Sakata, Osami; Yang, Anli; Yamauchi, Ryosuke; Taguchi, Munetaka; Matsuda, Akifumi; Yoshimoto, Mamoru

    2014-07-01

    The core-level and valence-band electronic structures of LixNi1-xO epitaxial thin films with x = 0, 0.27, and 0.48 were studied by hard X-ray photoelectron spectroscopy. A double peak structure, consisting of a main peak and a shoulder peak, and a satellite structure were observed in the Ni 2p3/2 core-level spectra. The intensity ratio of the shoulder to main peak in this double peak structure increased with increasing lithium content in LixNi1-xO. This lithium doping dependence of the Ni 2p3/2 core-level spectra was investigated using an extended cluster model, which included the Zhang-Rice (ZR) doublet bound states arising from a competition between O 2p - Ni 3d hybridization and the Ni on-site Coulomb interaction. The results indicated that the change in the intensity ratio in the main peak is because of a reduction in the ZR doublet bound states from lithium substitutions. This strongly suggests that holes compensating Li doping in LixNi1-xO are of primarily ZR character.

  9. Study on the chemical stability of catalyst counter electrodes for dye-sensitized solar cells using a simple X-ray photoelectron spectroscopy-based method

    NASA Astrophysics Data System (ADS)

    Yun, Dong-Jin; Kim, Jungmin; Chung, Jongwon; Park, SungHoon; Baek, WoonJoong; Kim, Yongsu; Kim, Seongheon; Kwon, Young-Nam; Chung, JaeGwan; Kyoung, Yongkoo; Kim, Ki-Hong; Heo, Sung

    2014-12-01

    Since the chemical/electrical stability and catalytic activity are essential conditions for catalyst counter electrodes (CCEs) in dye-sensitized solar cells (DSSCs), a simple dipping method is employed for evaluating the chemical stability of CCE candidates in an iodine-based liquid electrolyte (I-electrolyte). The chemical stabilities and transition mechanisms of the CCEs are successfully analyzed by studying the chemical transitions in X-ray photoelectron spectroscopy (XPS) core levels after dipping in the I-electrolyte. All films including the Pt film undergo degradation depending on the type of material. While dipping in the I-electrolyte, Cu and Au films scarcely dissolves as their respective metal sulfides, and the Al film gradually loss its metallic properties owing to Al2O3 growth. On the other hand, a previously unknown transition mechanism of organic conducting CCEs is determined based on the proposed method. Compared to the other metal films, the poly(3,4-ethylenedioxythiophene) poly(styrenesulfonate) (PEDOT:PSS) and multi wall carbon nanotube (MWCNT)/PEDOT:PSS films undergo an entirely unique transition mechanism, which results from the chemical adsorption of organic molecules onto PEDOT:PSS molecules in the I-electrolyte. Consequently, these chemical structure transitions correspond well to the degrees of alternation in the electrical properties of DSSCs with all the investigated CCEs.

  10. Kinetics of the sulfur oxidation on palladium: A combined in situ x-ray photoelectron spectroscopy and density-functional study

    SciTech Connect

    Gotterbarm, Karin; Hoefert, Oliver; Lorenz, Michael P. A.; Streber, Regine; Papp, Christian; Luckas, Nicola; Vines, Francesc; Steinrueck, Hans-Peter; Goerling, Andreas

    2012-03-07

    We studied the reaction kinetics of sulfur oxidation on the Pd(100) surface by in situ high resolution x-ray photoelectron spectroscopy and ab initio density functional calculations. Isothermal oxidation experiments were performed between 400 and 500 K for small amounts ({approx}0.02 ML) of preadsorbed sulfur, with oxygen in large excess. The main stable reaction intermediate found on the surface is SO{sub 4}, with SO{sub 2} and SO{sub 3} being only present in minor amounts. Density-functional calculations depict a reaction energy profile, which explains the sequential formation of SO{sub 2}, SO{sub 3}, and eventually SO{sub 4}, also highlighting that the in-plane formation of SO from S and O adatoms is the rate limiting step. From the experiments we determined the activation energy of the rate limiting step to be 85 {+-} 6 kJ mol{sup -1} by Arrhenius analysis, matching the calculated endothermicity of the SO formation.

  11. Cation profiling of passive films on stainless steel formed in sulphuric and acetic acid by deconvolution of angle-resolved X-ray photoelectron spectra

    NASA Astrophysics Data System (ADS)

    Högström, Jonas; Fredriksson, Wendy; Edstrom, Kristina; Björefors, Fredrik; Nyholm, Leif; Olsson, Claes-Olof A.

    2013-11-01

    An approach for determining depth gradients of metal-ion concentrations in passive films on stainless steel using angle-resolved X-ray photoelectron spectroscopy (ARXPS) is described. The iterative method, which is based on analyses of the oxidised metal peaks, provides increased precision and hence allows faster ARXPS measurements to be carried out. The method was used to determine the concentration depth profiles for molybdenum, iron and chromium in passive films on 316L/EN 1.4432 stainless steel samples oxidised in 0.5 M H2SO4 and acetic acid diluted with 0.02 M Na2B4O7 · 10H2O and 1 M H2O, respectively. The molybdenum concentration in the film is pin-pointed to the oxide/metal interface and the films also contained an iron-ion-enriched surface layer and a chromium-ion-dominated middle layer. Although films of similar composition and thickness (i.e., about 2 nm) were formed in the two electrolytes, the corrosion currents were found to be three orders of magnitude larger in the acetic acid solution. The differences in the layer composition, found for the two electrolytes as well as different oxidation conditions, can be explained based on the oxidation potentials of the metals and the dissolution rates of the different metal ions.

  12. Surface change in titanium subhydride between 25 and 700/sup 0/C studied by Auger electron spectroscopy and x-ray photoelectron spectroscopy

    SciTech Connect

    Wang, P.S.; Carlson, R.S.; Wittberg, T.N.

    1982-07-09

    The surface sensitive spectroscopic techniques of Auger electron spectroscopy (AES) and x-ray photoelectron spectroscopy (XPS) have been applied to the study of the oxide dissolution of titanium and titanium subhydride. In an earlier study using AES, it was shown that the rate of oxygen dissolution into titanium increased sharply at approx. 350/sup 0/C. These data correlated well with physical property measurements that indicated an exothermic reaction was occurring at these temperatures which corresponded to the reaction of free Ti with atmospheric oxygen. In the present study the work has been expanded to include studies of TiH/sub x/ (x = 1.15, 1.62). It has been found that dissolution of the native oxide on titanium subhydride occurs at a temperature substantially higher (approx. 500/sup 0/C) than that required for titanium. It appears that the outward diffusion of hydrogen is inhibiting the inward diffusion of oxygen on the sub-hydride samples at temperatures below 500/sup 0/C.

  13. Temperature effects on Li4Ti5O12 electrode/electrolyte interfaces at the first cycle: A X-ray Photoelectron Spectroscopy and Scanning Auger Microscopy study

    NASA Astrophysics Data System (ADS)

    Gieu, J.-B.; Courrèges, C.; El Ouatani, L.; Tessier, C.; Martinez, H.

    2016-06-01

    Li4Ti5O12-based negative electrodes for Lithium-ion batteries are of interest because of the high reversibility of Li+ insertion/extraction. In this study, the surface of cycled electrodes is analysed by X-ray Photoelectron Spectroscopy (XPS) and Scanning Auger Microscopy (SAM) to investigate the effects of cycling temperature (room temperature, 60 °C and 85 °C) upon the solid electrolyte interphase (SEI) formation, which plays a major role in batteries electrochemical performances. Half-cells, with a vinylene carbonate containing electrolyte, are galvanostatically cycled at different steps of the first cycle: the mid-plateau during the first discharge, the end of the first discharge at 1.2 V and the end of the first charge at 2.0 V. XPS analysis evidences that higher temperatures promote the formation of a thicker SEI, which can explain the increase of the irreversible capacity with temperature. SAM mappings (allowing high spatial resolution ∼10-100 nm) evidence that this SEI homogeneously covers the electrode surface, regardless of the cycling temperature. During charge, the SEI is partially dissolved at room temperature, more slightly at 60 °C whereas at 85 °C, no clear evidence of layer thinning is observed. The SEI chemical composition is also investigated and reveals a majority of organic species and an increasing proportion of LiF with the temperature.

  14. X-ray photoelectron spectroscopic and electrochemical impedance spectroscopic analysis of RuO2-Ta2O5 thick film pH sensors.

    PubMed

    Manjakkal, Libu; Cvejin, Katarina; Kulawik, Jan; Zaraska, Krzysztof; Socha, Robert P; Szwagierczak, Dorota

    2016-08-10

    The paper reports on investigation of the pH sensing mechanism of thick film RuO2-Ta2O5 sensors by using X-ray photoelectron spectroscopy (XPS) and electrochemical impedance spectroscopy (EIS). Interdigitated conductimetric pH sensors were screen printed on alumina substrates. The microstructure and elemental composition of the films were examined by scanning electron microscopy and energy dispersive spectroscopy. The XPS studies revealed the presence of Ru ions at different oxidation states and the surface hydroxylation of the sensing layer increasing with increasing pH. The EIS analysis carried out in the frequency range 10 Hz-2 MHz showed that the electrical parameters of the sensitive electrodes in the low frequency range were distinctly dependent on pH. The charge transfer and ionic exchange occurring at metal oxide-solution interface were indicated as processes responsible for the sensing mechanism of thick film RuO2-Ta2O5 pH sensors. PMID:27282750

  15. Aging of Zerovalent Iron in Synthetic Groundwater: X-ray Photoelectron Spectroscopy Depth Profiling Characterization and Depassivation with Uniform Magnetic Field.

    PubMed

    Xu, Hanyang; Sun, Yuankui; Li, Jinxiang; Li, Fengmin; Guan, Xiaohong

    2016-08-01

    Scanning electron microscopy (SEM), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS) depth profiling were employed to characterize the aged zerovalent iron (AZVI) samples incubated in synthetic groundwater. The AZVI samples prepared under different conditions exhibited the passive layers of different morphologies, amounts, and constituents. Owing to the accumulation of iron oxides on their surface, all the prepared AZVI samples were much less reactive than the pristine ZVI for Se(IV) removal. However, the reactivity of all AZVI samples toward Se(IV) sequestration could be significantly enhanced by applying a uniform magnetic field (UMF). Moreover, the flux intensity of UMF necessary to depassivate an AZVI sample was strongly dependent on the properties of its passive layer. The UMF of 1 mT was strong enough to restore the reactivity of the AZVI samples with Fe3O4 as the major constituent of the passive film or with a thin layer of α-Fe2O3 and γ-FeOOH in the external passive film. The flux intensity of UMF necessary to depassivate the AZVI samples would increase to 2 mT or even 5 mT if the AZVI samples were covered with passive films being thicker, denser, and contained more γ-FeOOH and α-Fe2O3. Furthermore, increasing the flux intensity of UMF facilitated the reduction of Se(IV) to Se(0) by AZVI samples. PMID:27384928

  16. Influence of polymolybdate adsorbates on electrooxidation of ethanol at PtRu nanoparticles: Combined electrochemical, mass spectrometric and X-ray photoelectron spectroscopic studies

    NASA Astrophysics Data System (ADS)

    Gralec, Barbara; Lewera, Adam; Kulesza, Pawel J.

    2016-05-01

    The role Keggin-type phosphomolybdate (PMo12O403-) ions (adsorbed on carbon-supported PtRu, PtRu/C) on electrooxidation of ethanol is addressed here. The combined results obtained using Differential Electrochemical Mass Spectrometry, X-ray Photoelectron Spectroscopy and Cyclic Voltammetry are consistent with the view that presence of the Keggin-type polyoxometallate, phosphomolybdate, ions (adsorbates) leads to enlargement of the current densities associated with electrooxidation of ethanol at potentials greater than 700 mV vs. RHE. This increase of the anodic currents is correlated with the higher acetaldehyde yield which is likely to reflect changes in the reaction kinetics (e.g. more dynamic dehydrogenation of ethanol leading to acetaldehyde) or in the reaction mechanism defined by the preferential surface modification resulting not only in faster kinetics but also in higher selectivity with respect to acetaldehyde production. It is apparent from the spectroscopic data that modification of PtRu/C nanoparticles with phosphomolybdate ions leads to suppression of the formation of Ru surface oxides.

  17. The Evolution of Ga and As Core Levels in the Formation of Fe/GaAs(001): A High Resolution Soft X-ray Photoelectron Spectroscopic Study

    SciTech Connect

    Thompson, J W; Neal, J R; Shen, T H; Morton, S A; Tobin, J G; Waddill, G D; Matthew, J D; Greig, D; Hopkinson, M

    2006-12-08

    A high resolution soft x-ray photoelectron spectroscopic study of Ga and As 3d core levels has been conducted for Fe/GaAs (001) as a function of Fe thickness. This work has provided unambiguous evidence of substrate disrupting chemical reactions induced by the Fe overlayer--a quantitative analysis of the acquired spectra indicates significantly differing behavior of Ga and As during Fe growth, and our observations have been compared with existing theoretical models. Our results demonstrate that the outdiffusing Ga and As remain largely confined to the interface region, forming a thin intermixed layer. Whereas at low coverages Fe has little influence on the underlying GaAs substrate, the onset of substrate disruption when the Fe thickness reaches 3.5 {angstrom} results in major changes in the energy distribution curves (EDCs) of both As and Ga 3d cores. Our quantitative analysis suggests the presence of two new As environments of metallic character; one bound to the interfacial region and another which, as confirmed by in-situ oxidation experiments, surface segregates and persists over a wide range of overlayer thickness. Analysis of the corresponding Ga 3d EDCs found not two, but three new environments--also metallic in nature. Two of the three are interface-resident whereas the third undergoes outdiffusion at low Fe coverages. Based on the variations of the integrated intensities of each component, we present a schematic of the proposed chemical make-up of the Fe/GaAs (001) system.

  18. "Un-annealed and Annealed Pd Ultra-Thin Film on SiC Characterized by Scanning Probe Microscopy and X-ray Photoelectron Spectroscopy"

    NASA Technical Reports Server (NTRS)

    Lu, W. J.; Shi, D. T.; Elshot, K.; Bryant, E.; Lafate, K.; Chen, H.; Burger, A.; Collins, W. E.

    1998-01-01

    Pd/SiC has been used as a hydrogen and a hydrocarbon gas sensor operated at high temperature. UHV (Ultra High Vacuum)-Scanning Tunneling Microscopy (STM), Atomic Force Microscopy (AFM) and X-ray Photoelectron Spectroscopy (XPS) techniques were applied to study the relationship between the morphology and chemical compositions for Pd ultra-thin films on SiC (less than 30 angstroms) at different annealing temperatures. Pd ultra-thin film on 6H-SiC was prepared by the RF sputtering method. The morphology from UHV-STM and AFM shows that the Pd thin film was well deposited on SiC substrate, and the Pd was partially aggregated to round shaped participates at an annealing temperature of 300 C. At 400 C, the amount of surface participates decreases, and some strap shape participates appear. From XPS, Pd2Si was formed on the surface after annealing at 300 C, and all Pd reacted with SiC to form Pd2Si after annealing at 400 C. The intensity of the XPS Pd peak decreases enormously at 400 C. The Pd film diffused into SiC, and the Schottky barrier height has almost no changes. The work shows the Pd sicilides/SiC have the same electronic properties with Pd/SiC, and explains why the Pd/SiC sensor still responds to hydrogen at high operating temperatures.

  19. Electronic structure of (Ge2Sb2Te5)1-x(In3SbTe2)x investigated by x-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Benayad, Anass; Kang, YounSeon; Shin, Hyun-Joon; Kim, Kihong; Suh, Dong-Seok; Kim, KiJoon; Kim, CheolKyu; Lee, Tae-Yon; Noh, Jin-Seo; Lee, JaeCheol; Khang, YoonHo

    2009-08-01

    We have investigated the core levels and the valence band of (Ge2Sb2Te5)1-x(In3Sb1Te2)x quaternary phase system (IGST) by means of x-ray photoelectron spectroscopy. A systematic shift of Sb 3d and Ge 2p core-level peaks toward lower binding energies side was observed with increasing indium amount, whereas the In 3d and Te 3d core peaks showed less change. The Sb 3d and Ge 2p core-level shift is attributed to an increase in the electronic charge of p-electrons dependent of indium amount. The valence band spectra show a distinct change in the sp configuration with indium concentration change. The change in the local bonding as the indium amount increase has a profound impact on both local atomic arrangement and amorphous-to-crystalline transformation temperature. The difference in the photoemission spectra have been discussed according to a simple structural model suggesting that the Na site in IGST can be occupied by Te, Sb, In, and vacancy, whereas in GST it is occupied only by Te.

  20. 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 PAGESBeta

    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

  1. Hard X-ray photoelectron spectroscopy of Li{sub x}Ni{sub 1−x}O epitaxial thin films with a high lithium content

    SciTech Connect

    Kumara, L. S. R. Yang, Anli; Sakata, Osami; Yamauchi, Ryosuke; Matsuda, Akifumi; Yoshimoto, Mamoru; Taguchi, Munetaka

    2014-07-28

    The core-level and valence-band electronic structures of Li{sub x}Ni{sub 1−x}O epitaxial thin films with x = 0, 0.27, and 0.48 were studied by hard X-ray photoelectron spectroscopy. A double peak structure, consisting of a main peak and a shoulder peak, and a satellite structure were observed in the Ni 2p{sub 3/2} core-level spectra. The intensity ratio of the shoulder to main peak in this double peak structure increased with increasing lithium content in Li{sub x}Ni{sub 1−x}O. This lithium doping dependence of the Ni 2p{sub 3/2} core-level spectra was investigated using an extended cluster model, which included the Zhang–Rice (ZR) doublet bound states arising from a competition between O 2p – Ni 3d hybridization and the Ni on-site Coulomb interaction. The results indicated that the change in the intensity ratio in the main peak is because of a reduction in the ZR doublet bound states from lithium substitutions. This strongly suggests that holes compensating Li doping in Li{sub x}Ni{sub 1−x}O are of primarily ZR character.

  2. Degradation of all-vanadium redox flow batteries (VRFB) investigated by electrochemical impedance and X-ray photoelectron spectroscopy: Part 2 electrochemical degradation

    NASA Astrophysics Data System (ADS)

    Derr, Igor; Bruns, Michael; Langner, Joachim; Fetyan, Abdulmonem; Melke, Julia; Roth, Christina

    2016-09-01

    Electrochemical degradation (ED) of carbon felt electrodes was investigated by cycling of a flow through all-vanadium redox flow battery (VRFB) and conducting half-cell measurements with two reference electrodes inside the test bench. ED was detected using half-cell and full-cell electrochemical impedance spectroscopy (EIS) at different states of charge (SOC). Reversing the polarity of the battery to recover cell performance was performed with little success. Renewing the electrolyte after a certain amount of cycles restored the capacity of the battery. X-ray photoelectron spectroscopy (XPS) reveals that the amount of surface functional increases by more than a factor of 3 for the negative side as well as for the positive side. Scanning electron microscope (SEM) images show a peeling of the fiber surface after cycling the felts, which leads to a loss of electrochemically active surface area (ECSA). Long term cycling shows that ED has a stronger impact on the negative half-cell [V(II)/V(III)] than the positive half-cell [V(IV)/V(V)] and that the negative half-cell is the rate-determining half-cell for the VRFB.

  3. Surface characterization of 7S and 11S globulin powders from soy protein examined by X-ray photoelectron spectroscopy and scanning electron microscopy.

    PubMed

    Zhao, Xiaoyan; Chen, Jun; Zhu, Qingjun; Du, Fangling; Ao, Qiang; Liu, Jie

    2011-09-01

    In this study the surface composition of 7S and 11S globulin powders from soybean proteins by aqueous buffer and reverse micelle extractions had been examined using X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). Analysis by XPS revealed that the O and N atomic percentage of 7S and 11S globulin surfaces from bis(2-ethylhexyl) sodium sulfosuccinate (AOT) reverse micelle was higher than from aqueous buffer, but the C atomic percentage was lower. The O/C ratio of the 7S globulin powder from aqueous buffer and reverse micelle was similar while significant differences were obtained in the O/C ratio of the 11S globulin powder, N/C atom ratios of the 7S and 11S globulin powders and high-resolution XPS C 1s, N 1s, O 1s spectra. Powder microstructure after reverse micelle treatment showed the presence of small pores, indicating the effect of reverse micelle on the 7S and 11S globulin structure. The obtained results indicated that the reverse micelle could affect the C, O and N components on the surface of soybean proteins. PMID:21555209

  4. Auger and X-ray PhotoelectronSpectroscopy Study of the Density ofOxygen States in Bismuth, Aluminum, Silicon, and Uranium Oxides

    SciTech Connect

    Teterin, Yu A.; Ivanov, K.E.; Teterin, A. Yu; Lebedev, A.M.; Utkin, I.O.; Vukchevich, L.

    1998-08-03

    The correlation of relative partial electron density at the oxygen ions with the intensity of Auger O KLL lines in Bi2O3, Al2O3, SiO2 and UO2 has been determined by Auger and X-ray photoelectron spectroscopic methods. The dependence of the relative intensities of Auger O KL2-3L2-3 and O KL1L2-3-lines was characterized from the binding energy of O 1s electrons. The electron density of the outer valence levels of oxygen increases as the relative intensities of Anger OKL2-3L2-3 and O KL1L2-3-lines increase. The fine structure observed in the O KL1L2-3 Auger and the O 2s XPS spectra has been explained by the formation of inner valence molecular orbitals (IVMO) from the interaction of electrons of the O 2s and filled metal ns shells.

  5. Chemical order in Ge{sub x}As{sub y}Se{sub 1-x-y} glasses probed by high resolution X-ray photoelectron spectroscopy

    SciTech Connect

    Xu, S. W.; Wang, R. P.; Luther-Davies, B.; Kovalskiy, A.; Miller, A. C.; Jain, H.

    2014-02-28

    We have measured high-resolution x-ray photoelectron spectra of Ge{sub x}As{sub y}Se{sub 1-x-y} glasses with a mean coordination number (MCN) from 2.2 to 2.78. The valence band spectra showed that a number of Se–Se–Se trimers can be found in Se-rich samples, whilst multiband features induced by phase separation can be observed in extremely Se-poor samples. When the Ge, As, and Se 3d spectra were decomposed into several doublets, which correspond, respectively, to different chemical environments, the perfect AsSe{sub 3/2} pyramidal and GeSe{sub 4/2} tetrahedral structures in Se-rich samples gradually evolved into defect structures, including As–As and Ge–Ge homopolar bonds, with increasing Ge and As concentrations. Two transition-like features were found at MCN = 2.5 and 2.64–2.72 that correspond first to the disappearance of Se-chains in the glass network and, subsequently, destruction of the perfect GeSe{sub 4/2} tetrahedral structures, respectively.

  6. Spectroscopic ellipsometry and x-ray photoelectron spectroscopy of La{sub 2}O{sub 3} thin films deposited by reactive magnetron sputtering

    SciTech Connect

    Atuchin, V. V.; Kalinkin, A. V.; Kochubey, V. A.; Kruchinin, V. N.; Vemuri, R. S.; Ramana, C. V.

    2011-03-15

    Lanthanum oxide (La{sub 2}O{sub 3}) films were grown by the reactive dc magnetron sputtering and studied their structural, chemical and optical parameters. La{sub 2}O{sub 3} films were deposited onto Si substrates by sputtering La-metal in a reactive gas (Ar+O{sub 2}) mixture at a substrate temperature of 200 deg. C Reflection high-energy electron diffraction measurements confirm the amorphous state of La{sub 2}O{sub 3} films. Chemical analysis of the top-surface layers evaluated with x-ray photoelectron spectroscopy indicates the presence of a layer modified by hydroxylation due to interaction with atmosphere. Optical parameters of a-La{sub 2}O{sub 3} were determined with spectroscopic ellipsometry (SE). There is no optical absorption over spectral range {lambda}=250-1100 nm. Dispersion of refractive index of a-La{sub 2}O{sub 3} was defined by fitting of SE parameters over {lambda}=250-1100 nm.

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

    SciTech Connect

    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.

  8. Resolving CuO chain and CuO2 plane contributions to the YBa2Cu3O7 -δ valence band by standing-wave excited hard x-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Thiess, S.; Lee, T.-L.; Aruta, C.; Lin, C. T.; Venturini, F.; Brookes, N. B.; Cowie, B. C. C.; Zegenhagen, J.

    2015-08-01

    We analyzed the valence band (VB) of the 90 K high-temperature superconductor YBa2Cu3O7 -δ by photoelectron spectroscopy under standing-wave excitation employing hard x rays. Precisely positioning the standing-wave intensity in the unit cell allows selectively probing the VB yield from the CuO chains and CuO2 planes, respectively. Both contribute strongly over the whole VB but the spectral weight of the planes is significantly higher than the chains within about 2 eV from the Fermi level. In the x-ray regime, the major contribution to the VB emission is coming from Cu 3 d .

  9. X-ray Photoelectron Diffraction (XPD) Study of the Growth of Cu on clean and O-precovered Ru(0001).

    NASA Astrophysics Data System (ADS)

    Ruebush, S. R.; Couch, R. E.; Fadley, C. S.; Thevuthasan, S.

    1996-03-01

    We have studied the growth of Cu on clean and O-precovered Ru(0001) for the first time with XPD, measuring experimental O 1s (E_kin=958 eV), Cu 2p3/2 (E_kin=554 eV), and Ru 3d (E_kin=1206eV) intensities over nearly the full 2π solid angle above the surface for Cu coverages from submonolayer up to many monolayers. We have analyzed our data using single and multiple scattering diffraction calculations. We have found a continuous Cu interlayer spacing from 1.84 Åat 1 ML to about 2.00 Åat 8 ML, with the bulk Cu spacing being 2.08 ÅWe have also studied the effect that a surfactant such as oxygen has on the growth of Cu. Our XPD studies show that all oxygen floats on the Cu surface. In addition, a preliminary analysis of our data suggests a tendency towards island growth for about 1-3 ML. We will compare our results with prior theoretical and experimental studies of this system.

  10. 77 FR 12226 - Sadex Corp.; Filing of Food Additive Petition (Animal Use); Electron Beam and X-Ray Sources for...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-02-29

    ... Petition (Animal Use); Electron Beam and X-Ray Sources for Irradiation of Poultry Feed and Poultry Feed... regulations be amended to provide for the safe use of electron beam and x-ray sources for irradiation of... use of electron beam and x- ray sources for irradiation of poultry feed and poultry feed...

  11. NH{sub 3} adsorption and decomposition on Ir(110): A combined temperature programmed desorption and high resolution fast x-ray photoelectron spectroscopy study

    SciTech Connect

    Weststrate, C.J.; Bakker, J.W.; Rienks, E.D.L.; Lizzit, S.; Petaccia, L.; Baraldi, A.; Vinod, C.P.; Nieuwenhuys, B.E.

    2005-05-08

    The adsorption and decomposition of NH{sub 3} on Ir(110) has been studied in the temperature range from 80 K to 700 K. By using high-energy resolution x-ray photoelectron spectroscopy it is possible to distinguish chemically different surface species. At low temperature a NH{sub 3} multilayer, which desorbs at {approx}110 K, was observed. The second layer of NH{sub 3} molecules desorbs around 140 K, in a separate desorption peak. Chemisorbed NH{sub 3} desorbs in steps from the surface and several desorption peaks are observed between 200 and 400 K. A part of the NH{sub 3ad} decomposes into NH{sub ad} between 225 and 300 K. NH{sub ad} decomposes into N{sub ad} between 400 K and 500 K and the hydrogen released in this process immediately desorbs. N{sub 2} desorption takes place between 500 and 700 K via N{sub ad} combination. The steady state decomposition reaction of NH{sub 3} starts at 500 K. The maximum reaction rate is observed between 540 K and 610 K. A model is presented to explain the occurrence of a maximum in the reaction rate. Hydrogenation of N{sub ad} below 400 K results in NH{sub ad}. No NH{sub 2ad} or NH{sub 3ad}/NH{sub 3} were observed. The hydrogenation of NH{sub ad} only takes place above 400 K. On the basis of the experimental findings an energy scheme is presented to account for the observations.

  12. X-ray photoelectron spectroscopy of fast-frozen hematite colloids in aqueous solutions. 5. Halide ion (F-, Cl-, Br-, I-) adsorption.

    PubMed

    Shimizu, Kenichi; Shchukarev, Andrey; Kozin, Philipp A; Boily, Jean-François

    2013-02-26

    Halide anion (F(-), Cl(-), Br(-), and I(-)) adsorption and its impact on sodium adsorption at the hematite/water interface were studied by cryogenic X-ray photoelectron spectroscopy (XPS). Measurements were carried out on frozen, centrifuged wet hematite pastes that were previously equilibrated in 50 mM electrolytic solutions in the pH 2-11 range. XPS-derived halide ion surface loadings decreased in the order F(-) > I(-) ≈ Cl(-) > Br(-), whereas sodium loadings were in the order Na(F) > Na(I) > Na(Br) > Na(Cl). The greater sodium loadings in NaF and in NaI resulted from larger anion loadings in these systems. Bromide ion had the lowest loading among all halide ions despite having a charge-to-size ratio that is intermediate between those of Cl(-) and I(-). This unexpected result may have arisen from specific properties of the hematite/water interface, such as water structure and electric double layer thickness. Fluoride ion adsorption proceeded via the formation of hydrogen bonds with the surface hydroxo groups (e.g., ≡Fe-OH(2)···F(-) or ≡Fe-OH···F(-)). Surface-bound fluoride ions exert a greater charge-screening effect than the other halide anions, as demonstrated by considerably small zeta potential values. Fe-F bond formation was excluded as a possible interfacial process as the F 1s peak binding energy (684.2 eV) was more comparable to that of NaF (684.6 eV) than FeF(3) (685.4 eV). Overall, these findings motivate further refinements of existing thermodynamic adsorption models for predicting the ionic composition of hematite particle surfaces contacted with sodium halide aqueous solutions. PMID:23347248

  13. Direct determination of the band offset in atomic layer deposited ZnO/hydrogenated amorphous silicon heterojunctions from X-ray photoelectron spectroscopy valence band spectra

    SciTech Connect

    Korte, L. Rößler, R.; Pettenkofer, C.

    2014-05-28

    The chemical composition and band alignment at the heterointerface between atomic layer deposition-grown zinc oxide (ZnO) and hydrogenated amorphous silicon (a-Si:H) is investigated using monochromatized X-ray photoelectron spectroscopy. A new approach for obtaining the valence band offset ΔE{sub V} is developed, which consists in fitting the valence band (VB) spectrum obtained for a-Si:H with a thin ZnO overlayer as the sum of experimentally obtained VB spectra of a bulk a-Si:H film and a thick ZnO film. This approach allows obtaining ΔE{sub V} = 2.71 ± 0.15 eV with a minimum of assumptions, and also yields information on the change in band bending of both substrate and ZnO film. The band offset results are compared to values obtained using the usual approach of comparing valence band edge-to-core level energy differences, ΔE{sub B,CL} − ΔE{sub B,VB}. Furthermore, a theoretical value for the VB offset is calculated from the concept of charge neutrality level line-up, using literature data for the charge neutrality levels and the experimentally determined ZnO/a-Si:H interface dipole. The thus obtained value of ΔE{sub V}{sup CNL} = 2.65 ± 0.3 eV agrees well with the experimental ΔE{sub V}.

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

    SciTech Connect

    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.

  15. Transformation of amyloid-like fibers, formed from an elastin-based biopolymer, into a hydrogel: an X-ray photoelectron spectroscopy and atomic force microscopy study.

    PubMed

    Flamia, R; Salvi, A M; D'Alessio, L; Castle, J E; Tamburro, A M

    2007-01-01

    Previous studies have revealed the propensity of elastin-based biopolymers to form amyloid-like fibers when dissolved in water. These are of interest when considered as "ancestral units" of elastin in which they represent the simplest sequences in the hydrophobic regions of the general type XxxGlyGlyZzzGly (Xxx, Zzz = Val, Leu). We normally refer to these biopolymers based on elastin or related to elastin units as "elastin-like polypeptides". The requirement of water for the formation of amyloids seems quite interesting and deserves investigation, the water representing the natural transport medium in human cells. As a matter of fact, the "natural" supramolecular organization of elastin is in the form of beaded-string-like filaments and not in the form of amyloids whose "in vivo" deposition is associated with some important human diseases. Our work is directed, therefore, to understanding the mechanism by which such hydrophobic sequences form amyloids and any conditions by which they might regress to a non-amyloid filament. The elastin-like sequence here under investigation is the ValGlyGlyValGly pentapeptide that has been previously analyzed both in its monomer and polymer form. In particular, we have focused our investigation on the apparent stability of amyloids formed from poly(ValGlyGlyValGly), and we have observed these fibers evolving to a hydrogel after prolonged aging in water. We will show how atomic force microscopy can be combined with X-ray photoelectron spectroscopy to gain an insight into the spontaneous organization of an elastin-like polypeptide driven by interfacial interactions. The results are discussed also in light of fractal-like assembly and their implications from a biomedical point of view. PMID:17206798

  16. Depth profiling of the elemental surface composition of the oral microorganism S. salivarius HB and fibrillar mutants by X-ray photoelectron spectroscopy.

    PubMed

    van der Mei, H C; Handley, P S; Busscher, H J

    1992-02-01

    X-ray photoelectron spectroscopy (XPS) on microbial cell surfaces requires freeze-drying of cells, and as a result, the cell surface appendages flatten out on the cell surface and form a collapsed fibrillar mass. At present, it is unclear how the density, length and composition of these fibrils influence the elemental surface composition as probed by XPS. The sampling depth of XPS can be varied by changing the electron take-off angle. In this article, we made a depth profiling of the collapsed fibrillar mass of Streptococcus salivarius HB and fibril-deficient mutants by angle-dependent XPS. Methylamine tungstate negative staining and ruthenium red staining followed by sectioning revealed distinct classes of fibrils with various lengths on each of the strains. Interpretation of the angle dependence of the oxygen/carbon (O/C) and phosphorus/carbon (P/C) surface concentration ratios of these strains was difficult. However, the angle dependence of the nitrogen/carbon (N/C) surface concentration ratio could be fully interpreted: N/C did not vary with sampling depth on a bald strain, S. salivarius HBC12 and on S. salivarius HB7, a strain with a dense array of fibrils of uniform length. N/C decreased with sampling depth in case of a sparsely fibrillated strain, S. salivarius HBV51 and eventually reached the value observed for the bald strain, HBC12. A high N/C at small sampling depth was observed for S. salivarius HB with protruding, protein rich fibrils. We conclude that elemental depth profiling of microbial cell surfaces by XPS can be interpreted to coincide with structural and biochemical information on the cell surface as obtained by electron microscopy and can therefore be considered as a useful technique to study structural features of cell surfaces in combination with electron microscopy. PMID:1284785

  17. In situ x-ray photoelectron spectroscopic and density-functional studies of Si atoms adsorbed on a C60 film.

    PubMed

    Onoe, Jun; Nakao, Aiko; Hara, Toshiki

    2004-12-01

    The interaction between C(60) and Si atoms has been investigated for Si atoms adsorbed on a C(60) film using in situ x-ray photoelectron spectroscopy (XPS) and density-functional (DFT) calculations. Analysis of the Si 2p core peak identified three kinds of Si atoms adsorbed on the film: silicon suboxides (SiO(x)), bulk Si crystal, and silicon atoms bound to C(60). Based on the atomic percent ratio of silicon to carbon, we estimated that there was approximately one Si atom bound to each C(60) molecule. The Si 2p peak due to the Si-C(60) interaction demonstrated that a charge transfer from the Si atom to the C(60) molecule takes place at room temperature, which is much lower than the temperature of 670 K at which the charge transfer was observed for C(60) adsorbed on Si(001) and (111) clean surfaces [Sakamoto et al., Phys. Rev. B 60, 2579 (1999)]. The number of electrons transferred between the C(60) molecule and Si atom was estimated to be 0.59 based on XPS results, which is in good agreement with the DFT result of 0.63 for a C(60)Si with C(2v) symmetry used as a model cluster. Furthermore, the shift in binding energy of both the Si 2p and C 1s core peaks before and after Si-atom deposition was experimentally obtained to be +2.0 and -0.4 eV, respectively. The C(60)Si model cluster provides the shift of +2.13 eV for the Si 2p core peak and of -0.28 eV for the C 1s core peak, which are well corresponding to those experimental results. The covalency of the Si-C(60) interaction was also discussed in terms of Mulliken overlap population between them. PMID:15634092

  18. Validity of automated x-ray photoelectron spectroscopy algorithm to determine the amount of substance and the depth distribution of atoms

    SciTech Connect

    Tougaard, Sven

    2013-05-15

    The author reports a systematic study of the range of validity of a previously developed algorithm for automated x-ray photoelectron spectroscopy analysis, which takes into account the variation in both peak intensity and the intensity in the background of inelastically scattered electrons. This test was done by first simulating spectra for the Au4d peak with gold atoms distributed in the form of a wide range of nanostructures, which includes overlayers with varying thickness, a 5 A layer of atoms buried at varying depths and a substrate covered with an overlayer of varying thickness. Next, the algorithm was applied to analyze these spectra. The algorithm determines the number of atoms within the outermost 3 {lambda} of the surface. This amount of substance is denoted AOS{sub 3{lambda}} (where {lambda} is the electron inelastic mean free path). In general the determined AOS{sub 3{lambda}} is found to be accurate to within {approx}10-20% depending on the depth distribution of the atoms. The algorithm also determines a characteristic length L, which was found to give unambiguous information on the depth distribution of the atoms for practically all studied cases. A set of rules for this parameter, which relates the value of L to the depths where the atoms are distributed, was tested, and these rules were found to be generally valid with only a few exceptions. The results were found to be rather independent of the spectral energy range (from 20 to 40 eV below the peak energy) used in the analysis.

  19. Competition between organics and bromide at the aqueous solution-air interface as seen from ozone uptake kinetics and X-ray photoelectron spectroscopy.

    PubMed

    Lee, Ming-Tao; Brown, Matthew A; Kato, Shunsuke; Kleibert, Armin; Türler, Andreas; Ammann, Markus

    2015-05-14

    A more detailed understanding of the heterogeneous chemistry of halogenated species in the marine boundary layer is required. Here, we studied the reaction of ozone (O3) with NaBr solutions in the presence and absence of citric acid (C6H8O7) under ambient conditions. Citric acid is used as a proxy for oxidized organic material present at the ocean surface or in sea spray aerosol. On neat NaBr solutions, the observed kinetics is consistent with bulk reaction-limited uptake, and a second-order rate constant for the reaction of O3 + Br(-) is 57 ± 10 M(-1) s(-1). On mixed NaBr-citric acid aqueous solutions, the uptake kinetics was faster than that predicted by bulk reaction-limited uptake and also faster than expected based on an acid-catalyzed mechanism. X-ray photoelectron spectroscopy (XPS) on a liquid microjet of the same solutions at 1.0 × 10(-3)-1.0 × 10(-4) mbar was used to obtain quantitative insight into the interfacial composition relative to that of the bulk solutions. It revealed that the bromide anion becomes depleted by 30 ± 10% while the sodium cation gets enhanced by 40 ± 20% at the aqueous solution-air interface of a 0.12 M NaBr solution mixed with 2.5 M citric acid in the bulk, attributed to the role of citric acid as a weak surfactant. Therefore, the enhanced reactivity of bromide solutions observed in the presence of citric acid is not necessarily attributable to a surface reaction but could also result from an increased solubility of ozone at higher citric acid concentrations. Whether the acid-catalyzed chemistry may have a larger effect on the surface than in the bulk to offset the effect of bromide depletion also remains open. PMID:25530167

  20. Thermal stability of surface freezing films in Ga-based alloys: an x-ray photoelectron spectroscopy and scanning tunneling microscopy study.

    PubMed

    Halka, V; Freyland, W

    2007-07-21

    We have investigated the thickness and surface structure of surface freezing films in Ga-Bi and Ga-Pb alloys over a wide temperature range between room temperature and the respective surface freezing transitions by x-ray photoelectron spectroscopy (XPS) and scanning tunnelling microscopy (STM). For the example of a Ga-Bi alloy dilute in Bi, XPS measurements show that the surface freezing film has a nearly constant value of approximately 25 A between the surface freezing temperature of 130 degrees C and room temperature if the sample is cooled slowly (5 Kh). On heating to 130 degrees C the film thickness exhibits a clear hysteresis on melting. On quenching the alloy sample (>100 Kh) the film thickness increases by almost a factor of 10. These observations indicate that the surface freezing films are metastable. The surface structure of the surface freezing films of various Ga-rich Ga-Bi and Ga-Pb alloys has been probed for the first time by STM at different temperatures below and above the bulk eutectic point. Atomically resolved STM images show the surface structures of pure Bi (0001) and Pb (111), respectively, at room temperature. On heating above the eutectic temperature the surface structure of the films does not change significantly as judged from the size and thickness of Pb or Bi terraces. These observations together with the film thickness variation with temperature indicate that the surface freezing films behave like a metastable independent surface phase. These results together with the wetting characteristics of these alloys suggest that surface freezing in these systems is a first order surface phase transition between wetting and metastable surface freezing films. The energy barrier for nucleation is strongly reduced due to a lowering of the interfacial energy if the nucleus is completely immersed in the respective wetting layer. PMID:17655450

  1. Electronic structure of rare-earth chromium antimonides RECrSb3 (RE=La-Nd, Sm, Gd-Dy, Yb) by X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Crerar, Shane J.; Mar, Arthur; Grosvenor, Andrew P.

    2012-12-01

    The electronic structure of the ternary rare-earth chromium antimonides RECrSb3 (RE=La-Nd, Sm, Gd-Dy, Yb) has been examined by high-resolution X-ray photoelectron spectroscopy (XPS) for the first time. The RE 3d or 4d core-line spectra are substantially complicated by the presence of satellite peaks but their general resemblance to those of RE2O3 tends to support the presence of trivalent RE atoms in RECrSb3. However, the Yb 4d spectrum of YbCrSb3 also shows peaks that are characteristic of divalent ytterbium. The Cr 2p core-line spectra exhibit asymmetric lineshapes and little change in binding energy (BE) relative to Cr metal, providing strong evidence for electronic delocalization. The Sb 3d core-line spectra reveal slightly negative BE shifts relative to elemental antimony, supporting the presence of anionic Sb species in RECrSb3. The experimental valence band spectrum of LaCrSb3 matches well with the calculated density of states, and it can be fitted to component peaks belonging to individual atoms to yield an average formulation that agrees well with expectations (“La3+Cr3+(Sb2-)3”). On progressing from LaCrSb3 to NdCrSb3, the 4f-band in the valence band spectra grows in intensity and shifts to higher BE. The valence band spectrum for YbCrSb3 also supports the presence of divalent ytterbium.

  2. Investigations on the low voltage cathodoluminescence stability and surface chemical behaviour using Auger and X-ray photoelectron spectroscopy on LiSrBO{sub 3}:Sm{sup 3+} phosphor

    SciTech Connect

    Pitale, Shreyas S.; Nagpure, I.M.; Kumar, Vinay; Ntwaeaborwa, O.M.; Terblans, J.J.; Swart, H.C.

    2011-07-15

    Highlights: {yields} Stable orange-red cathodoluminescence observed from LiSrBO{sub 3}:Sm{sup 3+} phosphor. {yields} In situ Auger electron spectroscopy, while monitoring the CL output reduction, reveals surface concentration modification of Li, Sr, B and O atoms. {yields} X-ray photoelectron spectroscopy confirms the formation of SrO{sub 2} layer due to the electron stimulated surface chemical reactions (ESSCRs). This layer is possibly contributing to the surface chemical stability and prevents further degradation. -- Abstract: Orange-red emissive LiSrBO{sub 3}:Sm{sup 3+} phosphors were synthesized through the solid-state reaction method. Under UV radiation (221 nm) and low-voltage electron beam (2 keV, 12 mA/cm{sup 2}) excitation, the Sm{sup 3+} doped LiSrBO{sub 3} phosphor shows emission corresponding to the characteristic {sup 4}G{sub 5/2}-{sup 6}H{sub 7/2} transitions of Sm{sup 3+} with the strongest emission at 601 nm. A high stability of cathodoluminescence (CL) emission during prolong electron bombardment with low-energy electrons was observed. Surface sensitive diagnostic tools such as Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS) were used to study the surface chemistry. AES results revealed modifications in the surface concentrations of Li, Sr, B, O and C on the surface of the LiSrBO{sub 3}:Sm{sup 3+} phosphor as indicated by the changes in their Auger peak to peak heights (APPH) as a function of electron dose. Observed changes in the high resolution XPS spectra of the LiSrBO{sub 3}:Sm{sup 3+} surface irradiated with the low energy electron beam provide evidence of compositional and structural changes as a result of the electron beam stimulated surface chemical reactions (ESSCRs). Additional SrO{sub 2} was identified by XPS on the phosphor surface after it received an electron dose of 300 C/cm{sup 2} together with the increase in the concentrations of chemical species containing the B-C-O bonding. The new surface chemical

  3. Development of cosmic x-ray polarimeter

    NASA Astrophysics Data System (ADS)

    Hayato, Asami; Tamagawa, Toru; Tsunoda, Naoko; Hashimoto, Shigehira; Miyamoto, Masao; Kohama, Mitsuhiro; Tokanai, Fuyuki; Hamagaki, Hideki; Inuzuka, Masahide; Miyasaka, Hiromasa; Sakurai, Ikuya; Makishima, Kazuo

    2006-06-01

    We present a performance study of a cosmic X-ray polarimeter which is based on the photoelectric effect in gas, and sensitive to a few to 30 keV range. In our polarimeter, the key device would be the 50 μm pitch Gas Electron Multiplier (GEM). We have evaluated the modulation factor using highly polarized X-ray, provided by a synchrotron accelerator. In the analysis, we selected events by the eccentricity of the charge cloud of the photoelectron track. As a result, we obtained the relationship between the selection criteria for the eccentricity and the modulation factors; for example, when we selected the events which have their eccentricity of > 0.95, the polarimeter exhibited with the modulation factor of 0.32. In addition, we estimated the Minimum Detectable Polarization degree (MDP) of Crab Nebula with our polarimeter and found 10 ksec observation is enough to detect the polarization, if we adopt suitable X-ray mirrors.

  4. Surface redox properties of lanthanum chromium nickel oxide, lanthanum strontium cobalt oxide, and silver explored via in-situ x-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Vovk, Gregory

    The surface redox properties of LaCr0.6Ni0.4O 3 (powder), La0.5Sr0.5CoO3 (thin film) and silver (powder) were investigated using X-ray photoelectron spectroscopy (XPS). In order to control the oxidation state of a sample in ultra high vacuum (UHV) conditions, it was incorporated as the working electrode in a solid state electrochemical cell with the following configuration: (sample|YSZ|Pd:PdO)), where YSZ is 8 mol% yttria-stabilized zirconia, an oxide ion conducting electrolyte and Pd:PdO is a palladium-palladium oxide powder mixture serving as the reference electrode and an oxygen reservoir. Reduction/oxidation of the sample was initiated by applying an external bias voltage to the sample. It was found that the surface of LaCr0.6Ni0.4O 3 and LaNiO3 powders could be reversibly reduced and oxidized electrochemically to changes involving La, Cr, Ni, and to a lesser extent, O surface atoms. Binding energy shifts (with respect to the La 3d5/2 peak) were seen for the Cr 2p, Ni 3p, and O 1s peaks. The La 3d peaks did not shift noticeably upon reduction, but did exhibit La 3d5/2 parent:satellite ratio changes. The reduced surfaces of LaCr0.6Ni 0.4O3 and LaNiO3 were found to be active in adsorbing CO2, an indication of the increased Lewis basicity of these surfaces upon electrochemical reduction. La0.5Sr0.5CoO3 thin films displayed similar La 3d5/2 parent:satellite ratio changes as to those seen on LaCr0.6Ni0.4O3 and LaNiO3. The electronic behavior of the B-cation, Co, showed localized electronic changes. Furthermore, the surface stoichiometry of La0.5Sr0.5CoO 3 was rich in La and Sr and displayed irreversible binding energy changes in the Sr 3d and O 1s XPS signals. Two different species of oxygen and strontium were always present on the La0.5Sr0.5CoO3 surface. Ag showed reversible changes to O 1s XPS binding energy shifts and amounts. Although this behavior is in agreement with previous reports, the results were complicated by the reversible movement of sodium arising

  5. X-ray photoelectron spectroscopy and structural analysis of amorphous SiO{sub x}N{sub y} films deposited at low temperatures

    SciTech Connect

    Cova, P.; Poulin, S.; Masut, R.A.

    2005-11-01

    We establish, using a tetrahedral model, the bonding properties of amorphous silicon oxynitride (a-SiO{sub x}N{sub y}) films deposited at low temperatures (LTs) by electron-cyclotron resonance chemical-vapor deposition (ECRCVD) on several substrates and under various conditions of gas flows and total gas pressure in a dilute mixture of SiH{sub 4}+N{sub 2} in Ar. The atomic percentage of each tetrahedral unit incorporated in the film network is calculated from the deconvolution of the high-resolution x-ray photoelectron spectroscopy (XPS) spectra in the Si 2p{sub 3/2} region and corroborated by the results obtained from both survey scans and the high-resolution XPS spectra in the N 1s region. The Si{sub 3}N{sub 4} phase is the most important one and the only bonding unit which is incorporated in all our LT ECRCVD SiO{sub x}N{sub y} films. The incorporation of all the other component tetrahedrons depends strongly on growth conditions. The threshold values of the N/Si atomic ratio for which intrinsic defects, such as Si-Si bonds, are not incorporated in the network depend on the O/Si ratio incorporated in the films, mainly due to the competition between oxygen and nitrogen atoms in their reaction with silicon dangling bonds. The effect of the total gas pressure on the atomic percentages of the oxidation states present in the LT ECRCVD SiO{sub x}N{sub y} films is qualitatively similar to the effect of the ion bombarding energy or the plasma density. O-N bonds are present only in samples having high amount of oxygen and nitrogen in their networks. For these films, our results show unambiguously the presence of the N-Si{sub 2}O tetrahedron and suggest that N-Si{sub 3-{nu}}O{sub {nu}} tetrahedrons with {nu}{>=}2 are not incorporated in their networks. A correlation is observed between the N-Si{sub 2}O and the Si-O{sub 3}(ON) tetrahedrons whose component peak is localized at (104.0{+-}0.2) eV in the Si 2p{sub 3/2} region of the XPS data, which suggests that both bonding

  6. X-ray photoelectron spectroscopy study of the nucleation processes and chemistry of CdS thin films deposited by sublimation on different solar cell substrate materials

    SciTech Connect

    Espinos, J.P.; Martin-Concepcion, A.I.; Mansilla, C.; Yubero, F.; Gonzalez-Elipe, A.R.

    2006-07-15

    Cadmium sulfide has been deposited by evaporation on five different substrates: CdTe, ZnO, Ag, TiO{sub 2}, and partially reduced titanium oxide (i.e., TiO{sub 1.73}). The deposition rate and the evolution of the Cd/S ratio on the different substrates have been determined by x-ray photoelectron spectroscopy. The growth mode of the films has been also studied by analyzing the shape of the backgrounds behind the photoemission peaks (peak shape analysis). It has been found that, under completely equivalent conditions, the deposition efficiency (i.e., sticking coefficient) is large on CdTe and TiO{sub 1.73}, but very small on ZnO and TiO{sub 2}. Silver constitutes an intermediate situation characterized by a long induction period where the deposition rate is small and a later increase in deposition efficiency comparable to that on CdTe. For the initial stages of deposition, below an equivalent monolayer, it has been also found that the Cd/S ratio is smaller than unity on TiO{sub 1.73} and ZnO but larger than unity on CdTe and Ag substrates. For sufficiently long deposition times the Cd/S ratio on the surface reaches unity. Except for silver substrate, cadmium appears as Cd{sup 2+} and sulfur as S{sup -2} species at the initial stages of deposition. On the silver surface, cadmium adsorbs as Cd{sup 0} at low coverage. Peak shape analysis has shown that cadmium sulfide grows according to layer-by-layer mechanism (Frank-van de Merwe model) when the substrates are CdTe and TiO{sub 1.73}, but large particles are formed that do not cover the surface for ZnO and Ag substrates (Volmer-Weber growth model). These results are consistent with the different chemical affinities of the substrate towards the atoms of cadmium and sulfur produced during the evaporation of the cadmium sulfide.

  7. Electronic structure of rare-earth chromium antimonides RECrSb{sub 3} (RE=La-Nd, Sm, Gd-Dy, Yb) by X-ray photoelectron spectroscopy

    SciTech Connect

    Crerar, Shane J.; Mar, Arthur; Grosvenor, Andrew P.

    2012-12-15

    The electronic structure of the ternary rare-earth chromium antimonides RECrSb{sub 3} (RE=La-Nd, Sm, Gd-Dy, Yb) has been examined by high-resolution X-ray photoelectron spectroscopy (XPS) for the first time. The RE 3d or 4d core-line spectra are substantially complicated by the presence of satellite peaks but their general resemblance to those of RE{sub 2}O{sub 3} tends to support the presence of trivalent RE atoms in RECrSb{sub 3}. However, the Yb 4d spectrum of YbCrSb{sub 3} also shows peaks that are characteristic of divalent ytterbium. The Cr 2p core-line spectra exhibit asymmetric lineshapes and little change in binding energy (BE) relative to Cr metal, providing strong evidence for electronic delocalization. The Sb 3d core-line spectra reveal slightly negative BE shifts relative to elemental antimony, supporting the presence of anionic Sb species in RECrSb{sub 3}. The experimental valence band spectrum of LaCrSb{sub 3} matches well with the calculated density of states, and it can be fitted to component peaks belonging to individual atoms to yield an average formulation that agrees well with expectations ('La{sup 3+}Cr{sup 3+}(Sb{sup 2-}){sub 3}'). On progressing from LaCrSb{sub 3} to NdCrSb{sub 3}, the 4f-band in the valence band spectra grows in intensity and shifts to higher BE. The valence band spectrum for YbCrSb{sub 3} also supports the presence of divalent ytterbium. - Graphical Abstract: In their valence band spectra, the 4f-band intensifies and shifts to higher BE on progressing from LaCrSb{sub 3} to NdCrSb{sub 3}. Highlights: Black-Right-Pointing-Pointer High-resolution core-line and valence band XPS spectra were measured for RECrSb{sub 3}. Black-Right-Pointing-Pointer Divalent Yb is present in YbCrSb{sub 3}, in contrast to trivalent RE in other members. Black-Right-Pointing-Pointer Asymmetric Cr 2p spectral lineshape confirms delocalization of Cr valence electrons. Black-Right-Pointing-Pointer Small negative Sb 3d BE shifts support assignment of

  8. Deduction of the chemical state and the electronic structure of Nd{sub 2}Fe{sub 14}B compound from X-ray photoelectron spectroscopy core-level and valence-band spectra

    SciTech Connect

    Wang, Jing; Liang, Le; Zhang, Lanting E-mail: lmsun@sjtu.edu.cn; Sun, Limin E-mail: lmsun@sjtu.edu.cn; Hirano, Shinichi

    2014-10-28

    Characterization of chemical state and electronic structure of the technologically important Nd{sub 2}Fe{sub 14}B compound is attractive for understanding the physical nature of its excellent magnetic properties. X-ray photoelectron spectroscopy (XPS) study of such rare-earth compound is important and also challenging due to the easy oxidation of surface and small photoelectron cross-sections of rare-earth 4f electrons and B 2p electrons, etc. Here, we reported an investigation based on XPS spectra of Nd{sub 2}Fe{sub 14}B compound as a function of Ar ion sputtering time. The chemical state of Fe and that of B in Nd{sub 2}Fe{sub 14}B compound can be clearly determined to be 0 and −3, respectively. The Nd in Nd{sub 2}Fe{sub 14}B compound is found to have the chemical state of close to +3 instead of +3 as compared with the Nd in Nd{sub 2}O{sub 3}. In addition, by comparing the valence-band spectrum of Nd{sub 2}Fe{sub 14}B compound to that of the pure Fe, the contributions from Nd, Fe, and B to the valence-band structure of Nd{sub 2}Fe{sub 14}B compound is made more clear. The B 2p states and B 2s states are identified to be at ∼11.2 eV and ∼24.6 eV, respectively, which is reported for the first time. The contribution from Nd 4f states can be identified both in XPS core-level spectrum and XPS valence-band spectrum. Although Nd 4f states partially hybridize with Fe 3d states, Nd 4f states are mainly localized in Nd{sub 2}Fe{sub 14}B compound.

  9. Epitaxial BaTiO{sub 3}(100) films on Pt(100): A low-energy electron diffraction, scanning tunneling microscopy, and x-ray photoelectron spectroscopy study

    SciTech Connect

    Foerster, Stefan; Huth, Michael; Schindler, Karl-Michael; Widdra, Wolf

    2011-09-14

    The growth of epitaxial ultrathin BaTiO{sub 3} films on a Pt(100) substrate has been studied by scanning tunneling microscopy (STM), low-energy electron diffraction (LEED), and x-ray photoelectron spectroscopy (XPS). The films have been prepared by radio-frequency-assisted magnetron sputter deposition at room temperature and develop a long-range order upon annealing at 900 K in O{sub 2}. By adjusting the Ar and O{sub 2} partial pressures of the sputter gas, the stoichiometry was tuned to match that of a BaTiO{sub 3}(100) single crystal as determined by XPS. STM reveals the growth of continuous BaTiO{sub 3} films with unit cell high islands on top. With LEED already for monolayer thicknesses, the formation of a BaTiO{sub 3}(100)-(1 x 1) structure has been observed. Films of 2-3 unit cell thickness show a brilliant (1 x 1) LEED pattern for which an extended set of LEED I-V data has been acquired. At temperatures above 1050 K the BaTiO{sub 3} thin film starts to decay by formation of vacancy islands. In addition (4 x 4) and (3 x 3) surface reconstructions develop upon prolonged heating.

  10. Synthesis, structure, electronic spectroscopy, photophysics, electrochemistry, and X-ray photoelectron spectroscopy of highly-electron-deficient [5,10,15,20-tetrakis(perfluoroalkyl)porphinato]zinc(II ) complexes and their free base derivatives

    SciTech Connect

    Goll, J.G.; Moore, K.T.; Therien, M.J.; Ghosh, A.

    1996-09-04

    The synthesis, optical spectroscopy, photophysical properties, electrochemistry, and X-ray photoelectron spectroscopy of a series of [5,10,15,20-tetrakis(perfluoroalkyl)porphinato]zinc(II ) complexes and their free base analogs are reported. The title compounds were prepared by a condensation methodology that utilizes perfluoro-1-(2`-pyrrolyl)-1-alkanol precursors and employs continuous water removal throughout the course of the reaction to yield the meso perfluorocarbon-substituted porphyrins. The nature of the porphyrin-pendant meso-perfluoroalkyl group exerts considerable influence over the macrocycle`s solubility properties. The structure of the monopyridyl adduct of [5,10,15,20-tetrakis(heptafluoropropyl)porphinato] zinc(II) features an S{sub 4}-distorted porphyrin core; X-ray data are given. Electrochemical studies carried out on these porphyrin and (porphinato)zinc(II) complexes indicate that meso-perfluoroalkylporphyrins are among the most electron-deficient porphyrinic species known. X-ray photoelectron spectroscopy experiments corroborate the electron poor nature of these systems and evince extreme stabilization of the nitrogen ls orbitals, consonant with particularly effective removal of electron density from the macrocycle by the meso-perfluoroalkyl moieties that is modulated by {sigma}-symmetry orbitals. 27 refs., 8 figs., 6 tabs.

  11. Chest x-ray

    MedlinePlus

    ... Images Aortic rupture, chest x-ray Lung cancer, frontal chest x-ray Adenocarcinoma - chest x-ray Coal ... cancer - chest x-ray Lung nodule, right middle lobe - chest x-ray Lung mass, right upper lung - ...

  12. A study of internal structure in components made by additive manufacturing process using 3 D X-ray tomography

    NASA Astrophysics Data System (ADS)

    Raguvarun, K.; Balasubramaniam, Krishnan; Rajagopal, Prabhu; Palanisamy, Suresh; Nagarajah, Romesh; Hoye, Nicholas; Curiri, Dominic; Kapoor, Ajay

    2015-03-01

    Additive manufacturing methods are gaining increasing popularity for rapidly and efficiently manufacturing parts and components in the industrial context, as well as for domestic applications. However, except when used for prototyping or rapid visualization of components, industries are concerned with the load carrying capacity and strength achievable by additive manufactured parts. In this paper, the wire-arc additive manufacturing (AM) process based on gas tungsten arc welding (GTAW) has been examined for the internal structure and constitution of components generated by the process. High-resolution 3D X-ray tomography is used to gain cut-views through wedge-shaped parts created using this GTAW additive manufacturing process with titanium alloy materials. In this work, two different control conditions for the GTAW process are considered. The studies reveal clusters of porosities, located in periodic spatial intervals along the sample cross-section. Such internal defects can have a detrimental effect on the strength of the resulting AM components, as shown in destructive testing studies. Closer examination of this phenomenon shows that defect clusters are preferentially located at GTAW traversal path intervals. These results highlight the strong need for enhanced control of process parameters in ensuring components with minimal defects and higher strength.

  13. A study of internal structure in components made by additive manufacturing process using 3 D X-ray tomography

    SciTech Connect

    Raguvarun, K. Balasubramaniam, Krishnan Rajagopal, Prabhu; Palanisamy, Suresh; Nagarajah, Romesh; Kapoor, Ajay; Hoye, Nicholas; Curiri, Dominic

    2015-03-31

    Additive manufacturing methods are gaining increasing popularity for rapidly and efficiently manufacturing parts and components in the industrial context, as well as for domestic applications. However, except when used for prototyping or rapid visualization of components, industries are concerned with the load carrying capacity and strength achievable by additive manufactured parts. In this paper, the wire-arc additive manufacturing (AM) process based on gas tungsten arc welding (GTAW) has been examined for the internal structure and constitution of components generated by the process. High-resolution 3D X-ray tomography is used to gain cut-views through wedge-shaped parts created using this GTAW additive manufacturing process with titanium alloy materials. In this work, two different control conditions for the GTAW process are considered. The studies reveal clusters of porosities, located in periodic spatial intervals along the sample cross-section. Such internal defects can have a detrimental effect on the strength of the resulting AM components, as shown in destructive testing studies. Closer examination of this phenomenon shows that defect clusters are preferentially located at GTAW traversal path intervals. These results highlight the strong need for enhanced control of process parameters in ensuring components with minimal defects and higher strength.

  14. A transmissive x-ray polarimeter design for hard x-ray focusing telescopes

    NASA Astrophysics Data System (ADS)

    Li, Hong; Feng, Hua; Ji, Jianfeng; Deng, Zhi; He, Li; Zeng, Ming; Li, Tenglin; Liu, Yinong; Heng, Peiying; Wu, Qiong; Han, Dong; Dong, Yongwei; Lu, Fangjun; Zhang, Shuangnan

    2015-08-01

    The X-ray Timing and Polarization (XTP) is a mission concept for a future space borne X-ray observatory and is currently selected for early phase study. We present a new design of X-ray polarimeter based on the time projection gas chamber. The polarimeter, placed above the focal plane, has an additional rear window that allows hard X-rays to penetrate (a transmission of nearly 80% at 6 keV) through it and reach the detector on the focal plane. Such a design is to compensate the low detection efficiency of gas detectors, at a low cost of sensitivity, and can maximize the science return of multilayer hard X-ray telescopes without the risk of moving focal plane instruments. The sensitivity in terms of minimum detectable polarization, based on current instrument configuration, is expected to be 3% for a 1mCrab source given an observing time of 105 s. We present preliminary test results, including photoelectron tracks and modulation curves, using a test chamber and polarized X-ray sources in the lab.

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

    SciTech Connect

    Tobin, J G

    2011-03-17

    The subjects of discussion included: VUV photoelectron spectroscopy, X-ray photoelectron spectroscopy, Synchrotron-radiation-based photoelectron spectroscopy, Soft x-ray absorption spectroscopy, Soft x-ray emission spectroscopy, Inverse photoelectron spectroscopy, Bremstrahlung Isochromat Spectroscopy, Low energy IPES, Resonant inverse photoelectron spectroscopy.

  16. Beam Damage of HS (CH2)15 COOH Terminated Self Assembled Monolayer (SAM) as Observed by X-Ray Photoelectron Spectroscopy

    SciTech Connect

    Engelhard, Mark H.; Tarasevich, Barbara J.; Baer, Donald R.

    2011-10-25

    XPS spectra of HS(CH{sub 2}){sub 15} COOH terminated a self assembled monolayer (SAM)sample was collected over a period of 242 minutes to determine specimen damage during long exposures to monochromatic Al Ka x-rays. For this COOH terminated SAM we measured the loss of oxygen as a function of time by rastering a focused 100 W, 100 um diameter x-ray beam over a 1.4 mm x 0.2 mm area of the sample.

  17. In situ oxidation study of copper, tin, and copper-tin intermetallics at low temperatures by x-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Wang, Dong-Ning

    The initial oxidation behavior of metallic copper, tin, and three single-phase Cu-Sn alloys (an alpha phase solid solution alloy, and the intermetallic compounds varepsilon-Cusb3Sn and eta-Cusb6Snsb5) has been investigated by X-ray Photoelectron Spectroscopy (XPS) at temperatures of 150sp°C, 200sp°C, and 350sp°C. The oxidation studies are performed in an XPS chamber with pure oxygen. Tin metal oxidizes to produce a combination of SnO and SnOsb2 at both 150sp°C and 200sp°C. The oxide layer consists mainly of SnO with a small fraction of SnOsb2 concentrated near the top of the surface. The oxide growth on tin metal follows a logarithmic law at 150sp°C and a parabolic law at 200sp°C. Copper metal oxidizes to Cusb2O at temperatures below 350sp°C. At 350sp°C, a graded structure of Cusb2O as the inner layer and CuO near the surface forms after 50 minutes. The copper growth kinetics follows the cubic law at all three temperatures, and the calculated activation energy of copper oxide growth is 61 kJ/mol. For all of the Cu-Sn alloys, the tin is preferentially oxidized at all temperatures; oxidation of the copper component in the two intermetallics (varepsilon-Cusb3Sn and eta-Cusb6Snsb5) is strongly suppressed. Copper oxidation is observed in the varepsilon phase oxidation only after 30 minutes at 350sp°C; no copper oxidation is seen in the eta-Cusb6Snsb5 phase under the time-temperature conditions studied. At all three temperatures, the oxide layer on the eta-Cusb6Snsb5 phase consists of the mixed tin oxides, similar to that observed for oxidation of tin metal. However, the SnOsb2/SnO ratio on the eta-Cusb6Snsb5 phase is higher than that on the tin metal. For the varepsilon-Cusb3Sn phase, at temperatures lower than 350sp°C, the oxide layer also consists of both of the tin oxides, with a higher SnOsb2/SnO ratio than the tin metal. At 350sp°C, after 30 minutes the copper component in the varepsilon phase starts to oxidize. As a result, the oxide layer changes from

  18. Assigning Oxidation States to Organic Compounds via Predictions from X-Ray Photoelectron Spectroscopy: A Discussion of Approaches and Recommended Improvements

    ERIC Educational Resources Information Center

    Gupta, Vipul; Ganegoda, Hasitha; Engelhard, Mark H.; Terry, Jeff; Linford, Matthew R.

    2014-01-01

    The traditional assignment of oxidation states to organic molecules is problematic. Accordingly, in 1999, Calzaferri proposed a simple and elegant solution that is based on the similar electronegativities of carbon and hydrogen: hydrogen would be assigned an oxidation state of zero when bonded to carbon. Here, we show that X-ray photoelectron…

  19. In situ x-ray photoelectron spectroscopy and capacitance voltage characterization of plasma treatments for Al{sub 2}O{sub 3}/AlGaN/GaN stacks

    SciTech Connect

    Qin, Xiaoye; Lucero, Antonio; Azcatl, Angelica; Kim, Jiyoung; Wallace, Robert M.

    2014-07-07

    We investigate the Al{sub 2}O{sub 3}/AlGaN/GaN metal-oxide-semiconductor structure pretreated by O{sub 2} anneals, N{sub 2} remote plasma, and forming gas remote plasma prior to atomic layer deposition of Al{sub 2}O{sub 3} using in situ X-ray photoelectron spectroscopy, low energy electron diffraction, and capacitance- voltage measurements. Plasma pretreatments reduce the Ga-oxide/oxynitride formation and the interface state density, while inducing a threshold voltage instability.

  20. X-ray photoelectron study of Bi{sub 2}Sr{sub 2}CaCu{sub 2{minus}x}Co{sub x}O{sub {approximately}8}

    SciTech Connect

    Man, N.K.; Hien, T.D.; Kumari, K.; Venkatesh, S.; Garg, K.B.; Sinh, N.K.; Phuc, N.X.

    1999-05-30

    An X-ray photoelectron spectroscopy study has been performed on well characterized Bi{sub 2}Sr{sub 2}CaCu{sub 2{minus}x}Co{sub x}O{sup {approximately}8} (x = 0, 0.02 and 0.1) samples. There is a shift in the Sr binding energy with Co concentration, which is related to the change in {Tc}. This relationship can be understood by the change of hole concentration in the CuO{sub 2} planes as a result of Cobalt doping. The results of Bi 4f and Co 2p core level spectra are also discussed in detail.

  1. Correlation between Charge State of Insulating NaCl Surfaces and Ionic Mobility Induced by Water Adsorption: A Combined Ambient Pressure X-ray Photoelectron Spectroscopy and Scanning Force Microscopy Study

    SciTech Connect

    Verdaguer, Albert; Jose Segura, Juan; Fraxedas, Jordi; Bluhm, Hendrik; Salmeron, Miquel

    2008-09-03

    In situ ambient pressure X-ray photoelectron spectroscopy (APPES) and scanning force microscopy were used to characterize the surface discharge induced by water layers grown on (001) surfaces of sodium chloride single crystals. The APPES studies show that both kinetic energy (KE) and full width at half-maximum (FWHM) of the Na 2s and Cl 2p core level peaks, monitored as a function of relative humidity (RH), mimic surface conductivity curves measured using scanning force microscopy. The KE position and FWHM of the core level peaks therefore are directly related to the solvation and diffusion of ions at the NaCl(100) surface upon adsorption of water.

  2. Electronic structure of the (Nd{sub 1−x}Dy{sub x}){sub 2}Fe{sub 14}B (0 ≤ x ≤ 1) system studied by X-ray photoelectron spectroscopy

    SciTech Connect

    Wang, Jing; Liang, Le; Yang, Bin; Sun, Li-min; Zhang, Lan-ting; Hirano, Shin-ichi

    2015-09-15

    Systematic characterization of electronic structures in the (Nd{sub 1−x}Dy{sub x}){sub 2}Fe{sub 14}B system, especially the 4f behavior, provides an insight to the physical nature of the evolution of magnetic properties. A series of X-ray photoelectron spectroscopy (XPS) core-level and valence-band spectra were used to study the electronic structures. It was found that substitution of Dy for Nd in Nd{sub 2}Fe{sub 14}B results in a nonlinear variation in the evolution of electronic structures. Only the finite coupling between the Nd 4f states and the Fe 3d states is found at both the Nd-rich regime and the Dy-rich regime. When the Dy concentration and the Nd concentration approach to be equal, a strong coupling between the Nd 4f states and the Fe 3d states is found, which results in a bonding state between them. Additionally, the 4f components in the (Nd{sub 1−x}Dy{sub x}){sub 2}Fe{sub 14}B system are ascribed to three parts: 1) the individual contribution of the Dy 4f states, which emerges just after the Dy-substitution; 2) the contribution of the coupling between the Nd 4f states and the Dy 4f states, which arises only when 0.4 ≤ x ≤ 0.6; 3) the associated contributions of the Nd 4f states and the Dy 4f states, where the contribution of the Nd 4f states and that of the Dy 4f states are prominent in the Nd-rich regime and Dy-rich regime, respectively.

  3. Visible light absorbance enhanced by nitrogen embedded in the surface layer of Mn-doped sodium niobate crystals, detected by ultra violet - visible spectroscopy, x-ray photoelectron spectroscopy, and electric conductivity tests

    NASA Astrophysics Data System (ADS)

    Molak, A.; Pilch, M.

    2016-05-01

    Sodium niobate crystals doped with manganese ions, Na(NbMn)O3, were annealed in a nitrogen N2 flow at 600, 670, and 930 K. It was verified that simultaneous doping with Mn ions and annealing in nitrogen enhanced the photocatalytic features of sodium niobate. The transmission in the ultraviolet-visible range was measured at room temperature. The absorbance edge is in the range from 3.4 to 2.3 eV. The optical band gap Egap = 1.2-1.3 eV was evaluated using the Tauc relation. Crystals annealed at 670 K and 930 K exhibited an additional shift of the absorption edge of ˜20-40 nm toward longer wavelengths. The optical energy gap narrowed as a result of the superimposed effect of Mn and N co-doping. The x-ray photoelectron spectroscopy test showed that N ions incorporated into the surface layer. The valence band consisted of O 2p states hybridized with Nb 4d, Mn 3d, and N 2s states. The disorder detected in the surroundings of Nb and O ions decreased due to annealing. The binding energy of oxygen ions situated within the surface layer was EB ≈ 531 eV. The other contributions were assigned to molecular contamination. The contribution centered at 535.5 eV vanished after annealing at 600 K and 670 K. The contribution centered at 534 eV vanished after annealing at 930 K. The N2 annealing partly removed carbonates from the surfaces of the samples. In the 480-950 K range, the electric conductivity activation energy, Ea = 0.7-1.2 eV, was comparable with the optical Egap. The electric permittivity showed dispersion in the 0.1-800 kHz range that corresponds to the occurrence of defects.

  4. Consequences of Electron-Density Manipulations on the X-ray Photoelectron Spectroscopic Properties of Ferrocenyl-β-diketonato Complexes of Manganese(III). Structure of [Mn(FcCOCHCOCH3)3].

    PubMed

    Buitendach, Blenerhassitt E; Erasmus, Elizabeth; Landman, Marilé; Niemantsverdriet, J W Hans; Swarts, Jannie C

    2016-03-01

    Reaction of [Mn3(OAc)6O·3H2O](+) (1) with ferrocenyl β-diketones of the type FcCOCH2COR with R = CF3 (2a) and CH3 (2b), Ph = C6H5 (2c), and Fc = Fe(II)(η(5)-C5H4)(η(5)-C5H5) (2d) yielded a series of ferrocene-functionalized β-diketonato manganese(III) complexes 3a-3d, respectively, of general formula [Mn(FcCOCHCOR)3]. The mixed-ligand β-diketonato complex [Mn(FcCOCHCOFc)2(FcCOCHCOCH3)] (4) was obtained by reacting mixtures of diketones 2b and 2d with 1. A single-crystal X-ray structure determination of 3b (Z = 2, triclinic, space group P1̅) highlighted a weak axial elongating Jahn-Teller effect and a high degree of bond conjugation. An X-ray photoelectron spectroscopic study, by virtue of linear relationships between group electronegativities of ligand R groups, χR, or ∑χR, and binding energies of both the Fe 2p3/2 and Mn 2p3/2 photoelectron lines, confirmed communication between molecular fragments of 2a-2d as well as 3a-3d. This unprecedented observation allows prediction of binding energies from known β-diketonato side group χR values. PMID:26886078

  5. Micro-X-Ray Fluorescence, Micro-X-Ray Absorption Spectroscopy, and Micro-X-Ray Diffraction Investigation of Lead Speciation after the Addition of Different Phosphorus Amendments to a Smelter-Contaminated Soil

    EPA Science Inventory

    The stabilization of Pb on additions of P to contaminated soils and mine spoil materials has been well documented. It is clear from the literature that different P sources result in different efficacies of Pb stabilization in the same contaminated material. We hypothesized that...

  6. Beam damage of poly(2-chloroethyl methylacrylate) [PCEMA] films as observed by x-ray photoelectron spectroscopy at 143 K, 303 K, and 373 K

    SciTech Connect

    Engelhard, Mark H.; Baer, Donald R.; Lea, Alan S.

    2003-03-08

    X-ray beam damage is often observed during surface analysis of beam sensitive materials as indicated in the introduction to this issue and in a wide variety of references. While damage occurs in a wide range of materials, those that are most susceptible to damage are materials that contain low energy covalent bonds such as polymers or other organic materials. Even amongst the relatively easily damaged polymers, there is a wide range of damage rates. The focus of this submission is on poly(2-chloroethyl methylacrylate) [PCEMA] films. In order to determine the extent to which localized sample heating could influence damage rates the temperature of the substrate holding the PECMA was controlled during irradiation. PCEMA presumably degrades primarily by photo-ionization, resulting in the production of HCl through H and Cl bond cleavage. PCEMA has been recommended as a polymer for use as a reference for evaluating x-ray damage. PCEMA has been shown to be more sensitive to degradation than PVC which has also been used as a damage sensitive material useful for comparison of damage rates. Measurements of several relatively common materials on one instrument can provide a data base that allows damage rates on one instrument to be linked or compared to other damage data in the literature. Therefore for purposes of comparison, damage rates for bulk PVC at the same three different temperatures used for the PCEMA data have been collected and are also presented in this volume. Other data collected at the same x-ray parameters include thin films of PVC (for which damage rates are essentially identical to the bulk material) and of poly(acrylonitrile) PAN which is more stable that either PCEMA or PVC.

  7. X-ray diffraction and photoelectron spectroscopy studies of MoO 2 as catalyst for the partial oxidation of isooctane

    NASA Astrophysics Data System (ADS)

    Marin-Flores, Oscar; Scudiero, L.; Ha, Su

    2009-08-01

    X-ray diffraction (XRD), X-ray photoemission (XPS) as well as ultraviolet photoemission (UPS) spectroscopy experiments on MoO 2 powders were carried out to examine the bulk, the core level energies, and the electronic structure of MoO 2 samples that were employed as catalysts for the partial oxidation of isooctane. Five fresh 0.5-g MoO 2 samples were exposed for 0, 0.5, 9, 20, and 43 h to identical reforming environments and their spent samples were analyzed using the techniques mentioned above. Our results indicate the rapid appearance of an intermediate Mo phase with a binding energy of 228.5 eV and whose concentration progressively increases with time. The oxidation state for this new phase was graphically estimated to approximately +2.6 and assigned to the compound Mo 2O 3, which forms on the catalyst surface as a result of its exposure to the reforming environment. The electronic structure probed by UPS reveals two bands, one at 1.62 eV and another at 0.55 eV below the Fermi level, that decrease with the increasing time on stream. These results correlate very well with the drop in the catalytic performance of MoO 2 for the partial oxidation of isooctane and with the decline in the concentration of dioxide (Mo 4+) detected not only on the catalyst surface, but also in the bulk structure, as confirmed by our XRD analysis.

  8. Rotational Doppler effect in x-ray photoionization

    SciTech Connect

    Sun Yuping; Wang Chuankui; Gel'mukhanov, Faris

    2010-11-15

    The energy of the photoelectron experiences a red or blue Doppler shift when the molecule recedes from the detector or approaches him. This results in a broadening of the photoelectron line due to the translational thermal motion. However, the molecules also have rotational degrees of freedom and we show that the translational Doppler effect has its rotational counterpart. This rotational Doppler effect leads to an additional broadening of the spectral line of the same magnitude as the Doppler broadening caused by translational thermal motion. The rotational Doppler broadening as well as the rotational recoil broadening is sensitive to the molecular orbital from which the photoelectron is ejected. This broadening should be taken into account in analysis of x-ray photoemission spectra of super-high resolution and it can be directly observed using x-ray pump-probe spectroscopy.

  9. X-ray diffraction analysis of LiCu2O2 crystals with additives of silver atoms

    NASA Astrophysics Data System (ADS)

    Sirotinkin, V. P.; Bush, A. A.; Kamentsev, K. E.; Dau, H. S.; Yakovlev, K. A.; Tishchenko, E. A.

    2015-09-01

    Silver-containing LiCu2O2 crystals up to 4 × 8 × 8 mm in size were grown by the crystallization of 80(1- x)CuO · 20 x AgNO3 · 20Li2CO3 (0 ≤ х ≤ 0.5) mixture melt. According to the X-ray spectral and Rietveld X-ray diffraction data, the maximum amount of silver incorporated in the LiCu2O2 structure is about 4 at % relative to the copper content. It was established that silver atoms occupy statistically crystallographic positions of lithium atoms. The incorporation of silver atoms is accompanied by a noticeable increase in parameter с of the LiCu2O2 rhombic unit cell, a slight increase in parameter а, and a slight decrease in parameter b.

  10. In situ time-resolved X-ray diffraction of tobermorite formation in autoclaved aerated concrete: Influence of silica source reactivity and Al addition

    SciTech Connect

    Matsui, Kunio; Kikuma, Jun; Tsunashima, Masamichi; Ishikawa, Tetsuji; Matsuno, Shin-ya; Ogawa, Akihiro; Sato, Masugu

    2011-05-15

    The hydrothermal formation of tobermorite during the processing of autoclaved aerated concrete was investigated by in situ X-ray diffraction (XRD) analysis. High-energy X-rays from a synchrotron radiation source in combination with a newly developed autoclave cell and a photon-counting pixel array detector were used. To investigate the effects of the silica source, reactive quartz from chert and less-reactive quartz from quartz sand were used as starting materials. The effect of Al addition on tobermorite formation was also studied. In all cases, C-S-H, hydroxylellestadite and katoite were clearly observed as intermediates. Acceleration of tobermorite formation by Al addition was clearly observed. However, Al addition did not affect the dissolution rate of quartz. Two pathways, via C-S-H and katoite, were also observed in the Al-containing system. These results suggest that the structure of initially formed C-S-H is important for the subsequent tobermorite formation reactions.

  11. Understanding the role of buried interface charges in a metal-oxide-semiconductor stack of Ti/Al{sub 2}O{sub 3}/Si using hard x-ray photoelectron spectroscopy

    SciTech Connect

    Church, J. R.; Opila, R. L.; Weiland, C.

    2015-04-27

    Hard X-ray photoelectron spectroscopy (HAXPES) analyses were carried out on metal-oxide-semiconductor (MOS) samples consisting of Si, thick and thin Al{sub 2}O{sub 3}, and a Ti metal cap. Using Si 1s and C 1s core levels for an energy reference, the Al 1s and Si 1s spectra were analyzed to reveal information about the location and roles of charges throughout the MOS layers. With different oxide thicknesses (2 nm and 23 nm), the depth sensitivity of HAXPES is exploited to probe different regions in the MOS structure. Post Ti deposition results indicated unexpected band alignment values between the thin and thick films, which are explained by the behavior of mobile charge within the Al{sub 2}O{sub 3} layer.

  12. In-operando and non-destructive analysis of the resistive switching in the Ti/HfO2/TiN-based system by hard x-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Bertaud, Thomas; Sowinska, Malgorzata; Walczyk, Damian; Thiess, Sebastian; Gloskovskii, Andrei; Walczyk, Christian; Schroeder, Thomas

    2012-10-01

    Resistive switching in Ti/HfO2/TiN was investigated in-operando by hard x-ray photoelectron spectroscopy. In comparison with the virgin-state, ON- and OFF-states show enhanced Ti/TiOx/HfO2 interface oxidation, resulting from an oxygen-gettering activity of Ti. The formed TiOx layer acts in the resistive switching process as an oxygen reservoir in exchange with the non-stoichiometric HfO2-δ. A Ti1+/Ti3+ valence change redox reaction occurs between OFF- and ON-states. The peak shifts are attributed to space charge potentials created by the varying oxygen vacancy concentration at the interface. A push-pull model of oxygen vacancies as a function of voltage polarity is proposed to describe the mechanism.

  13. Surface and interface analysis of a Roman lead pipe ``fistula'': microchemistry of the soldering at the join, as seen by scanning Auger microscopy and X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Paparazzo, Ernesto

    1994-01-01

    Scanning Auger microscopy (SAM) and X-ray photoelectron spectroscopy (XPS) are used to study the surface and interface chemical composition of a Roman lead pipe (fistula). Experimental evidence is provided that the Romans used tin for soldering the join, and the chemical nature of the single elements, e.g. whether in metallic or combined form, is identified. SAM discloses the segregation of the chemical elements with a sub-micron spatial resolution, and large deviations in the quantitative results are found relative to the large-area averaged XPS results. Elemental depth profiles are obtained from all over the body of the pipe: we find that the lead is less oxidized at the join, and this region contains many more hydrocarbon species, which we interpret as deriving from the use of oil for anti-oxidizing purposes. Our experimental findings are consistent with Plinius' report on the lead-tin soldering techniques used in the Roman world.

  14. Room-temperature oxidation of a GaAs(001) surface induced by the interaction of hyperthermal atomic oxygen and studied by x-ray photoelectron spectroscopy and ion scattering spectroscopy

    NASA Astrophysics Data System (ADS)

    Wolan, John T.; Mount, Charles K.; Hoflund, Gar B.

    1998-03-01

    In this study a hyperthermal oxygen atom source has been used to form an oxide layer on an Ar+-sputtered GaAs(001) surface at room temperature, and this layer has been examined using x-ray photoelectron spectroscopy (XPS) and ion scattering spectroscopy (ISS). XPS data indicate that the Ga in the near-surface region is oxidized predominantly to Ga2O3 with a significant contribution from GaAsO4 while the As is oxidized predominantly to an AsOx species with significant contributions from As2O3 and GaAsO4 and/or As2O5. The oxide layer thickness is estimated to be about 25 Å, and the XPS Ga:As atom ratio increases from 1.1 to 1.6 during the oxidation. The ISS data indicate that the resulting oxide layer formed is more electrically insulating than a native oxide layer on this surface.

  15. Angle-resolved X-ray photoelectron spectroscopy of topmost surface for LaNiO 3 thin film grown on SrTiO 3 substrate by laser molecular beam epitaxy

    NASA Astrophysics Data System (ADS)

    Chen, P.; Xu, S. Y.; Lin, J.; Ong, C. K.; Cui, D. F.

    1999-01-01

    The LaNiO 3 thin film was grown on SrTiO 3 (001) substrate by computer-controlled laser molecular beam epitaxy (laser MBE). In situ monitoring of the growing film surface was performed with a reflection high energy electron diffraction (RHEED). Angle-resolved X-ray photoelectron spectroscopy (ARXPS) indicated that the terminating plane of the LaNiO 3 film was the LaO atomic plane, and the SrTiO 3 (001) surfaces of as-supplied substrate as well as HF-pretreated substrate were predominantly terminated with TiO atomic plane. The structural conversion of the topmost atomic layer from NiO to LaO occurred during the LaNiO 3 epitaxial growth process.

  16. Direct measurement of band offset at the interface between CdS and Cu{sub 2}ZnSnS{sub 4} using hard X-ray photoelectron spectroscopy

    SciTech Connect

    Tajima, Shin; Kataoka, Keita; Takahashi, Naoko; Kimoto, Yasuji; Fukano, Tatsuo; Hasegawa, Masaki; Hazama, Hirofumi

    2013-12-09

    We directly and non-destructively measured the valence band offset at the interface between CdS and Cu{sub 2}ZnSnS{sub 4} (CZTS) using hard X-ray photoelectron spectroscopy (HAXPES), which can measure the electron state of the buried interface because of its large analysis depth. These measurements were made using the following real devices; CZTS(t = 700 nm), CdS(t = 100 nm)/CZTS(t = 700 nm), and CdS(t = 5 nm)/CZTS(t = 700 nm) films formed on Mo coated glass. The valence band spectra were measured by HAXPES using an X-ray photon energy of 8 keV. The value of the valence band offset at the interface between CdS and CZTS was estimated as 1.0 eV by fitting the spectra. The conduction band offset could be deduced as 0.0 eV from the obtained valence band offset and the band gap energies of CdS and CZTS.

  17. Effects of rare-earth substitution in the oxyarsenides REFeAsO (RE=Ce, Pr, Nd, Sm, Gd) and CeNiAsO by X-ray photoelectron and absorption spectroscopy

    SciTech Connect

    Blanchard, Peter E.R.; Cavell, Ronald G.; Mar, Arthur

    2010-08-16

    X-ray photoelectron spectroscopy (XPS) and X-ray absorption near-edge spectroscopy (XANES) have been applied to examine the electronic structure of the rare-earth transition-metal oxyarsenides REFeAsO (RE=Ce, Pr, Nd, Sm, Gd) and CeNiAsO. Within the metal-arsenic layer [MAs], the bonding character is predominantly covalent and the As atoms are anionic, as implied by the small energy shifts in the M 2p and As 3d XPS spectra. Within the rare-earth-oxygen layer [REO], the bonding character is predominantly ionic, as implied by the similarity of the O 1s binding energies to those in highly ionic oxides. Substitution with a smaller RE element increases the O 1s binding energy, a result of an enhanced Madelung potential. The Ce 3d XPS and Ce L{sub 3}-edge XANES spectra have lineshapes and energies that confirm the presence of trivalent cerium in CeFeAsO and CeNiAsO. A population analysis of the valence band spectrum of CeNiAsO supports the formal charge assignment [Ce{sup 3+}O{sup 2-}][Ni{sup 2+}As{sup 3-}].

  18. 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

    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.

  19. Amorphous nonstoichiometric Ge1-x-Cx:H compounds obtained by radiolysis-chemical vapor deposition of germane/ethyne or germane/allene systems: A bonding and microstructure investigation performed by x-ray photoelectron spectroscopy and Raman spectroscopy

    NASA Astrophysics Data System (ADS)

    Benzi, Paola; Bottizzo, Elena; Demaria, Chiara; Infante, Guido; Iucci, Giovanna; Polzonetti, Giovanni

    2007-06-01

    Hydrogenated germanium carbides have been produced by x-ray activated-chemical vapor deposition from germane/ethyne or germane/allene systems. The chemical composition and structure of the reaction products as a function of the hydrocarbon percentage in the irradiated mixture and of the solid annealing temperature have been studied and discussed. Bonding and microstructure of these alloys have been investigated by x-ray photoelectron spectroscopy and Raman spectroscopy. The results indicate that the solids are formed by a randomly bound network of carbon, germanium and hydrogen atoms with composition, and characteristics and properties variable with the radiolysis experimental conditions. The spectra show the presence of Ge-C bonds and a partial polymerlike character of the films with hydrogen atoms bonded both to germanium and carbon. Clustered-germanium zones dispersed in the material matrix are also evidenced. The results suggest that the conductive properties of the materials are related to the density of these amorphous clusters. The annealing causes compositional and structural transformations becoming more drastic with temperature.

  20. X-Rays

    MedlinePlus

    X-rays are a type of radiation called electromagnetic waves. X-ray imaging creates pictures of the inside of ... different amounts of radiation. Calcium in bones absorbs x-rays the most, so bones look white. Fat ...

  1. Cosmic x ray physics

    NASA Technical Reports Server (NTRS)

    Mccammon, Dan; Cox, D. P.; Kraushaar, W. L.; Sanders, W. T.

    1990-01-01

    The annual progress report on Cosmic X Ray Physics is presented. Topics studied include: the soft x ray background, proportional counter and filter calibrations, the new sounding rocket payload: X Ray Calorimeter, and theoretical studies.

  2. Cosmic x ray physics

    NASA Technical Reports Server (NTRS)

    Mccammon, Dan; Cox, D. P.; Kraushaar, W. L.; Sanders, W. T.

    1991-01-01

    The annual progress report on Cosmic X Ray Physics for the period 1 Jan. to 31 Dec. 1990 is presented. Topics studied include: soft x ray background, new sounding rocket payload: x ray calorimeter, and theoretical studies.

  3. Joint x-ray

    MedlinePlus

    X-ray - joint; Arthrography; Arthrogram ... x-ray technologist will help you position the joint to be x-rayed on the table. Once in place, pictures are taken. The joint may be moved into other positions for more ...

  4. Clarifying the chemical state of additives in membranes for polymer electrolyte fuel cells by X-ray absorption fine structure

    NASA Astrophysics Data System (ADS)

    Tanuma, Toshihiro; Itoh, Takanori

    2016-02-01

    Cerium and manganese compounds are used in the membrane for polymer electrolyte fuel cells (PEFCs) as radical scavengers to mitigate chemical degradation of the membrane. The chemical states of cerium and manganese in the membrane were investigated using a fluorescence X-ray absorption fine structure (XAFS) technique. Membrane electrode assemblies (MEAs) were subjected to open circuit voltage (OCV) condition, under which hydroxyl radicals attack the membrane; a shift in absorption energy in X-ray absorption near edge structure (XANES) spectra was compared between Ce- and Mn-containing membranes before and after OCV testing. In the case of the Ce-containing MEA, there was no significant difference in XANES spectra before and after OCV testing, whereas in the case of the Mn-containing MEA, there was an obvious shift in XANES absorption energy after OCV testing, indicating that Mn atoms with higher valence state than 2+ exist in the membrane after OCV testing. This can be attributed to the difference in the rate of reduction; the reaction of Ce4+ with ·OOH is much faster than that of Mn3+ with ·OOH, leaving some of the Mn atoms with higher valence state. It was confirmed that cerium and manganese redox couples reduced the attack from radicals, mitigating membrane degradation.

  5. Electronic structure of copper halides CuI and CuCl: A comparative X-Ray photoelectron and absorption spectroscopy study

    NASA Astrophysics Data System (ADS)

    Generalov, A. V.; Vinogradov, A. S.

    2013-06-01

    The energy distributions of the occupied and unoccupied electronic states for copper halides CuCl and CuI have been investigated using X-ray photoemission and absorption spectroscopy with a highenergy resolution on the equipment of the Russian-German beamline for outlet and monochromatization of synchrotron radiation from the electron storage ring BESSY II. A quasi-molecular analysis of the obtained experimental spectra has revealed that there is a fundamental similarity of the energy structures of the valence band and the conduction band of copper halides Cu X ( X = Cl, I) due to the identical atomic structure of the studied compounds. The differences in the positions of individual energy subbands in the valence band and the conduction band of Cu X and in their intensities in the spectra are associated with different degrees of hybridization of the Cu 3 d, 4 s and X( n + 1) s, np valence states, as well as with different sizes of structural units (CuCl4 and CuI4 quasi-molecules) of the studied crystals.

  6. Hunting liquid micro-pockets in snow and ice: Phase transition in salt solutions at the bulk and interface with X-ray photoelectron spectroscopy.

    NASA Astrophysics Data System (ADS)

    Bartels-Rausch, Thorsten; Orlando, Fabrizio; Kong, Xiangrui; Waldner, Astrid; Artiglia, Luca; Ammann, Markus; Huthwelker, Thomas

    2016-04-01

    Sea salt, and in particular chloride, is an important reactant in the atmosphere. Chloride in air-borne sea salt aerosol is - once chemically converted to a molecular halogen (Cl2, BrCl) and released to the atmosphere - well known as important atmospheric reactant, driving large-scale changes to the atmospheric composition and in particular to ozone levels in remote areas, but also in coastal mega cities. Similar chemistry has been proposed for sea salt deposits in polar snow covers. A crucial factor determining the overall reactivity is the local physical environment of the chloride ion. For example, the reactivity of liquid aerosols decreases significantly upon crystallization. Surprisingly, the phases of NaCl-containing systems are still under debate, partially due to the limited availability of in situ measurements directly probing the local environment at the surface of frozen NaCl-water binary systems. Using core electron spectroscopy of the oxygen atoms in water, we previously showed that these systems follow the phase rules at the air-ice interface. This finding contrasts some earlier observations, where the presence of liquid below the eutectic point of bulk solutions was postulated. In the present study, we present new electron yield near-edge X-ray absorption fine structure spectroscopy (NEXAFS) data obtained at near-ambient pressures up to 20 mbar of NaCl frozen solutions. The method is sensitive to small changes in the local environment of the chlorine atom. The measurements were performed at the PHOENIX beamline at SLS. The study indicates frapant differences in the phases of NaCl - water mixtures at temperatures blow the freezing point for the surface of the ice vs. the bulk. This has significant impact on modelling chemical reactions in snow or ice and it's environmental consequences.

  7. Aortic arch calcification on chest X-ray combined with coronary calcium score show additional benefit for diagnosis and outcome in patients with angina

    PubMed Central

    Woo, Jong Shin; Kim, Weon; Kwon, Se Hwan; Youn, Hyo Chul; Kim, Hyun Soo; Kim, Jin Bae; Kim, Soo Joong; Kim, Woo-Shik; Kim, Kwon Sam

    2016-01-01

    Background The coronary artery calcium (CAC) and aortic arch calcification (AoAC) are individually associated with cardiovascular disease and outcome. This study investigated the predictive value of AoAC combined with CAC for cardiovascular diagnosis and outcome in patients with angina. Methods A total of 2018 stable angina patients who underwent chest X-ray and cardiac multi-detector computed tomography were followed up for four years to assess adverse events, which were categorized as cardiac death, stroke, myocardial infarction, or repeated revascularization. The extent of AoAC on chest X-ray was graded on a scale from 0 to 3. Results During the four years of follow-up, 620 patients were treated by coronary stenting and 153 (7%) adverse events occurred. A higher grade of AoAC was associated with a higher CAC score. Cox regression showed that the CAC score, but not AoAC, were associated with adverse events. In patients with CAC score < 400, AoAC showed an additive predictive value in detecting significant coronary artery disease (CAD). A gradual increases in the risk of adverse events were noted if AoAC was present in patients with similar CAC score. Conclusions As AoAC is strongly correlated with the CAC score regardless of age or gender, careful evaluation of CAD would be required in patients with AoAC on conventional chest X-rays. PMID:27103916

  8. Microgap x-ray detector

    SciTech Connect

    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.

  9. Microgap x-ray detector

    DOEpatents

    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.

  10. Chest x-ray

    MedlinePlus

    Chest radiography; Serial chest x-ray; X-ray - chest ... You stand in front of the x-ray machine. You will be told to hold your breath when the x-ray is taken. Two images are usually taken. You will ...

  11. GEMS X-ray Polarimeter Performance Simulations

    NASA Technical Reports Server (NTRS)

    Baumgartner, Wayne H.; Strohmayer, Tod; Kallman, Tim; Black, J. Kevin; Hill, Joanne; Swank, Jean

    2012-01-01

    The Gravity and Extreme Magnetism Small explorer (GEMS) is an X-ray polarization telescope selected as a NASA small explorer satellite mission. The X-ray Polarimeter on GEMS uses a Time Projection Chamber gas proportional counter to measure the polarization of astrophysical X-rays in the 2-10 keV band by sensing the direction of the track of the primary photoelectron excited by the incident X-ray. We have simulated the expected sensitivity of the polarimeter to polarized X-rays. We use the simulation package Penelope to model the physics of the interaction of the initial photoelectron with the detector gas and to determine the distribution of charge deposited in the detector volume. We then model the charge diffusion in the detector,and produce simulated track images. Within the track reconstruction algorithm we apply cuts on the track shape and focus on the initial photoelectron direction in order to maximize the overall sensitivity of the instrument, using this technique we have predicted instrument modulation factors nu(sub 100) for 100% polarized X-rays ranging from 10% to over 60% across the 2-10 keV X-ray band. We also discuss the simulation program used to develop and model some of the algorithms used for triggering, and energy measurement of events in the polarimeter.

  12. Organobase catalyzed 1,4-conjugate addition of 4-hydroxycoumarin on chalcones: Synthesis, NMR and single-crystal X-ray diffraction studies of novel warfarin analogues

    NASA Astrophysics Data System (ADS)

    Talhi, Oualid; Fernandes, José A.; Pinto, Diana C. G. A.; Almeida Paz, Filipe A.; Silva, Artur M. S.

    2015-08-01

    The synthesis of a new series of warfarin analogues by convenient organobase catalyzed 1,4-conjugate addition of 4-hydroxycoumarin to chalcone derivatives is described. 1H NMR spectroscopy evidenced the presence of a predominant acyclic open-form together with the cyclic hemiketal tautomers of the resulting Michael adducts. The acyclic open-form has been unequivocally proved by single-crystal X-ray diffraction analysis. The use of the B ring ortho-hydroxychalcone synthons in this reaction has led to a diastereoselective synthesis of warfarin bicyclo[3.3.1]nonane ketal derivatives.

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

    DOEpatents

    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.

  14. Effect of additives on distributions of lamellar structures in sheared polymer: a study of synchrotron small-angle x-ray scattering

    NASA Astrophysics Data System (ADS)

    Zhu, Peng-Wei; Edward, Graham; Nichols, Lance

    2009-12-01

    The effects of additives on the distributions of lamellar morphology and orientation in sheared isotactic polypropylene were investigated using the small beam of synchrotron small-angle x-ray scattering. The Cu-phthalocyanine can template the lamellar orientation even under low shear rates, whereas the ultramarine blue cannot. The surface contact is suggested to play a role in stabilizing the formation of oriented nuclei which subsequently direct the growth of oriented lamellae. The additives have no notable effects on the long spacing in the shear region. However, at high shear rates, they decrease the thickness of crystalline lamellae or increase the thickness of amorphous lamellae. Since the additives increase the degree of volume crystalline in the shear region, the number of crystalline lamellae should be increased. The results are helpful in designing and selecting suitable additives for controlling lamellar morphology and orientation.

  15. Origin and Tunability of Unusually Large Surface Capacitance in Doped Cerium Oxide Studied by Ambient-Pressure X-Ray Photoelectron Spectroscopy.

    PubMed

    Gopal, Chirranjeevi Balaji; Gabaly, Farid El; McDaniel, Anthony H; Chueh, William C

    2016-06-01

    The volumetric redox (chemical) capacitance of the surface of CeO2-δ films is quantified in situ to be 100-fold larger than the bulk values under catalytically relevant conditions. Sm addition slightly lowers the surface oxygen nonstoichiometry, but effects a 10-fold enhancement in surface chemical capacitance by mitigating defect interactions, highlighting the importance of differential nonstoichiometry for catalysis. PMID:27031580

  16. The Solid Electrolyte Interphase a key parameter of the high performance of Sb in sodium-ion batteries: Comparative X-ray Photoelectron Spectroscopy study of Sb/Na-ion and Sb/Li-ion batteries

    NASA Astrophysics Data System (ADS)

    Bodenes, Lucille; Darwiche, Ali; Monconduit, Laure; Martinez, Hervé

    2015-01-01

    To understand the origin of the better performance of Sb electrode i) vs Na than vs Li and ii) formulated with CarboxyMethyl Cellulose (CMC) in water rather than with PolyVinylidene diFluoride (PVdF) in N-Methyl-2-Pyrrolidone (NMP), X-ray Photoelectron Spectroscopy (XPS) and electrochemical tests have been carried out to carefully investigate the chemical composition of the SEI layer formed at the Sb electrode surface in the Li- and Na-system, with the different binders. Sb electrodes were cycled using a standard EC/PC/3DMC (1 M LiPF6) electrolyte containing Vinylene Carbonate (VC) and FluoroEthylene Carbonate (FEC) for Li system and a standard Propylene Carbonate PC (1 M NaClO4) electrolyte containing FEC for Na system. Surface analysis was performed by a combined XPS core peaks and quantification data analysis to establish the main components of the Solid Electrolyte Interphase film (SEI). The key observation is that the thickness of the SEI layer is strongly related to the nature of the polymer binder used in the formulation and that its chemical nature is different in Li and Na batteries. Much favorable SEI in the case of Sb-CMC/Na seems to participate to the excellent performance of this electrode.

  17. Accurate argon cluster-ion sputter yields: Measured yields and effect of the sputter threshold in practical depth-profiling by x-ray photoelectron spectroscopy and secondary ion mass spectrometry

    NASA Astrophysics Data System (ADS)

    Cumpson, Peter J.; Portoles, Jose F.; Barlow, Anders J.; Sano, Naoko

    2013-09-01

    Argon Gas Cluster-Ion Beam sources are likely to become widely used on x-ray photoelectron spectroscopy and secondary ion mass spectrometry instruments in the next few years. At typical energies used for sputter depth profiling the average argon atom in the cluster has a kinetic energy comparable with the sputter threshold, meaning that for the first time in practical surface analysis a quantitative model of sputter yields near threshold is needed. We develop a simple equation based on a very simple model. Though greatly simplified it is likely to have realistic limiting behaviour and can be made useful for estimating sputter yields by fitting its three parameters to experimental data. We measure argon cluster-ion sputter yield using a quartz crystal microbalance close to the sputter threshold, for silicon dioxide, poly(methyl methacrylate), and polystyrene and (along with data for gold from the existing literature) perform least-squares fits of our new sputter yield equation to this data. The equation performs well, with smaller residuals than for earlier empirical models, but more importantly it is very easy to use in the design and quantification of sputter depth-profiling experiments.

  18. A hard X-ray photoelectron spectroscopy study on the solid electrolyte interphase of a lithium 4,5-dicyano-2-(trifluoromethyl)imidazolide based electrolyte for Si-electrodes

    NASA Astrophysics Data System (ADS)

    Lindgren, Fredrik; Xu, Chao; Maibach, Julia; Andersson, Anna M.; Marcinek, Marek; Niedzicki, Leszek; Gustafsson, Torbjörn; Björefors, Fredrik; Edström, Kristina

    2016-01-01

    This report focuses on the relatively new salt, lithium 4,5-dicyano-2-(trifluoromethyl)imidazolide (LiTDI), and its functionality together with a silicon based composite electrode in a half-cell lithium ion battery context. LiTDI is a promising alternative to the commonly used LiPF6 salt because it does not form HF which can decompose the oxide layer on Si. The formation of a solid electrolyte interphase (SEI) as well as the development of the active Si-particles are investigated during the first electrochemical lithiation and de-lithiation. Characterizations are carried out at different state of charge with scanning electron microscopy (SEM) as well as hard x-ray photoelectron spectroscopy (HAXPES) at two different photon energies. This enables a depth resolved picture of the reaction processes and gives an idea of the chemical buildup of the SEI. The SEI is formed by solvent and LiTDI decomposition products and its composition is similar to SEI formed by other carbonate based electrolytes. The LiTDI salt or its decomposition products are not in itself reactive towards the active Si-material and no unwanted side reactions occurs with the active Si-particles. Despite some decomposition of the LiTDI salt, it is a promising alternative for electrolytes aimed towards Si-based electrodes.

  19. Electronic structure of (Ge{sub 2}Sb{sub 2}Te{sub 5}){sub 1-x}(In{sub 3}SbTe{sub 2}){sub x} investigated by x-ray photoelectron spectroscopy

    SciTech Connect

    Benayad, Anass; Kim, Kihong; Lee, JaeCheol; Kang, YounSeon; Suh, Dong-Seok; Kim, KiJoon; Kim, CheolKyu; Lee, Tae-Yon; Noh, Jin-Seo; Khang, YoonHo; Shin, Hyun-Joon

    2009-08-15

    We have investigated the core levels and the valence band of (Ge{sub 2}Sb{sub 2}Te{sub 5}){sub 1-x}(In{sub 3}Sb{sub 1}Te{sub 2}){sub x} quaternary phase system (IGST) by means of x-ray photoelectron spectroscopy. A systematic shift of Sb 3d and Ge 2p core-level peaks toward lower binding energies side was observed with increasing indium amount, whereas the In 3d and Te 3d core peaks showed less change. The Sb 3d and Ge 2p core-level shift is attributed to an increase in the electronic charge of p-electrons dependent of indium amount. The valence band spectra show a distinct change in the sp configuration with indium concentration change. The change in the local bonding as the indium amount increase has a profound impact on both local atomic arrangement and amorphous-to-crystalline transformation temperature. The difference in the photoemission spectra have been discussed according to a simple structural model suggesting that the Na site in IGST can be occupied by Te, Sb, In, and vacancy, whereas in GST it is occupied only by Te.

  20. Valence and origin of metal-insulator transition in Mn doped SrRuO 3 studied by electrical transport, X-ray photoelectron spectroscopy and LSDA+ U calculation

    NASA Astrophysics Data System (ADS)

    Sahu, Ranjan K.; Pandey, Sudhir K.; Pathak, L. C.

    2011-03-01

    We have studied the valence and electronic properties of Mn doped SrRuO 3 using electrical transport measurement, X-ray photoelectron spectroscopy (XPS) and local (spin) density approximation plus Coulomb interaction strength calculation (LSDA+ U). The resistivity data revealed that the system undergoes transition from metal to insulator at the critical Mn doping level, x˜0.2, which is accompanied by the structural transition from orthorhombic to tetragonal crystal symmetry. Besides, the significant reduction of the spectral weight at the coherent zone (0.8 eV) of the valence band is observed for x>0.2. The core XPS spectra suggest that both the transition elements exist in the mixed ionic pair, Ru +4/Ru +5↔Mn +3/Mn +4. The detail analysis of the results suggests that the Coulomb correlation effect in conjugation with localization of the charge carriers predominate over the mixed ionic pair effect and responsible for the metal-insulator transition in the series.

  1. Band alignment of HfO{sub 2}/Al{sub 0.25}Ga{sub 0.75}N determined by x-ray photoelectron spectroscopy: Effect of SiH{sub 4} surface treatment

    SciTech Connect

    Samuel Owen, Man Hon E-mail: yeo@ieee.org; Amin Bhuiyan, Maruf; Zhou, Qian; Yeo, Yee-Chia E-mail: yeo@ieee.org; Zhang, Zheng; Sheng Pan, Ji

    2014-03-03

    The band-alignment of atomic layer deposited (ALD)-HfO{sub 2}/Al{sub 0.25}Ga{sub 0.75}N was studied by high resolution x-ray photoelectron spectroscopy measurements for both the non-passivated and SiH{sub 4} passivated AlGaN surfaces. The valence band offset and the conduction band offset for the ALD-HfO{sub 2}/Al{sub 0.25}Ga{sub 0.75}N interface were found to be 0.43 eV and 1.47 eV, respectively, for the non-passivated sample, and 0.59 eV and 1.31 eV, respectively, for the SiH{sub 4}-passivated sample. The difference in the band alignment is dominated by the band bending or band shift in the AlGaN substrate as a result of the different interlayers formed by the two surface preparations.

  2. 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

    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.

  3. Study of high-temperature hydrogen reduced Pt0/TiO2 by X-ray photoelectron spectroscopy combined with argon ion sputtering—Diffusion-encapsulation effect in relation to strong metal-support interaction

    NASA Astrophysics Data System (ADS)

    Zhang, Jingwei; Zhang, Min; Jin, Zhensheng; Wang, Jingju; Zhang, Zhijun

    2012-02-01

    X-ray photoelectron spectroscopy combined with Ar+ ion sputtering has been used to analyze the variation in the valence and concentration of Pt, Ti, and O of Pt0/TiO2 reduced by H2 at elevated temperature. It is confirmed that titanium oxide of low-valence is transferred onto the surface of Pt0 particulates to encapsulate the surface via a strong metal-support interaction under reducing atmosphere. It is also found for the first time that Pt0 atom is diffused into the lattice of TiO2 to occupy the oxygen vacancy (VOrad rad ) and accept one electron from adjacent Ti3+ forming a localized Pt-sbnd Ti4+ bond. This differs from the strong metal-support interaction under oxidizing atmosphere. Namely, although the Pt0 atom is also diffused into the lattice of TiO2 under oxidizing atmosphere, it replaces Ti atom and forms a Pt2+sbnd O2- bond. Moreover, the strong metal-support interaction under oxidizing atmosphere results in increased photocatalytic activity of Pt0/TiO2, while the strong metal-support interaction under reducing atmosphere leads to decreased photocatalytic activity of Pt0/TiO2.

  4. Investigation of solid electrolyte interface (SEI) film on LiCoO2 cathode in fluoroethylene carbonate (FEC)-containing electrolyte by 2D correlation X-ray photoelectron spectroscopy (XPS)

    NASA Astrophysics Data System (ADS)

    Park, Yeonju; Shin, Su Hyun; Hwang, Hoon; Lee, Sung Man; Kim, Sung Phil; Choi, Hyun Chul; Jung, Young Mee

    2014-07-01

    The effects of fluoroethylene carbonate (FEC) on the electrochemical performance of the LiCoO2 cathode were investigated by galvanostatic charge-discharge testing and cyclic voltammetry (CV). It was found that FEC has a positive effect on cycling stability and also improves cell performance. We also studied solid electrolyte interface (SEI) film on the LiCoO2 cathode, using X-ray photoelectron spectroscopy (XPS) and 2D correlation spectroscopy. The 2D correlation XPS spectra showed that, initially, the polyvinylidene fluoride (PVdF) binder and electrolyte components are decomposed, after which SEI components are formed on the LiCoO2 cathode surface. In the FEC-containing electrolyte, the polycarbonate components are more abundant than in the FEC-free electrolyte. The formed carbonates in SEI film can act as Li+-conducting materials in reducing the electrode/electrolyte interfacial impedance. This hypothesis is supported by the results of an electrochemical impedance spectrum (EIS) analysis.

  5. Investigation of chemical wet-etch surface modification of Ga[sub 0. 5]In[sub 0. 5]P using photoluminescence, X-ray photoelectron spectroscopy, capacitance measurements, and photocurrent-voltage curves

    SciTech Connect

    Kocha, S.S.; Peterson, M.W.; Nelson, A.J.; Rosenwaks, Y.; Arent, D.J.; Turner, J.A. )

    1995-01-12

    Epitaxial Ga[sub 0.5]In[sub 0.5]P films, deposited lattice-matched to GaAs by atmospheric pressure organometallic vapor phase epitaxy, were subjected to various wet-etching processes and the resulting surface was characterized. The steady-state photoluminescence (PL) peak intensity was found to increase 5-fold with some etches, indicating lowered surface recombination rates as a result of etching. Average PL decay times estimated from time-resolved photoluminescence studies also exhibited a correspondingly significant enhancement. Capacitance-voltage and photocurrent-voltage measurements were carried out to investigate changes in energetics of the band edges or alteration in kinetics as a result of the treatments. High resolution X-ray photoelectron spectroscopy revealed a variation of the oxidized species of P, Ga, and In on the surface with etching and were correlated to the PL results. The amount of oxidized material on the surface was lowered after etching in concentrated H[sub 2]SO[sub 4], 1:20:1 HCl:CH[sub 3]COOH:H[sub 2]O[sub 2], and 1:20:1 HCl:H[sub 3]PO[sub 4]:H[sub 2]O[sub 2] and concurred with observations of a higher steady-state PL intensity and longer carrier lifetimes. A nitric acid or aqua regia etch on the other hand yielded an oxide-rich surface with diminished PL. 30 refs., 10 figs., 2 tabs.

  6. 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/HfO2/TiN cells

    NASA Astrophysics Data System (ADS)

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

    2014-05-01

    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/HfO2 interface chemistry and physics of resistive switching Ti/HfO2/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/HfO2 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/HfO2 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.

  7. 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

    Zhang, Bo; 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 lnρ-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.

  8. 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

    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.

  9. 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

    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.

  10. Accurate argon cluster-ion sputter yields: Measured yields and effect of the sputter threshold in practical depth-profiling by x-ray photoelectron spectroscopy and secondary ion mass spectrometry

    SciTech Connect

    Cumpson, Peter J.; Portoles, Jose F.; Barlow, Anders J.; Sano, Naoko

    2013-09-28

    Argon Gas Cluster-Ion Beam sources are likely to become widely used on x-ray photoelectron spectroscopy and secondary ion mass spectrometry instruments in the next few years. At typical energies used for sputter depth profiling the average argon atom in the cluster has a kinetic energy comparable with the sputter threshold, meaning that for the first time in practical surface analysis a quantitative model of sputter yields near threshold is needed. We develop a simple equation based on a very simple model. Though greatly simplified it is likely to have realistic limiting behaviour and can be made useful for estimating sputter yields by fitting its three parameters to experimental data. We measure argon cluster-ion sputter yield using a quartz crystal microbalance close to the sputter threshold, for silicon dioxide, poly(methyl methacrylate), and polystyrene and (along with data for gold from the existing literature) perform least-squares fits of our new sputter yield equation to this data. The equation performs well, with smaller residuals than for earlier empirical models, but more importantly it is very easy to use in the design and quantification of sputter depth-profiling experiments.

  11. Determination of the limit of detection by X-ray photoelectron spectroscopy for As, Zn and Pb oxides in SiO2 matrix as model systems for environmental investigations

    NASA Astrophysics Data System (ADS)

    Atzei, Davide; Elsener, Bernhard; Fantauzzi, Marzia; Brundu, Fabio; Rossi, Antonella

    2016-07-01

    In this work the detection limits of arsenic, zinc and lead in silica matrix by X-ray photoelectron spectroscopy (XPS) analysis were evaluated. These elements were selected since they are particularly relevant in environmental investigations. Pure oxides and several binary mixtures with silica at different concentrations of As (III), Zn (II) and Pb (II) oxides obtained by ball milling were analysed by XPS. Inductive-coupled plasma optical emission spectroscopy (ICP-OES) was also exploited for determining their bulk concentration. The linear response of XPS intensity vs weighed (at%) was confirmed. Three different models were here applied to estimate the limit of detection (LOD) of arsenic, zinc and lead and the results were in good agreement. Under the experimental conditions here adopted, the calculated LODs (at%) of arsenic, zinc, and lead as pure oxides and in silica matrix were found to range between 0.1 and 0.3, between 0.04 and 0.1 and between 0.03 and 0.04 respectively.

  12. X-ray photoelectron diffraction study of dopant effects in La{sub 0.7}X{sub 0.3}MnO{sub 3} (X = La, Sr, Ca, Ce) thin films

    SciTech Connect

    Raisch, C.; Glaser, M.; Chasse, T.; Langheinrich, C.; Chasse, A.; Werner, R.; Kleiner, R.; Koelle, D.

    2013-02-14

    We present and discuss element-specific x-ray photoelectron diffraction (XPD) patterns of La, Mn, O and the dopant ions Ca, Sr and Ce of various La{sub 0.7}X{sub 0.3}MnO (LXMO) films grown epitaxially on SrTiO{sub 3}(001) substrates. The recorded XPD polar scans are explained in the framework of multiple-scattering cluster calculations, where in general a very good agreement between experimental and theoretical data has been found. Results for all thin films are compatible with a tetragonally distorted cubic perovskite structure with similar MnO{sub 6} network. Strong evidence for Mn-site termination was found in all thin films. Dopant locations on A-type sites were clearly confirmed for Sr in LSMO and Ca in LCMO films by means of XPD polar scans. The absence of surface-sensitive Ce3d diffraction features for Ce in LCeMO points to non-equivalent Ce sites and related near-surface disorder.

  13. Investigation of Lithium Insertion Mechanisms of a Thin-Film Si Electrode by Coupling Time-of-Flight Secondary-Ion Mass Spectrometry, X-ray Photoelectron Spectroscopy, and Focused-Ion-Beam/SEM.

    PubMed

    Bordes, Arnaud; De Vito, Eric; Haon, Cédric; Secouard, Christophe; Montani, Alexandre; Marcus, Philippe

    2015-12-23

    Silicon is a serious candidate to replace graphite in electrodes because it offers a specific capacity almost 10 times higher than that of carbonaceous materials. However, cycling performances of Si electrodes remain very limited because of the huge volume changes upon alloying and dealloying with lithium. A fine understanding of the lithiation mechanism of silicon electrodes will help to design more robust architectures. In this work, an amorphous silicon thin film has been used as a model for a better understanding of lithiation mechanism. Lithium distribution in the Si layer has been thoroughly investigated by coupling powerful characterization tools: X-ray photoelectron spectroscopy (XPS) and secondary-ion mass spectrometry (ToF-SIMS). In particular, cross-analysis of different lithiation states has been carried out. A lithiation front moving forward over the state of charge has been highlighted. The quantification of the LixSi alloy indicates a lithium amount much higher than that of the Li/Si ratio estimated in previous studies. This anomaly leads to a description of the lithiation mechanism based on the presence of fast diffusion paths for Li throughout the Si layer. These paths would be a second driving force for silicon alloying and lithium segregation at the collector interface. SEM observations of a FIB cut corroborate this mechanism. PMID:26618212

  14. Formation of a ZnO/ZnS interface passivation layer on (NH4)2S treated In0.53Ga0.47As: Electrical and in-situ X-ray photoelectron spectroscopy characterization

    NASA Astrophysics Data System (ADS)

    Lucero, Antonio T.; Byun, Young-Chul; Qin, Xiaoye; Cheng, Lanxia; Kim, Hyoungsub; Wallace, Robert M.; Kim, Jiyoung

    2016-08-01

    Atomic layer deposition is used to convert an (NH4)2S cleaned p-In0.53Ga0.47As with diethylzinc (DEZ) and water, resulting in the formation of a ZnO/ZnS interfacial passivation layer (IPL). The process is studied using in-situ X-ray photoelectron spectroscopy. DEZ reacts with sulfur and oxygen present on the surface, chemically reducing arsenic 3+ and gallium 3+ to lower oxidation states. The sulfur concentration remains constant during the deposition process while the oxygen concentration on the surface remains small, confirming that the IPL is composed of both ZnO and ZnS. Measurements of metal–oxide–semiconductor capacitors with HfO2 for the dielectric show that the ZnO/ZnS IPL can nearly eliminate frequency dispersion (<1% per frequency decade) in accumulation and results in small hysteresis (<60 mV) with a D it in the 1011 eV‑1 cm‑2 range in the midgap. Frequency dispersion is observed in the depletion region and is attributed to minority carrier generation from the ZnO present in the IPL.

  15. Dental x-rays

    MedlinePlus

    X-ray - teeth; Radiograph - dental; Bitewings; Periapical film; Panoramic film ... dentist's office. There are many types of dental x-rays. Some are: Bitewing Periapical Palatal (also called occlusal) ...

  16. X-ray (image)

    MedlinePlus

    X-rays are a form of ionizing radiation that can penetrate the body to form an image on ... will be shades of gray depending on density. X-rays can provide information about obstructions, tumors, and other ...

  17. X-Ray Lasers

    ERIC Educational Resources Information Center

    Chapline, George; Wood, Lowell

    1975-01-01

    Outlines the prospects of generating coherent x rays using high-power lasers and indentifies problem areas in their development. Indicates possible applications for coherent x rays in the fields of chemistry, biology, and crystallography. (GS)

  18. X Ray Topography

    ERIC Educational Resources Information Center

    Balchin, A. A.

    1974-01-01

    Discusses some aspects in X-ray topography, including formation of dislocations, characteristics of stacking faults, x-ray contrast in defect inspection, Berg-Barrett technique, and Lang traversing crystal and Borrmann's methods. (CC)

  19. Extremity x-ray

    MedlinePlus

    ... degenerative) Bone tumor Broken bone (fracture) Dislocated bone Osteomyelitis (infection) Other conditions for which the test may ... Bone tumor Bone x-ray Broken bone Clubfoot Osteomyelitis X-ray Update Date 10/22/2014 Updated ...

  20. Imaging local electric fields produced upon synchrotron X-ray exposure

    PubMed Central

    Dettmar, Christopher M.; Newman, Justin A.; Toth, Scott J.; Becker, Michael; Fischetti, Robert F.; Simpson, Garth J.

    2015-01-01

    Electron–hole separation following hard X-ray absorption during diffraction analysis of soft materials under cryogenic conditions produces substantial local electric fields visualizable by second harmonic generation (SHG) microscopy. Monte Carlo simulations of X-ray photoelectron trajectories suggest the formation of substantial local electric fields in the regions adjacent to those exposed to X-rays, indicating a possible electric-field–induced SHG (EFISH) mechanism for generating the observed signal. In studies of amorphous vitreous solvents, analysis of the SHG spatial profiles following X-ray microbeam exposure was consistent with an EFISH mechanism. Within protein crystals, exposure to 12-keV (1.033-Å) X-rays resulted in increased SHG in the region extending ∼3 μm beyond the borders of the X-ray beam. Moderate X-ray exposures typical of those used for crystal centering by raster scanning through an X-ray beam were sufficient to produce static electric fields easily detectable by SHG. The X-ray–induced SHG activity was observed with no measurable loss for longer than 2 wk while maintained under cryogenic conditions, but disappeared if annealed to room temperature for a few seconds. These results provide direct experimental observables capable of validating simulations of X-ray–induced damage within soft materials. In addition, X-ray–induced local fields may potentially impact diffraction resolution through localized piezoelectric distortions of the lattice. PMID:25552555

  1. X-Ray Imaging

    MedlinePlus

    ... Brain Surgery Imaging Clinical Trials Basics Patient Information X-Ray Imaging Print This Page X-ray imaging is perhaps the most familiar type of imaging. Images produced by X-rays are due to the different absorption rates of ...

  2. X-Rays

    MedlinePlus

    X-rays are a type of radiation called electromagnetic waves. X-ray imaging creates pictures of the inside of your ... different amounts of radiation. Calcium in bones absorbs x-rays the most, so bones look white. Fat and ...

  3. Hand x-ray

    MedlinePlus

    X-ray - hand ... A hand x-ray is taken in a hospital radiology department or your health care provider's office by an ... technician. You will be asked to place your hand on the x-ray table, and keep it ...

  4. Sinus x-ray

    MedlinePlus

    Paranasal sinus radiography; X-ray - sinuses ... sinus x-ray is taken in a hospital radiology department. Or the x-ray may be taken ... Brown J, Rout J. ENT, neck, and dental radiology. In: Adam A, Dixon AK, Gillard JH Schaefer- ...

  5. A New NIST Database for the Simulation of Electron Spectra for Surface Analysis (SESSA): Application to Angle-Resolved X-ray Photoelectron Spectroscopy of HfO2, ZrO2, HfSiO4, and ZrSiO4 Films on Silicon

    SciTech Connect

    Powell, C.J.; Smekal, W.; Werner, W.S.M.

    2005-09-09

    We describe a new NIST database for the Simulation of Electron Spectra for Surface Analysis (SESSA). This database provides data for the many parameters needed in quantitative Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS). In addition, AES and XPS spectra can be simulated for layered samples. The simulated spectra, for layer compositions and thicknesses specified by the user, can be compared with measured spectra. The layer compositions and thicknesses can then be adjusted to find maximum consistency between simulated and measured spectra. In this way, AES and XPS can provide more detailed characterization of multilayer thin-film materials. We report on the use of SESSA for determining the thicknesses of HfO2, ZrO2, HfSiO4, and ZrSiO4 films on Si by angle-resolved XPS. Practical effective attenuation lengths (EALs) have been computed from SESSA as a function of film thickness and photoelectron emission angle (i.e., to simulate the effects of tilting the sample). These EALs have been compared with similar values obtained from the NIST Electron Effective-Attenuation-Length Database (SRD 82). Generally good agreement was found between corresponding EAL values, but there were differences for film thicknesses less than the inelastic mean free path of the photoelectrons in the overlayer film. These differences are due to a simplifying approximation in the algorithm used to compute EALs in SRD 82. SESSA, with realistic cross sections for elastic and inelastic scattering in the film and substrate materials, is believed to provide more accurate EALs than SRD 82 for thin-film thickness measurements, particularly in applications where the film and substrate have different electron-scattering properties.

  6. A New NIST Database for the Simulation of Electron Spectra for Surface Analysis (SESSA): Application to Angle-Resolved X-ray Photoelectron Spectroscopy of HfO2, ZrO2, HfSiO4, and ZrSiO4 Films on Silicon

    NASA Astrophysics Data System (ADS)

    Powell, C. J.; Smekal, W.; Werner, W. S. M.

    2005-09-01

    We describe a new NIST database for the Simulation of Electron Spectra for Surface Analysis (SESSA). This database provides data for the many parameters needed in quantitative Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS). In addition, AES and XPS spectra can be simulated for layered samples. The simulated spectra, for layer compositions and thicknesses specified by the user, can be compared with measured spectra. The layer compositions and thicknesses can then be adjusted to find maximum consistency between simulated and measured spectra. In this way, AES and XPS can provide more detailed characterization of multilayer thin-film materials. We report on the use of SESSA for determining the thicknesses of HfO2, ZrO2, HfSiO4, and ZrSiO4 films on Si by angle-resolved XPS. Practical effective attenuation lengths (EALs) have been computed from SESSA as a function of film thickness and photoelectron emission angle (i.e., to simulate the effects of tilting the sample). These EALs have been compared with similar values obtained from the NIST Electron Effective-Attenuation-Length Database (SRD 82). Generally good agreement was found between corresponding EAL values, but there were differences for film thicknesses less than the inelastic mean free path of the photoelectrons in the overlayer film. These differences are due to a simplifying approximation in the algorithm used to compute EALs in SRD 82. SESSA, with realistic cross sections for elastic and inelastic scattering in the film and substrate materials, is believed to provide more accurate EALs than SRD 82 for thin-film thickness measurements, particularly in applications where the film and substrate have different electron-scattering properties.

  7. Transformation from Multilamellar to Unilamellar Vesicles by Addition of a Cationic Lipid to PEGylated Liposomes Explored with Synchrotron Small Angle X-ray Scattering

    NASA Astrophysics Data System (ADS)

    Sakuragi, Mina; Koiwai, Kazunori; Nakamura, Kouji; Masunaga, Hiroyasu; Ogawa, Hiroki; Sakurai, Kazuo

    2011-01-01

    PEGylated liposomes composed of a benzamidine derivative (TRX), hydrogenated soybean phosphatidylcholine (HSPC), and N-(monomethoxy-polyethyleneglycolcarbamyl) distearoyl phosphatidylethanolamine (PEG-PE) were examined in terms of how the addition of TRX affects their structures with small angle x-ray scattering (SAXS) as well as transmission electron microscopy (TEM). TEM images showed the presence of unilamella vesicles for both with and without TRX, though a small amount of multilamella vesicles were observed in absence of TRX. We analyzed SAXS profiles at contained TRX composition combined with contrast variation technique by adding PEG solution and unilamella vesicle model could be reproduced. Subsequently, we analyzed SAXS profiles at no TRX composition. The mixture model of unilamella and multilamella vesicle was reconstructed and we estimated about 10 % multilamella vesicles from a fitting parameter.

  8. Growth of an Ultrathin Zirconia Film on Pt3Zr Examined by High-Resolution X-ray Photoelectron Spectroscopy, Temperature-Programmed Desorption, Scanning Tunneling Microscopy, and Density Functional Theory

    PubMed Central

    2014-01-01

    Ultrathin (∼3 Å) zirconium oxide films were grown on a single-crystalline Pt3Zr(0001) substrate by oxidation in 1 × 10–7 mbar of O2 at 673 K, followed by annealing at temperatures up to 1023 K. The ZrO2 films are intended to serve as model supports for reforming catalysts and fuel cell anodes. The atomic and electronic structure and composition of the ZrO2 films were determined by synchrotron-based high-resolution X-ray photoelectron spectroscopy (HR-XPS) (including depth profiling), low-energy electron diffraction (LEED), scanning tunneling microscopy (STM), and density functional theory (DFT) calculations. Oxidation mainly leads to ultrathin trilayer (O–Zr–O) films on the alloy; only a small area fraction (10–15%) is covered by ZrO2 clusters (thickness ∼0.5–10 nm). The amount of clusters decreases with increasing annealing temperature. Temperature-programmed desorption (TPD) of CO was utilized to confirm complete coverage of the Pt3Zr substrate by ZrO2, that is, formation of a closed oxide overlayer. Experiments and DFT calculations show that the core level shifts of Zr in the trilayer ZrO2 films are between those of metallic Zr and thick (bulklike) ZrO2. Therefore, the assignment of such XPS core level shifts to substoichiometric ZrOx is not necessarily correct, because these XPS signals may equally well arise from ultrathin ZrO2 films or metal/ZrO2 interfaces. Furthermore, our results indicate that the common approach of calculating core level shifts by DFT including final-state effects should be taken with care for thicker insulating films, clusters, and bulk insulators. PMID:25688293

  9. LiNi(0.5)Mn(1.5)O4 high-voltage cathode coated with Li4Ti5O12: a hard X-ray photoelectron spectroscopy (HAXPES) study.

    PubMed

    Sachs, Malte; Gellert, Michael; Chen, Min; Drescher, Hans-Jörg; Kachel, Stefan Renato; Zhou, Han; Zugermeier, Malte; Gorgoi, Mihaela; Roling, Bernhard; Gottfried, J Michael

    2015-12-21

    A Li4Ti5O12 (LTO) film was coated as buffer layer onto a LiNi0.5Mn1.5O4 (LNMO) high-voltage cathode, and after cycling of the cathode in a battery electrolyte, the LTO film was investigated by means of synchrotron radiation based hard X-ray photoelectron spectroscopy (HAXPES). By tuning the photon energy between 2 keV and 6 keV, we obtained non-destructive depth profiles of the coating material with probing depths ranging from 6 nm to 20 nm. The coating was found to be covered by a few nanometers thin surface layer resulting from electrolyte decomposition. This layer consisted predominantly of organic polymers as well as metal fluorides and fluorophosphates. A positive influence of the Li4Ti5O12 coating with regard to the size and stability of the surface layer was found. The coating itself consisted of a uniform mixture of Li(I), Ti(IV), Ni(II) and Mn(IV) oxides that most likely adopted a spinel structure by forming a solid solution of the two spinels LiNi0.5Mn1.5O4 and Li4Ti5O12 with Li, Mn, Ni and Ti cations mixing on the spinel octahedral sites. The diffusion of Ni and Mn ions into the Li4Ti5O12 lattice occurred during the heat treatment when preparing the cathode. The doping of Li4Ti5O12 with the open d-shell ions Ni(2+) (d(8)) and Mn(4+) (d(3)) should increase the electronic conductivity of the coating significantly, as was found in previous studies. The complex signal structure of the Ti 2p, Ni 2p and Mn 2p core levels provides insight into the chemical nature of the transition metal ions. PMID:26563554

  10. 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

    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.

  11. Atomic force microscopy and x-ray photoelectron spectroscopy investigations of the morphology and chemistry of a PdCl2/SnCl2 electroless plating catalysis system adsorbed onto shape memory alloy particles

    NASA Astrophysics Data System (ADS)

    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 (SnO2 and PdO) and hydroxide [Sn(OH)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)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.

  12. Panoramic Dental X-Ray

    MedlinePlus

    ... X-ray? What is Panoramic X-ray? Panoramic radiography , also called panoramic x-ray , is a two- ... Exams Dental Cone Beam CT X-ray, Interventional Radiology and Nuclear Medicine Radiation Safety About this Site ...

  13. X-ray binaries

    NASA Technical Reports Server (NTRS)

    1976-01-01

    Satellite X-ray experiments and ground-based programs aimed at observation of X-ray binaries are discussed. Experiments aboard OAO-3, OSO-8, Ariel 5, Uhuru, and Skylab are included along with rocket and ground-based observations. Major topics covered are: Her X-1, Cyg X-3, Cen X-3, Cyg X-1, the transient source A0620-00, other possible X-ray binaries, and plans and prospects for future observational programs.

  14. Bulk sensitive hard x-ray photoemission electron microscopy

    SciTech Connect

    Patt, M. Wiemann, C.; Weber, N.; Escher, M.; Merkel, M.; Gloskovskii, A.; Drube, W.; Schneider, C. M.

    2014-11-15

    Hard x-ray photoelectron spectroscopy (HAXPES) has now matured into a well-established technique as a bulk sensitive probe of the electronic structure due to the larger escape depth of the highly energetic electrons. In order to enable HAXPES studies with high lateral resolution, we have set up a dedicated energy-filtered hard x-ray photoemission electron microscope (HAXPEEM) working with electron kinetic energies up to 10 keV. It is based on the NanoESCA design and also preserves the performance of the instrument in the low and medium energy range. In this way, spectromicroscopy can be performed from threshold to hard x-ray photoemission. The high potential of the HAXPEEM approach for the investigation of buried layers and structures has been shown already on a layered and structured SrTiO{sub 3} sample. Here, we present results of experiments with test structures to elaborate the imaging and spectroscopic performance of the instrument and show the capabilities of the method to image bulk properties. Additionally, we introduce a method to determine the effective attenuation length of photoelectrons in a direct photoemission experiment.

  15. Noise variance analysis using a flat panel x-ray detector: A method for additive noise assessment with application to breast CT applications

    SciTech Connect

    Yang Kai; Huang, Shih-Ying; Packard, Nathan J.; Boone, John M.

    2010-07-15

    Purpose: A simplified linear model approach was proposed to accurately model the response of a flat panel detector used for breast CT (bCT). Methods: Individual detector pixel mean and variance were measured from bCT projection images acquired both in air and with a polyethylene cylinder, with the detector operating in both fixed low gain and dynamic gain mode. Once the coefficients of the linear model are determined, the fractional additive noise can be used as a quantitative metric to evaluate the system's efficiency in utilizing x-ray photons, including the performance of different gain modes of the detector. Results: Fractional additive noise increases as the object thickness increases or as the radiation dose to the detector decreases. For bCT scan techniques on the UC Davis prototype scanner (80 kVp, 500 views total, 30 frames/s), in the low gain mode, additive noise contributes 21% of the total pixel noise variance for a 10 cm object and 44% for a 17 cm object. With the dynamic gain mode, additive noise only represents approximately 2.6% of the total pixel noise variance for a 10 cm object and 7.3% for a 17 cm object. Conclusions: The existence of the signal-independent additive noise is the primary cause for a quadratic relationship between bCT noise variance and the inverse of radiation dose at the detector. With the knowledge of the additive noise contribution to experimentally acquired images, system modifications can be made to reduce the impact of additive noise and improve the quantum noise efficiency of the bCT system.

  16. X-ray beamsplitter

    DOEpatents

    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.

  17. X-ray beamsplitter

    DOEpatents

    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.

  18. X-ray - skeleton

    MedlinePlus

    A skeletal x-ray is an imaging test used to look at the bones. It is used to detect fractures , tumors, or ... in the health care provider's office by an x-ray technologist. You will lie on a table or ...

  19. Extremity x-ray

    MedlinePlus

    An extremity x-ray is an image of the hands, wrist, feet, ankle, leg, thigh, forearm humerus or upper arm, hip, shoulder ... term "extremity" often refers to a human limb. X-rays are a form of radiation that passes through ...

  20. X-ray Spectrometry.

    ERIC Educational Resources Information Center

    Markowicz, Andrzej A.; Van Grieken, Rene E.

    1984-01-01

    Provided is a selective literature survey of X-ray spectrometry from late 1981 to late 1983. Literature examined focuses on: excitation (photon and electron excitation and particle-induced X-ray emission; detection (wavelength-dispersive and energy-dispersive spectrometry); instrumentation and techniques; and on such quantitative analytical…